CN104987851B - One kind electrolysis door filling polyurethane cellular glue and preparation method thereof - Google Patents
One kind electrolysis door filling polyurethane cellular glue and preparation method thereof Download PDFInfo
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- 229920002635 polyurethane Polymers 0.000 title claims abstract description 54
- 239000004814 polyurethane Substances 0.000 title claims abstract description 54
- 230000001413 cellular effect Effects 0.000 title claims abstract description 41
- 239000003292 glue Substances 0.000 title claims abstract description 38
- 238000005868 electrolysis reaction Methods 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 229920001730 Moisture cure polyurethane Polymers 0.000 claims abstract description 23
- 229920005989 resin Polymers 0.000 claims abstract description 21
- 239000011347 resin Substances 0.000 claims abstract description 21
- 239000003381 stabilizer Substances 0.000 claims abstract description 14
- 239000006260 foam Substances 0.000 claims abstract description 9
- 239000000945 filler Substances 0.000 claims abstract description 7
- 239000004088 foaming agent Substances 0.000 claims abstract description 5
- -1 polymethylene Polymers 0.000 claims description 48
- 229920001228 polyisocyanate Polymers 0.000 claims description 43
- 239000005056 polyisocyanate Substances 0.000 claims description 43
- 229920006389 polyphenyl polymer Polymers 0.000 claims description 40
- 229920000570 polyether Polymers 0.000 claims description 38
- 238000003756 stirring Methods 0.000 claims description 33
- 239000003054 catalyst Substances 0.000 claims description 22
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 19
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 13
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 12
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical group CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 12
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 12
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- SNZYOYGFWBZAQY-UHFFFAOYSA-N 2-ethyl-2-(hydroxymethyl)propane-1,3-diol;2-methyloxirane Chemical compound CC1CO1.CCC(CO)(CO)CO SNZYOYGFWBZAQY-UHFFFAOYSA-N 0.000 claims description 8
- NNPPMTNAJDCUHE-UHFFFAOYSA-N isobutane Chemical compound CC(C)C NNPPMTNAJDCUHE-UHFFFAOYSA-N 0.000 claims description 8
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 claims description 8
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- RGSFGYAAUTVSQA-UHFFFAOYSA-N pentamethylene Natural products C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 claims description 7
- SYBYTAAJFKOIEJ-UHFFFAOYSA-N 3-Methylbutan-2-one Chemical compound CC(C)C(C)=O SYBYTAAJFKOIEJ-UHFFFAOYSA-N 0.000 claims description 6
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 6
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
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- 239000003960 organic solvent Substances 0.000 claims description 6
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims description 6
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 5
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 5
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 4
- 239000002585 base Substances 0.000 claims description 4
- 239000001282 iso-butane Substances 0.000 claims description 4
- QWTDNUCVQCZILF-UHFFFAOYSA-N isopentane Chemical compound CCC(C)C QWTDNUCVQCZILF-UHFFFAOYSA-N 0.000 claims description 4
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- 239000005995 Aluminium silicate Substances 0.000 claims description 3
- SVYKKECYCPFKGB-UHFFFAOYSA-N N,N-dimethylcyclohexylamine Chemical compound CN(C)C1CCCCC1 SVYKKECYCPFKGB-UHFFFAOYSA-N 0.000 claims description 3
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 claims description 3
- 235000012211 aluminium silicate Nutrition 0.000 claims description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 3
- 239000006229 carbon black Substances 0.000 claims description 3
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- 239000012972 dimethylethanolamine Substances 0.000 claims description 3
- YGANSGVIUGARFR-UHFFFAOYSA-N dipotassium dioxosilane oxo(oxoalumanyloxy)alumane oxygen(2-) Chemical compound [O--].[K+].[K+].O=[Si]=O.O=[Al]O[Al]=O YGANSGVIUGARFR-UHFFFAOYSA-N 0.000 claims description 3
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052627 muscovite Inorganic materials 0.000 claims description 3
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- 239000004408 titanium dioxide Substances 0.000 claims description 3
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000010456 wollastonite Substances 0.000 claims description 3
- 229910052882 wollastonite Inorganic materials 0.000 claims description 3
- HXKKHQJGJAFBHI-UHFFFAOYSA-N 1-aminopropan-2-ol Chemical compound CC(O)CN HXKKHQJGJAFBHI-UHFFFAOYSA-N 0.000 claims description 2
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 2
- AFABGHUZZDYHJO-UHFFFAOYSA-N dimethyl butane Natural products CCCC(C)C AFABGHUZZDYHJO-UHFFFAOYSA-N 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims description 2
- 229940102253 isopropanolamine Drugs 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims 2
- 229910052757 nitrogen Inorganic materials 0.000 claims 2
