WO2021112135A1 - Compound and molded object - Google Patents
Compound and molded object Download PDFInfo
- Publication number
- WO2021112135A1 WO2021112135A1 PCT/JP2020/044901 JP2020044901W WO2021112135A1 WO 2021112135 A1 WO2021112135 A1 WO 2021112135A1 JP 2020044901 W JP2020044901 W JP 2020044901W WO 2021112135 A1 WO2021112135 A1 WO 2021112135A1
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- WO
- WIPO (PCT)
- Prior art keywords
- group
- compound
- epoxy resin
- carbon atoms
- resin
- Prior art date
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- 150000001875 compounds Chemical class 0.000 title claims abstract description 137
- 239000003822 epoxy resin Substances 0.000 claims abstract description 111
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 111
- -1 siloxane compound Chemical class 0.000 claims abstract description 109
- 229910052751 metal Inorganic materials 0.000 claims abstract description 99
- 239000011342 resin composition Substances 0.000 claims abstract description 83
- 239000000843 powder Substances 0.000 claims abstract description 76
- 239000000126 substance Substances 0.000 claims abstract description 56
- 239000002184 metal Substances 0.000 claims description 96
- 125000004432 carbon atom Chemical group C* 0.000 claims description 38
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 24
- 125000000962 organic group Chemical group 0.000 claims description 17
- 125000003118 aryl group Chemical group 0.000 claims description 15
- 125000003700 epoxy group Chemical group 0.000 claims description 11
- 125000000217 alkyl group Chemical group 0.000 claims description 10
- 125000003545 alkoxy group Chemical group 0.000 claims description 8
- 125000001033 ether group Chemical group 0.000 claims description 7
- 125000002947 alkylene group Chemical group 0.000 claims description 6
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 6
- 229920001281 polyalkylene Polymers 0.000 claims description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 125000001183 hydrocarbyl group Chemical group 0.000 claims 1
- 239000000047 product Substances 0.000 description 80
- 238000001723 curing Methods 0.000 description 59
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 37
- 239000003795 chemical substances by application Substances 0.000 description 31
- 239000005011 phenolic resin Substances 0.000 description 29
- 229910045601 alloy Inorganic materials 0.000 description 28
- 239000000956 alloy Substances 0.000 description 28
- 239000002245 particle Substances 0.000 description 24
- 238000012360 testing method Methods 0.000 description 24
- 229920003986 novolac Polymers 0.000 description 20
- 229920005989 resin Polymers 0.000 description 19
- 239000011347 resin Substances 0.000 description 19
- 238000000465 moulding Methods 0.000 description 18
- 239000001993 wax Substances 0.000 description 17
- 238000010438 heat treatment Methods 0.000 description 16
- 239000007822 coupling agent Substances 0.000 description 12
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 12
- QFLWZFQWSBQYPS-AWRAUJHKSA-N (3S)-3-[[(2S)-2-[[(2S)-2-[5-[(3aS,6aR)-2-oxo-1,3,3a,4,6,6a-hexahydrothieno[3,4-d]imidazol-4-yl]pentanoylamino]-3-methylbutanoyl]amino]-3-(4-hydroxyphenyl)propanoyl]amino]-4-[1-bis(4-chlorophenoxy)phosphorylbutylamino]-4-oxobutanoic acid Chemical compound CCCC(NC(=O)[C@H](CC(O)=O)NC(=O)[C@H](Cc1ccc(O)cc1)NC(=O)[C@@H](NC(=O)CCCCC1SC[C@@H]2NC(=O)N[C@H]12)C(C)C)P(=O)(Oc1ccc(Cl)cc1)Oc1ccc(Cl)cc1 QFLWZFQWSBQYPS-AWRAUJHKSA-N 0.000 description 11
- 238000004898 kneading Methods 0.000 description 11
- 239000000203 mixture Substances 0.000 description 11
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 9
- 239000003063 flame retardant Substances 0.000 description 9
- 239000002994 raw material Substances 0.000 description 9
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- 238000004519 manufacturing process Methods 0.000 description 8
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 8
- 150000002989 phenols Chemical class 0.000 description 8
- SMQUZDBALVYZAC-UHFFFAOYSA-N salicylaldehyde Chemical compound OC1=CC=CC=C1C=O SMQUZDBALVYZAC-UHFFFAOYSA-N 0.000 description 8
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 7
- 125000003710 aryl alkyl group Chemical group 0.000 description 7
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- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 7
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- 230000000052 comparative effect Effects 0.000 description 6
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- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 5
- 239000000654 additive Substances 0.000 description 5
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- 239000011812 mixed powder Substances 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
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- 238000001721 transfer moulding Methods 0.000 description 5
- NAWXUBYGYWOOIX-SFHVURJKSA-N (2s)-2-[[4-[2-(2,4-diaminoquinazolin-6-yl)ethyl]benzoyl]amino]-4-methylidenepentanedioic acid Chemical compound C1=CC2=NC(N)=NC(N)=C2C=C1CCC1=CC=C(C(=O)N[C@@H](CC(=C)C(O)=O)C(O)=O)C=C1 NAWXUBYGYWOOIX-SFHVURJKSA-N 0.000 description 4
- KJCVRFUGPWSIIH-UHFFFAOYSA-N 1-naphthol Chemical compound C1=CC=C2C(O)=CC=CC2=C1 KJCVRFUGPWSIIH-UHFFFAOYSA-N 0.000 description 4
- 125000000094 2-phenylethyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])C([H])([H])* 0.000 description 4
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 4
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- 125000003342 alkenyl group Chemical group 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 description 4
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 4
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 4
- 125000004369 butenyl group Chemical group C(=CCC)* 0.000 description 4
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 4
- 239000004202 carbamide Substances 0.000 description 4
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229920001971 elastomer Polymers 0.000 description 4
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 125000003187 heptyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 4
- 125000006038 hexenyl group Chemical group 0.000 description 4
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 4
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
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- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 4
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- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 description 3
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 239000006087 Silane Coupling Agent Substances 0.000 description 3
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- HECLRDQVFMWTQS-RGOKHQFPSA-N 1755-01-7 Chemical compound C1[C@H]2[C@@H]3CC=C[C@@H]3[C@@H]1C=C2 HECLRDQVFMWTQS-RGOKHQFPSA-N 0.000 description 2
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- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910002796 Si–Al Inorganic materials 0.000 description 1
- 229910009038 Sn—P Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 125000002723 alicyclic group Chemical group 0.000 description 1
- 239000004844 aliphatic epoxy resin Substances 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 150000001343 alkyl silanes Chemical class 0.000 description 1
- 229910000828 alnico Inorganic materials 0.000 description 1
- CEGOLXSVJUTHNZ-UHFFFAOYSA-K aluminium tristearate Chemical compound [Al+3].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CEGOLXSVJUTHNZ-UHFFFAOYSA-K 0.000 description 1
- 229940063655 aluminum stearate Drugs 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 description 1
- LLEMOWNGBBNAJR-UHFFFAOYSA-N biphenyl-2-ol Chemical compound OC1=CC=CC=C1C1=CC=CC=C1 LLEMOWNGBBNAJR-UHFFFAOYSA-N 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 125000004106 butoxy group Chemical group [*]OC([H])([H])C([H])([H])C(C([H])([H])[H])([H])[H] 0.000 description 1
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N butyric aldehyde Natural products CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 description 1
- 239000008116 calcium stearate Substances 0.000 description 1
- 235000013539 calcium stearate Nutrition 0.000 description 1
- HIAAVKYLDRCDFQ-UHFFFAOYSA-L calcium;dodecanoate Chemical compound [Ca+2].CCCCCCCCCCCC([O-])=O.CCCCCCCCCCCC([O-])=O HIAAVKYLDRCDFQ-UHFFFAOYSA-L 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- UPHIPHFJVNKLMR-UHFFFAOYSA-N chromium iron Chemical compound [Cr].[Fe] UPHIPHFJVNKLMR-UHFFFAOYSA-N 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 1
- 229930003836 cresol Natural products 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- CZZYITDELCSZES-UHFFFAOYSA-N diphenylmethane Chemical compound C=1C=CC=CC=1CC1=CC=CC=C1 CZZYITDELCSZES-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- GFQOFGWPGYRLAO-UHFFFAOYSA-N dodecanamide;ethene Chemical compound C=C.CCCCCCCCCCCC(N)=O.CCCCCCCCCCCC(N)=O GFQOFGWPGYRLAO-UHFFFAOYSA-N 0.000 description 1
- POULHZVOKOAJMA-UHFFFAOYSA-M dodecanoate Chemical compound CCCCCCCCCCCC([O-])=O POULHZVOKOAJMA-UHFFFAOYSA-M 0.000 description 1
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- SWSBIGKFUOXRNJ-CVBJKYQLSA-N ethene;(z)-octadec-9-enamide Chemical compound C=C.CCCCCCCC\C=C/CCCCCCCC(N)=O.CCCCCCCC\C=C/CCCCCCCC(N)=O SWSBIGKFUOXRNJ-CVBJKYQLSA-N 0.000 description 1
- ZJOLCKGSXLIVAA-UHFFFAOYSA-N ethene;octadecanamide Chemical compound C=C.CCCCCCCCCCCCCCCCCC(N)=O.CCCCCCCCCCCCCCCCCC(N)=O ZJOLCKGSXLIVAA-UHFFFAOYSA-N 0.000 description 1
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000002223 garnet Substances 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 150000004668 long chain fatty acids Chemical class 0.000 description 1
- 235000019359 magnesium stearate Nutrition 0.000 description 1
- 229910001004 magnetic alloy Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- 239000004200 microcrystalline wax Substances 0.000 description 1
- 239000006082 mold release agent Substances 0.000 description 1
- PECBPCUKEFYARY-ZPHPHTNESA-N n-[(z)-octadec-9-enyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCCCCCCCC\C=C/CCCCCCCC PECBPCUKEFYARY-ZPHPHTNESA-N 0.000 description 1
- GOQYKNQRPGWPLP-UHFFFAOYSA-N n-heptadecyl alcohol Natural products CCCCCCCCCCCCCCCCCO GOQYKNQRPGWPLP-UHFFFAOYSA-N 0.000 description 1
- DJWFNQUDPJTSAD-UHFFFAOYSA-N n-octadecyloctadecanamide Chemical compound CCCCCCCCCCCCCCCCCCNC(=O)CCCCCCCCCCCCCCCCC DJWFNQUDPJTSAD-UHFFFAOYSA-N 0.000 description 1
- NXPPAOGUKPJVDI-UHFFFAOYSA-N naphthalene-1,2-diol Chemical compound C1=CC=CC2=C(O)C(O)=CC=C21 NXPPAOGUKPJVDI-UHFFFAOYSA-N 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- LYRFLYHAGKPMFH-UHFFFAOYSA-N octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(N)=O LYRFLYHAGKPMFH-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- FATBGEAMYMYZAF-KTKRTIGZSA-N oleamide Chemical compound CCCCCCCC\C=C/CCCCCCCC(N)=O FATBGEAMYMYZAF-KTKRTIGZSA-N 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 150000004965 peroxy acids Chemical class 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229920002312 polyamide-imide Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 239000004848 polyfunctional curative Substances 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 125000002572 propoxy group Chemical group [*]OC([H])([H])C(C([H])([H])[H])([H])[H] 0.000 description 1
- 229920005604 random copolymer Polymers 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- 229910000702 sendust Inorganic materials 0.000 description 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- IYMSIPPWHNIMGE-UHFFFAOYSA-N silylurea Chemical compound NC(=O)N[SiH3] IYMSIPPWHNIMGE-UHFFFAOYSA-N 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- TXDNPSYEJHXKMK-UHFFFAOYSA-N sulfanylsilane Chemical compound S[SiH3] TXDNPSYEJHXKMK-UHFFFAOYSA-N 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 150000003609 titanium compounds Chemical class 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical compound [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 1
- 125000002256 xylenyl group Chemical class C1(C(C=CC=C1)C)(C)* 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
- ODNJVAVDJKOYFK-GRVYQHKQSA-L zinc;(9z,12z)-octadeca-9,12-dienoate Chemical compound [Zn+2].CCCCC\C=C/C\C=C/CCCCCCCC([O-])=O.CCCCC\C=C/C\C=C/CCCCCCCC([O-])=O ODNJVAVDJKOYFK-GRVYQHKQSA-L 0.000 description 1
- 150000003755 zirconium compounds Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/541—Silicon-containing compounds containing oxygen
- C08K5/5415—Silicon-containing compounds containing oxygen containing at least one Si—O bond
- C08K5/5419—Silicon-containing compounds containing oxygen containing at least one Si—O bond containing at least one Si—C bond
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0856—Iron
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
Definitions
- the present invention relates to a compound and a molded product.
- the compound containing the metal powder and the resin composition is used as a raw material for various industrial products such as an inductor, an electromagnetic wave shield, or a bond magnet, depending on the physical characteristics of the metal powder (see Patent Document 1 below).
- An object of the present invention is to provide a compound capable of obtaining a molded product having both heat resistance and withstand voltage resistance, and a molded product having the compound.
- the compound according to one aspect of the present invention comprises a metal element-containing powder and a resin composition
- the resin composition contains an epoxy resin and a compound having a siloxane bond (chemical clond) and has a siloxane bond.
- the content of the compound is 20 parts by mass or less with respect to 100 parts by mass of the epoxy resin
- the compound having a siloxane bond includes a siloxane compound having a structure represented by the following chemical formula (1).
- n is an integer of 2 to 200
- R 1 and R 2 are independently alkyl groups having 1 to 10 carbon atoms, aryl groups having 6 to 10 carbon atoms, and 1 carbon group. It is a monovalent organic group having an alkoxy group of ⁇ 10, an epoxy group, a monovalent organic group having a carboxy group, or a polyalkylene ether group having 3 to 500 carbon atoms.
- the siloxane compound may further have a structural unit represented by the following chemical formula (2).
- R 3 is an alkylene group having 1 to 10 carbon atoms.
- the compound according to one aspect of the present invention may contain a compound represented by the following chemical formula (3) as a siloxane compound.
- n is an integer of 2 to 200
- m 1 and m 2 are independently integers of 1 to 200, and are R 4 , R 5 , R 6 and R 7.
- Each of them independently has an alkyl group having 1 to 10 carbon atoms, an aryl group having 6 to 10 carbon atoms, an alkoxy group having 1 to 10 carbon atoms, a monovalent organic group having an epoxy group, and a monovalent organic group having a carboxy group.
- It is a divalent hydrocarbon group having 1 to 10 carbon atoms which may contain a structure.
- the compound according to one aspect of the present invention may contain at least one of a biphenylene aralkyl type epoxy resin and an isocyanate-modified epoxy resin as the epoxy resin.
- the content of the metal element-containing powder may be 90% by mass or more and less than 100% by mass.
- the molded product according to one aspect of the present invention includes the above compound.
- a compound capable of obtaining a molded product having both heat resistance and withstand voltage resistance, and a molded product having the compound.
- the compound according to the present embodiment includes a metal element-containing powder and a resin composition.
- the metal element-containing powder is composed of a plurality of (many) metal element-containing particles.
- the metal element-containing powder may contain, for example, at least one selected from the group consisting of elemental metals, alloys and metal compounds.
- the resin composition contains at least an epoxy resin and a compound having a siloxane bond. A compound having a siloxane bond may be referred to as a "siloxane compound".
- the resin composition may contain other components in addition to the epoxy resin and the siloxane compound.
- the resin composition may contain a curing agent.
- the resin composition may contain a curing accelerator.
- the resin composition may contain additives.
- the resin composition is a component that can include an epoxy resin, a siloxane compound, a curing agent, a curing accelerator, and an additive, and is a remaining component (nonvolatile component) excluding an organic solvent and a metal element-containing powder. Good.
- the additive is a component of the rest of the resin composition excluding the resin, the siloxane compound, the curing agent and the curing accelerator.
- the additive is, for example, a coupling agent or a flame retardant.
- the resin composition may contain wax as an additive.
- the compound may be a powder (compound powder).
- the compound according to this embodiment contains a predetermined amount of a siloxane compound which is a kind of elastomer.
- a siloxane compound which is a kind of elastomer.
- the reason why the heat resistance and withstand voltage resistance of the molded product obtained from the compound are improved by the predetermined amount of the siloxane compound is not clear, but the inventors speculate the following possibilities.
- the addition of the siloxane compound improves the fluidity of the contained components and suppresses the generation of internal voids during molding.
- the compatibility between the metal element-containing powder and the epoxy resin is low, and it is considered that the characteristics are deteriorated from the interface between the two. This is because the compatibility between the two can be improved by adding the siloxane compound.
- the action and effect according to the present invention are not limited to the above items.
- the compound may include a metal element-containing powder and a resin composition adhering to the surface of each metal element-containing particle constituting the metal element-containing powder.
- the resin composition may cover the entire surface of the particles, or may cover only a part of the surface of the particles.
- the compound may include an uncured resin composition and a metal element-containing powder.
- the compound may include a semi-cured product of the resin composition (for example, a B-stage resin composition) and a metal element-containing powder.
- the compound may comprise both an uncured resin composition and a semi-cured resin composition.
- the compound may consist of a metal element-containing powder and a resin composition.
- the content of the metal element-containing powder in the compound is 90% by mass or more and less than 100% by mass, 90% by mass or more and 99.8% by mass or less, 92% by mass or more and 99.5% by mass or less, based on the total mass of the compound. It may be 94% by mass or more and 98.5% by mass or less, or 94% by mass or more and 97.5% by mass or less.
- the compound may contain other fillers (eg, silica fillers) in addition to the metal element-containing powder.
- the content of the resin composition in the compound is 0.2% by mass or more and 10% by mass or less, or 4% by mass or more, based on the total mass of the compound (for example, the total mass of the metal element-containing powder and the resin composition). It may be 6% by mass or less.
- the content of the siloxane compound in the compound is 20 parts by mass or less with respect to 100 parts by mass of the epoxy resin, but may be 17.5 parts by mass or less, and may be 15 parts by mass or less.
- the lower limit of the content of the siloxane compound in the compound is not particularly limited, but from the viewpoint of moldability and the like, it may be 0.1 part by mass or more and 5 parts by mass or more with respect to 100 parts by mass of the epoxy resin. It may be 7.5 parts by mass or more, and may be 10 parts by mass or more.
- the average particle size of the metal element-containing powder is not particularly limited, but may be, for example, 1 ⁇ m or more and 300 ⁇ m or less.
- the average particle size may be measured, for example, by a particle size distribution meter.
- the shape of the individual metal element-containing particles constituting the metal element-containing powder is not limited, and may be, for example, spherical, flat, prismatic, or needle-shaped.
- the compound may include a plurality of types of metal element-containing powders having different average particle sizes.
- the molded product can be used as various industrial products or their raw materials. It can be used.
- Industrial products manufactured using the compound may be, for example, automobiles, medical equipment, electronic equipment, electrical equipment, information and communication equipment, home appliances, audio equipment, and general industrial equipment.
- the compound may be used as a raw material for a bond magnet.
- the compound when the compound contains a soft magnetic powder such as a Fe—Si—Cr based alloy or ferrite as the metal element-containing powder, the compound may be used as an inductor (for example, an EMI filter) or a raw material for a transformer (for example, a magnetic core).
- a molded product for example, a sheet formed from the compound may be used as an electromagnetic wave shield.
- the resin composition has a function as a binder of the metal element-containing particles constituting the metal element-containing powder, and imparts mechanical strength to the molded product formed from the compound.
- the resin composition is filled between the metal element-containing particles when the compound is molded at high pressure using a mold, and the metal element-containing particles are bound to each other.
- the cured product of the resin composition binds the metal element-containing particles more firmly, and the mechanical strength of the molded product is improved.
- the resin composition contains at least an epoxy resin as a thermosetting resin.
- the compound contains an epoxy resin having relatively excellent fluidity among thermosetting resins, the fluidity, storage stability, and moldability of the compound are improved.
- the compound may contain other resins in addition to the epoxy resin as long as the effects of the present invention are not impaired.
- the resin composition may contain at least one of a phenol resin and a polyamide-imide resin as a thermosetting resin.
- the resin composition may function as a curing agent for the epoxy resin.
- the resin composition may include a thermoplastic resin.
- the thermoplastic resin may be at least one selected from the group consisting of, for example, acrylic resin, polyethylene, polypropylene, polystyrene, polyvinyl chloride, and polyethylene terephthalate.
- the resin composition may contain both a thermosetting resin and a thermoplastic resin.
- the resin composition may contain a silicone resin.
- the epoxy resin may be, for example, a resin having two or more epoxy groups in one molecule.
- the epoxy resin may be, for example, a resin having three or more epoxy groups in one molecule.
- the epoxy resin may be a polyfunctional epoxy resin.
- Epoxy resins include, for example, biphenyl type epoxy resin, stillben type epoxy resin, diphenylmethane type epoxy resin, sulfur atom-containing epoxy resin, novolak type epoxy resin, dicyclopentadiene type epoxy resin, salicylaldehyde type epoxy resin, naphthols and phenol.
- Copolymerization type epoxy resin aralkyl type phenol resin epoxidized product, bisphenol type epoxy resin, epoxy resin containing bisphenol skeleton, alcoholic glycidyl ether type epoxy resin, paraxylylene and / or metaxylylene modified phenol resin glycidyl ether Type epoxy resin, glycidyl ether type epoxy resin of terpen-modified phenol resin, cyclopentadiene type epoxy resin, glycidyl ether type epoxy resin of polycyclic aromatic ring-modified phenol resin, glycidyl ether type epoxy resin of naphthalene ring-containing phenol resin, glycidyl ester type Epoxy resin, glycidyl type or methyl glycidyl type epoxy resin, alicyclic epoxy resin, halogenated phenol novolac type epoxy resin, orthocresol novolac type epoxy resin, hydroquinone type epoxy resin, trimethylolpropane type epoxy resin, and ole
- the epoxy resins include biphenyl type epoxy resin, orthocresol novolac type epoxy resin, phenol novolac type epoxy resin, bisphenol type epoxy resin, epoxy resin having a bisphenol skeleton, and salicylaldehyde novolac type epoxy resin. And at least one selected from the group consisting of naphthol novolac type epoxy resins.
- the epoxy resin may be a crystalline epoxy resin. Although the molecular weight of the crystalline epoxy resin is relatively low, the crystalline epoxy resin has a relatively high melting point and is excellent in fluidity.
- the crystalline epoxy resin (highly crystalline epoxy resin) may be at least one selected from the group consisting of, for example, a hydroquinone type epoxy resin, a bisphenol type epoxy resin, a thioether type epoxy resin, and a biphenyl type epoxy resin.
- Commercially available crystalline epoxy resins include, for example, Epicron 860, Epicron 1050, Epicron 1055, Epicron 2050, Epicron 3050, Epicron 4050, Epicron 7050, Epicron HM-091, Epicron HM-101, Epicron N-730A, Epicron N.
- YX- It may be at least one selected from the group consisting of 4000, YX-4000H, YL4121H, and YX-8800 (above, trade name manufactured by Mitsubishi Chemical Corporation).
- the resin composition is, as an epoxy resin, at least one of a biphenylene aralkyl type epoxy resin and an isocyanate-modified epoxy resin. May include one type.
- the resin composition may contain both a biphenylene aralkyl type epoxy resin and an isocyanate-modified epoxy resin as the epoxy resin.
- the commercially available product of the biphenylene aralkyl type epoxy resin may be, for example, NC-3000 manufactured by Nippon Kayaku Co., Ltd.
- the commercially available product of the isocyanate-modified epoxy resin may be, for example, AER-4001 manufactured by Asahi Kasei Corporation (formerly Asahi Kasei E-Materials Corporation).
- the resin composition may contain a polyfunctional epoxy resin from the viewpoint of easily improving the heat resistance and withstand voltage of the molded product.
- Examples of commercially available products of the polyfunctional epoxy resin include VG-3101L manufactured by Printec Co., Ltd.
- the resin composition may contain one of the above epoxy resins.
- the resin composition may contain a plurality of types of epoxy resins among the above.
- the curing agent is classified into a curing agent that cures the epoxy resin in the range of low temperature to room temperature and a heat curing type curing agent that cures the epoxy resin with heating.
- Hardeners that cure epoxy resins in the low to room temperature range are, for example, aliphatic polyamines, polyaminoamides, and polymercaptans.
- the heat-curable curing agent is, for example, aromatic polyamine, acid anhydride, phenol novolac resin, dicyandiamide (DICY) and the like.
- the curing agent may be preferably a heat-curing type curing agent, more preferably a phenol resin, and further preferably a phenol novolac resin.
- a phenol novolac resin as a curing agent, it is easy to obtain a cured product of an epoxy resin having a high glass transition point. As a result, the heat resistance and mechanical strength of the molded product are likely to be improved.
- the phenol resin is, for example, an aralkyl type phenol resin, a dicyclopentadiene type phenol resin, a salicylaldehyde type phenol resin, a novolac type phenol resin, a copolymerized phenol resin of a benzaldehyde type phenol and an aralkyl type phenol, a paraxylylene and / or a metaxylylene modification.
- phenol resin From the group consisting of phenol resin, melamine-modified phenol resin, terpen-modified phenol resin, dicyclopentadiene-type naphthol resin, cyclopentadiene-modified phenol resin, polycyclic aromatic ring-modified phenol resin, biphenyl-type phenol resin, and triphenylmethane-type phenol resin. It may be at least one of the choices.
- the phenol resin may be a copolymer composed of two or more of the above.
- Tamanol 758 manufactured by Arakawa Chemical Industry Co., Ltd., HP-850N manufactured by Hitachi Kasei Co., Ltd., or the like may be used.
- the phenol novolac resin may be, for example, a resin obtained by condensing or co-condensing phenols and / or naphthols and aldehydes under an acidic catalyst.
- the phenols constituting the phenol novolac resin may be at least one selected from the group consisting of, for example, phenol, cresol, xylenol, resorcin, catechol, bisphenol A, bisphenol F, phenylphenol and aminophenol.
- the naphthols constituting the phenol novolac resin may be at least one selected from the group consisting of, for example, ⁇ -naphthol, ⁇ -naphthol and dihydroxynaphthalene.
- the aldehydes constituting the phenol novolac resin may be at least one selected from the group consisting of, for example, formaldehyde, acetaldehyde, propionaldehyde, benzaldehyde and salicylaldehyde.
- Examples of commercially available phenol novolac resins include HF-3M and MEW-1800 manufactured by Meiwa Kasei Co., Ltd.
- the curing agent may be, for example, a compound having two phenolic hydroxyl groups in one molecule.
- the compound having two phenolic hydroxyl groups in one molecule may be at least one selected from the group consisting of, for example, resorcin, catechol, bisphenol A, bisphenol F, and substituted or unsubstituted biphenol.
- the resin composition may contain one of the above phenol resins.
- the resin composition may include a plurality of types of phenol resins among the above.
- the resin composition may contain one of the above curing agents.
- the resin composition may contain a plurality of types of curing agents among the above.
- the ratio of the active group (phenolic OH group) in the curing agent that reacts with the epoxy group in the epoxy resin is preferably 0.5 to 1.5 equivalents, more preferably 0.5 to 1.5 equivalents with respect to 1 equivalent of the epoxy group in the epoxy resin. May be 0.6 to 1.4 equivalents, more preferably 0.8 to 1.2 equivalents.
- the ratio of active groups in the curing agent is less than 0.5 equivalent, it is difficult to obtain a sufficient elastic modulus of the obtained cured product.
- the ratio of active groups in the curing agent exceeds 1.5 equivalents, the mechanical strength of the molded product formed from the compound after curing tends to decrease. However, even when the ratio of active groups in the curing agent is out of the above range, the effect according to the present invention can be obtained.
- the curing accelerator (catalyst) is not limited as long as it is a composition that reacts with the epoxy resin to accelerate the curing of the epoxy resin.
- the curing accelerator may be, for example, an alkyl group-substituted imidazole or an imidazole such as benzimidazole.
- the resin composition may include a kind of curing accelerator.
- the resin composition may include a plurality of types of curing accelerators. When the resin composition contains a curing accelerator, the moldability and releasability of the compound are likely to be improved. Further, when the resin composition contains a curing accelerator, the mechanical strength of the molded product (for example, an electronic component) manufactured by using the compound is improved, and the compound is stored in a high temperature and high humidity environment.
- imidazole-based curing accelerators include, for example, 2MZ-H, C11Z, C17Z, 1,2DMZ, 2E4MZ, 2PZ-PW, 2P4MZ, 1B2MZ, 1B2PZ, 2MZ-CN, C11Z-CN, 2E4MZ-CN, 2PZ.
- -At least one selected from the group consisting of CN, C11Z-CNS, 2P4MHZ, TPZ, and SFZ (above, trade name manufactured by Shikoku Chemicals Corporation) may be used.
- the curing accelerator for example, a urea-based catalyst may be used.
- examples of commercially available urea-based catalysts include U-CAT3512T manufactured by Sun Appro Co., Ltd.
- the amount of the curing accelerator to be blended is not particularly limited as long as it can obtain the curing promoting effect.
- the amount of the curing accelerator blended is preferably 0.1 part by mass or more and 30 parts by mass with respect to 100 parts by mass of the epoxy resin.
- it may be more preferably 1 part by mass or more and 15 parts by mass or less.
- the content of the curing accelerator is preferably 0.001 part by mass or more and 5 parts by mass or less with respect to 100 parts by mass in total of the mass of the epoxy resin and the curing agent (for example, phenol resin).
- the blending amount of the curing accelerator is less than 0.1 parts by mass, it is difficult to obtain a sufficient curing promoting effect.
- the blending amount of the curing accelerator exceeds 30 parts by mass, the storage stability of the compound tends to decrease. However, even when the blending amount and content of the curing accelerator are out of the above range, the effect according to the present invention can be obtained.
- the resin composition contains a compound having a siloxane bond (siloxane compound).
- the siloxane bond is a bond containing two silicon atoms (Si) and one oxygen atom (O), and may be represented by —Si—O—Si—.
- the compound having a siloxane bond may be a polysiloxane compound.
- the resin composition may contain one kind of siloxane compound, and may contain a plurality of kinds of siloxane compounds. From the viewpoint that the molding shrinkage of the compound is easily reduced and the heat resistance and withstand voltage of the molded product are easily improved, the resin composition preferably contains the first siloxane compound described later as the siloxane compound.
- the resin composition may contain only the first siloxane compound as the siloxane compound, or may further contain the second siloxane compound.
- the resin composition may contain both the first siloxane compound and the second siloxane compound.
- the resin composition may contain a siloxane compound other than the first siloxane compound and the second siloxane compound. The details of the first siloxane compound and the second siloxane compound will be described below.
- the first siloxane compound may have a structural unit represented by the following chemical formula (1).
- a structural unit can simply be called a "structure”.
- the structural unit represented by the following chemical formula (1) may be expressed as "structural unit 1".
- n is an integer of 2 to 200
- R 1 and R 2 are independently alkyl groups having 1 to 10 carbon atoms, aryl groups having 6 to 10 carbon atoms, and 1 to 1 carbon atoms. It is a monovalent organic group having 10 alkoxy groups, an epoxy group, a monovalent organic group having a carboxy group, or a polyalkylene ether group having 3 to 500 carbon atoms.
- a plurality of R 1 present in the first siloxane compound may be the same or different from each other.
- Plural R 2 present in the first siloxane compound may be the same or different from each other.
- R 1 and R 2 may be the same or different from each other.
- the first siloxane compound may have a repeating unit represented by the above chemical formula (1).
- the first siloxane compound preferably further has a structural unit represented by the following chemical formula (2). ..
- the structural unit represented by the following chemical formula (2) may be expressed as "structural unit 2".
- R 3 is an alkylene group having 1 to 10 carbon atoms.
- the first siloxane compound may have a plurality of structural units 2. Plural R 3 present in the first siloxane compound may be the same or different from each other.
- the first siloxane compound may have a repeating unit represented by the above chemical formula (2).
- the first siloxane compound is preferably a compound represented by the following chemical formula (3).
- the compound represented by the following chemical formula (3) may be referred to as "Compound 3".
- n is an integer of 2 to 200.
- m 1 and m 2 is an integer from 1 to 200 independently.
- R 4 , R 5 , R 6 and R 7 each independently have an alkyl group having 1 to 10 carbon atoms, an aryl group having 6 to 10 carbon atoms, an alkoxy group having 1 to 10 carbon atoms, and an epoxy group.
- R 8 and R 9 is an alkylene group having 1 to 10 carbon atoms independently.
- Each of R 10 and R 11 is a divalent hydrocarbon group having 1 to 10 carbon atoms which may contain an ether structure independently. It can also be said that each of R 10 and R 11 is a divalent hydrocarbon group having 1 to 10 carbon atoms, which may independently contain an oxygen atom or may be bonded via an oxygen atom. ..
- Plural R 4 present in compound 3 may be the same or different from each other.
- a plurality of R 5 present in the compound 3 may be the same or different from each other.
- R 4 , R 5 , R 6 and R 7 may be the same or different from each other.
- a plurality of R 8 present in compound 3 may be the same or different from each other.
- a plurality of R 9 present in compound 3 may be the same or different from each other.
- R 8 and R 9 may be the same or different from each other.
- the weight average molecular weight (Mw) of Compound 3 may be, for example, 4000 or more and 20000 or less.
- Commercially available products of Compound 3 may be, for example, DBL-C31, DBL-C32, etc. manufactured by Gelest Co., Ltd.
- the second siloxane compound has a structural unit represented by the following chemical formula (4) and the following chemical formula (5). It is preferable to have a structural unit represented by).
- the structural unit represented by the following chemical formula (4) may be expressed as "structural unit 4".
- the structural unit represented by the following chemical formula (5) may be expressed as "structural unit 5".
- R 12 is a monovalent hydrocarbon group having 1 to 12 carbon atoms.
- R 17 is an organic group having 1 or more carbon atoms.
- R 12 is, for example, an alkyl group such as a methyl group, an ethyl group, a propyl group, a butyl group, an isopropyl group, an isobutyl group, a t-butyl group, a pentyl group, a hexyl group, a heptyl group, an octyl group and a 2-ethylhexyl group; Alkenyl groups such as vinyl group, allyl group, butenyl group, pentenyl group and hexenyl group; aryl groups such as phenyl group, trill group, xsilyl group, naphthyl group and biphenyl group; aralkyl groups such as benzyl group and phenethyl group. It's okay.
- R 12 is preferably a methyl group or a phenyl group.
- the second siloxane compound may have a plurality of structural units 4.
- the plurality of R 12s present in the second siloxane compound may be the same as or different from each other.
- the second siloxane compound may have a repeating unit represented by the above chemical formula (4).
- R 13 and R 14 are independently monovalent hydrocarbon groups having 1 to 12 carbon atoms.
- R 13 is, for example, an alkyl group such as a methyl group, an ethyl group, a propyl group, a butyl group, an isopropyl group, an isobutyl group, a t-butyl group, a pentyl group, a hexyl group, a heptyl group, an octyl group and a 2-ethylhexyl group; Alkenyl groups such as vinyl group, allyl group, butenyl group, pentenyl group and hexenyl group; aryl groups such as phenyl group, trill group, xsilyl group, naphthyl group and biphenyl group; aralkyl groups such as benzyl group and phenethyl group. It's okay.
- R 13 is preferably a methyl group or a phenyl group.
- R 14 is, for example, an alkyl group such as a methyl group, an ethyl group, a propyl group, a butyl group, an isopropyl group, an isobutyl group, a t-butyl group, a pentyl group, a hexyl group, a heptyl group, an octyl group and a 2-ethylhexyl group; Alkenyl groups such as vinyl group, allyl group, butenyl group, pentenyl group and hexenyl group; aryl groups such as phenyl group, trill group, xsilyl group, naphthyl group and biphenyl group; aralkyl groups such as benzyl group and phenethyl group. It's okay.
- R 14 is preferably a methyl group or a phenyl group.
- the second siloxane compound may have a plurality of structural units 5.
- the plurality of R 13s present in the second siloxane compound may be the same as or different from each other.
- the plurality of R 14s present in the second siloxane compound may be the same as or different from each other.
- R 13 and R 14 may be the same or different from each other.
- the second siloxane compound may have a repeating unit represented by the above chemical formula (5).
- the terminal of the molecule of the second siloxane compound is preferably any one of R 12 , R 13 , R 14 , hydroxyl group and alkoxy group.
- the alkoxy group may be, for example, a methoxy group, an ethoxy group, a propoxy group, or a butoxy group.
- the second siloxane compound preferably has a structural unit represented by the following chemical formula (6).
- the structural unit represented by the following chemical formula (6) may be expressed as "structural unit 6".
- R 15 is a monovalent hydrocarbon group having 1 to 12 carbon atoms.
- R 16 is a monovalent organic group having an epoxy group.
- R 15 is, for example, a methyl group, an ethyl group, a propyl group, a butyl group, an isopropyl group, an isobutyl group, t- butyl group, a pentyl group, a hexyl group, heptyl group, and an octyl group, a 2-ethylhexyl group; Alkenyl groups such as vinyl group, allyl group, butenyl group, pentenyl group and hexenyl group; aryl groups such as phenyl group, trill group, xsilyl group, naphthyl group and biphenyl group; aralkyl groups such as benzyl group and phenethyl group. It's okay.
- R 13 is preferably a methyl group or a phenyl group.
- R 16 is, for example, 2,3-epoxypropyl group, 3,4-epoxybutyl group, 4,5-epoxypentyl group, 2-glycidoxyethyl group, 3-glycidoxypropyl group, 4-glycid. It may be a xybutyl group, a 2- (3,4-epoxycyclohexyl) ethyl group, a 3- (3,4-epoxycyclohexyl) propyl group, or the like. R 16 is preferably a 3-glycidoxypropyl group.
- the second siloxane compound may have a plurality of structural units 6.
- a plurality of R 15 present in the second siloxane compound may be the same or different from each other.
- the plurality of R 16s present in the second siloxane compound may be the same as or different from each other.
- the second siloxane compound may have a repeating unit represented by the above chemical formula (6).
- the second siloxane compound is a structural unit represented by the following chemical formula (7) and the following chemical formula (8). It is preferable that the compound has at least one structural unit selected from the group consisting of the structural unit represented by, the structural unit represented by the following chemical formula (9), and the structural unit represented by the following chemical formula (10). ..
- the structural unit represented by the following chemical formula (7) may be expressed as "structural unit 7".
- the structural unit represented by the following chemical formula (8) may be expressed as "structural unit 8".
- the structural unit represented by the following chemical formula (9) may be expressed as "structural unit 9".
- structural unit 10 The structural unit represented by the following chemical formula (10) may be expressed as "structural unit 10".
- a compound having at least one structural unit selected from the group consisting of the structural unit 7, the structural unit 8, the structural unit 9, and the structural unit 10 may be referred to as “compound 11”.
- Compound 11 may have all of structural unit 7, structural unit 8, structural unit 9, and structural unit 10.
- R 18 is an organic group having 1 or more carbon atoms.
- R 19 is an organic group having 1 or more carbon atoms.
- Compound 11 may have a plurality of structural units 7. Compound 11 may have a repeating unit represented by the above chemical formula (7). Compound 11 may have a plurality of structural units 8. Compound 11 may have a repeating unit represented by the above chemical formula (8). Compound 11 may have a plurality of structural units 9. Compound 11 may have a repeating unit represented by the above chemical formula (9). Compound 11 may have a plurality of structural units 10. Compound 11 may have a repeating unit represented by the above chemical formula (10).
- the commercially available product of Compound 11 may be, for example, AY42-119 manufactured by Toray Dow Corning Co., Ltd.
- the epoxy equivalent of the second siloxane compound may be 500 or more and 4000 or less, or 1000 or more and 2500 or less. When the epoxy equivalent is within the above range, the fluidity of the compound is likely to be improved and the moldability is likely to be improved.
- the softening point of the second siloxane compound is preferably 40 ° C. or higher and 120 ° C. or lower, and more preferably 50 ° C. or higher and 100 ° C. or lower. When the softening point is within the above range, the mechanical strength of the molded product formed from the compound is likely to be improved.
- the softening point of the second siloxane compound may be adjusted by the molecular weight, structure (for example, content ratio of each structural unit) of the second siloxane compound, the type of organic group bonded to the silicon atom, and the like. From the viewpoint of improving the fluidity of the compound, it is preferable to adjust the softening point by the content of the aryl group in the second siloxane compound.
- the aryl group may be, for example, a phenyl group, a tolyl group, a xsilyl group, a naphthyl group, a biphenyl group or the like.
- the aryl group is preferably a phenyl group. It is more preferable to adjust the softening point by the content of the phenyl group in the monovalent organic group bonded to the silicon atom in the second siloxane compound.
- the content of the phenyl group may be adjusted to preferably 60 mol% or more and 100 mol% or less, more preferably 70 mol% or more and 85 mol% or less.
- the weight average molecular weight (Mw) of the second siloxane compound may be 1000 or more and 30,000 or less, preferably 2000 or more and 20000 or less, and more preferably 3000 or more and 10000 or less.
- the weight average molecular weight (Mw) may be measured by gel permeation chromatography (GPC) and may be a value converted using a standard polystyrene calibration curve.
- the second siloxane compound is preferably a random copolymer.
- the resin composition may contain one of the above siloxane compounds, and may contain a plurality of the above siloxane compounds.
- the coupling agent improves the adhesion between the resin composition and the metal element-containing particles constituting the metal element-containing powder, and improves the flexibility and mechanical strength of the molded product formed from the compound.
- the coupling agent may be at least one selected from the group consisting of, for example, a silane compound (silane coupling agent), a titanium compound, an aluminum compound (aluminum chelate), and an aluminum / zirconium compound.
- the silane coupling agent may be at least one selected from the group consisting of, for example, epoxysilane, mercaptosilane, aminosilane, alkylsilane, ureidosilane, acid anhydride-based silane, and vinylsilane. In particular, an aminophenyl-based silane coupling agent is preferable.
- the resin composition may contain one of the above-mentioned coupling agents, and may contain a plurality of of the above-mentioned coupling agents.
- the compound may contain a flame retardant.
- the flame retardant is at least one selected from the group consisting of, for example, a bromine-based flame retardant, a scale flame retardant, a hydrated metal compound-based flame retardant, a silicone-based flame retardant, a nitrogen-containing compound, a hindered amine compound, an organic metal compound, and an aromatic empra. May be.
- the resin composition may contain one of the above flame retardants, and may contain a plurality of the above flame retardants.
- the resin composition may contain wax.
- the wax enhances the fluidity of the compound in the molding of the compound (for example, transfer molding) and functions as a mold release agent.
- the wax may be at least one of fatty acids such as higher fatty acids and fatty acid esters.
- the wax is, for example, fatty acids such as montanic acid, stearic acid, 12-oxystearic acid, laurate or esters thereof; zinc stearate, calcium stearate, barium steaenoate, aluminum stearate, magnesium stearate, calcium laurate, Fatty acid salts such as zinc linoleate, calcium ricinolate, zinc 2-ethylhexoneate; stearic acid amide, oleic acid amide, erucate amide, bechenic acid amide, palmitate amide, laurate amide, hydroxystearic acid amide, methylene bisstearate Acid amide, ethylene bisstearic acid amide, ethylene bislauric acid amide, distearyl adipate amide, ethylene bisoleic acid amide, diorail adipic acid amide, N-stearyl stearic acid amide, N-oleyl stearic acid amide, N-stearyl Fatty
- Polyethers made of materials; Silicone compounds such as silicone oil and silicone grease; Fluorine compounds such as fluorine oil, fluorine grease, and fluorine-containing resin powder; and paraffin wax, polyethylene wax, amide wax, polypropylene wax, and ester wax.
- Carnauba, waxes such as microwax; at least one selected from the group consisting of.
- LICOWAX-OP manufactured by Clariant Chemicals Co., Ltd.
- As a commercial product of natural wax Carnauba Wax No. 1 manufactured by Ceralica NODA Co., Ltd. 1 is mentioned.
- release agent examples include metal soap composed of a bond between a metal and a long-chain fatty acid such as montanic acid, stearic acid, 12-oxystearic acid, and lauric acid.
- metal soaps include powder base L manufactured by NOF CORPORATION.
- the metal element-containing powder may contain, for example, at least one selected from the group consisting of elemental metals, alloys and metal compounds.
- the metal element-containing powder may consist of, for example, at least one selected from the group consisting of elemental metals, alloys and metal compounds.
- the alloy may include at least one selected from the group consisting of solid solutions, eutectic and intermetallic compounds.
- the alloy may be, for example, stainless steel (Fe—Cr based alloy, Fe—Ni—Cr based alloy, etc.).
- the metal compound may be, for example, an oxide such as ferrite.
- the metal element-containing powder may contain one kind of metal element or a plurality of kinds of metal elements.
- the metal element contained in the metal element-containing powder may be, for example, a base metal element, a noble metal element, a transition metal element, or a rare earth element.
- the compound may contain one kind of metal element-containing powder, and may contain a plurality of kinds of metal element-containing powders having different compositions.
- the metal element-containing powder is not limited to the above composition.
- the metal elements contained in the metal element-containing powder include, for example, iron (Fe), copper (Cu), titanium (Ti), manganese (Mn), cobalt (Co), nickel (Ni), zinc (Zn), and aluminum (Zn). Al), tin (Sn), chromium (Cr), barium (Ba), strontium (Sr), lead (Pb), silver (Ag), praseodymium (Pr), neodymium (Nd), samarium (Sm) and dysprosium ( It may be at least one selected from the group consisting of Dy).
- the metal element-containing powder may further contain an element other than the metal element.
- the metal element-containing powder may contain, for example, oxygen ( ⁇ ), beryllium (Be), phosphorus (P), boron (B), or silicon (Si).
- the metal element-containing powder may be a magnetic powder.
- the metal element-containing powder may be a soft magnetic alloy or a ferromagnetic alloy.
- the metal element-containing powder includes, for example, Fe-Si alloy, Fe—Si—Al alloy (Sendust), Fe—Ni alloy (Permalloy), Fe—Cu—Ni alloy (Permalloy), Fe—Co alloy.
- the metal element-containing powder may be a copper alloy such as a Cu—Sn-based alloy, a Cu—Sn—P-based alloy, a Cu—Ni-based alloy, or a Cu—Be-based alloy.
- the metal element-containing powder may contain one of the above elements and compositions, and may contain a plurality of of the above elements and compositions.
- the metal element-containing powder may be Fe alone.
- the metal element-containing powder may be an iron-containing alloy (Fe-based alloy).
- the Fe-based alloy may be, for example, a Fe—Si—Cr based alloy or an Nd—Fe—B based alloy.
- the metal element-containing powder may be at least one of amorphous iron powder and carbonyl iron powder. When the metal element-containing powder contains at least one of Fe simple substance and Fe-based alloy, it is easy to prepare a molded product having a high space factor and excellent magnetic properties from the compound.
- the metal element-containing powder may be an Fe amorphous alloy.
- Fe amorphous alloy powders include, for example, AW2-08, KUAMET-6B2, KUAMET 9A4-II (above, trade name manufactured by Epson Atmix Co., Ltd.), DAP MS3, DAP MS7, DAP MSA10, DAP PB, etc. From DAP PC, DAP MKV49, DAP 410L, DAP 430L, DAP HYB series (above, product name manufactured by Daido Special Steel Co., Ltd.), MH45D, MH28D, MH25D, and MH20D (above, product name manufactured by Kobe Steel Co., Ltd.) At least one selected from the group may be used.
- the metal element-containing powder and the resin composition are mixed while being heated.
- the metal element-containing powder and the resin composition may be kneaded with a kneader, a roll, a stirrer, or the like while being heated.
- the resin composition adheres to a part or the whole of the surface of the metal element-containing particles constituting the metal element-containing powder to coat the metal element-containing particles, and the resin composition.
- Part or all of the epoxy resin in the material becomes a semi-cured product.
- the result is a compound.
- a compound may be obtained by further adding wax to the powder obtained by heating and mixing the metal element-containing powder and the resin composition.
- the resin composition and wax may be mixed in advance.
- a curing agent such as a metal element-containing powder, a siloxane compound, an epoxy resin, or a phenol resin, a curing accelerator, and a coupling agent may be kneaded in a tank.
- the metal element-containing powder, the siloxane compound and the coupling agent are put into the tank and mixed, the epoxy resin, the curing agent and the curing accelerator may be put into the tank to knead the raw materials in the tank. ..
- the curing accelerator After kneading the siloxane compound, the epoxy resin, the curing agent, and the coupling agent in the tank, the curing accelerator may be put in the tank, and the raw materials in the tank may be further kneaded.
- a mixed powder of an epoxy resin, a curing agent, and a curing accelerator (resin mixed powder) is prepared in advance, and then a metal element-containing powder, a siloxane compound, and a coupling agent are kneaded to prepare a metal mixed powder. Subsequently, the metal mixed powder and the above resin mixed powder may be kneaded.
- the kneading time depends on the type of the kneading machine, the volume of the kneading machine, and the production amount of the compound, but for example, it is preferably 1 minute or more, more preferably 2 minutes or more, and 3 minutes or more. Is even more preferable.
- the kneading time is preferably 20 minutes or less, more preferably 15 minutes or less, and even more preferably 10 minutes or less. If the kneading time is less than 1 minute, the kneading is insufficient, the moldability of the compound is impaired, and the degree of curing of the compound varies.