- KPAPHODVWOVUJL-UHFFFAOYSA-N 1-benzofuran;1h-indene Chemical compound C1=CC=C2CC=CC2=C1.C1=CC=C2OC=CC2=C1 KPAPHODVWOVUJL-UHFFFAOYSA-N 0.000 claims 1
- 239000012298 atmosphere Substances 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- POLCUAVZOMRGSN-UHFFFAOYSA-N dipropyl ether Chemical compound CCCOCCC POLCUAVZOMRGSN-UHFFFAOYSA-N 0.000 claims 1
- 150000002148 esters Chemical class 0.000 claims 1
- 150000002170 ethers Chemical class 0.000 claims 1
- 235000013312 flour Nutrition 0.000 claims 1
- 235000013847 iso-butane Nutrition 0.000 claims 1
- 150000002527 isonitriles Chemical class 0.000 claims 1
- 125000005474 octanoate group Chemical group 0.000 claims 1
- 125000004817 pentamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 4
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 239000004721 Polyphenylene oxide Substances 0.000 description 36
- 239000000853 adhesive Substances 0.000 description 18
- 230000001070 adhesive effect Effects 0.000 description 18
- 150000002009 diols Chemical class 0.000 description 13
- 230000007613 environmental effect Effects 0.000 description 12
- 238000005187 foaming Methods 0.000 description 11
- 229910052782 aluminium Inorganic materials 0.000 description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 10
- 238000002485 combustion reaction Methods 0.000 description 10
- 239000012948 isocyanate Substances 0.000 description 9
- 150000002513 isocyanates Chemical class 0.000 description 9
- IANQTJSKSUMEQM-UHFFFAOYSA-N 1-benzofuran Chemical compound C1=CC=C2OC=CC2=C1 IANQTJSKSUMEQM-UHFFFAOYSA-N 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 229920005862 polyol Polymers 0.000 description 6
- 150000003077 polyols Chemical class 0.000 description 6
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 description 4
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- DMEGYFMYUHOHGS-UHFFFAOYSA-N heptamethylene Natural products C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 description 3
- 239000003208 petroleum Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000008096 xylene Substances 0.000 description 3
- GTEXIOINCJRBIO-UHFFFAOYSA-N 2-[2-(dimethylamino)ethoxy]-n,n-dimethylethanamine Chemical compound CN(C)CCOCCN(C)C GTEXIOINCJRBIO-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- AYOHIQLKSOJJQH-UHFFFAOYSA-N dibutyltin Chemical compound CCCC[Sn]CCCC AYOHIQLKSOJJQH-UHFFFAOYSA-N 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
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- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
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- 231100000331 toxic Toxicity 0.000 description 2
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- YEYKMVJDLWJFOA-UHFFFAOYSA-N 2-propoxyethanol Chemical compound CCCOCCO YEYKMVJDLWJFOA-UHFFFAOYSA-N 0.000 description 1
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- 229920005830 Polyurethane Foam Polymers 0.000 description 1
- WUGQZFFCHPXWKQ-UHFFFAOYSA-N Propanolamine Chemical compound NCCCO WUGQZFFCHPXWKQ-UHFFFAOYSA-N 0.000 description 1
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- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 description 1
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Landscapes
- Adhesives Or Adhesive Processes (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
本发明属于化工的技术领域,公开了一种电解门填充用聚氨酯蜂窝胶及其制备方法。所述聚氨酯蜂窝胶,由以下按重量份数计的组分制备而成:自制聚氨酯预聚体80~100,发泡剂150~180,泡沫稳定剂2~5,增粘树脂35~40以及活性填料50~80。本发明所制备的聚氨酯蜂窝胶环保,无毒无污染、性能好、泡沫细腻均匀、成本低、固化速度合理;并且本发明的制备方法简单,易于实现,可应用于电解门领域。The invention belongs to the technical field of chemical industry, and discloses a polyurethane cellular glue for filling an electrolytic door and a preparation method thereof. The polyurethane cellular glue is prepared from the following components in parts by weight: self-made polyurethane prepolymer 80-100, foaming agent 150-180, foam stabilizer 2-5, tackifying resin 35-40 and Active filler 50-80. The polyurethane cellular glue prepared by the invention is environmentally friendly, non-toxic and pollution-free, has good performance, fine and uniform foam, low cost, and reasonable curing speed; and the preparation method of the invention is simple and easy to implement, and can be applied to the field of electrolysis doors.
Description
技术领域technical field
本发明属于化工的技术领域,具体涉及一种电解门填充用聚氨酯蜂窝胶及其制备方法。The invention belongs to the technical field of chemical industry, and in particular relates to a polyurethane cellular glue for filling an electrolytic door and a preparation method thereof.
背景技术Background technique
电解门技术是一种新型的室内门制备技术,电解门主材采用电解板,内填充聚合物,其具有美观大方、防腐蚀、抗变形、耐用等特点。作为电解门的填充物应具有耐压和粘结力强等特点。但是在现有的技术中,填充物一般含有挥发性有毒有污染的物质,并且其力学性能较差。目前电解门内置填充物主要采用聚氨酯发泡蜂窝胶。Electrolytic door technology is a new type of indoor door preparation technology. The main material of electrolytic door is electrolytic plate, which is filled with polymer. It has the characteristics of beautiful appearance, corrosion resistance, deformation resistance and durability. The filler used as the electrolytic door should have the characteristics of pressure resistance and strong adhesion. However, in the prior art, fillers generally contain volatile, toxic and polluting substances, and their mechanical properties are poor. At present, the built-in filling of the electrolytic door mainly adopts polyurethane foamed honeycomb glue.