- the resin composition for example, epoxy resin and phenol resin
- the heating temperature is, for example, a semi-cured epoxy resin (B-stage epoxy resin) and a cured epoxy resin (C-stage epoxy resin). Any temperature may be used as long as the production of the epoxy is suppressed.
- the heating temperature may be lower than the activation temperature of the curing accelerator.
- the heating temperature is, for example, preferably 50 ° C. or higher, more preferably 60 ° C. or higher, and even more preferably 70 ° C.
- the heating temperature is preferably 150 ° C. or lower, more preferably 120 ° C. or lower, and even more preferably 110 ° C. or lower.
- the resin composition in the tank softens and easily covers the surface of the metal element-containing particles constituting the metal element-containing powder, and a semi-cured epoxy resin is easily formed. Complete curing of the epoxy resin during kneading is likely to be suppressed.
- the molded product according to the present embodiment may include the above-mentioned compound.
- the molded product is at least one selected from the group consisting of an uncured resin composition, a semi-cured product of the resin composition (B-stage resin composition), and a cured product of the resin composition (C-stage resin composition). May include.
- the molded product may be a cured product of the above compound.
- the method for producing a molded product according to the present embodiment may include a step of pressurizing the compound in a mold.
- the method for producing the molded product may include only the step of pressurizing the compound in the mold, and may include other steps in addition to the step.
- the method for producing the molded product may include a first step, a second step, and a third step. The details of each step will be described below.
- the compound is prepared by the above method.
- a molded product (B stage molded product) is obtained by pressurizing the compound in the mold.
- the resin composition is filled between the individual metal element-containing particles constituting the metal element-containing powder.
- the resin composition then functions as a binder and binds the metal element-containing particles to each other.
- transfer molding of the compound may be carried out.
- the compound may be pressurized at 5 MPa or more and 50 MPa or less.
- the higher the molding pressure the easier it is to obtain a molded product having excellent mechanical strength.
- the molding pressure is preferably 8 MPa or more and 20 MPa or less.
- the density of the molded product formed by transfer molding may be preferably 75% or more and 86% or less, and more preferably 80% or more and 86% or less with respect to the true density of the compound. When the density of the molded product is 75% or more and 86% or less, it is easy to obtain a molded product having excellent mechanical strength.
- the second step and the third step may be carried out collectively.
- the molded product is cured by heat treatment to obtain a C-stage molded product.
- the compound according to the present embodiment contains a siloxane compound which is a kind of elastomer, the elasticity of the entire compound is reduced, and the stress acting on the compound due to the molding shrinkage (thermosetting) of the compound is reduced. As a result, the molding shrinkage rate of the compound is reduced in the process of forming the molded product by thermosetting the compound. Further, as described above, the mechanism is not clear, but since the compound according to the present embodiment contains a predetermined amount of a siloxane compound which is a kind of elastomer, the heat resistance and withstand voltage resistance of the molded product obtained from the compound are improved. To do.
- the temperature of the heat treatment may be a temperature at which the resin composition in the molded product is sufficiently cured.
- the temperature of the heat treatment may be preferably 100 ° C. or higher and 300 ° C. or lower, and more preferably 110 ° C. or higher and 250 ° C. or lower.
- the heat treatment temperature exceeds 300 ° C., the metal element-containing powder is oxidized or the cured resin product is deteriorated by a small amount of oxygen inevitably contained in the heat treatment atmosphere.
- the heat treatment temperature holding time is preferably several minutes or more and 10 hours or less, more preferably 3 minutes. It may be 8 hours or less.
- Example 1 [Preparation of compound] 50 g of biphenylene aralkyl type epoxy resin, 50 g of polyfunctional epoxy resin, 14.5 g of phenol novolac resin 1 (curing agent), 23.6 g of phenol novolac resin 2 (curing agent), 5.9 g of urea catalyst (curing agent) Curing accelerator), 7.5 g of zinc chloride type metal soap (release agent), 2.0 g of montanic acid ester (release agent (wax)), and 4.0 g of natural wax (release agent (wax)). )) was put into a plastic container. A resin mixture was prepared by mixing these raw materials in a plastic container for 10 minutes.
- the resin mixture corresponds to all other components of the resin composition except the siloxane compound and the coupling agent.
- the biphenylene aralkyl type epoxy resin NC-3000 manufactured by Nippon Kayaku Co., Ltd. was used.
- the polyfunctional epoxy resin VG-3101L manufactured by Printec Co., Ltd. was used.
- the phenol novolac resin 1 HF-3M manufactured by Meiwa Kasei Co., Ltd. was used.
- MEW-1800 manufactured by Meiwa Kasei Co., Ltd. was used.
- As the urea catalyst U-CAT3512T manufactured by Sun Appro Co., Ltd. was used.
- gincrowlate type metal soap powder base L manufactured by NOF CORPORATION was used.
- montanic acid ester LICOWAX-OP manufactured by Clariant Chemicals Co., Ltd. was used.
- As a natural wax Carnauba Wax No. 1 manufactured by Ceralica NODA Co., Ltd. 1 was used.
- Amorphous iron powder 1 and amorphous iron powder 2 were uniformly mixed for 5 minutes with a pressurized twin-screw kneader (manufactured by Nihon Spindle Manufacturing Co., Ltd., capacity 5 L) to prepare 3741 g of metal element-containing powder.
- the content of the amorphous iron powder 1 in the metal element-containing powder was 82% by mass.
- the content of the amorphous iron powder 2 in the metal element-containing powder was 18% by mass.
- the above resin mixture was added to the contents of the twin-screw kneader, and the contents were melted and kneaded for 15 minutes while maintaining the temperature of the contents at 120 ° C.
- the kneaded product obtained by the above melting and kneading was cooled to room temperature, and then the kneaded product was crushed with a hammer until the kneaded product had a predetermined particle size.
- the above-mentioned "melting” means melting at least a part of the resin composition in the contents of the biaxial kneader.
- the metal element-containing powder in the compound does not melt during the compound preparation process.
- amorphous iron powder 1 KUAMET 9A4-II 053C03 (average particle size 24 ⁇ m) manufactured by Epson Atmix Co., Ltd. was used.
- amorphous iron powder 2 AW2-08 (average particle size 5.3 ⁇ m) manufactured by Epson Atmix Co., Ltd. was used.
- methacryloxyoctyltrimethoxysilane KBM-5803 manufactured by Shin-Etsu Chemical Co., Ltd. was used.
- 3-mercaptopropyltrimethoxysilane KBM-803 manufactured by Shin-Etsu Chemical Co., Ltd. was used.
- the caprolactone-modified dimethyl silicone DBL-C32 manufactured by Gelest was used. This caprolactone-modified dimethyl silicone is a compound represented by the above chemical formula (3).
- the compound of Example 1 was prepared by the above method.
- the content of the metal element-containing powder in the compound was 95.5% by mass.
- the bending elongation rate ⁇ (unit:%) was calculated based on the following mathematical formula (C).
- P is the load (unit: N) when the test piece is broken.
- Lv is the distance (unit: mm) between the two fulcrums.
- W is the width (unit: mm) of the test piece.
- T is the thickness (unit: mm) of the test piece.
- F / Y is the gradient (unit: N / mm) of the straight line portion of the load-deflection curve.
- S is the deflection (unit: mm) of the test piece immediately before the test piece is destroyed.
- the high-voltage line and the ground wire were connected to the high-voltage output terminal and the ground terminal of the high-voltage amplifier, respectively.
- the waveform output of the function generator was input to the high-voltage amplifier, and a test voltage was generated so as to boost the voltage from 0 V to a maximum of 2000 V at a rate of 10 V per second, and applied to the test piece.
- the voltage at the time when the current passing through the test piece exceeded 10 mA was read.
- stainless steel electrodes were placed at different positions on the test piece, and a voltage was applied in the same manner. It was repeated a predetermined number of times, and the average value of the read voltages was taken as the withstand voltage (dielectric breakdown voltage: V / mm) of the test piece.
- the compound according to the present invention has high industrial value because a molded product having both heat resistance and withstand voltage can be obtained.
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Abstract
A compound comprising a metallic-element-containing powder and a resin composition, wherein the resin composition comprises an epoxy resin and one or more compounds each having a siloxane bond, the compounds having a siloxane bond being contained in an amount of 20 parts by mass or less per 100 parts by mass of the epoxy resin and including a siloxane compound having a structure represented by chemical formula (1).
Description
本発明は、コンパウンド及び成形体に関する。
The present invention relates to a compound and a molded product.
金属粉末及び樹脂組成物を含むコンパウンドは、金属粉末の諸物性に応じて、例えば、インダクタ、電磁波シールド、又はボンド磁石等の多様な工業製品の原材料として利用される（下記特許文献１参照。）
The compound containing the metal powder and the resin composition is used as a raw material for various industrial products such as an inductor, an electromagnetic wave shield, or a bond magnet, depending on the physical characteristics of the metal powder (see Patent Document 1 below).
インダクタ等の工業製品には、熱や電圧に対する耐性が要求される場合がある。本発明は、耐熱性及び耐電圧性を共に有する成形体を得ることが可能なコンパウンド、及び当該コンパウンドを備える成形体を提供することを目的とする。
Industrial products such as inductors may be required to withstand heat and voltage. An object of the present invention is to provide a compound capable of obtaining a molded product having both heat resistance and withstand voltage resistance, and a molded product having the compound.
本発明の一側面に係るコンパウンドは、金属元素含有粉と、樹脂組成物と、を備え、樹脂組成物が、エポキシ樹脂、及びシロキサン結合を有する化合物（ｃｈｅｍｉｃａｌ ｃоｍｐоｕｎｄ）を含有し、シロキサン結合を有する化合物の含有量が、エポキシ樹脂１００質量部に対して、２０質量部以下であり、シロキサン結合を有する化合物が、下記化学式（１）で表される構造を有するシロキサン化合物を含む。
［前記化学式（１）中、ｎは２～２００の整数であり、Ｒ１及びＲ２其々は独立に、炭素数１～１０のアルキル基、炭素数６～１０のアリール基、炭素数１～１０のアルコキシ基、エポキシ基を有する１価の有機基、カルボキシ基を有する１価の有機基、又は炭素数３～５００のポリアルキレンエーテル基である。］
The compound according to one aspect of the present invention comprises a metal element-containing powder and a resin composition, and the resin composition contains an epoxy resin and a compound having a siloxane bond (chemical clond) and has a siloxane bond. The content of the compound is 20 parts by mass or less with respect to 100 parts by mass of the epoxy resin, and the compound having a siloxane bond includes a siloxane compound having a structure represented by the following chemical formula (1).
[In the chemical formula (1), n is an integer of 2 to 200, and R 1 and R 2 are independently alkyl groups having 1 to 10 carbon atoms, aryl groups having 6 to 10 carbon atoms, and 1 carbon group. It is a monovalent organic group having an alkoxy group of ~ 10, an epoxy group, a monovalent organic group having a carboxy group, or a polyalkylene ether group having 3 to 500 carbon atoms. ]
本発明の一側面に係る上記コンパウンドでは、シロキサン化合物が、下記化学式（２）で表される構造単位をさらに有してよい。
In the above compound according to one aspect of the present invention, the siloxane compound may further have a structural unit represented by the following chemical formula (2).
本発明の一側面に係る上記コンパウンドは、シロキサン化合物として、下記化学式（３）で表される化合物を含んでよい。
The compound according to one aspect of the present invention may contain a compound represented by the following chemical formula (3) as a siloxane compound.
本発明の一側面に係る上記コンパウンドは、エポキシ樹脂として、ビフェニレンアラルキル型エポキシ樹脂及びイソシアネート変性エポキシ樹脂のうちの少なくとも一種を含んでよい。
The compound according to one aspect of the present invention may contain at least one of a biphenylene aralkyl type epoxy resin and an isocyanate-modified epoxy resin as the epoxy resin.
本発明の一側面に係る上記コンパウンドでは、金属元素含有粉の含有量が、９０質量％以上１００質量％未満であってよい。
In the above compound according to one aspect of the present invention, the content of the metal element-containing powder may be 90% by mass or more and less than 100% by mass.
本発明の一側面に係る成形体は、上記コンパウンドを備える。
The molded product according to one aspect of the present invention includes the above compound.
本発明によれば、耐熱性及び耐電圧性を共に有する成形体を得ることが可能なコンパウンド、及び当該コンパウンドを備える成形体が提供される。
According to the present invention, there is provided a compound capable of obtaining a molded product having both heat resistance and withstand voltage resistance, and a molded product having the compound.
以下、本発明の好適な実施形態について説明する。ただし、本発明は下記実施形態に何ら限定されるものではない。
Hereinafter, preferred embodiments of the present invention will be described. However, the present invention is not limited to the following embodiments.
＜コンパウンドの概要＞
本実施形態に係るコンパウンドは、金属元素含有粉と、樹脂組成物と、を備える。金属元素含有粉は、複数（多数）の金属元素含有粒子から構成される。金属元素含有粉（金属元素含有粒子）は、例えば、金属単体、合金及び金属化合物からなる群より選ばれる少なくとも一種を含有してよい。樹脂組成物は少なくとも、エポキシ樹脂、及びシロキサン結合を有する化合物を含有する。シロキサン結合を有する化合物は、「シロキサン化合物」と表記される場合がある。樹脂組成物は、エポキシ樹脂及びシロキサン化合物に加えて、他の成分を含有してよい。例えば、樹脂組成物は、硬化剤を含有してよい。樹脂組成物は、硬化促進剤を含有してよい。樹脂組成物は、添加剤を含有してよい。樹脂組成物は、エポキシ樹脂、シロキサン化合物、硬化剤、硬化促進剤及び添加剤を包含し得る成分であって、有機溶媒と金属元素含有粉とを除く残りの成分（不揮発性成分）であってよい。添加剤とは、樹脂組成物のうち、樹脂、シロキサン化合物、硬化剤及び硬化促進剤を除く残部の成分である。添加剤は、例えば、カップリング剤又は難燃剤等である。樹脂組成物が添加剤としてワックスを含有してもよい。コンパウンドは、粉末（コンパウンド粉）であってよい。 <Outline of compound>
The compound according to the present embodiment includes a metal element-containing powder and a resin composition. The metal element-containing powder is composed of a plurality of (many) metal element-containing particles. The metal element-containing powder (metal element-containing particles) may contain, for example, at least one selected from the group consisting of elemental metals, alloys and metal compounds. The resin composition contains at least an epoxy resin and a compound having a siloxane bond. A compound having a siloxane bond may be referred to as a "siloxane compound". The resin composition may contain other components in addition to the epoxy resin and the siloxane compound. For example, the resin composition may contain a curing agent. The resin composition may contain a curing accelerator. The resin composition may contain additives. The resin composition is a component that can include an epoxy resin, a siloxane compound, a curing agent, a curing accelerator, and an additive, and is a remaining component (nonvolatile component) excluding an organic solvent and a metal element-containing powder. Good. The additive is a component of the rest of the resin composition excluding the resin, the siloxane compound, the curing agent and the curing accelerator. The additive is, for example, a coupling agent or a flame retardant. The resin composition may contain wax as an additive. The compound may be a powder (compound powder).
本実施形態に係るコンパウンドは、金属元素含有粉と、樹脂組成物と、を備える。金属元素含有粉は、複数（多数）の金属元素含有粒子から構成される。金属元素含有粉（金属元素含有粒子）は、例えば、金属単体、合金及び金属化合物からなる群より選ばれる少なくとも一種を含有してよい。樹脂組成物は少なくとも、エポキシ樹脂、及びシロキサン結合を有する化合物を含有する。シロキサン結合を有する化合物は、「シロキサン化合物」と表記される場合がある。樹脂組成物は、エポキシ樹脂及びシロキサン化合物に加えて、他の成分を含有してよい。例えば、樹脂組成物は、硬化剤を含有してよい。樹脂組成物は、硬化促進剤を含有してよい。樹脂組成物は、添加剤を含有してよい。樹脂組成物は、エポキシ樹脂、シロキサン化合物、硬化剤、硬化促進剤及び添加剤を包含し得る成分であって、有機溶媒と金属元素含有粉とを除く残りの成分（不揮発性成分）であってよい。添加剤とは、樹脂組成物のうち、樹脂、シロキサン化合物、硬化剤及び硬化促進剤を除く残部の成分である。添加剤は、例えば、カップリング剤又は難燃剤等である。樹脂組成物が添加剤としてワックスを含有してもよい。コンパウンドは、粉末（コンパウンド粉）であってよい。 <Outline of compound>
The compound according to the present embodiment includes a metal element-containing powder and a resin composition. The metal element-containing powder is composed of a plurality of (many) metal element-containing particles. The metal element-containing powder (metal element-containing particles) may contain, for example, at least one selected from the group consisting of elemental metals, alloys and metal compounds. The resin composition contains at least an epoxy resin and a compound having a siloxane bond. A compound having a siloxane bond may be referred to as a "siloxane compound". The resin composition may contain other components in addition to the epoxy resin and the siloxane compound. For example, the resin composition may contain a curing agent. The resin composition may contain a curing accelerator. The resin composition may contain additives. The resin composition is a component that can include an epoxy resin, a siloxane compound, a curing agent, a curing accelerator, and an additive, and is a remaining component (nonvolatile component) excluding an organic solvent and a metal element-containing powder. Good. The additive is a component of the rest of the resin composition excluding the resin, the siloxane compound, the curing agent and the curing accelerator. The additive is, for example, a coupling agent or a flame retardant. The resin composition may contain wax as an additive. The compound may be a powder (compound powder).
本実施形態に係るコンパウンドは、エラストマーの一種であるシロキサン化合物を所定量含有する。所定量のシロキサン化合物によりコンパウンドから得られる成形体の耐熱性及び耐電圧性が向上する理由は定かではないが、発明者らは次のような可能性を推察している。第一に、シロキサン化合物を添加することで含有成分の流動性が向上し、成形時に内部ボイドの発生を抑制できるためであると考える。第二に、金属元素含有粉とエポキシ樹脂との相溶性が低く、両者の界面から特性低下がもたらされると考えられるが、シロキサン化合物を添加することで両者の相溶性を向上できるためであると考える。ただし、本発明に係る作用効果は、上記の事項に限定されない。
The compound according to this embodiment contains a predetermined amount of a siloxane compound which is a kind of elastomer. The reason why the heat resistance and withstand voltage resistance of the molded product obtained from the compound are improved by the predetermined amount of the siloxane compound is not clear, but the inventors speculate the following possibilities. First, it is considered that the addition of the siloxane compound improves the fluidity of the contained components and suppresses the generation of internal voids during molding. Secondly, the compatibility between the metal element-containing powder and the epoxy resin is low, and it is considered that the characteristics are deteriorated from the interface between the two. This is because the compatibility between the two can be improved by adding the siloxane compound. Think. However, the action and effect according to the present invention are not limited to the above items.
コンパウンドは、金属元素含有粉と、当該金属元素含有粉を構成する個々の金属元素含有粒子の表面に付着した樹脂組成物と、を備えてよい。樹脂組成物は、当該粒子の表面の全体を覆っていてもよく、当該粒子の表面の一部のみを覆っていてもよい。コンパウンドは、未硬化の樹脂組成物と、金属元素含有粉と、を備えてよい。コンパウンドは、樹脂組成物の半硬化物（例えばＢステージの樹脂組成物）と、金属元素含有粉と、を備えてよい。コンパウンドは、未硬化の樹脂組成物、及び樹脂組成物の半硬化物の両方を備えてもよい。コンパウンドは、金属元素含有粉と樹脂組成物とからなっていてよい。
The compound may include a metal element-containing powder and a resin composition adhering to the surface of each metal element-containing particle constituting the metal element-containing powder. The resin composition may cover the entire surface of the particles, or may cover only a part of the surface of the particles. The compound may include an uncured resin composition and a metal element-containing powder. The compound may include a semi-cured product of the resin composition (for example, a B-stage resin composition) and a metal element-containing powder. The compound may comprise both an uncured resin composition and a semi-cured resin composition. The compound may consist of a metal element-containing powder and a resin composition.
コンパウンドにおける金属元素含有粉の含有量は、コンパウンド全体の質量に対して、９０質量％以上１００質量％未満、９０質量％以上９９．８質量％以下、９２質量％以上９９．５質量％以下、９４質量％以上９８．５質量％以下、又は９４質量％以上９７．５質量％以下であってよい。コンパウンドは、金属元素含有粉に加えて、他の充填材（例えば、シリカのフィラー）を含有してもよい。
The content of the metal element-containing powder in the compound is 90% by mass or more and less than 100% by mass, 90% by mass or more and 99.8% by mass or less, 92% by mass or more and 99.5% by mass or less, based on the total mass of the compound. It may be 94% by mass or more and 98.5% by mass or less, or 94% by mass or more and 97.5% by mass or less. The compound may contain other fillers (eg, silica fillers) in addition to the metal element-containing powder.
コンパウンドにおける樹脂組成物の含有量は、コンパウンド全体の質量（例えば、金属元素含有粉及び樹脂組成物の質量の合計）に対して、０．２質量％以上１０質量％以下、又は４質量％以上６質量％以下であってよい。
The content of the resin composition in the compound is 0.2% by mass or more and 10% by mass or less, or 4% by mass or more, based on the total mass of the compound (for example, the total mass of the metal element-containing powder and the resin composition). It may be 6% by mass or less.
コンパウンドにおけるシロキサン化合物の含有量は、エポキシ樹脂１００質量部に対して、２０質量部以下であるが、１７．５質量部以下であってよく、１５質量部以下であってよい。シロキサン化合物の含有量が上記の範囲内である場合、成形体の耐熱性及び耐電圧性が両立される。一方、コンパウンドにおけるシロキサン化合物の含有量の下限は特に限定されないが、成形性等の観点から、エポキシ樹脂１００質量部に対して、０．１質量部以上であってよく、５質量部以上であってよく、７．５質量部以上であってよく、１０質量部以上であってよい。
The content of the siloxane compound in the compound is 20 parts by mass or less with respect to 100 parts by mass of the epoxy resin, but may be 17.5 parts by mass or less, and may be 15 parts by mass or less. When the content of the siloxane compound is within the above range, both heat resistance and withstand voltage resistance of the molded product are compatible. On the other hand, the lower limit of the content of the siloxane compound in the compound is not particularly limited, but from the viewpoint of moldability and the like, it may be 0.1 part by mass or more and 5 parts by mass or more with respect to 100 parts by mass of the epoxy resin. It may be 7.5 parts by mass or more, and may be 10 parts by mass or more.
金属元素含有粉の平均粒子径は、特に限定されないが、例えば、１μｍ以上３００μｍ以下であってよい。平均粒子径は、例えば粒度分布計によって測定されてよい。金属元素含有粉を構成する個々の金属元素含有粒子の形状は限定されないが、例えば、球状、扁平形状、角柱状又は針状であってよい。コンパウンドは、平均粒子径が異なる複数種の金属元素含有粉を備えてよい。
The average particle size of the metal element-containing powder is not particularly limited, but may be, for example, 1 μm or more and 300 μm or less. The average particle size may be measured, for example, by a particle size distribution meter. The shape of the individual metal element-containing particles constituting the metal element-containing powder is not limited, and may be, for example, spherical, flat, prismatic, or needle-shaped. The compound may include a plurality of types of metal element-containing powders having different average particle sizes.
コンパウンドに含まれる金属元素含有粉の組成又は組合せに応じて、コンパウンドから形成される成形体の電磁気的特性等の諸特性を自在に制御し、当該成形体を様々な工業製品又はそれらの原材料に利用することができる。コンパウンドを用いて製造される工業製品は、例えば、自動車、医療機器、電子機器、電気機器、情報通信機器、家電製品、音響機器、及び一般産業機器であってよい。例えば、コンパウンドが金属元素含有粉としてＳｍ‐Ｆｅ‐Ｎ系合金又はＮｄ‐Ｆｅ‐Ｂ系合金等の永久磁石を含む場合、コンパウンドは、ボンド磁石の原材料として利用されてよい。コンパウンドが金属元素含有粉としてＦｅ‐Ｓｉ‐Ｃｒ系合金又はフェライト等の軟磁性粉を含む場合、コンパウンドは、インダクタ（例えばＥＭＩフィルタ）又はトランスの原材料（例えば磁芯）として利用されてよい。コンパウンドが金属元素含有粉として鉄と銅とを含む場合、コンパウンドから形成された成形体（例えばシート）は、電磁波シールドとして利用されてよい。
Depending on the composition or combination of the metal element-containing powder contained in the compound, various properties such as the electromagnetic properties of the molded product formed from the compound can be freely controlled, and the molded product can be used as various industrial products or their raw materials. It can be used. Industrial products manufactured using the compound may be, for example, automobiles, medical equipment, electronic equipment, electrical equipment, information and communication equipment, home appliances, audio equipment, and general industrial equipment. For example, when the compound contains a permanent magnet such as a Sm-Fe-N alloy or an Nd-Fe-B alloy as a metal element-containing powder, the compound may be used as a raw material for a bond magnet. When the compound contains a soft magnetic powder such as a Fe—Si—Cr based alloy or ferrite as the metal element-containing powder, the compound may be used as an inductor (for example, an EMI filter) or a raw material for a transformer (for example, a magnetic core). When the compound contains iron and copper as metal element-containing powder, a molded product (for example, a sheet) formed from the compound may be used as an electromagnetic wave shield.
＜コンパウンドの組成＞
（樹脂組成物）
樹脂組成物は、金属元素含有粉を構成する金属元素含有粒子の結合材（バインダ）としての機能を有し、コンパウンドから形成される成形体に機械的強度を付与する。例えば、樹脂組成物は、金型を用いてコンパウンドが高圧で成形される際に、金属元素含有粒子の間に充填され、金属元素含有粒子を互いに結着する。成形体中の樹脂組成物を硬化させることにより、樹脂組成物の硬化物が金属元素含有粒子同士をより強固に結着して、成形体の機械的強度が向上する。 <Composite composition>
(Resin composition)
The resin composition has a function as a binder of the metal element-containing particles constituting the metal element-containing powder, and imparts mechanical strength to the molded product formed from the compound. For example, the resin composition is filled between the metal element-containing particles when the compound is molded at high pressure using a mold, and the metal element-containing particles are bound to each other. By curing the resin composition in the molded product, the cured product of the resin composition binds the metal element-containing particles more firmly, and the mechanical strength of the molded product is improved.
（樹脂組成物）
樹脂組成物は、金属元素含有粉を構成する金属元素含有粒子の結合材（バインダ）としての機能を有し、コンパウンドから形成される成形体に機械的強度を付与する。例えば、樹脂組成物は、金型を用いてコンパウンドが高圧で成形される際に、金属元素含有粒子の間に充填され、金属元素含有粒子を互いに結着する。成形体中の樹脂組成物を硬化させることにより、樹脂組成物の硬化物が金属元素含有粒子同士をより強固に結着して、成形体の機械的強度が向上する。 <Composite composition>
(Resin composition)
The resin composition has a function as a binder of the metal element-containing particles constituting the metal element-containing powder, and imparts mechanical strength to the molded product formed from the compound. For example, the resin composition is filled between the metal element-containing particles when the compound is molded at high pressure using a mold, and the metal element-containing particles are bound to each other. By curing the resin composition in the molded product, the cured product of the resin composition binds the metal element-containing particles more firmly, and the mechanical strength of the molded product is improved.
樹脂組成物は、熱硬化性樹脂として、少なくともエポキシ樹脂を含有する。コンパウンドが、熱硬化性樹脂の中でも比較的に流動性に優れたエポキシ樹脂を含むことにより、コンパウンドの流動性、保存安定性、及び成形性が向上する。ただし、本発明の効果が阻害されない限りにおいて、コンパウンドはエポキシ樹脂に加えて他の樹脂を含んでもよい。例えば、樹脂組成物は、熱硬化性樹脂として、フェノール樹脂及びポリアミドイミド樹脂のうち少なくも一種を含んでもよい。樹脂組成物がエポキシ樹脂及びフェノール樹脂の両方を含む場合、フェノール樹脂はエポキシ樹脂の硬化剤として機能してもよい。樹脂組成物は、熱可塑性樹脂を含んでもよい。熱可塑性樹脂は、例えば、アクリル樹脂、ポリエチレン、ポリプロピレン、ポリスチレン、ポリ塩化ビニル、及びポリエチレンテレフタレートからなる群より選ばれる少なくとも一種であってよい。樹脂組成物は、熱硬化性樹脂及び熱可塑性樹脂の両方を含んでよい。樹脂組成物は、シリコーン樹脂を含んでもよい。
The resin composition contains at least an epoxy resin as a thermosetting resin. When the compound contains an epoxy resin having relatively excellent fluidity among thermosetting resins, the fluidity, storage stability, and moldability of the compound are improved. However, the compound may contain other resins in addition to the epoxy resin as long as the effects of the present invention are not impaired. For example, the resin composition may contain at least one of a phenol resin and a polyamide-imide resin as a thermosetting resin. When the resin composition contains both an epoxy resin and a phenol resin, the phenol resin may function as a curing agent for the epoxy resin. The resin composition may include a thermoplastic resin. The thermoplastic resin may be at least one selected from the group consisting of, for example, acrylic resin, polyethylene, polypropylene, polystyrene, polyvinyl chloride, and polyethylene terephthalate. The resin composition may contain both a thermosetting resin and a thermoplastic resin. The resin composition may contain a silicone resin.
エポキシ樹脂は、例えば、１分子中に２個以上のエポキシ基を有する樹脂であってよい。エポキシ樹脂は、例えば、１分子中に３個以上のエポキシ基を有する樹脂であってよい。エポキシ樹脂は、多官能型エポキシ樹脂であってよい。エポキシ樹脂は、例えば、ビフェニル型エポキシ樹脂、スチルベン型エポキシ樹脂、ジフェニルメタン型エポキシ樹脂、硫黄原子含有型エポキシ樹脂、ノボラック型エポキシ樹脂、ジシクロペンタジエン型エポキシ樹脂、サリチルアルデヒド型エポキシ樹脂、ナフトール類とフェノール類との共重合型エポキシ樹脂、アラルキル型フェノール樹脂のエポキシ化物、ビスフェノール型エポキシ樹脂、ビスフェノール骨格を含有するエポキシ樹脂、アルコール類のグリシジルエーテル型エポキシ樹脂、パラキシリレン及び／又はメタキシリレン変性フェノール樹脂のグリシジルエーテル型エポキシ樹脂、テルペン変性フェノール樹脂のグリシジルエーテル型エポキシ樹脂、シクロペンタジエン型エポキシ樹脂、多環芳香環変性フェノール樹脂のグリシジルエーテル型エポキシ樹脂、ナフタレン環含有フェノール樹脂のグリシジルエーテル型エポキシ樹脂、グリシジルエステル型エポキシ樹脂、グリシジル型又はメチルグリシジル型のエポキシ樹脂、脂環型エポキシ樹脂、ハロゲン化フェノールノボラック型エポキシ樹脂、オルソクレゾールノボラック型エポキシ樹脂、ハイドロキノン型エポキシ樹脂、トリメチロールプロパン型エポキシ樹脂、及びオレフィン結合を過酢酸等の過酸で酸化して得られる線状脂肪族エポキシ樹脂からなる群より選ばれる少なくとも一種であってよい。
The epoxy resin may be, for example, a resin having two or more epoxy groups in one molecule. The epoxy resin may be, for example, a resin having three or more epoxy groups in one molecule. The epoxy resin may be a polyfunctional epoxy resin. Epoxy resins include, for example, biphenyl type epoxy resin, stillben type epoxy resin, diphenylmethane type epoxy resin, sulfur atom-containing epoxy resin, novolak type epoxy resin, dicyclopentadiene type epoxy resin, salicylaldehyde type epoxy resin, naphthols and phenol. Copolymerization type epoxy resin, aralkyl type phenol resin epoxidized product, bisphenol type epoxy resin, epoxy resin containing bisphenol skeleton, alcoholic glycidyl ether type epoxy resin, paraxylylene and / or metaxylylene modified phenol resin glycidyl ether Type epoxy resin, glycidyl ether type epoxy resin of terpen-modified phenol resin, cyclopentadiene type epoxy resin, glycidyl ether type epoxy resin of polycyclic aromatic ring-modified phenol resin, glycidyl ether type epoxy resin of naphthalene ring-containing phenol resin, glycidyl ester type Epoxy resin, glycidyl type or methyl glycidyl type epoxy resin, alicyclic epoxy resin, halogenated phenol novolac type epoxy resin, orthocresol novolac type epoxy resin, hydroquinone type epoxy resin, trimethylolpropane type epoxy resin, and olefin bond It may be at least one selected from the group consisting of linear aliphatic epoxy resins obtained by oxidation with a peracid such as peracetic acid.
流動性に優れている観点において、エポキシ樹脂は、ビフェニル型エポキシ樹脂、オルソクレゾールノボラック型エポキシ樹脂、フェノールノボラック型エポキシ樹脂、ビスフェノール型エポキシ樹脂、ビスフェノール骨格を有するエポキシ樹脂、サリチルアルデヒドノボラック型エポキシ樹脂、及びナフトールノボラック型エポキシ樹脂からなる群より選ばれる少なくとも一種であってよい。
From the viewpoint of excellent fluidity, the epoxy resins include biphenyl type epoxy resin, orthocresol novolac type epoxy resin, phenol novolac type epoxy resin, bisphenol type epoxy resin, epoxy resin having a bisphenol skeleton, and salicylaldehyde novolac type epoxy resin. And at least one selected from the group consisting of naphthol novolac type epoxy resins.
エポキシ樹脂は、結晶性のエポキシ樹脂であってよい。結晶性のエポキシ樹脂の分子量は比較的低いにもかかわらず、結晶性のエポキシ樹脂は比較的高い融点を有し、且つ流動性に優れる。結晶性のエポキシ樹脂（結晶性の高いエポキシ樹脂）は、例えば、ハイドロキノン型エポキシ樹脂、ビスフェノール型エポキシ樹脂、チオエーテル型エポキシ樹脂、及びビフェニル型エポキシ樹脂からなる群より選ばれる少なくとも一種であってよい。結晶性のエポキシ樹脂の市販品は、例えば、エピクロン８６０、エピクロン１０５０、エピクロン１０５５、エピクロン２０５０、エピクロン３０５０、エピクロン４０５０、エピクロン７０５０、エピクロンＨＭ‐０９１、エピクロンＨＭ‐１０１、エピクロンＮ‐７３０Ａ、エピクロンＮ‐７４０、エピクロンＮ‐７７０、エピクロンＮ‐７７５、エピクロンＮ‐８６５、エピクロンＨＰ‐４０３２Ｄ、エピクロンＨＰ‐７２００Ｌ、エピクロンＨＰ‐７２００、エピクロンＨＰ‐７２００Ｈ、エピクロンＨＰ‐７２００ＨＨ、エピクロンＨＰ‐７２００ＨＨＨ、エピクロンＨＰ‐４７００、エピクロンＨＰ‐４７１０、エピクロンＨＰ‐４７７０、エピクロンＨＰ‐５０００、エピクロンＨＰ‐６０００、Ｎ５００Ｐ‐２、及びＮ５００Ｐ‐１０（以上、ＤＩＣ株式会社製の商品名）、ＮＣ‐３０００、ＮＣ‐３０００‐Ｌ、ＮＣ‐３０００‐Ｈ、ＮＣ‐３１００、ＣＥＲ‐３０００‐Ｌ、ＮＣ‐２０００‐Ｌ、ＸＤ‐１０００、ＮＣ‐７０００‐Ｌ、ＮＣ‐７３００‐Ｌ、ＥＰＰＮ‐５０１Ｈ、ＥＰＰＮ‐５０１ＨＹ、ＥＰＰＮ‐５０２Ｈ、ＥＯＣＮ‐１０２０、ＥＯＣＮ‐１０２Ｓ、ＥＯＣＮ‐１０３Ｓ、ＥＯＣＮ‐１０４Ｓ、ＣＥＲ‐１０２０、ＥＰＰＮ‐２０１、ＢＲＥＮ‐Ｓ、ＢＲＥＮ‐１０Ｓ（以上、日本化薬株式会社製の商品名）、ＹＸ‐４０００、ＹＸ‐４０００Ｈ、ＹＬ４１２１Ｈ、及びＹＸ‐８８００（以上、三菱ケミカル株式会社製の商品名）からなる群より選ばれる少なくとも一種であってよい。
The epoxy resin may be a crystalline epoxy resin. Although the molecular weight of the crystalline epoxy resin is relatively low, the crystalline epoxy resin has a relatively high melting point and is excellent in fluidity. The crystalline epoxy resin (highly crystalline epoxy resin) may be at least one selected from the group consisting of, for example, a hydroquinone type epoxy resin, a bisphenol type epoxy resin, a thioether type epoxy resin, and a biphenyl type epoxy resin. Commercially available crystalline epoxy resins include, for example, Epicron 860, Epicron 1050, Epicron 1055, Epicron 2050, Epicron 3050, Epicron 4050, Epicron 7050, Epicron HM-091, Epicron HM-101, Epicron N-730A, Epicron N. -740, Epicron N-770, Epicron N-775, Epicron N-865, Epicron HP-4032D, Epicron HP-7200L, Epicron HP-7200, Epicron HP-7200H, Epicron HP-7200HH, Epicron HP-7200HH, Epicron HP -4700, Epicron HP-4710, Epicron HP-4770, Epicron HP-5000, Epicron HP-6000, N500P-2, and N500P-10 (hereinafter, trade names manufactured by DIC Corporation), NC-3000, NC-3000. -L, NC-3000-H, NC-3100, CER-3000-L, NC-2000-L, XD-1000, NC-7000-L, NC-7300-L, EPPN-501H, EPPN-501HY, EPPN -502H, EOCN-1020, EOCN-102S, EOCN-103S, EOCN-104S, CER-1020, EPPN-201, BREN-S, BREN-10S (above, trade name manufactured by Nippon Kayaku Co., Ltd.), YX- It may be at least one selected from the group consisting of 4000, YX-4000H, YL4121H, and YX-8800 (above, trade name manufactured by Mitsubishi Chemical Corporation).
コンパウンドの成形収縮率が低減され易く、また成形体の耐熱性及び耐電圧性が向上し易い観点から、樹脂組成物は、エポキシ樹脂として、ビフェニレンアラルキル型エポキシ樹脂及びイソシアネート変性エポキシ樹脂のうちの少なくとも一種を含んでよい。樹脂組成物は、エポキシ樹脂として、ビフェニレンアラルキル型エポキシ樹脂及びイソシアネート変性エポキシ樹脂の両方を含んでよい。ビフェニレンアラルキル型エポキシ樹脂の市販品は、例えば、日本化薬株式会社製のＮＣ‐３０００であってよい。イソシアネート変性エポキシ樹脂の市販品は、例えば、旭化成株式会社（旧旭化成イーマテリアルズ株式会社）製のＡＥＲ‐４００１であってよい。成形体の耐熱性及び耐電圧性が向上し易い観点から、樹脂組成物は、多官能型エポキシ樹脂を含んでよい。多官能型エポキシ樹脂の市販品としては、例えば、株式会社プリンテック製のＶＧ－３１０１Ｌ等が挙げられる。
From the viewpoint that the molding shrinkage of the compound is easily reduced and the heat resistance and withstand voltage of the molded product are easily improved, the resin composition is, as an epoxy resin, at least one of a biphenylene aralkyl type epoxy resin and an isocyanate-modified epoxy resin. May include one type. The resin composition may contain both a biphenylene aralkyl type epoxy resin and an isocyanate-modified epoxy resin as the epoxy resin. The commercially available product of the biphenylene aralkyl type epoxy resin may be, for example, NC-3000 manufactured by Nippon Kayaku Co., Ltd. The commercially available product of the isocyanate-modified epoxy resin may be, for example, AER-4001 manufactured by Asahi Kasei Corporation (formerly Asahi Kasei E-Materials Corporation). The resin composition may contain a polyfunctional epoxy resin from the viewpoint of easily improving the heat resistance and withstand voltage of the molded product. Examples of commercially available products of the polyfunctional epoxy resin include VG-3101L manufactured by Printec Co., Ltd.
樹脂組成物は、上記のうち一種のエポキシ樹脂を含有してよい。樹脂組成物は、上記のうち複数種のエポキシ樹脂を含有してもよい。
The resin composition may contain one of the above epoxy resins. The resin composition may contain a plurality of types of epoxy resins among the above.
硬化剤は、低温から室温の範囲でエポキシ樹脂を硬化させる硬化剤と、加熱に伴ってエポキシ樹脂を硬化させる加熱硬化型硬化剤と、に分類される。低温から室温の範囲でエポキシ樹脂を硬化させる硬化剤は、例えば、脂肪族ポリアミン、ポリアミノアミド、及びポリメルカプタン等である。加熱硬化型硬化剤は、例えば、芳香族ポリアミン、酸無水物、フェノールノボラック樹脂、及びジシアンジアミド（ＤＩＣＹ）等である。
The curing agent is classified into a curing agent that cures the epoxy resin in the range of low temperature to room temperature and a heat curing type curing agent that cures the epoxy resin with heating. Hardeners that cure epoxy resins in the low to room temperature range are, for example, aliphatic polyamines, polyaminoamides, and polymercaptans. The heat-curable curing agent is, for example, aromatic polyamine, acid anhydride, phenol novolac resin, dicyandiamide (DICY) and the like.
低温から室温の範囲でエポキシ樹脂を硬化させる硬化剤を用いた場合、エポキシ樹脂の硬化物のガラス転移点は低く、エポキシ樹脂の硬化物は軟らかい傾向がある。その結果、コンパウンドから形成された成形体も軟らかくなり易い。一方、成形体の耐熱性を向上させる観点から、硬化剤は、好ましくは加熱硬化型の硬化剤、より好ましくはフェノール樹脂、さらに好ましくはフェノールノボラック樹脂であってよい。特に硬化剤としてフェノールノボラック樹脂を用いることで、ガラス転移点が高いエポキシ樹脂の硬化物が得られ易い。その結果、成形体の耐熱性及び機械的強度が向上し易い。
When a curing agent that cures the epoxy resin in the range of low temperature to room temperature is used, the glass transition point of the cured product of the epoxy resin is low, and the cured product of the epoxy resin tends to be soft. As a result, the molded product formed from the compound also tends to be soft. On the other hand, from the viewpoint of improving the heat resistance of the molded product, the curing agent may be preferably a heat-curing type curing agent, more preferably a phenol resin, and further preferably a phenol novolac resin. In particular, by using a phenol novolac resin as a curing agent, it is easy to obtain a cured product of an epoxy resin having a high glass transition point. As a result, the heat resistance and mechanical strength of the molded product are likely to be improved.
フェノール樹脂は、例えば、アラルキル型フェノール樹脂、ジシクロペンタジエン型フェノール樹脂、サリチルアルデヒド型フェノール樹脂、ノボラック型フェノール樹脂、ベンズアルデヒド型フェノールとアラルキル型フェノールとの共重合型フェノール樹脂、パラキシリレン及び／又はメタキシリレン変性フェノール樹脂、メラミン変性フェノール樹脂、テルペン変性フェノール樹脂、ジシクロペンタジエン型ナフトール樹脂、シクロペンタジエン変性フェノール樹脂、多環芳香環変性フェノール樹脂、ビフェニル型フェノール樹脂、及びトリフェニルメタン型フェノール樹脂からなる群より選ばれる少なくとも一種であってよい。フェノール樹脂は、上記のうちの２種以上から構成される共重合体であってもよい。フェノール樹脂の市販品としては、例えば、荒川化学工業株式会社製のタマノル７５８、又は日立化成株式会社製のＨＰ‐８５０Ｎ等を用いてもよい。
The phenol resin is, for example, an aralkyl type phenol resin, a dicyclopentadiene type phenol resin, a salicylaldehyde type phenol resin, a novolac type phenol resin, a copolymerized phenol resin of a benzaldehyde type phenol and an aralkyl type phenol, a paraxylylene and / or a metaxylylene modification. From the group consisting of phenol resin, melamine-modified phenol resin, terpen-modified phenol resin, dicyclopentadiene-type naphthol resin, cyclopentadiene-modified phenol resin, polycyclic aromatic ring-modified phenol resin, biphenyl-type phenol resin, and triphenylmethane-type phenol resin. It may be at least one of the choices. The phenol resin may be a copolymer composed of two or more of the above. As a commercially available phenol resin, for example, Tamanol 758 manufactured by Arakawa Chemical Industry Co., Ltd., HP-850N manufactured by Hitachi Kasei Co., Ltd., or the like may be used.
フェノールノボラック樹脂は、例えば、フェノール類及び／又はナフトール類と、アルデヒド類と、を酸性触媒下で縮合又は共縮合させて得られる樹脂であってよい。フェノールノボラック樹脂を構成するフェノール類は、例えば、フェノール、クレゾール、キシレノール、レゾルシン、カテコール、ビスフェノールＡ、ビスフェノールＦ、フェニルフェノール及びアミノフェノールからなる群より選ばれる少なくとも一種であってよい。フェノールノボラック樹脂を構成するナフトール類は、例えば、α‐ナフトール、β‐ナフトール及びジヒドロキシナフタレンからなる群より選ばれる少なくとも一種であってよい。フェノールノボラック樹脂を構成するアルデヒド類は、例えば、ホルムアルデヒド、アセトアルデヒド、プロピオンアルデヒド、ベンズアルデヒド及びサリチルアルデヒドからなる群より選ばれる少なくとも一種であってよい。フェノールノボラック樹脂の市販品としては、例えば、明和化成株式会社製のＨＦ－３Ｍ、ＭＥＷ－１８００等が挙げられる。
The phenol novolac resin may be, for example, a resin obtained by condensing or co-condensing phenols and / or naphthols and aldehydes under an acidic catalyst. The phenols constituting the phenol novolac resin may be at least one selected from the group consisting of, for example, phenol, cresol, xylenol, resorcin, catechol, bisphenol A, bisphenol F, phenylphenol and aminophenol. The naphthols constituting the phenol novolac resin may be at least one selected from the group consisting of, for example, α-naphthol, β-naphthol and dihydroxynaphthalene. The aldehydes constituting the phenol novolac resin may be at least one selected from the group consisting of, for example, formaldehyde, acetaldehyde, propionaldehyde, benzaldehyde and salicylaldehyde. Examples of commercially available phenol novolac resins include HF-3M and MEW-1800 manufactured by Meiwa Kasei Co., Ltd.
硬化剤は、例えば、１分子中に２個のフェノール性水酸基を有する化合物であってもよい。１分子中に２個のフェノール性水酸基を有する化合物は、例えば、レゾルシン、カテコール、ビスフェノールＡ、ビスフェノールＦ、及び置換又は非置換のビフェノールからなる群より選ばれる少なくとも一種であってよい。
The curing agent may be, for example, a compound having two phenolic hydroxyl groups in one molecule. The compound having two phenolic hydroxyl groups in one molecule may be at least one selected from the group consisting of, for example, resorcin, catechol, bisphenol A, bisphenol F, and substituted or unsubstituted biphenol.
樹脂組成物は、上記のうち一種のフェノール樹脂を含有してよい。樹脂組成物は、上記のうち複数種のフェノール樹脂を備えてもよい。樹脂組成物は、上記のうち一種の硬化剤を含有してよい。樹脂組成物は、上記のうち複数種の硬化剤を含有してもよい。
The resin composition may contain one of the above phenol resins. The resin composition may include a plurality of types of phenol resins among the above. The resin composition may contain one of the above curing agents. The resin composition may contain a plurality of types of curing agents among the above.
エポキシ樹脂中のエポキシ基と反応する硬化剤中の活性基（フェノール性ＯＨ基）の比率は、エポキシ樹脂中のエポキシ基１当量に対して、好ましくは０．５～１．５当量、より好ましくは０．６～１．４当量、さらに好ましくは０．８～１．２当量であってよい。硬化剤中の活性基の比率が０．５当量未満である場合、得られる硬化物の充分な弾性率が得られ難い。一方、硬化剤中の活性基の比率が１．５当量を超える場合、コンパウンドから形成された成形体の硬化後の機械的強度が低下する傾向がある。ただし、硬化剤中の活性基の比率が上記範囲外である場合であっても、本発明に係る効果は得られる。
The ratio of the active group (phenolic OH group) in the curing agent that reacts with the epoxy group in the epoxy resin is preferably 0.5 to 1.5 equivalents, more preferably 0.5 to 1.5 equivalents with respect to 1 equivalent of the epoxy group in the epoxy resin. May be 0.6 to 1.4 equivalents, more preferably 0.8 to 1.2 equivalents. When the ratio of active groups in the curing agent is less than 0.5 equivalent, it is difficult to obtain a sufficient elastic modulus of the obtained cured product. On the other hand, when the ratio of active groups in the curing agent exceeds 1.5 equivalents, the mechanical strength of the molded product formed from the compound after curing tends to decrease. However, even when the ratio of active groups in the curing agent is out of the above range, the effect according to the present invention can be obtained.