聚氨酯发泡蜂窝胶具有优良的物理机械性能、声学性能、电学性能和耐化学性能等品质,其市场正在持续增长,特别是在建筑、汽车、轮船、保温材料行业上应用比较广泛。发泡型聚氨酯胶黏剂可水与湿气固化,固化后具有与塑料类似的强度,又具有类橡胶的韧性,同时粘结强度高、耐油、耐水、耐高温、耐冲击、耐震动、电绝缘性好等特点,且容易加工。Polyurethane foamed cellular glue has excellent physical and mechanical properties, acoustic properties, electrical properties, and chemical resistance properties. Its market is growing continuously, especially in construction, automobiles, ships, and thermal insulation materials. Foamed polyurethane adhesive can be cured by water and moisture. After curing, it has the strength similar to that of plastic and has rubber-like toughness. At the same time, it has high bonding strength, oil resistance, water resistance, high temperature resistance, impact resistance, vibration resistance, electrical Good insulation and other characteristics, and easy processing.
常用于聚氨酯发泡胶的二异氰酸酯有脂肪酸与芳香族类型。但是脂肪酸型二异氰酸酯改善胶黏剂内聚强度并不是很明显。芳香族二氰酸酯虽然能够显著改善内聚强度,但是一般常用的芳香型二异氰酸酯如甲苯二异氰酸酯、二苯基甲烷二异氰酸酯有不同程度的不足。甲苯二异氰酸酯具有蒸汽压大、易挥发特点,故其危害性大。二苯基甲烷二异氰酸酯有较前者毒性小、反应速度快等优势,但是纯净物在常温下一般为固体使用不便,此外其活性高容易形成二聚体产生凝胶。Diisocyanates commonly used in polyurethane foams are fatty acid and aromatic types. However, the improvement of the cohesive strength of the adhesive by fatty acid diisocyanate is not obvious. Although aromatic dicyanate can significantly improve cohesive strength, commonly used aromatic diisocyanate such as toluene diisocyanate and diphenylmethane diisocyanate have deficiencies in varying degrees. Toluene diisocyanate has the characteristics of high vapor pressure and easy volatility, so it is very harmful. Diphenylmethane diisocyanate has the advantages of less toxicity and faster reaction than the former, but the pure product is generally solid at room temperature and inconvenient to use. In addition, its high activity easily forms dimers to produce gels.
公开号为CN 102295910A的中国专利公开了一种高强度聚氨酯蜂窝胶及其制备方法,该方法制备出的聚氨酯蜂窝胶粘度稳定,但是该报道的聚氨酯发泡蜂窝胶主要采用甲苯二异氰酸酯与自制聚醚多元醇合成的预聚体为基料。甲苯二异氰酸酯挥发性强、毒性强的特点,因此该聚氨酯蜂窝胶环保性能有待改善。此外自制聚醚多元醇工艺复杂和应用性能有待提高等缺陷。The Chinese patent with the publication number CN 102295910A discloses a high-strength polyurethane cellular adhesive and a preparation method thereof. The polyurethane cellular adhesive prepared by the method has a stable viscosity, but the reported polyurethane foaming cellular adhesive mainly uses toluene diisocyanate and self-made The prepolymer synthesized by polyether polyol is used as the base material. Toluene diisocyanate is highly volatile and toxic, so the environmental performance of the polyurethane cellular adhesive needs to be improved. In addition, the self-made polyether polyol has disadvantages such as complex process and application performance to be improved.
发明内容Contents of the invention
为了克服现有技术的缺点和不足,本发明的首要目的在于提供一种电解门填充用聚氨酯蜂窝胶。本发明的聚氨酯蜂窝胶环保性能高,无毒无污染、黏结强度高、泡沫细腻均匀、成本低、固化速度合理;克服了现有产品的环保性能差,粘结强度不高、固化速度过快等缺陷,满足了日益增长的环保要求与技术提高的电解门行业应用要求。In order to overcome the shortcomings and deficiencies of the prior art, the primary purpose of the present invention is to provide a polyurethane cellular glue for electrolytic door filling. The polyurethane honeycomb glue of the present invention has high environmental protection performance, non-toxic and pollution-free, high bonding strength, fine and uniform foam, low cost, and reasonable curing speed; it overcomes the poor environmental protection performance of existing products, low bonding strength and too fast curing speed And other defects, to meet the growing environmental protection requirements and technical improvement of the electrolytic door industry application requirements.
本发明的另一目的在于提供上述电解门填充用聚氨酯蜂窝胶的制备方法。Another object of the present invention is to provide a preparation method of the above-mentioned polyurethane cellular glue for filling the electrolytic door.