硬化促進剤（触媒）は、例えば、エポキシ樹脂と反応してエポキシ樹脂の硬化を促進させる組成物であれば限定されない。硬化促進剤は、例えば、アルキル基置換イミダゾール、又はベンゾイミダゾール等のイミダゾール類であってよい。樹脂組成物は、一種の硬化促進剤を備えてよい。樹脂組成物は、複数種の硬化促進剤を備えてもよい。樹脂組成物が硬化促進剤を含有することにより、コンパウンドの成形性及び離型性が向上し易い。また、樹脂組成物が硬化促進剤を含有することにより、コンパウンドを用いて製造された成形体（例えば、電子部品）の機械的強度が向上したり、高温・高湿な環境下におけるコンパウンドの保存安定性が向上したりする。イミダゾール系硬化促進剤の市販品としては、例えば、２ＭＺ‐Ｈ、Ｃ１１Ｚ、Ｃ１７Ｚ、１，２ＤＭＺ、２Ｅ４ＭＺ、２ＰＺ‐ＰＷ、２Ｐ４ＭＺ、１Ｂ２ＭＺ、１Ｂ２ＰＺ、２ＭＺ‐ＣＮ、Ｃ１１Ｚ‐ＣＮ、２Ｅ４ＭＺ‐ＣＮ、２ＰＺ‐ＣＮ、Ｃ１１Ｚ‐ＣＮＳ、２Ｐ４ＭＨＺ、ＴＰＺ、及びＳＦＺ（以上、四国化成工業株式会社製の商品名）からなる群より選ばれる少なくとも一種を用いてよい。硬化促進剤（触媒）として、例えば、ウレア系触媒を用いてもよい。ウレア系触媒の市販品としては、例えば、サンアプロ株式会社製のＵ－ＣＡＴ３５１２Ｔが挙げられる。
The curing accelerator (catalyst) is not limited as long as it is a composition that reacts with the epoxy resin to accelerate the curing of the epoxy resin. The curing accelerator may be, for example, an alkyl group-substituted imidazole or an imidazole such as benzimidazole. The resin composition may include a kind of curing accelerator. The resin composition may include a plurality of types of curing accelerators. When the resin composition contains a curing accelerator, the moldability and releasability of the compound are likely to be improved. Further, when the resin composition contains a curing accelerator, the mechanical strength of the molded product (for example, an electronic component) manufactured by using the compound is improved, and the compound is stored in a high temperature and high humidity environment. Stability is improved. Commercially available imidazole-based curing accelerators include, for example, 2MZ-H, C11Z, C17Z, 1,2DMZ, 2E4MZ, 2PZ-PW, 2P4MZ, 1B2MZ, 1B2PZ, 2MZ-CN, C11Z-CN, 2E4MZ-CN, 2PZ. -At least one selected from the group consisting of CN, C11Z-CNS, 2P4MHZ, TPZ, and SFZ (above, trade name manufactured by Shikoku Chemicals Corporation) may be used. As the curing accelerator (catalyst), for example, a urea-based catalyst may be used. Examples of commercially available urea-based catalysts include U-CAT3512T manufactured by Sun Appro Co., Ltd.
硬化促進剤の配合量は、硬化促進効果が得られる量であればよく、特に限定されない。ただし、樹脂組成物の吸湿時の硬化性及び流動性を改善する観点からは、硬化促進剤の配合量は、１００質量部のエポキシ樹脂に対して、好ましくは０．１質量部以上３０質量部以下、より好ましくは１質量部以上１５質量部以下であってよい。硬化促進剤の含有量は、エポキシ樹脂及び硬化剤（例えばフェノール樹脂）の質量の合計１００質量部に対して０．００１質量部以上５質量部以下であることが好ましい。硬化促進剤の配合量が０．１質量部未満である場合、十分な硬化促進効果が得られ難い。硬化促進剤の配合量が３０質量部を超える場合、コンパウンドの保存安定性が低下し易い。ただし、硬化促進剤の配合量及び含有量が上記範囲外である場合であっても、本発明に係る効果は得られる。
The amount of the curing accelerator to be blended is not particularly limited as long as it can obtain the curing promoting effect. However, from the viewpoint of improving the curability and fluidity of the resin composition during moisture absorption, the amount of the curing accelerator blended is preferably 0.1 part by mass or more and 30 parts by mass with respect to 100 parts by mass of the epoxy resin. Hereinafter, it may be more preferably 1 part by mass or more and 15 parts by mass or less. The content of the curing accelerator is preferably 0.001 part by mass or more and 5 parts by mass or less with respect to 100 parts by mass in total of the mass of the epoxy resin and the curing agent (for example, phenol resin). When the blending amount of the curing accelerator is less than 0.1 parts by mass, it is difficult to obtain a sufficient curing promoting effect. When the blending amount of the curing accelerator exceeds 30 parts by mass, the storage stability of the compound tends to decrease. However, even when the blending amount and content of the curing accelerator are out of the above range, the effect according to the present invention can be obtained.
樹脂組成物は、シロキサン結合を有する化合物（シロキサン化合物）を含有する。シロキサン結合は、２つのケイ素原子（Ｓｉ）と１つの酸素原子（Ｏ）とを含む結合であり、－Ｓｉ－Ｏ－Ｓｉ－で表されてよい。シロキサン結合を有する化合物はポリシロキサン化合物であってよい。樹脂組成物は、一種のシロキサン化合物を含有してよく、複数種のシロキサン化合物を含有してもよい。コンパウンドの成形収縮率が低減され易く、また成形体の耐熱性及び耐電圧性が向上し易い観点から、樹脂組成物は、シロキサン化合物として、後述される第１シロキサン化合物を含有することが好ましい。樹脂組成物は、シロキサン化合物として、第１シロキサン化合物のみを含有してもよく、さらに第２シロキサン化合物を含有してもよい。樹脂組成物は、第１シロキサン化合物及び第２シロキサン化合物の両方を含有してもよい。樹脂組成物は、第１シロキサン化合物及び第２シロキサン化合物以外のシロキサン化合物を含有してもよい。以下では、第１シロキサン化合物及び第２シロキサン化合物の詳細を説明する。
The resin composition contains a compound having a siloxane bond (siloxane compound). The siloxane bond is a bond containing two silicon atoms (Si) and one oxygen atom (O), and may be represented by —Si—O—Si—. The compound having a siloxane bond may be a polysiloxane compound. The resin composition may contain one kind of siloxane compound, and may contain a plurality of kinds of siloxane compounds. From the viewpoint that the molding shrinkage of the compound is easily reduced and the heat resistance and withstand voltage of the molded product are easily improved, the resin composition preferably contains the first siloxane compound described later as the siloxane compound. The resin composition may contain only the first siloxane compound as the siloxane compound, or may further contain the second siloxane compound. The resin composition may contain both the first siloxane compound and the second siloxane compound. The resin composition may contain a siloxane compound other than the first siloxane compound and the second siloxane compound. The details of the first siloxane compound and the second siloxane compound will be described below.
第１シロキサン化合物は、下記化学式（１）で表される構造単位を有してよい。構造単位を単に「構造」ということができる。下記化学式（１）で表される構造単位は、「構造単位１」と表記される場合がある。
The first siloxane compound may have a structural unit represented by the following chemical formula (1). A structural unit can simply be called a "structure". The structural unit represented by the following chemical formula (1) may be expressed as "structural unit 1".
上記化学式（１）中、ｎは２～２００の整数であり、Ｒ１及びＲ２其々は独立に、炭素数１～１０のアルキル基、炭素数６～１０のアリール基、炭素数１～１０のアルコキシ基、エポキシ基を有する１価の有機基、カルボキシ基を有する１価の有機基、又は炭素数３～５００のポリアルキレンエーテル基である。
In the above chemical formula (1), n is an integer of 2 to 200, and R 1 and R 2 are independently alkyl groups having 1 to 10 carbon atoms, aryl groups having 6 to 10 carbon atoms, and 1 to 1 carbon atoms. It is a monovalent organic group having 10 alkoxy groups, an epoxy group, a monovalent organic group having a carboxy group, or a polyalkylene ether group having 3 to 500 carbon atoms.
第１シロキサン化合物中に存在する複数のＲ１は、互いに同じであっても異なってもよい。第１シロキサン化合物中に存在する複数のＲ２は、互いに同じであっても異なってもよい。Ｒ１及びＲ２は、互いに同じであっても異なってもよい。第１シロキサン化合物は、上記化学式（１）で表される繰り返し単位を有してもよい。
A plurality of R 1 present in the first siloxane compound may be the same or different from each other. Plural R 2 present in the first siloxane compound may be the same or different from each other. R 1 and R 2 may be the same or different from each other. The first siloxane compound may have a repeating unit represented by the above chemical formula (1).
コンパウンドの成形収縮率が低減され易く、また成形体の耐熱性及び耐電圧性が向上し易い観点から、第１シロキサン化合物は、下記化学式（２）で表される構造単位をさらに有することが好ましい。下記化学式（２）で表される構造単位は、「構造単位２」と表記される場合がある。
From the viewpoint that the molding shrinkage of the compound is easily reduced and the heat resistance and withstand voltage of the molded product are easily improved, the first siloxane compound preferably further has a structural unit represented by the following chemical formula (2). .. The structural unit represented by the following chemical formula (2) may be expressed as "structural unit 2".
上記化学式（２）中、Ｒ３は、炭素数１～１０のアルキレン基である。
In the above chemical formula (2), R 3 is an alkylene group having 1 to 10 carbon atoms.
第１シロキサン化合物は、複数の構造単位２を有してよい。第１シロキサン化合物中に存在する複数のＲ３は、互いに同じであっても異なってもよい。第１シロキサン化合物は、上記化学式（２）で表される繰り返し単位を有してもよい。
The first siloxane compound may have a plurality of structural units 2. Plural R 3 present in the first siloxane compound may be the same or different from each other. The first siloxane compound may have a repeating unit represented by the above chemical formula (2).
コンパウンドの成形収縮率が低減され易く、また成形体の耐熱性及び耐電圧性が向上し易い観点から、第１シロキサン化合物は、下記化学式（３）で表される化合物であることが好ましい。下記化学式（３）で表される化合物は、「化合物３」と表記される場合がある。
From the viewpoint that the molding shrinkage rate of the compound is easily reduced and the heat resistance and withstand voltage resistance of the molded product are easily improved, the first siloxane compound is preferably a compound represented by the following chemical formula (3). The compound represented by the following chemical formula (3) may be referred to as "Compound 3".
上記化学式（３）中、ｎは、２～２００の整数である。ｍ１及びｍ２其々は独立に、１～２００の整数である。Ｒ４、Ｒ５、Ｒ６及びＲ７其々は独立に、炭素数１～１０のアルキル基、炭素数６～１０のアリール基、炭素数１～１０のアルコキシ基、エポキシ基を有する１価の有機基、カルボキシ基を有する１価の有機基、又は炭素数３～５００のポリアルキレンエーテル基である。Ｒ８及びＲ９其々は独立に、炭素数１～１０のアルキレン基である。Ｒ１０及びＲ１１其々は独立に、エーテル構造を含んでいてもよい炭素数１～１０の２価の炭化水素基である。Ｒ１０及びＲ１１其々は独立に、酸素原子を含んでいてもよい、或いは酸素原子を介して結合されていてもよい炭素数１～１０の２価の炭化水素基であるということもできる。
In the above chemical formula (3), n is an integer of 2 to 200. Each of m 1 and m 2 is an integer from 1 to 200 independently. R 4 , R 5 , R 6 and R 7 each independently have an alkyl group having 1 to 10 carbon atoms, an aryl group having 6 to 10 carbon atoms, an alkoxy group having 1 to 10 carbon atoms, and an epoxy group. , A monovalent organic group having a carboxy group, or a polyalkylene ether group having 3 to 500 carbon atoms. Each of R 8 and R 9 is an alkylene group having 1 to 10 carbon atoms independently. Each of R 10 and R 11 is a divalent hydrocarbon group having 1 to 10 carbon atoms which may contain an ether structure independently. It can also be said that each of R 10 and R 11 is a divalent hydrocarbon group having 1 to 10 carbon atoms, which may independently contain an oxygen atom or may be bonded via an oxygen atom. ..
化合物３中に存在する複数のＲ４は、互いに同じであっても異なってもよい。化合物３中に存在する複数のＲ５は、互いに同じであっても異なってもよい。Ｒ４、Ｒ５、Ｒ６及びＲ７は、互いに同じであっても異なってもよい。化合物３中に存在する複数のＲ８は、互いに同じであっても異なってもよい。化合物３中に存在する複数のＲ９は、互いに同じであっても異なってもよい。Ｒ８及びＲ９は、互いに同じであっても異なってもよい。化合物３の重量平均分子量（Ｍｗ）は、例えば、４０００以上２００００以下であってよい。
Plural R 4 present in compound 3 may be the same or different from each other. A plurality of R 5 present in the compound 3 may be the same or different from each other. R 4 , R 5 , R 6 and R 7 may be the same or different from each other. A plurality of R 8 present in compound 3 may be the same or different from each other. A plurality of R 9 present in compound 3 may be the same or different from each other. R 8 and R 9 may be the same or different from each other. The weight average molecular weight (Mw) of Compound 3 may be, for example, 4000 or more and 20000 or less.
化合物３の市販品は、例えば、Ｇｅｌｅｓｔ株式会社製のＤＢＬ‐Ｃ３１、ＤＢＬ‐Ｃ３２等であってよい。
Commercially available products of Compound 3 may be, for example, DBL-C31, DBL-C32, etc. manufactured by Gelest Co., Ltd.
コンパウンドの成形収縮率が低減され易く、また成形体の耐熱性及び耐電圧性が向上し易い観点から、第２シロキサン化合物は、下記化学式（４）で表される構造単位、及び下記化学式（５）で表される構造単位を有することが好ましい。下記化学式（４）で表される構造単位は、「構造単位４」と表記される場合がある。下記化学式（５）で表される構造単位は、「構造単位５」と表記される場合がある。
From the viewpoint that the molding shrinkage of the compound is easily reduced and the heat resistance and withstand voltage of the molded product are easily improved, the second siloxane compound has a structural unit represented by the following chemical formula (4) and the following chemical formula (5). It is preferable to have a structural unit represented by). The structural unit represented by the following chemical formula (4) may be expressed as "structural unit 4". The structural unit represented by the following chemical formula (5) may be expressed as "structural unit 5".
上記化学式（４）中、Ｒ１２は、炭素数１～１２の１価の炭化水素基である。Ｒ１７は炭素数１以上の有機基である。
In the above chemical formula (4), R 12 is a monovalent hydrocarbon group having 1 to 12 carbon atoms. R 17 is an organic group having 1 or more carbon atoms.
Ｒ１２は、例えば、メチル基、エチル基、プロピル基、ブチル基、イソプロピル基、イソブチル基、ｔ－ブチル基、ペンチル基、ヘキシル基、ヘプチル基、オクチル基、２－エチルヘキシル基等のアルキル基；ビニル基、アリル基、ブテニル基、ペンテニル基、ヘキセニル基等のアルケニル基；フェニル基、トリル基、キシリル基、ナフチル基、ビフェニル基等のアリール基；ベンジル基、フェネチル基等のアラルキル基等であってよい。Ｒ１２は、メチル基又はフェニル基であることが好ましい。
R 12 is, for example, an alkyl group such as a methyl group, an ethyl group, a propyl group, a butyl group, an isopropyl group, an isobutyl group, a t-butyl group, a pentyl group, a hexyl group, a heptyl group, an octyl group and a 2-ethylhexyl group; Alkenyl groups such as vinyl group, allyl group, butenyl group, pentenyl group and hexenyl group; aryl groups such as phenyl group, trill group, xsilyl group, naphthyl group and biphenyl group; aralkyl groups such as benzyl group and phenethyl group. It's okay. R 12 is preferably a methyl group or a phenyl group.
第２シロキサン化合物は、複数の構造単位４を有してよい。第２シロキサン化合物中に存在する複数のＲ１２は、互いに同じであっても異なってもよい。第２シロキサン化合物は、上記化学式（４）で表される繰り返し単位を有してもよい。
The second siloxane compound may have a plurality of structural units 4. The plurality of R 12s present in the second siloxane compound may be the same as or different from each other. The second siloxane compound may have a repeating unit represented by the above chemical formula (4).
上記化学式（５）中、Ｒ１３及びＲ１４其々は独立に、炭素数１～１２の１価の炭化水素基である。
In the above chemical formula (5), R 13 and R 14 are independently monovalent hydrocarbon groups having 1 to 12 carbon atoms.
Ｒ１３は、例えば、メチル基、エチル基、プロピル基、ブチル基、イソプロピル基、イソブチル基、ｔ－ブチル基、ペンチル基、ヘキシル基、ヘプチル基、オクチル基、２－エチルヘキシル基等のアルキル基；ビニル基、アリル基、ブテニル基、ペンテニル基、ヘキセニル基等のアルケニル基；フェニル基、トリル基、キシリル基、ナフチル基、ビフェニル基等のアリール基；ベンジル基、フェネチル基等のアラルキル基等であってよい。Ｒ１３は、メチル基又はフェニル基であることが好ましい。
R 13 is, for example, an alkyl group such as a methyl group, an ethyl group, a propyl group, a butyl group, an isopropyl group, an isobutyl group, a t-butyl group, a pentyl group, a hexyl group, a heptyl group, an octyl group and a 2-ethylhexyl group; Alkenyl groups such as vinyl group, allyl group, butenyl group, pentenyl group and hexenyl group; aryl groups such as phenyl group, trill group, xsilyl group, naphthyl group and biphenyl group; aralkyl groups such as benzyl group and phenethyl group. It's okay. R 13 is preferably a methyl group or a phenyl group.
Ｒ１４は、例えば、メチル基、エチル基、プロピル基、ブチル基、イソプロピル基、イソブチル基、ｔ－ブチル基、ペンチル基、ヘキシル基、ヘプチル基、オクチル基、２－エチルヘキシル基等のアルキル基；ビニル基、アリル基、ブテニル基、ペンテニル基、ヘキセニル基等のアルケニル基；フェニル基、トリル基、キシリル基、ナフチル基、ビフェニル基等のアリール基；ベンジル基、フェネチル基等のアラルキル基等であってよい。Ｒ１４は、メチル基又はフェニル基であることが好ましい。
R 14 is, for example, an alkyl group such as a methyl group, an ethyl group, a propyl group, a butyl group, an isopropyl group, an isobutyl group, a t-butyl group, a pentyl group, a hexyl group, a heptyl group, an octyl group and a 2-ethylhexyl group; Alkenyl groups such as vinyl group, allyl group, butenyl group, pentenyl group and hexenyl group; aryl groups such as phenyl group, trill group, xsilyl group, naphthyl group and biphenyl group; aralkyl groups such as benzyl group and phenethyl group. It's okay. R 14 is preferably a methyl group or a phenyl group.
第２シロキサン化合物は、複数の構造単位５を有してよい。第２シロキサン化合物中に存在する複数のＲ１３は、互いに同じであっても異なってもよい。第２シロキサン化合物中に存在する複数のＲ１４は、互いに同じであっても異なってもよい。Ｒ１３及びＲ１４は、互いに同じであっても異なってもよい。第２シロキサン化合物は、上記化学式（５）で表される繰り返し単位を有してもよい。
The second siloxane compound may have a plurality of structural units 5. The plurality of R 13s present in the second siloxane compound may be the same as or different from each other. The plurality of R 14s present in the second siloxane compound may be the same as or different from each other. R 13 and R 14 may be the same or different from each other. The second siloxane compound may have a repeating unit represented by the above chemical formula (5).
第２シロキサン化合物の保存安定性の観点から、第２シロキサン化合物の分子の末端は、Ｒ１２、Ｒ１３、Ｒ１４、水酸基及びアルコキシ基のうちのいずれか一つの基であることが好ましい。アルコキシ基は、例えば、メトキシ基、エトキシ基、プロプキシ基、又はブトキシ基であってよい。
From the viewpoint of storage stability of the second siloxane compound, the terminal of the molecule of the second siloxane compound is preferably any one of R 12 , R 13 , R 14 , hydroxyl group and alkoxy group. The alkoxy group may be, for example, a methoxy group, an ethoxy group, a propoxy group, or a butoxy group.
コンパウンドの成形収縮率が低減され易く、また成形体の耐熱性及び耐電圧性が向上し易い観点から、第２シロキサン化合物は、下記化学式（６）で表される構造単位を有することが好ましい。下記化学式（６）で表される構造単位は、「構造単位６」と表記される場合がある。
From the viewpoint that the molding shrinkage of the compound is easily reduced and the heat resistance and withstand voltage of the molded product are easily improved, the second siloxane compound preferably has a structural unit represented by the following chemical formula (6). The structural unit represented by the following chemical formula (6) may be expressed as "structural unit 6".
上記化学式（６）中、Ｒ１５は、炭素数１～１２の１価の炭化水素基である。Ｒ１６は、エポキシ基を有する１価の有機基である。
In the above chemical formula (6), R 15 is a monovalent hydrocarbon group having 1 to 12 carbon atoms. R 16 is a monovalent organic group having an epoxy group.
Ｒ１５は、例えば、メチル基、エチル基、プロピル基、ブチル基、イソプロピル基、イソブチル基、ｔ－ブチル基、ペンチル基、ヘキシル基、ヘプチル基、オクチル基、２－エチルヘキシル基等のアルキル基；ビニル基、アリル基、ブテニル基、ペンテニル基、ヘキセニル基等のアルケニル基；フェニル基、トリル基、キシリル基、ナフチル基、ビフェニル基等のアリール基；ベンジル基、フェネチル基等のアラルキル基等であってよい。Ｒ１３は、メチル基又はフェニル基であることが好ましい。
R 15 is, for example, a methyl group, an ethyl group, a propyl group, a butyl group, an isopropyl group, an isobutyl group, t- butyl group, a pentyl group, a hexyl group, heptyl group, and an octyl group, a 2-ethylhexyl group; Alkenyl groups such as vinyl group, allyl group, butenyl group, pentenyl group and hexenyl group; aryl groups such as phenyl group, trill group, xsilyl group, naphthyl group and biphenyl group; aralkyl groups such as benzyl group and phenethyl group. It's okay. R 13 is preferably a methyl group or a phenyl group.
Ｒ１６は、例えば、２，３－エポキシプロピル基、３，４－エポキシブチル基、４，５－エポキシペンチル基、２－グリシドキシエチル基、３－グリシドキシプロピル基、４－グリシドキシブチル基、２－（３，４－エポキシシクロヘキシル）エチル基、３－（３，４－エポキシシクロヘキシル）プロピル基等であってよい。Ｒ１６は、３－グリシドキシプロピル基であることが好ましい。
R 16 is, for example, 2,3-epoxypropyl group, 3,4-epoxybutyl group, 4,5-epoxypentyl group, 2-glycidoxyethyl group, 3-glycidoxypropyl group, 4-glycid. It may be a xybutyl group, a 2- (3,4-epoxycyclohexyl) ethyl group, a 3- (3,4-epoxycyclohexyl) propyl group, or the like. R 16 is preferably a 3-glycidoxypropyl group.
第２シロキサン化合物は、複数の構造単位６を有してよい。第２シロキサン化合物中に存在する複数のＲ１５は、互いに同じであっても異なってもよい。第２シロキサン化合物中に存在する複数のＲ１６は、互いに同じであっても異なってもよい。第２シロキサン化合物は、上記化学式（６）で表される繰り返し単位を有してもよい。
The second siloxane compound may have a plurality of structural units 6. A plurality of R 15 present in the second siloxane compound may be the same or different from each other. The plurality of R 16s present in the second siloxane compound may be the same as or different from each other. The second siloxane compound may have a repeating unit represented by the above chemical formula (6).
コンパウンドの成形収縮率が低減され易く、また成形体の耐熱性及び耐電圧性が向上し易い観点から、第２シロキサン化合物は、下記化学式（７）で表される構造単位、下記化学式（８）で表される構造単位、下記化学式（９）で表される構造単位、及び下記化学式（１０）で表される構造単位からなる群より選ばれる少なくとも一つの構造単位を有する化合物であることが好ましい。下記化学式（７）で表される構造単位は、「構造単位７」と表記される場合がある。下記化学式（８）で表される構造単位は、「構造単位８」と表記される場合がある。下記化学式（９）で表される構造単位は、「構造単位９」と表記される場合がある。下記化学式（１０）で表される構造単位は、「構造単位１０」と表記される場合がある。上記の構造単位７、構造単位８、構造単位９、及び構造単位１０からなる群より選ばれる少なくとも一つの構造単位を有する化合物は、「化合物１１」と表記される場合がある。化合物１１は、構造単位７、構造単位８、構造単位９、及び構造単位１０の全てを有してよい。
From the viewpoint that the molding shrinkage rate of the compound is easily reduced and the heat resistance and withstand voltage resistance of the molded product are easily improved, the second siloxane compound is a structural unit represented by the following chemical formula (7) and the following chemical formula (8). It is preferable that the compound has at least one structural unit selected from the group consisting of the structural unit represented by, the structural unit represented by the following chemical formula (9), and the structural unit represented by the following chemical formula (10). .. The structural unit represented by the following chemical formula (7) may be expressed as "structural unit 7". The structural unit represented by the following chemical formula (8) may be expressed as "structural unit 8". The structural unit represented by the following chemical formula (9) may be expressed as "structural unit 9". The structural unit represented by the following chemical formula (10) may be expressed as "structural unit 10". A compound having at least one structural unit selected from the group consisting of the structural unit 7, the structural unit 8, the structural unit 9, and the structural unit 10 may be referred to as “compound 11”. Compound 11 may have all of structural unit 7, structural unit 8, structural unit 9, and structural unit 10.
化合物１１は、複数の構造単位７を有してよい。化合物１１は、上記化学式（７）で表される繰り返し単位を有してもよい。化合物１１は、複数の構造単位８を有してよい。化合物１１は、上記化学式（８）で表される繰り返し単位を有してもよい。化合物１１は、複数の構造単位９を有してよい。化合物１１は、上記化学式（９）で表される繰り返し単位を有してもよい。化合物１１は、複数の構造単位１０を有してよい。化合物１１は、上記化学式（１０）で表される繰り返し単位を有してもよい。
Compound 11 may have a plurality of structural units 7. Compound 11 may have a repeating unit represented by the above chemical formula (7). Compound 11 may have a plurality of structural units 8. Compound 11 may have a repeating unit represented by the above chemical formula (8). Compound 11 may have a plurality of structural units 9. Compound 11 may have a repeating unit represented by the above chemical formula (9). Compound 11 may have a plurality of structural units 10. Compound 11 may have a repeating unit represented by the above chemical formula (10).
化合物１１の市販品は、例えば、東レ・ダウコーニング株式会社製のＡＹ４２‐１１９であってよい。
The commercially available product of Compound 11 may be, for example, AY42-119 manufactured by Toray Dow Corning Co., Ltd.
第２シロキサン化合物のエポキシ当量は、５００以上４０００以下、又は１０００以上２５００以下であってよい。エポキシ当量が上記範囲内である場合、コンパウンドの流動性が向上し易く、成形性が向上し易い。
The epoxy equivalent of the second siloxane compound may be 500 or more and 4000 or less, or 1000 or more and 2500 or less. When the epoxy equivalent is within the above range, the fluidity of the compound is likely to be improved and the moldability is likely to be improved.
第２シロキサン化合物の軟化点は、４０℃以上１２０℃以下であることが好ましく、５０℃以上１００℃以下であることがより好ましい。軟化点が上記範囲内である場合、コンパウンドから形成される成形体の機械的強度が向上し易い。第２シロキサン化合物の軟化点は、第２シロキサン化合物の分子量、構造（例えば、各構成単位の含有比率）、ケイ素原子に結合する有機基の種類等により調整されてよい。コンパウンドの流動性を向上する観点から、第２シロキサン化合物中のアリール基の含有量により軟化点を調整することが好ましい。アリール基は、例えば、フェニル基、トリル基、キシリル基、ナフチル基、ビフェニル基等であってよい。アリール基は、フェニル基であることが好ましい。第２シロキサン化合物中のケイ素原子に結合する一価の有機基中のフェニル基の含有量により、軟化点を調整することがより好ましい。上記フェニル基の含有量は、好ましくは６０モル％以上１００モル％以下、より好ましくは７０モル％以上８５モル％以下に調整されてよい。
The softening point of the second siloxane compound is preferably 40 ° C. or higher and 120 ° C. or lower, and more preferably 50 ° C. or higher and 100 ° C. or lower. When the softening point is within the above range, the mechanical strength of the molded product formed from the compound is likely to be improved. The softening point of the second siloxane compound may be adjusted by the molecular weight, structure (for example, content ratio of each structural unit) of the second siloxane compound, the type of organic group bonded to the silicon atom, and the like. From the viewpoint of improving the fluidity of the compound, it is preferable to adjust the softening point by the content of the aryl group in the second siloxane compound. The aryl group may be, for example, a phenyl group, a tolyl group, a xsilyl group, a naphthyl group, a biphenyl group or the like. The aryl group is preferably a phenyl group. It is more preferable to adjust the softening point by the content of the phenyl group in the monovalent organic group bonded to the silicon atom in the second siloxane compound. The content of the phenyl group may be adjusted to preferably 60 mol% or more and 100 mol% or less, more preferably 70 mol% or more and 85 mol% or less.
第２シロキサン化合物の重量平均分子量（Ｍｗ）は、１０００以上３００００以下、好ましくは２０００以上２００００以下、より好ましくは３０００以上１００００以下であってよい。重量平均分子量（Ｍｗ）は、ゲルパーミュエーションクロマトグラフィー（ＧＰＣ）で測定されてよく、標準ポリスチレン検量線を用いて換算された値であってよい。第２シロキサン化合物は、ランダム共重合体であることが好ましい。
The weight average molecular weight (Mw) of the second siloxane compound may be 1000 or more and 30,000 or less, preferably 2000 or more and 20000 or less, and more preferably 3000 or more and 10000 or less. The weight average molecular weight (Mw) may be measured by gel permeation chromatography (GPC) and may be a value converted using a standard polystyrene calibration curve. The second siloxane compound is preferably a random copolymer.
樹脂組成物は、上記のうち一種のシロキサン化合物を含有してよく、上記のうち複数種のシロキサン化合物を含有してもよい。
The resin composition may contain one of the above siloxane compounds, and may contain a plurality of the above siloxane compounds.
カップリング剤は、樹脂組成物と、金属元素含有粉を構成する金属元素含有粒子との密着性を向上させ、コンパウンドから形成される成形体の可撓性及び機械的強度を向上させる。カップリング剤は、例えば、シラン系化合物（シランカップリング剤）、チタン系化合物、アルミニウム化合物（アルミニウムキレート類）、及びアルミニウム／ジルコニウム系化合物からなる群より選ばれる少なくとも一種であってよい。シランカップリング剤は、例えば、エポキシシラン、メルカプトシラン、アミノシラン、アルキルシラン、ウレイドシラン、酸無水物系シラン及びビニルシランからなる群より選ばれる少なくとも一種であってよい。特に、アミノフェニル系のシランカップリング剤が好ましい。樹脂組成物は、上記のうち一種のカップリング剤を含有してよく、上記のうち複数種のカップリング剤を含有してもよい。
The coupling agent improves the adhesion between the resin composition and the metal element-containing particles constituting the metal element-containing powder, and improves the flexibility and mechanical strength of the molded product formed from the compound. The coupling agent may be at least one selected from the group consisting of, for example, a silane compound (silane coupling agent), a titanium compound, an aluminum compound (aluminum chelate), and an aluminum / zirconium compound. The silane coupling agent may be at least one selected from the group consisting of, for example, epoxysilane, mercaptosilane, aminosilane, alkylsilane, ureidosilane, acid anhydride-based silane, and vinylsilane. In particular, an aminophenyl-based silane coupling agent is preferable. The resin composition may contain one of the above-mentioned coupling agents, and may contain a plurality of of the above-mentioned coupling agents.
コンパウンドの環境安全性、リサイクル性、成形加工性及び低コストのために、コンパウンドは難燃剤を含んでよい。難燃剤は、例えば、臭素系難燃剤、鱗茎難燃剤、水和金属化合物系難燃剤、シリコーン系難燃剤、窒素含有化合物、ヒンダードアミン化合物、有機金属化合物及び芳香族エンプラからなる群より選ばれる少なくとも一種であってよい。樹脂組成物は、上記のうち一種の難燃剤を含有してよく、上記のうち複数種の難燃剤を含有してもよい。
Due to the environmental safety, recyclability, molding processability and low cost of the compound, the compound may contain a flame retardant. The flame retardant is at least one selected from the group consisting of, for example, a bromine-based flame retardant, a scale flame retardant, a hydrated metal compound-based flame retardant, a silicone-based flame retardant, a nitrogen-containing compound, a hindered amine compound, an organic metal compound, and an aromatic empra. May be. The resin composition may contain one of the above flame retardants, and may contain a plurality of the above flame retardants.
金型を用いてコンパウンドから成形体を形成する場合、樹脂組成物は、ワックスを含有してよい。ワックスは、コンパウンドの成形（例えばトランスファー成形）におけるコンパウンドの流動性を高めると共に、離型剤として機能する。ワックスは、高級脂肪酸等の脂肪酸、及び脂肪酸エステルのうち少なくともいずれか一つであってよい。
When forming a molded product from a compound using a mold, the resin composition may contain wax. The wax enhances the fluidity of the compound in the molding of the compound (for example, transfer molding) and functions as a mold release agent. The wax may be at least one of fatty acids such as higher fatty acids and fatty acid esters.
ワックスは、例えば、モンタン酸、ステアリン酸、１２－オキシステアリン酸、ラウリン酸等の脂肪酸類又はこれらのエステル；ステアリン酸亜鉛、ステアリン酸カルシウム、ステアエン酸バリウム、ステアリン酸アルミニウム、ステアリン酸マグネシウム、ラウリン酸カルシウム、リノール酸亜鉛、リシノール酸カルシウム、２－エチルヘキソイン酸亜鉛等の脂肪酸塩；ステアリン酸アミド、オレイン酸アミド、エルカ酸アミド、ベヘン酸アミド、パルミチン酸アミド、ラウリン酸アミド、ヒドロキシステアリン酸アミド、メチレンビスステアリン酸アミド、エチレンビスステアリン酸アミド、エチレンビスラウリン酸アミド、ジステアリルアジピン酸アミド、エチレンビスオレイン酸アミド、ジオレイルアジピン酸アミド、Ｎ－ステアリルステアリン酸アミド、Ｎ－オレイルステアリン酸アミド、Ｎ－ステアリルエルカ酸アミド、メチロールステアリン酸アミド、メチロールベヘン酸アミド等の脂肪酸アミド；ステアリン酸ブチル等の脂肪酸エステル；エチレングリコール、ステアリルアルコール等のアルコール類；ポリエチレングリコール、ポリプロピレングリコール、ポリテトラメチレングリコール及びこれらの変性物からなるポリエーテル類；シリコーンオイル、シリコーングリース等のシリコーン化合物；フッ素系オイル、フッ素系グリース、含フッ素樹脂粉末等のフッ素化合物；並びに、パラフィンワックス、ポリエチレンワックス、アマイドワックス、ポリプロピレンワックス、エステルワックス、カルナウバ、マイクロワックス等のワックス類；からなる群より選ばれる少なくとも一種であってよい。例えば、モンタン酸エステルの市販品としては、クラリアントケミカルズ株式会社製のＬＩＣＯＷＡＸ－ＯＰが挙げられる。例えば、天然ワックスの市販品としては、株式会社セラリカＮＯＤＡ製のカルナバワックスＮｏ．１が挙げられる。
The wax is, for example, fatty acids such as montanic acid, stearic acid, 12-oxystearic acid, laurate or esters thereof; zinc stearate, calcium stearate, barium steaenoate, aluminum stearate, magnesium stearate, calcium laurate, Fatty acid salts such as zinc linoleate, calcium ricinolate, zinc 2-ethylhexoneate; stearic acid amide, oleic acid amide, erucate amide, bechenic acid amide, palmitate amide, laurate amide, hydroxystearic acid amide, methylene bisstearate Acid amide, ethylene bisstearic acid amide, ethylene bislauric acid amide, distearyl adipate amide, ethylene bisoleic acid amide, diorail adipic acid amide, N-stearyl stearic acid amide, N-oleyl stearic acid amide, N-stearyl Fatty acid amides such as erucate amide, methylol stearic acid amide, methylol bechenic acid amide; fatty acid esters such as butyl stearate; alcohols such as ethylene glycol and stearyl alcohol; polyethylene glycol, polypropylene glycol, polytetramethylene glycol and modifications thereof. Polyethers made of materials; Silicone compounds such as silicone oil and silicone grease; Fluorine compounds such as fluorine oil, fluorine grease, and fluorine-containing resin powder; and paraffin wax, polyethylene wax, amide wax, polypropylene wax, and ester wax. , Carnauba, waxes such as microwax; at least one selected from the group consisting of. For example, as a commercially available product of montanic acid ester, LICOWAX-OP manufactured by Clariant Chemicals Co., Ltd. can be mentioned. For example, as a commercial product of natural wax, Carnauba Wax No. 1 manufactured by Ceralica NODA Co., Ltd. 1 is mentioned.
その他、離型剤としては、例えば、モンタン酸、ステアリン酸、１２－オキシステアリン酸、ラウリン酸等の長鎖脂肪酸と金属との結合で構成される金属石鹸が挙げられる。金属石鹸の市販品としては、例えば、日油株式会社製のパウダーベースＬ等が挙げられる。
Other examples of the release agent include metal soap composed of a bond between a metal and a long-chain fatty acid such as montanic acid, stearic acid, 12-oxystearic acid, and lauric acid. Examples of commercially available metal soaps include powder base L manufactured by NOF CORPORATION.
（金属元素含有粉）
金属元素含有粉（金属元素含有粒子）は、例えば、金属単体、合金及び金属化合物からなる群より選ばれる少なくとも一種を含有してよい。金属元素含有粉は、例えば、金属単体、合金及び金属化合物からなる群より選ばれる少なくとも一種からなっていてよい。合金は、固溶体、共晶及び金属間化合物からなる群より選ばれる少なくとも一種を含んでよい。合金とは、例えば、ステンレス鋼（Ｆｅ‐Ｃｒ系合金、Ｆｅ‐Ｎｉ‐Ｃｒ系合金等）であってよい。金属化合物とは、例えば、フェライト等の酸化物であってよい。金属元素含有粉は、一種の金属元素又は複数種の金属元素を含んでよい。金属元素含有粉に含まれる金属元素は、例えば、卑金属元素、貴金属元素、遷移金属元素、又は希土類元素であってよい。コンパウンドは、一種の金属元素含有粉を含んでよく、組成が異なる複数種の金属元素含有粉を含んでもよい。 (Metal element-containing powder)
The metal element-containing powder (metal element-containing particles) may contain, for example, at least one selected from the group consisting of elemental metals, alloys and metal compounds. The metal element-containing powder may consist of, for example, at least one selected from the group consisting of elemental metals, alloys and metal compounds. The alloy may include at least one selected from the group consisting of solid solutions, eutectic and intermetallic compounds. The alloy may be, for example, stainless steel (Fe—Cr based alloy, Fe—Ni—Cr based alloy, etc.). The metal compound may be, for example, an oxide such as ferrite. The metal element-containing powder may contain one kind of metal element or a plurality of kinds of metal elements. The metal element contained in the metal element-containing powder may be, for example, a base metal element, a noble metal element, a transition metal element, or a rare earth element. The compound may contain one kind of metal element-containing powder, and may contain a plurality of kinds of metal element-containing powders having different compositions.
金属元素含有粉（金属元素含有粒子）は、例えば、金属単体、合金及び金属化合物からなる群より選ばれる少なくとも一種を含有してよい。金属元素含有粉は、例えば、金属単体、合金及び金属化合物からなる群より選ばれる少なくとも一種からなっていてよい。合金は、固溶体、共晶及び金属間化合物からなる群より選ばれる少なくとも一種を含んでよい。合金とは、例えば、ステンレス鋼（Ｆｅ‐Ｃｒ系合金、Ｆｅ‐Ｎｉ‐Ｃｒ系合金等）であってよい。金属化合物とは、例えば、フェライト等の酸化物であってよい。金属元素含有粉は、一種の金属元素又は複数種の金属元素を含んでよい。金属元素含有粉に含まれる金属元素は、例えば、卑金属元素、貴金属元素、遷移金属元素、又は希土類元素であってよい。コンパウンドは、一種の金属元素含有粉を含んでよく、組成が異なる複数種の金属元素含有粉を含んでもよい。 (Metal element-containing powder)
The metal element-containing powder (metal element-containing particles) may contain, for example, at least one selected from the group consisting of elemental metals, alloys and metal compounds. The metal element-containing powder may consist of, for example, at least one selected from the group consisting of elemental metals, alloys and metal compounds. The alloy may include at least one selected from the group consisting of solid solutions, eutectic and intermetallic compounds. The alloy may be, for example, stainless steel (Fe—Cr based alloy, Fe—Ni—Cr based alloy, etc.). The metal compound may be, for example, an oxide such as ferrite. The metal element-containing powder may contain one kind of metal element or a plurality of kinds of metal elements. The metal element contained in the metal element-containing powder may be, for example, a base metal element, a noble metal element, a transition metal element, or a rare earth element. The compound may contain one kind of metal element-containing powder, and may contain a plurality of kinds of metal element-containing powders having different compositions.
金属元素含有粉は上記の組成物に限定されない。金属元素含有粉に含まれる金属元素は、例えば、鉄（Ｆｅ）、銅（Ｃｕ）、チタン（Ｔｉ）、マンガン（Ｍｎ）、コバルト（Ｃｏ）、ニッケル（Ｎｉ）、亜鉛（Ｚｎ）、アルミニウム（Ａｌ）、スズ（Ｓｎ）、クロム（Ｃｒ）、バリウム（Ｂａ）、ストロンチウム（Ｓｒ）、鉛（Ｐｂ）、銀（Ａｇ）、プラセオジム（Ｐｒ）、ネオジム（Ｎｄ）、サマリウム（Ｓｍ）及びジスプロシウム（Ｄｙ）からなる群より選ばれる少なくとも一種であってよい。金属元素含有粉は、金属元素以外の元素を更に含んでもよい。金属元素含有粉は、例えば、酸素（О）、ベリリウム（Ｂｅ）、リン（Ｐ）、ホウ素（Ｂ）、又はケイ素（Ｓｉ）を含んでもよい。金属元素含有粉は、磁性粉であってよい。金属元素含有粉は、軟磁性合金、又は強磁性合金であってよい。金属元素含有粉は、例えば、Ｆｅ‐Ｓｉ系合金、Ｆｅ‐Ｓｉ‐Ａｌ系合金（センダスト）、Ｆｅ‐Ｎｉ系合金（パーマロイ）、Ｆｅ‐Ｃｕ‐Ｎｉ系合金（パーマロイ）、Ｆｅ‐Ｃｏ系合金（パーメンジュール）、Ｆｅ‐Ｃｒ‐Ｓｉ系合金（電磁ステンレス鋼）、Ｎｄ‐Ｆｅ‐Ｂ系合金（希土類磁石）、Ｓｍ‐Ｆｅ‐Ｎ系合金（希土類磁石）、Ａｌ‐Ｎｉ‐Ｃｏ系合金（アルニコ磁石）及びフェライトからなる群より選ばれる少なくとも一種からなる磁性粉であってよい。フェライトは、例えば、スピネルフェライト、六方晶フェライト、又はガーネットフェライトであってよい。金属元素含有粉は、Ｃｕ‐Ｓｎ系合金、Ｃｕ‐Ｓｎ‐Ｐ系合金、Ｃｕ‐Ｎｉ系合金、又はＣｕ‐Ｂｅ系合金等の銅合金であってもよい。金属元素含有粉は、上記の元素及び組成物のうち一種を含んでよく、上記の元素及び組成物のうち複数種を含んでもよい。
The metal element-containing powder is not limited to the above composition. The metal elements contained in the metal element-containing powder include, for example, iron (Fe), copper (Cu), titanium (Ti), manganese (Mn), cobalt (Co), nickel (Ni), zinc (Zn), and aluminum (Zn). Al), tin (Sn), chromium (Cr), barium (Ba), strontium (Sr), lead (Pb), silver (Ag), praseodymium (Pr), neodymium (Nd), samarium (Sm) and dysprosium ( It may be at least one selected from the group consisting of Dy). The metal element-containing powder may further contain an element other than the metal element. The metal element-containing powder may contain, for example, oxygen (О), beryllium (Be), phosphorus (P), boron (B), or silicon (Si). The metal element-containing powder may be a magnetic powder. The metal element-containing powder may be a soft magnetic alloy or a ferromagnetic alloy. The metal element-containing powder includes, for example, Fe-Si alloy, Fe—Si—Al alloy (Sendust), Fe—Ni alloy (Permalloy), Fe—Cu—Ni alloy (Permalloy), Fe—Co alloy. (Permenzur), Fe-Cr-Si alloy (electromagnetic stainless steel), Nd-Fe-B alloy (rare earth magnet), Sm-Fe-N alloy (rare earth magnet), Al-Ni-Co alloy It may be a magnetic powder consisting of at least one selected from the group consisting of (alnico magnet) and ferrite. The ferrite may be, for example, spinel ferrite, hexagonal ferrite, or garnet ferrite. The metal element-containing powder may be a copper alloy such as a Cu—Sn-based alloy, a Cu—Sn—P-based alloy, a Cu—Ni-based alloy, or a Cu—Be-based alloy. The metal element-containing powder may contain one of the above elements and compositions, and may contain a plurality of of the above elements and compositions.
金属元素含有粉は、Ｆｅ単体であってもよい。金属元素含有粉は、鉄を含む合金（Ｆｅ系合金）であってもよい。Ｆｅ系合金は、例えば、Ｆｅ‐Ｓｉ‐Ｃｒ系合金、又はＮｄ‐Ｆｅ‐Ｂ系合金であってよい。金属元素含有粉は、アモルファス系鉄粉及びカルボニル鉄粉のうちの少なくともいずれかであってもよい。金属元素含有粉がＦｅ単体及びＦｅ系合金のうちの少なくともいずれかを含む場合、高い占積率を有し、且つ磁気特性に優れる成形体をコンパウンドから作製し易い。金属元素含有粉は、Ｆｅアモルファス合金であってもよい。Ｆｅアモルファス合金粉の市販品としては、例えば、ＡＷ２‐０８、ＫＵＡＭＥＴ‐６Ｂ２、ＫＵＡＭＥＴ ９Ａ４‐ＩＩ（以上、エプソンアトミックス株式会社製の商品名）、ＤＡＰ ＭＳ３、ＤＡＰ ＭＳ７、ＤＡＰ ＭＳＡ１０、ＤＡＰ ＰＢ、ＤＡＰ ＰＣ、ＤＡＰ ＭＫＶ４９、ＤＡＰ ４１０Ｌ、ＤＡＰ ４３０Ｌ、ＤＡＰ ＨＹＢシリーズ（以上、大同特殊鋼株式会社製の商品名）、ＭＨ４５Ｄ、ＭＨ２８Ｄ、ＭＨ２５Ｄ、及びＭＨ２０Ｄ（以上、神戸製鋼株式会社製の商品名）からなる群より選ばれる少なくとも一種が用いられてよい。
The metal element-containing powder may be Fe alone. The metal element-containing powder may be an iron-containing alloy (Fe-based alloy). The Fe-based alloy may be, for example, a Fe—Si—Cr based alloy or an Nd—Fe—B based alloy. The metal element-containing powder may be at least one of amorphous iron powder and carbonyl iron powder. When the metal element-containing powder contains at least one of Fe simple substance and Fe-based alloy, it is easy to prepare a molded product having a high space factor and excellent magnetic properties from the compound. The metal element-containing powder may be an Fe amorphous alloy. Commercially available Fe amorphous alloy powders include, for example, AW2-08, KUAMET-6B2, KUAMET 9A4-II (above, trade name manufactured by Epson Atmix Co., Ltd.), DAP MS3, DAP MS7, DAP MSA10, DAP PB, etc. From DAP PC, DAP MKV49, DAP 410L, DAP 430L, DAP HYB series (above, product name manufactured by Daido Special Steel Co., Ltd.), MH45D, MH28D, MH25D, and MH20D (above, product name manufactured by Kobe Steel Co., Ltd.) At least one selected from the group may be used.
＜コンパウンドの製造方法＞
コンパウンドの製造では、金属元素含有粉と樹脂組成物（樹脂組成物を構成する各成分）とを加熱しながら混合する。例えば、金属元素含有粉と樹脂組成物とを加熱しながらニーダー、ロール、攪拌機などで混練してよい。金属元素含有粉及び樹脂組成物の加熱及び混合により、樹脂組成物が金属元素含有粉を構成する金属元素含有粒子の表面の一部又は全体に付着して金属元素含有粒子を被覆し、樹脂組成物中のエポキシ樹脂の一部又は全部が半硬化物になる。その結果、コンパウンドが得られる。金属元素含有粉及び樹脂組成物の加熱及び混合によって得られた粉末に、さらにワックスを加えることによって、コンパウンドを得てもよい。予め樹脂組成物とワックスとが混合されていてもよい。 <Manufacturing method of compound>
In the production of the compound, the metal element-containing powder and the resin composition (each component constituting the resin composition) are mixed while being heated. For example, the metal element-containing powder and the resin composition may be kneaded with a kneader, a roll, a stirrer, or the like while being heated. By heating and mixing the metal element-containing powder and the resin composition, the resin composition adheres to a part or the whole of the surface of the metal element-containing particles constituting the metal element-containing powder to coat the metal element-containing particles, and the resin composition. Part or all of the epoxy resin in the material becomes a semi-cured product. The result is a compound. A compound may be obtained by further adding wax to the powder obtained by heating and mixing the metal element-containing powder and the resin composition. The resin composition and wax may be mixed in advance.