本发明的目的通过以下技术方案实现:The object of the present invention is achieved through the following technical solutions:
一种电解门填充用聚氨酯蜂窝胶,由以下按重量份数计的组分制备而成:A polyurethane cellular glue for electrolytic door filling, prepared from the following components in parts by weight:
所述自制聚氨酯预聚体通过以下方法制备得到:The self-made polyurethane prepolymer is prepared by the following method:
在氮气氛围中,于65~75℃,将聚醚多元醇滴入含有催化剂的多苯基多亚甲基多异氰酸酯溶液中,滴加完毕,继续反应2.5~3.5h,得到自制聚氨酯预聚体。In a nitrogen atmosphere, drop polyether polyol into polyphenyl polymethylene polyisocyanate solution containing catalyst at 65-75°C, after the addition is complete, continue to react for 2.5-3.5 hours to obtain self-made polyurethane prepolymer .
所述聚醚多元醇与多苯基多亚甲基多异氰酸酯的重量比为(30~60):(15~30);所述多苯基多亚甲基多异氰酸酯溶液是多苯基多亚甲基多异氰酸酯溶于有机溶剂制备得到,多苯基多亚甲基多异氰酸酯与有机溶剂的重量比为(15~30):(15~40)。所述滴加速度为20~30滴/min。The weight ratio of the polyether polyol to the polyphenyl polymethylene polyisocyanate is (30-60): (15-30); the polyphenyl polymethylene polyisocyanate solution is polyphenyl polymethylene polyisocyanate The methyl polyisocyanate is prepared by dissolving the organic solvent, and the weight ratio of the polyphenyl polymethylene polyisocyanate to the organic solvent is (15-30):(15-40). The dropping rate is 20-30 drops/min.
所述聚醚多元醇为羟值为37~61mgKOH/g聚氧化乙烯二醇或者羟值为42~112mgKOH/g三羟甲基丙烷-氧化丙烯聚醚的一种;所述聚醚多元醇使用前加热到120~140℃,保温反应60~80min。The polyether polyol is a kind of polyoxyethylene diol with a hydroxyl value of 37-61 mgKOH/g or a trimethylolpropane-propylene oxide polyether with a hydroxyl value of 42-112 mgKOH/g; the polyether polyol uses Pre-heat to 120-140°C and keep warm for 60-80 minutes.
所述多苯基多亚甲基多异氰酸酯中NCO质量分数为30~33%。The mass fraction of NCO in the polyphenyl polymethylene polyisocyanate is 30-33%.
所述催化剂为三亚乙基二胺、双(二甲基胺基乙基)醚、二甲基环己胺、二甲基乙醇胺、N,N-双(二亚氨基丙基)异丙醇胺、N-乙基吗啉、二月桂酸二丁基锡或辛酸亚锡中的一种以上。所述催化剂与多苯基多亚甲基多异氰酸酯的重量比为(0.03~0.07):(15~30)。The catalyst is triethylenediamine, bis(dimethylaminoethyl)ether, dimethylcyclohexylamine, dimethylethanolamine, N,N-bis(diiminopropyl)isopropanolamine , N-ethylmorpholine, dibutyltin dilaurate or stannous octoate. The weight ratio of the catalyst to the polyphenyl polymethylene polyisocyanate is (0.03-0.07): (15-30).
所述有机溶剂为乙酸乙酯、乙酸丙酯、甲乙酮、甲基异丙基酮、乙二醇单乙醚、乙二醇单丙醚、甲苯或二甲苯的一种以上。The organic solvent is one or more of ethyl acetate, propyl acetate, methyl ethyl ketone, methyl isopropyl ketone, ethylene glycol monoethyl ether, ethylene glycol monopropyl ether, toluene or xylene.
所述泡沫稳定剂为稳定剂B8404、B8863Z、B8454、Silbk 9000、Silbk 9020或Silbk9204的一种。The foam stabilizer is one of stabilizer B8404, B8863Z, B8454, Silbk 9000, Silbk 9020 or Silbk9204.
所述发泡剂为环戊烷、正戊烷、异戊烷、异丁烷、正丁烷或二氯甲烷的一种以上。The foaming agent is one or more of cyclopentane, n-pentane, isopentane, isobutane, n-butane or dichloromethane.
所述增粘树脂为石油树脂、萜烯树脂、古马隆树脂、松香树脂的一种;所述石油树脂为C5树脂或C9树脂中一种或两种。The tackifying resin is one of petroleum resin, terpene resin, coumarone resin and rosin resin; the petroleum resin is one or both of C5 resin or C9 resin.
所述活性填料为工业轻质325目碳酸钙、工业1000目高岭土、工业2000目硅灰石粉、工业350目细滑石粉、工业400目白云母、工业1000目钛白粉、工业400目重晶石粉或工业1000目炭黑的一种以上。The active filler is industrial light 325 mesh calcium carbonate, industrial 1000 mesh kaolin, industrial 2000 mesh wollastonite powder, industrial 350 mesh fine talcum powder, industrial 400 mesh muscovite, industrial 1000 mesh titanium dioxide, industrial 400 mesh barite powder or One or more types of industrial 1000 mesh carbon black.