コンパウンドの製造では、金属元素含有粉と樹脂組成物（樹脂組成物を構成する各成分）とを加熱しながら混合する。例えば、金属元素含有粉と樹脂組成物とを加熱しながらニーダー、ロール、攪拌機などで混練してよい。金属元素含有粉及び樹脂組成物の加熱及び混合により、樹脂組成物が金属元素含有粉を構成する金属元素含有粒子の表面の一部又は全体に付着して金属元素含有粒子を被覆し、樹脂組成物中のエポキシ樹脂の一部又は全部が半硬化物になる。その結果、コンパウンドが得られる。金属元素含有粉及び樹脂組成物の加熱及び混合によって得られた粉末に、さらにワックスを加えることによって、コンパウンドを得てもよい。予め樹脂組成物とワックスとが混合されていてもよい。 <Manufacturing method of compound>
In the production of the compound, the metal element-containing powder and the resin composition (each component constituting the resin composition) are mixed while being heated. For example, the metal element-containing powder and the resin composition may be kneaded with a kneader, a roll, a stirrer, or the like while being heated. By heating and mixing the metal element-containing powder and the resin composition, the resin composition adheres to a part or the whole of the surface of the metal element-containing particles constituting the metal element-containing powder to coat the metal element-containing particles, and the resin composition. Part or all of the epoxy resin in the material becomes a semi-cured product. The result is a compound. A compound may be obtained by further adding wax to the powder obtained by heating and mixing the metal element-containing powder and the resin composition. The resin composition and wax may be mixed in advance.
混練では、金属元素含有粉、シロキサン化合物、エポキシ樹脂、フェノール樹脂等の硬化剤、硬化促進剤、及びカップリング剤を槽内で混練してよい。金属元素含有粉、シロキサン化合物及びカップリング剤を槽内に投入して混合した後、エポキシ樹脂、硬化剤、及び硬化促進剤を槽内へ投入して、槽内の原料を混練してもよい。シロキサン化合物、エポキシ樹脂、硬化剤、カップリング剤を槽内で混練した後、硬化促進剤を槽内に入れて、更に槽内の原料を混練してもよい。予めエポキシ樹脂、硬化剤、及び硬化促進剤の混合粉（樹脂混合粉）を作製して、続いて、金属元素含有粉とシロキサン化合物とカップリング剤とを混練して金属混合粉を作製して、続いて、金属混合粉と上記の樹脂混合粉とを混練してもよい。
In kneading, a curing agent such as a metal element-containing powder, a siloxane compound, an epoxy resin, or a phenol resin, a curing accelerator, and a coupling agent may be kneaded in a tank. After the metal element-containing powder, the siloxane compound and the coupling agent are put into the tank and mixed, the epoxy resin, the curing agent and the curing accelerator may be put into the tank to knead the raw materials in the tank. .. After kneading the siloxane compound, the epoxy resin, the curing agent, and the coupling agent in the tank, the curing accelerator may be put in the tank, and the raw materials in the tank may be further kneaded. A mixed powder of an epoxy resin, a curing agent, and a curing accelerator (resin mixed powder) is prepared in advance, and then a metal element-containing powder, a siloxane compound, and a coupling agent are kneaded to prepare a metal mixed powder. Subsequently, the metal mixed powder and the above resin mixed powder may be kneaded.
混練時間は、混練機械の種類、混練機械の容積、コンパウンドの製造量にもよるが、例えば、１分以上であることが好ましく、２分以上であることがより好ましく、３分以上であることがさらに好ましい。また、混練時間は、２０分以下であることが好ましく、１５分以下であることがより好ましく、１０分以下であることがさらに好ましい。混練時間が１分未満である場合、混練が不十分であり、コンパウンドの成形性が損なわれ、コンパウンドの硬化度にばらつきが生じる。混練時間が２０分を超える場合、例えば、槽内で樹脂組成物（例えばエポキシ樹脂及びフェノール樹脂）の硬化が進み、コンパウンドの流動性及び成形性が損なわれ易い。槽内の原料を加熱しながらニーダーで混練する場合、加熱温度は、例えば、エポキシ樹脂の半硬化物（Ｂステージのエポキシ樹脂）が生成し、且つエポキシ樹脂の硬化物（Ｃステージのエポキシ樹脂）の生成が抑制される温度であればよい。加熱温度は、硬化促進剤の活性化温度よりも低い温度であってよい。加熱温度は、例えば、５０℃以上であることが好ましく、６０℃以上であることがより好ましく、７０℃以上であることがさらに好ましい。加熱温度は、１５０℃以下であることが好ましく、１２０℃以下であることがより好ましく、１１０℃以下であることがさらに好ましい。加熱温度が上記の範囲内である場合、槽内の樹脂組成物が軟化して金属元素含有粉を構成する金属元素含有粒子の表面を被覆し易く、エポキシ樹脂の半硬化物が生成し易く、混練中のエポキシ樹脂の完全な硬化が抑制され易い。
The kneading time depends on the type of the kneading machine, the volume of the kneading machine, and the production amount of the compound, but for example, it is preferably 1 minute or more, more preferably 2 minutes or more, and 3 minutes or more. Is even more preferable. The kneading time is preferably 20 minutes or less, more preferably 15 minutes or less, and even more preferably 10 minutes or less. If the kneading time is less than 1 minute, the kneading is insufficient, the moldability of the compound is impaired, and the degree of curing of the compound varies. When the kneading time exceeds 20 minutes, for example, the resin composition (for example, epoxy resin and phenol resin) is cured in the tank, and the fluidity and moldability of the compound are likely to be impaired. When the raw materials in the tank are kneaded with a kneader while heating, the heating temperature is, for example, a semi-cured epoxy resin (B-stage epoxy resin) and a cured epoxy resin (C-stage epoxy resin). Any temperature may be used as long as the production of the epoxy is suppressed. The heating temperature may be lower than the activation temperature of the curing accelerator. The heating temperature is, for example, preferably 50 ° C. or higher, more preferably 60 ° C. or higher, and even more preferably 70 ° C. or higher. The heating temperature is preferably 150 ° C. or lower, more preferably 120 ° C. or lower, and even more preferably 110 ° C. or lower. When the heating temperature is within the above range, the resin composition in the tank softens and easily covers the surface of the metal element-containing particles constituting the metal element-containing powder, and a semi-cured epoxy resin is easily formed. Complete curing of the epoxy resin during kneading is likely to be suppressed.
＜成形体＞
本実施形態に係る成形体は、上記のコンパウンドを備えてよい。成形体は、未硬化の樹脂組成物、樹脂組成物の半硬化物（Ｂステージの樹脂組成物）、及び樹脂組成物の硬化物（Ｃステージの樹脂組成物）からなる群より選ばれる少なくとも一種を含んでいてよい。成形体は、上記コンパウンドの硬化物であってよい。 <Molded body>
The molded product according to the present embodiment may include the above-mentioned compound. The molded product is at least one selected from the group consisting of an uncured resin composition, a semi-cured product of the resin composition (B-stage resin composition), and a cured product of the resin composition (C-stage resin composition). May include. The molded product may be a cured product of the above compound.
本実施形態に係る成形体は、上記のコンパウンドを備えてよい。成形体は、未硬化の樹脂組成物、樹脂組成物の半硬化物（Ｂステージの樹脂組成物）、及び樹脂組成物の硬化物（Ｃステージの樹脂組成物）からなる群より選ばれる少なくとも一種を含んでいてよい。成形体は、上記コンパウンドの硬化物であってよい。 <Molded body>
The molded product according to the present embodiment may include the above-mentioned compound. The molded product is at least one selected from the group consisting of an uncured resin composition, a semi-cured product of the resin composition (B-stage resin composition), and a cured product of the resin composition (C-stage resin composition). May include. The molded product may be a cured product of the above compound.
＜成形体の製造方法＞
本実施形態に係る成形体の製造方法は、コンパウンドを金型中で加圧する工程を備えてよい。成形体の製造方法は、コンパウンドを金型中で加圧する工程のみを備えてよく、当該工程に加えてその他の工程を備えてもよい。成形体の製造方法は、第一工程、第二工程及び第三工程を備えてもよい。以下では、各工程の詳細を説明する。 <Manufacturing method of molded product>
The method for producing a molded product according to the present embodiment may include a step of pressurizing the compound in a mold. The method for producing the molded product may include only the step of pressurizing the compound in the mold, and may include other steps in addition to the step. The method for producing the molded product may include a first step, a second step, and a third step. The details of each step will be described below.
本実施形態に係る成形体の製造方法は、コンパウンドを金型中で加圧する工程を備えてよい。成形体の製造方法は、コンパウンドを金型中で加圧する工程のみを備えてよく、当該工程に加えてその他の工程を備えてもよい。成形体の製造方法は、第一工程、第二工程及び第三工程を備えてもよい。以下では、各工程の詳細を説明する。 <Manufacturing method of molded product>
The method for producing a molded product according to the present embodiment may include a step of pressurizing the compound in a mold. The method for producing the molded product may include only the step of pressurizing the compound in the mold, and may include other steps in addition to the step. The method for producing the molded product may include a first step, a second step, and a third step. The details of each step will be described below.
第一工程では、上記の方法でコンパウンドを作製する。
In the first step, the compound is prepared by the above method.
第二工程では、コンパウンドを金型中で加圧することにより、成形体（Ｂステージの成形体）を得る。ここで、樹脂組成物が、金属元素含有粉を構成する個々の金属元素含有粒子間に充填される。そして樹脂組成物は、結合材（バインダ）として機能し、金属元素含有粒子同士を互いに結着する。
In the second step, a molded product (B stage molded product) is obtained by pressurizing the compound in the mold. Here, the resin composition is filled between the individual metal element-containing particles constituting the metal element-containing powder. The resin composition then functions as a binder and binds the metal element-containing particles to each other.
第二工程として、コンパウンドのトランスファー成形を実施してもよい。トランスファー成形では、コンパウンドを５ＭＰａ以上５０ＭＰａ以下で加圧してよい。成形圧力が高いほど、機械的強度に優れた成形体が得られ易い傾向がある。成形体の量産性及び金型の寿命を考慮した場合、成形圧力は８ＭＰａ以上２０ＭＰａ以下であることが好ましい。トランスファー成形によって形成される成形体の密度は、コンパウンドの真密度に対して、好ましくは７５％以上８６％以下、より好ましくは８０％以上８６％以下であってよい。成形体の密度が７５％以上８６％以下である場合、機械的強度に優れた成形体が得られ易い。トランスファー成形において、第二工程と第三工程とを一括して実施してもよい。
As the second step, transfer molding of the compound may be carried out. In transfer molding, the compound may be pressurized at 5 MPa or more and 50 MPa or less. The higher the molding pressure, the easier it is to obtain a molded product having excellent mechanical strength. Considering the mass productivity of the molded product and the life of the mold, the molding pressure is preferably 8 MPa or more and 20 MPa or less. The density of the molded product formed by transfer molding may be preferably 75% or more and 86% or less, and more preferably 80% or more and 86% or less with respect to the true density of the compound. When the density of the molded product is 75% or more and 86% or less, it is easy to obtain a molded product having excellent mechanical strength. In the transfer molding, the second step and the third step may be carried out collectively.
第三工程では、成形体を熱処理によって硬化させ、Ｃステージの成形体を得る。本実施形態に係るコンパウンドは、エラストマーの一種であるシロキサン化合物を含有するため、コンパウンド全体の弾性が低減され、コンパウンドの成形収縮（熱硬化）に伴ってコンパウンドに作用する応力が低減される。その結果、コンパウンドの熱硬化により成形体を形成する過程において、コンパウンドの成形収縮率が低減される。また、上述のとおりそのメカニズムは定かではないが、本実施形態に係るコンパウンドは、エラストマーの一種であるシロキサン化合物を所定量含有するため、コンパウンドから得られる成形体の耐熱性及び耐電圧性が向上する。熱処理の温度は、成形体中の樹脂組成物が十分に硬化する温度であればよい。熱処理の温度は、好ましくは１００℃以上３００℃以下、より好ましくは１１０℃以上２５０℃以下であってよい。成形体中の金属元素含有粉の酸化を抑制するために、熱処理を不活性雰囲気下で行うことが好ましい。熱処理温度が３００℃を超える場合、熱処理の雰囲気に不可避的に含まれる微量の酸素によって金属元素含有粉が酸化されたり、樹脂硬化物が劣化したりする。金属元素含有粉の酸化、及び樹脂硬化物の劣化を抑制しながら樹脂組成物を十分に硬化させるためには、熱処理温度の保持時間は、好ましくは数分以上１０時間以下、より好ましくは３分以上８時間以下であってよい。
In the third step, the molded product is cured by heat treatment to obtain a C-stage molded product. Since the compound according to the present embodiment contains a siloxane compound which is a kind of elastomer, the elasticity of the entire compound is reduced, and the stress acting on the compound due to the molding shrinkage (thermosetting) of the compound is reduced. As a result, the molding shrinkage rate of the compound is reduced in the process of forming the molded product by thermosetting the compound. Further, as described above, the mechanism is not clear, but since the compound according to the present embodiment contains a predetermined amount of a siloxane compound which is a kind of elastomer, the heat resistance and withstand voltage resistance of the molded product obtained from the compound are improved. To do. The temperature of the heat treatment may be a temperature at which the resin composition in the molded product is sufficiently cured. The temperature of the heat treatment may be preferably 100 ° C. or higher and 300 ° C. or lower, and more preferably 110 ° C. or higher and 250 ° C. or lower. In order to suppress the oxidation of the metal element-containing powder in the molded product, it is preferable to carry out the heat treatment in an inert atmosphere. When the heat treatment temperature exceeds 300 ° C., the metal element-containing powder is oxidized or the cured resin product is deteriorated by a small amount of oxygen inevitably contained in the heat treatment atmosphere. In order to sufficiently cure the resin composition while suppressing oxidation of the metal element-containing powder and deterioration of the cured resin product, the heat treatment temperature holding time is preferably several minutes or more and 10 hours or less, more preferably 3 minutes. It may be 8 hours or less.
以下では実施例及び比較例により本発明をさらに詳細に説明するが、本発明はこれらの例によって何ら限定されるものではない。
Hereinafter, the present invention will be described in more detail with reference to Examples and Comparative Examples, but the present invention is not limited to these examples.
（実施例１）
［コンパウンドの調製］
５０ｇのビフェニレンアラルキル型エポキシ樹脂、５０ｇの多官能型エポキシ樹脂、１４．５ｇのフェノールノボラック樹脂１（硬化剤）、２３．６ｇのフェノールノボラック樹脂２（硬化剤）、５．９ｇのウレア系触媒（硬化促進剤）、７．５ｇのジンクラウレート型金属石鹸（離型剤）、２．０ｇのモンタン酸エステル（離型剤（ワックス））、及び４．０ｇの天然ワックス（離型剤（ワックス））を、ポリ容器に投入した。これらの原料をポリ容器内で１０分間混合することにより、樹脂混合物を調製した。樹脂混合物とは、樹脂組成物のうち、シロキサン化合物及びカップリング剤を除く他の全成分に相当する。
ビフェニレンアラルキル型エポキシ樹脂としては、日本化薬株式会社製のＮＣ‐３０００を用いた。
多官能型エポキシ樹脂としては、株式会社プリンテック製のＶＧ－３１０１Ｌを用いた。
フェノールノボラック樹脂１としては、明和化成株式会社製のＨＦ－３Ｍを用いた。
フェノールノボラック樹脂２としては、明和化成株式会社製のＭＥＷ－１８００を用いた。
ウレア系触媒としては、サンアプロ株式会社製のＵ－ＣＡＴ３５１２Ｔを用いた。
ジンクラウレート型金属石鹸としては、日油株式会社製のパウダーベースＬを用いた。
モンタン酸エステルとしては、クラリアントケミカルズ株式会社製のＬＩＣＯＷＡＸ－ＯＰを用いた。
天然ワックスとしては、株式会社セラリカＮＯＤＡ製のカルナバワックスＮｏ．１を用いた。 (Example 1)
[Preparation of compound]
50 g of biphenylene aralkyl type epoxy resin, 50 g of polyfunctional epoxy resin, 14.5 g of phenol novolac resin 1 (curing agent), 23.6 g of phenol novolac resin 2 (curing agent), 5.9 g of urea catalyst (curing agent) Curing accelerator), 7.5 g of zinc chloride type metal soap (release agent), 2.0 g of montanic acid ester (release agent (wax)), and 4.0 g of natural wax (release agent (wax)). )) Was put into a plastic container. A resin mixture was prepared by mixing these raw materials in a plastic container for 10 minutes. The resin mixture corresponds to all other components of the resin composition except the siloxane compound and the coupling agent.
As the biphenylene aralkyl type epoxy resin, NC-3000 manufactured by Nippon Kayaku Co., Ltd. was used.
As the polyfunctional epoxy resin, VG-3101L manufactured by Printec Co., Ltd. was used.
As the phenol novolac resin 1, HF-3M manufactured by Meiwa Kasei Co., Ltd. was used.
As the phenol novolac resin 2, MEW-1800 manufactured by Meiwa Kasei Co., Ltd. was used.
As the urea catalyst, U-CAT3512T manufactured by Sun Appro Co., Ltd. was used.
As the gincrowlate type metal soap, powder base L manufactured by NOF CORPORATION was used.
As the montanic acid ester, LICOWAX-OP manufactured by Clariant Chemicals Co., Ltd. was used.
As a natural wax, Carnauba Wax No. 1 manufactured by Ceralica NODA Co., Ltd. 1 was used.
［コンパウンドの調製］
５０ｇのビフェニレンアラルキル型エポキシ樹脂、５０ｇの多官能型エポキシ樹脂、１４．５ｇのフェノールノボラック樹脂１（硬化剤）、２３．６ｇのフェノールノボラック樹脂２（硬化剤）、５．９ｇのウレア系触媒（硬化促進剤）、７．５ｇのジンクラウレート型金属石鹸（離型剤）、２．０ｇのモンタン酸エステル（離型剤（ワックス））、及び４．０ｇの天然ワックス（離型剤（ワックス））を、ポリ容器に投入した。これらの原料をポリ容器内で１０分間混合することにより、樹脂混合物を調製した。樹脂混合物とは、樹脂組成物のうち、シロキサン化合物及びカップリング剤を除く他の全成分に相当する。
ビフェニレンアラルキル型エポキシ樹脂としては、日本化薬株式会社製のＮＣ‐３０００を用いた。
多官能型エポキシ樹脂としては、株式会社プリンテック製のＶＧ－３１０１Ｌを用いた。
フェノールノボラック樹脂１としては、明和化成株式会社製のＨＦ－３Ｍを用いた。
フェノールノボラック樹脂２としては、明和化成株式会社製のＭＥＷ－１８００を用いた。
ウレア系触媒としては、サンアプロ株式会社製のＵ－ＣＡＴ３５１２Ｔを用いた。
ジンクラウレート型金属石鹸としては、日油株式会社製のパウダーベースＬを用いた。
モンタン酸エステルとしては、クラリアントケミカルズ株式会社製のＬＩＣＯＷＡＸ－ＯＰを用いた。
天然ワックスとしては、株式会社セラリカＮＯＤＡ製のカルナバワックスＮｏ．１を用いた。 (Example 1)
[Preparation of compound]
50 g of biphenylene aralkyl type epoxy resin, 50 g of polyfunctional epoxy resin, 14.5 g of phenol novolac resin 1 (curing agent), 23.6 g of phenol novolac resin 2 (curing agent), 5.9 g of urea catalyst (curing agent) Curing accelerator), 7.5 g of zinc chloride type metal soap (release agent), 2.0 g of montanic acid ester (release agent (wax)), and 4.0 g of natural wax (release agent (wax)). )) Was put into a plastic container. A resin mixture was prepared by mixing these raw materials in a plastic container for 10 minutes. The resin mixture corresponds to all other components of the resin composition except the siloxane compound and the coupling agent.
As the biphenylene aralkyl type epoxy resin, NC-3000 manufactured by Nippon Kayaku Co., Ltd. was used.
As the polyfunctional epoxy resin, VG-3101L manufactured by Printec Co., Ltd. was used.
As the phenol novolac resin 1, HF-3M manufactured by Meiwa Kasei Co., Ltd. was used.
As the phenol novolac resin 2, MEW-1800 manufactured by Meiwa Kasei Co., Ltd. was used.
As the urea catalyst, U-CAT3512T manufactured by Sun Appro Co., Ltd. was used.
As the gincrowlate type metal soap, powder base L manufactured by NOF CORPORATION was used.
As the montanic acid ester, LICOWAX-OP manufactured by Clariant Chemicals Co., Ltd. was used.
As a natural wax, Carnauba Wax No. 1 manufactured by Ceralica NODA Co., Ltd. 1 was used.
アモルファス系鉄粉１とアモルファス系鉄粉２とを、加圧式２軸ニーダー（日本スピンドル製造株式会社製、容量５Ｌ）で５分間均一に混合して、３７４１ｇの金属元素含有粉を調製した。金属元素含有粉におけるアモルファス系鉄粉１の含有量は、８２質量％であった。金属元素含有粉におけるアモルファス系鉄粉２の含有量は、１８質量％であった。１．９ｇのメタクリロキシオクチルトリメトキシシラン（カップリング剤）、１．９ｇの３－メルカプトプロピルトリメトキシシラン（カップリング剤）、及び１５ｇのカプロラクトン変性ジメチルシリコーン（シロキサン結合を有する化合物）を２軸ニーダー内の金属元素含有粉へ添加した。続いて、２軸ニーダーの内容物を９０℃になるまで加熱し、その温度を保持しながら、２軸ニーダーの内容物を１０分間混合した。続いて、上記の樹脂混合物を２軸ニーダーの内容物へ添加して、内容物の温度を１２０℃に保持しながら、内容物を１５分間溶融・混練した。以上の溶融・混練によって得られた混練物を室温まで冷却した後、混練物が所定の粒度を有するようになるまで混練物をハンマーで粉砕した。なお、上記の「溶融」とは、２軸ニーダーの内容物のうち樹脂組成物の少なくとも一部の溶融を意味する。コンパウンド中の金属元素含有粉は、コンパウンドの調製過程において溶融しない。
アモルファス系鉄粉１としては、エプソンアトミックス株式会社製のＫＵＡＭＥＴ ９Ａ４‐ＩＩ ０５３Ｃ０３（平均粒径２４μｍ）を用いた。
アモルファス系鉄粉２としては、エプソンアトミックス株式会社製のＡＷ２‐０８（平均粒径５．３μｍ）を用いた。
メタクリロキシオクチルトリメトキシシランとしては、信越化学工業株式会社製のＫＢＭ‐５８０３を用いた。
３－メルカプトプロピルトリメトキシシランとしては、信越化学工業株式会社製のＫＢＭ‐８０３を用いた。
カプロラクトン変性ジメチルシリコーンとしては、Ｇｅｌｅｓｔ社製のＤＢＬ‐Ｃ３２を用いた。このカプロラクトン変性ジメチルシリコーンは、上記の化学式（３）で表される化合物である。 Amorphous iron powder 1 and amorphous iron powder 2 were uniformly mixed for 5 minutes with a pressurized twin-screw kneader (manufactured by Nihon Spindle Manufacturing Co., Ltd., capacity 5 L) to prepare 3741 g of metal element-containing powder. The content of the amorphous iron powder 1 in the metal element-containing powder was 82% by mass. The content of the amorphous iron powder 2 in the metal element-containing powder was 18% by mass. 1.9 g of metharoxyoctyltrimethoxysilane (coupling agent), 1.9 g of 3-mercaptopropyltrimethoxysilane (coupling agent), and 15 g of caprolactone-modified dimethylsilicone (compound having a siloxane bond) biaxially It was added to the metal element-containing powder in the kneader. Subsequently, the contents of the twin-screw kneader were heated to 90 ° C., and the contents of the twin-screw kneader were mixed for 10 minutes while maintaining the temperature. Subsequently, the above resin mixture was added to the contents of the twin-screw kneader, and the contents were melted and kneaded for 15 minutes while maintaining the temperature of the contents at 120 ° C. The kneaded product obtained by the above melting and kneading was cooled to room temperature, and then the kneaded product was crushed with a hammer until the kneaded product had a predetermined particle size. The above-mentioned "melting" means melting at least a part of the resin composition in the contents of the biaxial kneader. The metal element-containing powder in the compound does not melt during the compound preparation process.
As the amorphous iron powder 1, KUAMET 9A4-II 053C03 (average particle size 24 μm) manufactured by Epson Atmix Co., Ltd. was used.
As the amorphous iron powder 2, AW2-08 (average particle size 5.3 μm) manufactured by Epson Atmix Co., Ltd. was used.