所述电解门填充用聚氨酯蜂窝胶的制备方法,具体包括以下步骤:The preparation method of the polyurethane cellular glue for filling the electrolysis door specifically comprises the following steps:
(1)在氮气的氛围下,于65~75℃,将泡沫稳定剂和增粘树脂加入自制聚氨酯预聚体中,搅拌1~2h,得到分散均匀的体系;(1) Add the foam stabilizer and tackifying resin to the self-made polyurethane prepolymer at 65-75°C under a nitrogen atmosphere, and stir for 1-2 hours to obtain a uniformly dispersed system;
(2)将步骤(1)中的体系降温至30~40℃,加入发泡剂与活性填料,继续搅拌30~40min,得到聚氨酯蜂窝胶。(2) Lower the temperature of the system in step (1) to 30-40°C, add foaming agent and active filler, and continue stirring for 30-40 minutes to obtain polyurethane cellular adhesive.
步骤(1)中所述搅拌的转速为300~500r/min;步骤(2)中所述搅拌的转速为400~600r/min。The rotational speed of stirring in step (1) is 300-500 r/min; the rotational speed of stirring in step (2) is 400-600 r/min.
所制备的聚氨酯蜂窝胶固含为70%~80%,粘度3000~4000mPa·s,铝板粘结强度1.5~2.0Mpa,剪切强度0.8~1.0Mpa,断裂伸长率60~80%,发泡倍率12~15,燃烧等级B2级,表干固化时间120~150min。The prepared polyurethane honeycomb glue has a solid content of 70% to 80%, a viscosity of 3000 to 4000mPa·s, an aluminum plate bond strength of 1.5 to 2.0Mpa, a shear strength of 0.8 to 1.0Mpa, and an elongation at break of 60 to 80%. The magnification is 12~15, the combustion level is B2, and the surface dry curing time is 120~150min.
本发明采用多苯基多亚甲基多异氰酸酯,是二苯基甲烷二异氰酸酯多聚体,活性与蒸汽压,比二苯基甲烷二异氰酸酯低,价格较其便宜。在相同质量下,多苯基多亚甲基多异氰酸酯具有更多的异氰酸酯根基团,在固化时与空气中的水反应生成更多的聚氨酯-脲键,其自身多异氰酸根能够起类似于自交联作用,故发泡胶形成分子量非常大的聚合物。聚合物中大量聚氨酯-脲键具有非常强的极性,宏观表现在与金属表面有非常强的粘结力。此外异氰酸酯基团含量高,固化速度快,与水产生的二氧化碳未扩散出就被固化在胶体层中,故本发明的发泡胶具有边固化边发泡、泡沫非常细腻均匀特点。The invention adopts polyphenyl polymethylene polyisocyanate, which is diphenylmethane diisocyanate multimer, has lower activity and vapor pressure than diphenylmethane diisocyanate, and is cheaper than it. Under the same mass, polyphenyl polymethylene polyisocyanate has more isocyanate groups, and reacts with water in the air to form more polyurethane-urea bonds during curing, and its own polyisocyanate can act similar to Self-crosslinking, so the styrofoam forms polymers with very large molecular weights. A large number of polyurethane-urea bonds in the polymer have very strong polarity, which is manifested in a very strong bond with the metal surface macroscopically. In addition, the content of isocyanate groups is high, the curing speed is fast, and the carbon dioxide produced with water is cured in the colloidal layer without diffusing out, so the foaming adhesive of the present invention has the characteristics of foaming while curing, and the foam is very fine and uniform.
与现有技术相比,本发明具有如下优点:Compared with prior art, the present invention has following advantage:
本发明的聚氨酯蜂窝胶性能较高,环保,无毒无污染、黏结强度高、泡沫细腻均匀、成本低、固化速度合理;本发明的制备方法简单,易于实现;该环保填充用聚氨酯蜂窝胶固含为70%~80%,粘度3000~4000mPa·s,铝板粘结强度1.5~2.0Mpa,剪切强度0.8~1.0Mpa,断裂伸长率60~80%,发泡倍率12~15,燃烧等级B2级,表干固化时间120~150min。The polyurethane cellular adhesive of the present invention has high performance, environmental protection, non-toxicity and pollution-free, high bonding strength, fine and uniform foam, low cost, and reasonable curing speed; the preparation method of the present invention is simple and easy to realize; the polyurethane cellular adhesive for environmental protection filling is solid The content is 70%~80%, the viscosity is 3000~4000mPa s, the bond strength of aluminum plate is 1.5~2.0Mpa, the shear strength is 0.8~1.0Mpa, the elongation at break is 60~80%, the expansion ratio is 12~15, and the combustion grade B2 level, surface dry curing time 120 ~ 150min.
具体实施方式detailed description
为更好地理解本发明,下面结合实施例对本发明作进一步的说明,但本发明的实施方式不限于此。In order to better understand the present invention, the present invention will be further described below in conjunction with examples, but the embodiments of the present invention are not limited thereto.
实施例1Example 1
一种电解门填充用聚氨酯蜂窝胶,通过以下方法制备得到:A kind of polyurethane cellular glue for electrolytic door filling, prepared by the following method:
(1)将50重量份羟值为37的聚氧化乙烯二醇加热到120℃,保温反应80min,使聚醚中的水分充分除去,得到去水的聚醚二元醇;(1) Heat 50 parts by weight of polyoxyethylene diol with a hydroxyl value of 37 to 120° C., heat-preserve and react for 80 minutes, fully remove the moisture in the polyether, and obtain dehydrated polyether diol;
(2)将20重量份的NCO质量分数为30%的多苯基多亚甲基多异氰酸酯和30重量份的乙酸乙酯搅拌均匀,加入0.05重量份三亚乙基二胺,得到含催化剂的多苯基多亚甲基多异氰酸酯溶液;(2) The NCO mass fraction of 20 parts by weight is 30% polyphenyl polymethylene polyisocyanate and the ethyl acetate of 30 parts by weight are stirred evenly, add 0.05 parts by weight of triethylenediamine, obtain the polyphenyl polymethylene polyisocyanate containing catalyst Phenyl polymethylene polyisocyanate solution;
(3)将步骤(2)的所有含催化剂的多苯基多亚甲基多异氰酸酯溶液升温至75℃,在氮气氛围下,将步骤(1)的所有聚醚二元醇滴入(滴加的速度请为20滴/min)到异氰酸酯溶液中,滴加完后,继续反应3.5h,得到自制的聚氨酯预聚体;(3) All the polyphenyl polymethylene polyisocyanate solutions containing the catalyst in step (2) are warmed up to 75°C, and under a nitrogen atmosphere, all the polyether diols in step (1) are dropped into (dropped The speed should be 20 drops/min) into the isocyanate solution. After the dropwise addition, continue to react for 3.5 hours to obtain a self-made polyurethane prepolymer;
(4)在氮气氛围以及75℃下,将2重量份稳定剂B8404的和35重量份松香树脂加入80重量份步骤(3)自制的聚氨酯预聚体中,搅拌2h(搅拌的转速为300r/min),得到分散均匀的体系;(4) In a nitrogen atmosphere and at 75°C, add 2 parts by weight of stabilizer B8404 and 35 parts by weight of rosin resin to 80 parts by weight of step (3) in the self-made polyurethane prepolymer, stir for 2h (the rotating speed of stirring is 300r/ min), to obtain a uniformly dispersed system;
(5)将步骤(4)的体系降温至30℃,加入100重量份的二氯甲烷、50重量份的环戊烷和50重量份的工业轻质325目碳酸钙,搅拌30min(转速为530r/min),得到聚氨酯蜂窝胶。(5) the system of step (4) is cooled to 30 DEG C, add the dichloromethane of 100 weight parts, the cyclopentane of 50 weight parts and the industrial light 325 order calcium carbonate of 50 weight parts, stir 30min (rotating speed is 530rr /min), to obtain polyurethane cellular glue.
所述聚氨酯蜂窝胶粘度3150mPa·s,铝板粘结强度1.5Mpa,剪切强度1.0Mpa,发泡倍率12,燃烧等级B2级,表干固化时间120min。The polyurethane honeycomb adhesive has a viscosity of 3150 mPa·s, an aluminum plate bonding strength of 1.5 Mpa, a shear strength of 1.0 Mpa, a foaming ratio of 12, a combustion grade of B2, and a curing time of 120 minutes.
实施列2Implementation column 2
一种电解门填充用聚氨酯蜂窝胶,通过以下方法制备得到:A kind of polyurethane cellular glue for electrolytic door filling, prepared by the following method:
(1)将60重量份羟值为56聚氧化乙烯二醇加热到140℃,保温反应60min,使聚醚中的水分充分除去,得到去水的聚醚二元醇;(1) heating 60 parts by weight of polyoxyethylene diol with a hydroxyl value of 56 to 140° C., and keeping it warm for 60 minutes to fully remove the moisture in the polyether to obtain dehydrated polyether diol;
(2)将25重量份的NCO质量分数为30%的多苯基多亚甲基多异氰酸酯和15重量份的甲苯搅拌均匀,加入0.03重量份双(二甲基胺基乙基)醚和0.01重量份三亚乙基二胺,得到含催化剂的多苯基多亚甲基多异氰酸酯溶液;(2) 25 parts by weight of NCO mass fraction are 30% polyphenyl polymethylene polyisocyanate and 15 parts by weight of toluene are stirred evenly, add 0.03 parts by weight of bis(dimethylaminoethyl) ether and 0.01 parts by weight parts by weight of triethylenediamine to obtain a catalyst-containing polyphenyl polymethylene polyisocyanate solution;