As the methacryloxyoctyltrimethoxysilane, KBM-5803 manufactured by Shin-Etsu Chemical Co., Ltd. was used.
As 3-mercaptopropyltrimethoxysilane, KBM-803 manufactured by Shin-Etsu Chemical Co., Ltd. was used.
As the caprolactone-modified dimethyl silicone, DBL-C32 manufactured by Gelest was used. This caprolactone-modified dimethyl silicone is a compound represented by the above chemical formula (3).
アモルファス系鉄粉１としては、エプソンアトミックス株式会社製のＫＵＡＭＥＴ ９Ａ４‐ＩＩ ０５３Ｃ０３（平均粒径２４μｍ）を用いた。
アモルファス系鉄粉２としては、エプソンアトミックス株式会社製のＡＷ２‐０８（平均粒径５．３μｍ）を用いた。
メタクリロキシオクチルトリメトキシシランとしては、信越化学工業株式会社製のＫＢＭ‐５８０３を用いた。
３－メルカプトプロピルトリメトキシシランとしては、信越化学工業株式会社製のＫＢＭ‐８０３を用いた。
カプロラクトン変性ジメチルシリコーンとしては、Ｇｅｌｅｓｔ社製のＤＢＬ‐Ｃ３２を用いた。このカプロラクトン変性ジメチルシリコーンは、上記の化学式（３）で表される化合物である。 Amorphous iron powder 1 and amorphous iron powder 2 were uniformly mixed for 5 minutes with a pressurized twin-screw kneader (manufactured by Nihon Spindle Manufacturing Co., Ltd., capacity 5 L) to prepare 3741 g of metal element-containing powder. The content of the amorphous iron powder 1 in the metal element-containing powder was 82% by mass. The content of the amorphous iron powder 2 in the metal element-containing powder was 18% by mass. 1.9 g of metharoxyoctyltrimethoxysilane (coupling agent), 1.9 g of 3-mercaptopropyltrimethoxysilane (coupling agent), and 15 g of caprolactone-modified dimethylsilicone (compound having a siloxane bond) biaxially It was added to the metal element-containing powder in the kneader. Subsequently, the contents of the twin-screw kneader were heated to 90 ° C., and the contents of the twin-screw kneader were mixed for 10 minutes while maintaining the temperature. Subsequently, the above resin mixture was added to the contents of the twin-screw kneader, and the contents were melted and kneaded for 15 minutes while maintaining the temperature of the contents at 120 ° C. The kneaded product obtained by the above melting and kneading was cooled to room temperature, and then the kneaded product was crushed with a hammer until the kneaded product had a predetermined particle size. The above-mentioned "melting" means melting at least a part of the resin composition in the contents of the biaxial kneader. The metal element-containing powder in the compound does not melt during the compound preparation process.
As the amorphous iron powder 1, KUAMET 9A4-II 053C03 (average particle size 24 μm) manufactured by Epson Atmix Co., Ltd. was used.
As the amorphous iron powder 2, AW2-08 (average particle size 5.3 μm) manufactured by Epson Atmix Co., Ltd. was used.
As the methacryloxyoctyltrimethoxysilane, KBM-5803 manufactured by Shin-Etsu Chemical Co., Ltd. was used.
As 3-mercaptopropyltrimethoxysilane, KBM-803 manufactured by Shin-Etsu Chemical Co., Ltd. was used.
As the caprolactone-modified dimethyl silicone, DBL-C32 manufactured by Gelest was used. This caprolactone-modified dimethyl silicone is a compound represented by the above chemical formula (3).
以上の方法により、実施例１のコンパウンドを調製した。コンパウンドにおける金属元素含有粉の含有量は９５．５質量％であった。
The compound of Example 1 was prepared by the above method. The content of the metal element-containing powder in the compound was 95.5% by mass.
（その他の実施例及び比較例）
原料処方を表１に示すように変更したこと以外は、実施例１と同様にして、その他の実施例及び比較例のコンパウンドを作製した。実施例１と同様の方法で、各例のコンパウンドに関する評価を行った。なお、表１に記載のＫＢＭ－４０３は、信越化学工業株式会社製の３－グリシドキシプロピルトリメトキシシランである。 (Other Examples and Comparative Examples)
Compounds of other Examples and Comparative Examples were prepared in the same manner as in Example 1 except that the raw material formulations were changed as shown in Table 1. The compound of each example was evaluated in the same manner as in Example 1. KBM-403 shown in Table 1 is 3-glycidoxypropyltrimethoxysilane manufactured by Shin-Etsu Chemical Co., Ltd.
原料処方を表１に示すように変更したこと以外は、実施例１と同様にして、その他の実施例及び比較例のコンパウンドを作製した。実施例１と同様の方法で、各例のコンパウンドに関する評価を行った。なお、表１に記載のＫＢＭ－４０３は、信越化学工業株式会社製の３－グリシドキシプロピルトリメトキシシランである。 (Other Examples and Comparative Examples)
Compounds of other Examples and Comparative Examples were prepared in the same manner as in Example 1 except that the raw material formulations were changed as shown in Table 1. The compound of each example was evaluated in the same manner as in Example 1. KBM-403 shown in Table 1 is 3-glycidoxypropyltrimethoxysilane manufactured by Shin-Etsu Chemical Co., Ltd.
［評価］
各実施例及び比較例のコンパウンドを用いて以下の評価を行った。結果を表１に示す。 [Evaluation]
The following evaluations were made using the compounds of each example and comparative example. The results are shown in Table 1.
各実施例及び比較例のコンパウンドを用いて以下の評価を行った。結果を表１に示す。 [Evaluation]
The following evaluations were made using the compounds of each example and comparative example. The results are shown in Table 1.
（耐熱性の評価：２５０℃曲げ試験）
各実施例及び比較例のコンパウンドを、成形金型温度１７５℃、成形圧力１３．５ＭＰａ、硬化時間３６０秒の条件でトランスファー成形した後、１７５℃で５．５時間ポストキュアすることによって、試験片を得た。試験片の寸法は、縦幅８０ｍｍ×横幅１０ｍｍ×厚さ３．０ｍｍであった。
恒温槽付きオートグラフを用いて、試験片に対して３点支持型の曲げ試験を実施した。オートグラフとしては、株式会社島津製作所製のＡＧＳ－５００Ａを用いた。恒温槽の温度は、２５０℃であった。曲げ試験では、２つの支点により試験片の一方の面を支持した。試験片の他方の面における２つの支点間の中央の位置に荷重を加えた。試験片が破壊されたときの荷重を測定した。曲げ試験の測定条件は、以下のとおりであった。
２つの支点間の距離Ｌｖ： ６４．０±０．５ｍｍ
ヘッドスピード： ２．０±０．２ｍｍ／分
チャートスピード： １００ｍｍ／分
チャートフルスケール： ４９０Ｎ（５０ｋｇｆ）
下記数式（Ａ）に基づいて、曲げ強度σ（単位：ＭＰａ）を算出した。下記数式（Ｂ）に基づいて、曲げ弾性率Ｅ（単位：ＧＰａ）を算出した。下記数式（Ｃ）に基づいて、曲げ伸び率ε（単位：％）を算出した。下記数式において、「Ｐ」は、試験片が破壊されたときの荷重（単位：Ｎ）である。「Ｌｖ」は、２つの支点間の距離（単位：ｍｍ）である。「Ｗ」は、試験片の横幅（単位：ｍｍ）である。「ｔ」は、試験片の厚さ（単位：ｍｍ）である。「Ｆ／Ｙ」は、荷重‐たわみ曲線の直線部分の勾配（単位：Ｎ／ｍｍ）である。「ｓ」は、試験片が破壊される直前の試験片のたわみ（単位：ｍｍ）である。
σ＝（３×Ｐ×Ｌｖ）／（２×Ｗ×ｔ２） （Ａ）
Ｅ＝［Ｌｖ３／（４×Ｗ×ｔ３）］×（Ｆ／Ｙ） （Ｂ）
ε＝（６００×ｓ×ｔ）／Ｌｖ２ （Ｃ） (Evaluation of heat resistance: 250 ° C bending test)
The compounds of each Example and Comparative Example were transfer-molded under the conditions of a molding die temperature of 175 ° C., a molding pressure of 13.5 MPa, and a curing time of 360 seconds, and then post-cured at 175 ° C. for 5.5 hours to test pieces. Got The dimensions of the test piece were 80 mm in length × 10 mm in width × 3.0 mm in thickness.
A three-point support type bending test was performed on the test piece using an autograph with a constant temperature bath. As the autograph, AGS-500A manufactured by Shimadzu Corporation was used. The temperature of the constant temperature bath was 250 ° C. In the bending test, one side of the test piece was supported by two fulcrums. A load was applied to the central position between the two fulcrums on the other surface of the test piece. The load when the test piece was broken was measured. The measurement conditions for the bending test were as follows.
Distance between two fulcrums Lv: 64.0 ± 0.5 mm
Head speed: 2.0 ± 0.2 mm / min Chart speed: 100 mm / min Chart full scale: 490N (50kgf)
The bending strength σ (unit: MPa) was calculated based on the following mathematical formula (A). The flexural modulus E (unit: GPa) was calculated based on the following mathematical formula (B). The bending elongation rate ε (unit:%) was calculated based on the following mathematical formula (C). In the following formula, "P" is the load (unit: N) when the test piece is broken. "Lv" is the distance (unit: mm) between the two fulcrums. “W” is the width (unit: mm) of the test piece. “T” is the thickness (unit: mm) of the test piece. "F / Y" is the gradient (unit: N / mm) of the straight line portion of the load-deflection curve. “S” is the deflection (unit: mm) of the test piece immediately before the test piece is destroyed.
σ = (3 × P × Lv) / (2 × W × t 2 ) (A)
E = [Lv 3 / (4 × W × t 3 )] × (F / Y) (B)
ε = (600 × s × t) / Lv 2 (C)
各実施例及び比較例のコンパウンドを、成形金型温度１７５℃、成形圧力１３．５ＭＰａ、硬化時間３６０秒の条件でトランスファー成形した後、１７５℃で５．５時間ポストキュアすることによって、試験片を得た。試験片の寸法は、縦幅８０ｍｍ×横幅１０ｍｍ×厚さ３．０ｍｍであった。
恒温槽付きオートグラフを用いて、試験片に対して３点支持型の曲げ試験を実施した。オートグラフとしては、株式会社島津製作所製のＡＧＳ－５００Ａを用いた。恒温槽の温度は、２５０℃であった。曲げ試験では、２つの支点により試験片の一方の面を支持した。試験片の他方の面における２つの支点間の中央の位置に荷重を加えた。試験片が破壊されたときの荷重を測定した。曲げ試験の測定条件は、以下のとおりであった。
２つの支点間の距離Ｌｖ： ６４．０±０．５ｍｍ
ヘッドスピード： ２．０±０．２ｍｍ／分
チャートスピード： １００ｍｍ／分
チャートフルスケール： ４９０Ｎ（５０ｋｇｆ）
下記数式（Ａ）に基づいて、曲げ強度σ（単位：ＭＰａ）を算出した。下記数式（Ｂ）に基づいて、曲げ弾性率Ｅ（単位：ＧＰａ）を算出した。下記数式（Ｃ）に基づいて、曲げ伸び率ε（単位：％）を算出した。下記数式において、「Ｐ」は、試験片が破壊されたときの荷重（単位：Ｎ）である。「Ｌｖ」は、２つの支点間の距離（単位：ｍｍ）である。「Ｗ」は、試験片の横幅（単位：ｍｍ）である。「ｔ」は、試験片の厚さ（単位：ｍｍ）である。「Ｆ／Ｙ」は、荷重‐たわみ曲線の直線部分の勾配（単位：Ｎ／ｍｍ）である。「ｓ」は、試験片が破壊される直前の試験片のたわみ（単位：ｍｍ）である。
σ＝（３×Ｐ×Ｌｖ）／（２×Ｗ×ｔ２） （Ａ）
Ｅ＝［Ｌｖ３／（４×Ｗ×ｔ３）］×（Ｆ／Ｙ） （Ｂ）
ε＝（６００×ｓ×ｔ）／Ｌｖ２ （Ｃ） (Evaluation of heat resistance: 250 ° C bending test)
The compounds of each Example and Comparative Example were transfer-molded under the conditions of a molding die temperature of 175 ° C., a molding pressure of 13.5 MPa, and a curing time of 360 seconds, and then post-cured at 175 ° C. for 5.5 hours to test pieces. Got The dimensions of the test piece were 80 mm in length × 10 mm in width × 3.0 mm in thickness.
A three-point support type bending test was performed on the test piece using an autograph with a constant temperature bath. As the autograph, AGS-500A manufactured by Shimadzu Corporation was used. The temperature of the constant temperature bath was 250 ° C. In the bending test, one side of the test piece was supported by two fulcrums. A load was applied to the central position between the two fulcrums on the other surface of the test piece. The load when the test piece was broken was measured. The measurement conditions for the bending test were as follows.
Distance between two fulcrums Lv: 64.0 ± 0.5 mm
Head speed: 2.0 ± 0.2 mm / min Chart speed: 100 mm / min Chart full scale: 490N (50kgf)
The bending strength σ (unit: MPa) was calculated based on the following mathematical formula (A). The flexural modulus E (unit: GPa) was calculated based on the following mathematical formula (B). The bending elongation rate ε (unit:%) was calculated based on the following mathematical formula (C). In the following formula, "P" is the load (unit: N) when the test piece is broken. "Lv" is the distance (unit: mm) between the two fulcrums. “W” is the width (unit: mm) of the test piece. “T” is the thickness (unit: mm) of the test piece. "F / Y" is the gradient (unit: N / mm) of the straight line portion of the load-deflection curve. “S” is the deflection (unit: mm) of the test piece immediately before the test piece is destroyed.
σ = (3 × P × Lv) / (2 × W × t 2 ) (A)
E = [Lv 3 / (4 × W × t 3 )] × (F / Y) (B)
ε = (600 × s × t) / Lv 2 (C)
（耐電圧性の評価：耐電圧試験）
各実施例及び比較例のコンパウンドを、成形金型温度１７５℃、成形圧力１３．５ＭＰａ、硬化時間３６０秒の条件でトランスファー成形した後、１７５℃で５．５時間ポストキュアすることによって、厚さ２．０ｍｍの試験片を作製した。
耐電圧試験に際し、絶縁板上に、接地線を接続したステンレス板、導電ゴム板、試験片、高圧線を接続した直径１０ｍｍのステンレス製電極を順に配置した。高圧線及び接地線を、高圧アンプの高圧出力端子、接地端子にそれぞれ接続した。ファンクションジェネレータの波形出力を高圧アンプに入力して、０Ｖから最大２０００Ｖまで毎秒１０Ｖの速度で昇圧するよう試験電圧を発生し、試験片に印加した。試験片を通過する電流が１０ｍＡを超過した時点の電圧を読み取った。次いで、試験片上の異なる位置にステンレス製電極を配置し、同様に電圧を印加した。所定回数繰り返し、読み取った電圧の平均値を試験片の耐電圧（絶縁破壊電圧：Ｖ／ｍｍ）とした。 (Evaluation of withstand voltage: Withstand voltage test)
The compounds of each Example and Comparative Example were transfer-molded under the conditions of a molding die temperature of 175 ° C., a molding pressure of 13.5 MPa, and a curing time of 360 seconds, and then post-cured at 175 ° C. for 5.5 hours to obtain a thickness. A 2.0 mm test piece was prepared.
In the withstand voltage test, a stainless steel plate to which the ground wire was connected, a conductive rubber plate, a test piece, and a stainless steel electrode having a diameter of 10 mm to which the high voltage wire was connected were arranged in this order on the insulating plate. The high-voltage line and the ground wire were connected to the high-voltage output terminal and the ground terminal of the high-voltage amplifier, respectively. The waveform output of the function generator was input to the high-voltage amplifier, and a test voltage was generated so as to boost the voltage from 0 V to a maximum of 2000 V at a rate of 10 V per second, and applied to the test piece. The voltage at the time when the current passing through the test piece exceeded 10 mA was read. Next, stainless steel electrodes were placed at different positions on the test piece, and a voltage was applied in the same manner. It was repeated a predetermined number of times, and the average value of the read voltages was taken as the withstand voltage (dielectric breakdown voltage: V / mm) of the test piece.
各実施例及び比較例のコンパウンドを、成形金型温度１７５℃、成形圧力１３．５ＭＰａ、硬化時間３６０秒の条件でトランスファー成形した後、１７５℃で５．５時間ポストキュアすることによって、厚さ２．０ｍｍの試験片を作製した。
耐電圧試験に際し、絶縁板上に、接地線を接続したステンレス板、導電ゴム板、試験片、高圧線を接続した直径１０ｍｍのステンレス製電極を順に配置した。高圧線及び接地線を、高圧アンプの高圧出力端子、接地端子にそれぞれ接続した。ファンクションジェネレータの波形出力を高圧アンプに入力して、０Ｖから最大２０００Ｖまで毎秒１０Ｖの速度で昇圧するよう試験電圧を発生し、試験片に印加した。試験片を通過する電流が１０ｍＡを超過した時点の電圧を読み取った。次いで、試験片上の異なる位置にステンレス製電極を配置し、同様に電圧を印加した。所定回数繰り返し、読み取った電圧の平均値を試験片の耐電圧（絶縁破壊電圧：Ｖ／ｍｍ）とした。 (Evaluation of withstand voltage: Withstand voltage test)
The compounds of each Example and Comparative Example were transfer-molded under the conditions of a molding die temperature of 175 ° C., a molding pressure of 13.5 MPa, and a curing time of 360 seconds, and then post-cured at 175 ° C. for 5.5 hours to obtain a thickness. A 2.0 mm test piece was prepared.
In the withstand voltage test, a stainless steel plate to which the ground wire was connected, a conductive rubber plate, a test piece, and a stainless steel electrode having a diameter of 10 mm to which the high voltage wire was connected were arranged in this order on the insulating plate. The high-voltage line and the ground wire were connected to the high-voltage output terminal and the ground terminal of the high-voltage amplifier, respectively. The waveform output of the function generator was input to the high-voltage amplifier, and a test voltage was generated so as to boost the voltage from 0 V to a maximum of 2000 V at a rate of 10 V per second, and applied to the test piece. The voltage at the time when the current passing through the test piece exceeded 10 mA was read. Next, stainless steel electrodes were placed at different positions on the test piece, and a voltage was applied in the same manner. It was repeated a predetermined number of times, and the average value of the read voltages was taken as the withstand voltage (dielectric breakdown voltage: V / mm) of the test piece.
本発明に係るコンパウンドは、耐熱性及び耐電圧性を共に有する成形体を得ることができるため、高い工業的な価値を有している。
The compound according to the present invention has high industrial value because a molded product having both heat resistance and withstand voltage can be obtained.
The compound according to the present invention has high industrial value because a molded product having both heat resistance and withstand voltage can be obtained.
Claims (6)
- 金属元素含有粉と、樹脂組成物と、を備え、
前記樹脂組成物が、エポキシ樹脂、及びシロキサン結合を有する化合物を含有し、
前記シロキサン結合を有する化合物の含有量が、前記エポキシ樹脂１００質量部に対して、２０質量部以下であり、
前記シロキサン結合を有する化合物が、下記化学式（１）で表される構造を有するシロキサン化合物を含む、コンパウンド。
The resin composition contains an epoxy resin and a compound having a siloxane bond.
The content of the compound having a siloxane bond is 20 parts by mass or less with respect to 100 parts by mass of the epoxy resin.
A compound in which the compound having a siloxane bond contains a siloxane compound having a structure represented by the following chemical formula (1).
- 前記シロキサン化合物が、下記化学式（２）で表される構造単位をさらに有する、
請求項１に記載のコンパウンド。
The compound according to claim 1.
- 前記シロキサン化合物として、下記化学式（３）で表される化合物を含む、
請求項１又は２に記載のコンパウンド。
The compound according to claim 1 or 2.
- 前記エポキシ樹脂として、ビフェニレンアラルキル型エポキシ樹脂及びイソシアネート変性エポキシ樹脂のうちの少なくとも一種を含む、
請求項１～３のいずれか一項に記載のコンパウンド。 The epoxy resin contains at least one of a biphenylene aralkyl type epoxy resin and an isocyanate-modified epoxy resin.
The compound according to any one of claims 1 to 3. - 前記金属元素含有粉の含有量が、９０質量％以上１００質量％未満である、
請求項１～４のいずれか一項に記載のコンパウンド。 The content of the metal element-containing powder is 90% by mass or more and less than 100% by mass.
The compound according to any one of claims 1 to 4. - 請求項１～５のいずれか一項に記載のコンパウンドを備える、成形体。
A molded product comprising the compound according to any one of claims 1 to 5.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2021562690A JPWO2021112135A1 (en) | 2019-12-03 | 2020-12-02 | |
| KR1020227016740A KR20220111255A (en) | 2019-12-03 | 2020-12-02 | compound and molded body |
| CN202080065528.0A CN114402030A (en) | 2019-12-03 | 2020-12-02 | Composite and molded article |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2019219060 | 2019-12-03 | ||
| JP2019-219060 | 2019-12-03 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2021112135A1 true WO2021112135A1 (en) | 2021-06-10 |
Family
ID=76221690
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/JP2020/044901 WO2021112135A1 (en) | 2019-12-03 | 2020-12-02 | Compound and molded object |
Country Status (5)
| Country | Link |
|---|---|
| JP (1) | JPWO2021112135A1 (en) |
| KR (1) | KR20220111255A (en) |
| CN (1) | CN114402030A (en) |
| TW (1) | TW202128875A (en) |
| WO (1) | WO2021112135A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPWO2022075186A1 (en) * | 2020-10-05 | 2022-04-14 |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06163225A (en) * | 1992-11-20 | 1994-06-10 | Sumitomo Metal Mining Co Ltd | Composition for bond magnet and bond magnet |
| JPH1167513A (en) * | 1997-08-11 | 1999-03-09 | Seiko Epson Corp | Rare earth bonded magnet |
| JP2010138384A (en) * | 2008-11-12 | 2010-06-24 | Hitachi Chem Co Ltd | Encapsulating liquid epoxy resin composition, electronic component device including element encapsulated with the encapsulating liquid epoxy resin composition, and wafer level chip size package |
| CN104371617A (en) * | 2013-08-12 | 2015-02-25 | 何书凤 | Production method of glue for filling casting slits |
| WO2019229960A1 (en) * | 2018-05-31 | 2019-12-05 | 日立化成株式会社 | Composition and molded object |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101899186B1 (en) * | 2011-05-13 | 2018-09-14 | 히타치가세이가부시끼가이샤 | Epoxy resin molding material for encapsulation and electronic component device |
| JP6159512B2 (en) | 2012-07-04 | 2017-07-05 | 太陽誘電株式会社 | Inductor |
-
2020
- 2020-12-02 WO PCT/JP2020/044901 patent/WO2021112135A1/en active Application Filing
- 2020-12-02 CN CN202080065528.0A patent/CN114402030A/en active Pending
- 2020-12-02 JP JP2021562690A patent/JPWO2021112135A1/ja active Pending
- 2020-12-02 KR KR1020227016740A patent/KR20220111255A/en unknown
- 2020-12-02 TW TW109142467A patent/TW202128875A/en unknown
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06163225A (en) * | 1992-11-20 | 1994-06-10 | Sumitomo Metal Mining Co Ltd | Composition for bond magnet and bond magnet |
| JPH1167513A (en) * | 1997-08-11 | 1999-03-09 | Seiko Epson Corp | Rare earth bonded magnet |
| JP2010138384A (en) * | 2008-11-12 | 2010-06-24 | Hitachi Chem Co Ltd | Encapsulating liquid epoxy resin composition, electronic component device including element encapsulated with the encapsulating liquid epoxy resin composition, and wafer level chip size package |
| CN104371617A (en) * | 2013-08-12 | 2015-02-25 | 何书凤 | Production method of glue for filling casting slits |
| WO2019229960A1 (en) * | 2018-05-31 | 2019-12-05 | 日立化成株式会社 | Composition and molded object |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPWO2022075186A1 (en) * | 2020-10-05 | 2022-04-14 | ||
| WO2022075186A1 (en) * | 2020-10-05 | 2022-04-14 | 住友ベークライト株式会社 | Resin molding material, molded body, and method for producing said molded body |
| JP7168131B2 (en) | 2020-10-05 | 2022-11-09 | 住友ベークライト株式会社 | Resin molding material, molded article, and method for producing the molded article |
Also Published As
| Publication number | Publication date |
|---|---|
| JPWO2021112135A1 (en) | 2021-06-10 |
| CN114402030A (en) | 2022-04-26 |
| TW202128875A (en) | 2021-08-01 |
| KR20220111255A (en) | 2022-08-09 |
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