(3)将步骤(2)的所有含催化剂的多苯基多亚甲基多异氰酸酯溶液升温至70℃,在氮气氛围中将步骤(1)中的聚醚二元醇滴入到异氰酸酯溶液中(滴加的速度为30滴/min),滴加完后,继续反应2.5h,得到自制的聚氨酯预聚体;(3) All the catalyst-containing polyphenyl polymethylene polyisocyanate solutions in step (2) are heated to 70°C, and the polyether diol in step (1) is dropped into the isocyanate solution in a nitrogen atmosphere (the speed of dropping is 30 drops/min), after dropping, continue reaction 2.5h, obtain self-made polyurethane prepolymer;
(4)在氮气氛围以及70℃下,将5重量份稳定剂B8863Z和40重量份石油树脂加入100重量份步骤(3)的自制的聚氨酯预聚体中,搅拌2h(搅拌的转速为500r/min),得到分散均匀的体系;(4) under nitrogen atmosphere and 70 DEG C, add 5 parts by weight of stabilizer B8863Z and 40 parts by weight of petroleum resin in the self-made polyurethane prepolymer of 100 parts by weight of step (3), stir for 2h (the rotating speed of stirring is 500r/ min), to obtain a uniformly dispersed system;
(5)将步骤(4)的体系降温至30℃,加入180重量份的环戊烷和40重量份的工业1000目高岭土和40重量份工业2000目硅灰石粉,搅拌30min(转速为560r/min),得到环保聚氨酯蜂窝胶。(5) The system of step (4) is cooled to 30 DEG C, add the cyclopentane of 180 weight parts and the industrial 1000 order kaolin of 40 weight parts and the industrial 2000 order wollastonite powder of 40 weight parts, stir 30min (rotating speed is 560r/ min), to obtain environmentally friendly polyurethane cellular glue.
该环保填充用聚氨酯蜂窝胶粘度3060mPa·s,铝板粘结强度1.6Mpa,剪切强度0.8Mpa,发泡倍率15,燃烧等级B2级,表干固化时间150min。The polyurethane honeycomb adhesive for environmental protection filling has a viscosity of 3060mPa·s, an aluminum plate bonding strength of 1.6Mpa, a shear strength of 0.8Mpa, a foaming ratio of 15, a combustion grade of B2, and a surface-dry curing time of 150min.
实施列3Implementation column 3
一种电解门填充用聚氨酯蜂窝胶,通过以下方法制备得到:A kind of polyurethane cellular glue for electrolytic door filling, prepared by the following method:
(1)将40重量份羟值为61的聚氧化乙烯二醇加热到120℃,保温反应80min,使聚醚中的水分充分除去,得到去水的聚醚二元醇;(1) Heat 40 parts by weight of polyoxyethylene diol with a hydroxyl value of 61 to 120° C., heat-preserve and react for 80 minutes, fully remove the moisture in the polyether, and obtain dehydrated polyether diol;
(2)将25重量份的NCO质量分数为30%的多苯基多亚甲基多异氰酸酯和15重量份的二甲苯搅拌均匀,加入0.03重量份二甲基环己胺和0.03重量份二月桂酸二丁基锡,得到含催化剂的多苯基多亚甲基多异氰酸酯溶液;(2) 25 parts by weight of NCO mass fraction are 30% polyphenyl polymethylene polyisocyanate and 15 parts by weight of xylene are stirred evenly, add 0.03 parts by weight of dimethylcyclohexylamine and 0.03 parts by weight of dilauric acid Acid dibutyltin, obtain the polyphenyl polymethylene polyisocyanate solution containing catalyst;
(3)将步骤(2)的所有含催化剂的多苯基多亚甲基多异氰酸酯溶液升温至65℃,在氮气氛围下,将步骤(1)中的聚醚二元醇滴入到异氰酸酯溶液中(滴加的速度为25滴/min),滴加完后,继续反应2.5h,得到自制的聚氨酯预聚体;(3) Warm up all the catalyst-containing polyphenyl polymethylene polyisocyanate solutions in step (2) to 65°C, and drop the polyether diol in step (1) into the isocyanate solution under nitrogen atmosphere (the speed of dropping is 25 drops/min), after dropwise addition, continue reaction 2.5h, obtain self-made polyurethane prepolymer;
(4)在氮气氛围以及65℃下,将5重量份稳定剂B8454和35重量份萜烯树脂加入90重量份步骤(3)的自制的聚氨酯预聚体中,搅拌1h(搅拌的转速为400r/min),得到分散均匀的体系;(4) In a nitrogen atmosphere and at 65°C, add 5 parts by weight of stabilizer B8454 and 35 parts by weight of terpene resin to the self-made polyurethane prepolymer of 90 parts by weight of step (3), stir for 1h (the rotating speed of stirring is 400r /min), to obtain a uniformly dispersed system;
(5)将步骤(4)的体系降温至35℃,加入160重量份的正丁烷和60重量份的工业400目重晶石粉,搅拌35min(搅拌的转速为480r/min),得到环保聚氨酯蜂窝胶。(5) Cool the system in step (4) to 35°C, add 160 parts by weight of n-butane and 60 parts by weight of industrial 400-mesh barite powder, stir for 35 minutes (the rotating speed of stirring is 480r/min), and obtain environmentally friendly polyurethane Honeycomb glue.
该环保填充用聚氨酯蜂窝胶粘度3258mPa·s,铝板粘结强度2.0Mpa,剪切强度1.0Mpa,发泡倍率13,燃烧等级B2级,表干固化时间135min。The polyurethane honeycomb adhesive for environmental protection filling has a viscosity of 3258mPa·s, an aluminum plate bonding strength of 2.0Mpa, a shear strength of 1.0Mpa, a foaming ratio of 13, a combustion grade of B2, and a surface-dry curing time of 135min.
实施列4Implementation column 4
一种电解门填充用聚氨酯蜂窝胶,通过以下方法制备得到:A kind of polyurethane cellular glue for electrolytic door filling, prepared by the following method:
(1)将50重量份羟值为42三羟甲基丙烷-氧化丙烯聚醚加热到140℃,保温反应80min,使聚醚中的水分充分除去,得到去水的聚醚二元醇;(1) Heating 50 parts by weight of trimethylolpropane-propylene oxide polyether with a hydroxyl value of 42 to 140° C., and keeping it warm for 80 minutes to fully remove the moisture in the polyether to obtain dehydrated polyether glycol;
(2)将15重量份的NCO质量分数为30%的多苯基多亚甲基多异氰酸酯和35重量份的乙酸丙酯搅拌均匀,加入0.07重量份二甲基乙醇胺,得到含催化剂的多苯基多亚甲基多异氰酸酯溶液;(2) The NCO mass fraction of 15 parts by weight is the polyphenyl polymethylene polyisocyanate of 30% and the propyl acetate of 35 parts by weight are stirred evenly, add 0.07 parts by weight of dimethylethanolamine, obtain the polyphenyl polyphenyl polyphenylene polyisocyanate containing catalyst Polymethylene polyisocyanate solution;
(3)将步骤(2)的所有含催化剂的多苯基多亚甲基多异氰酸酯溶液升温至70℃,在氮气氛围下,将步骤(1)中的聚醚三元醇滴入到异氰酸酯溶液中(滴加的速度为23滴/min),继续反应3h,得到自制的聚氨酯预聚体;(3) Warm up all the catalyst-containing polyphenyl polymethylene polyisocyanate solutions in step (2) to 70°C, and drop the polyether triol in step (1) into the isocyanate solution under a nitrogen atmosphere (the speed of dropping is 23 drops/min), continue to react 3h, obtain self-made polyurethane prepolymer;
(4)在氮气氛围以及70℃下,加入5重量份稳定剂Silbk 9000和40重量份古马隆树脂加入95重量份步骤(3)的自制的聚氨酯预聚体中,搅拌1.5h(搅拌的转速为350r/min),得到分散均匀的体系;(4) under nitrogen atmosphere and 70 ℃, add 5 parts by weight of stabilizer Silbk 9000 and 40 parts by weight of coumarone resin and add in the self-made polyurethane prepolymer of 95 parts by weight of step (3), stir for 1.5h (stirred Rotating speed is 350r/min), obtains the uniformly dispersed system;
(5)对步骤(4)的体系降温至40℃,加入170重量份的异丁烷和70重量份的工业400目白云母,搅拌38min(搅拌的转速为550r/min),得到环保聚氨酯蜂窝胶。(5) Cool the system of step (4) to 40°C, add 170 parts by weight of isobutane and 70 parts by weight of industrial 400 mesh muscovite, stir for 38min (the rotating speed of stirring is 550r/min), and obtain an environmentally friendly polyurethane cellular glue .
该环保填充用聚氨酯蜂窝胶粘度3368mPa·s,铝板粘结强度1.7Mpa,剪切强度0.9Mpa,发泡倍率12,燃烧等级B2级,表干固化时间125min。The polyurethane honeycomb adhesive for environmental protection filling has a viscosity of 3368mPa·s, an aluminum plate bonding strength of 1.7Mpa, a shear strength of 0.9Mpa, a foaming ratio of 12, a combustion grade of B2, and a surface-dry curing time of 125min.
实施列5Implementation column 5
一种电解门填充用聚氨酯蜂窝胶,通过以下方法制备得到:A kind of polyurethane cellular glue for electrolytic door filling, prepared by the following method:
(1)将55重量份羟值为67三羟甲基丙烷-氧化丙烯聚醚加热到130℃,保温反应70min,使聚醚中的水分充分除去,得到去水的聚醚二元醇;(1) Heating 55 parts by weight of trimethylolpropane-propylene oxide polyether with a hydroxyl value of 67 to 130° C., keeping the temperature for 70 minutes, and fully removing the moisture in the polyether to obtain dehydrated polyether glycol;
(2)将25重量份的NCO质量分数为33%的多苯基多亚甲基多异氰酸酯和20重量份的甲乙酮搅拌均匀,加入0.03重量份N,N-双(二亚氨基丙基)异丙醇胺,得到含催化剂的多苯基多亚甲基多异氰酸酯溶液;(2) Stir 25 parts by weight of polyphenyl polymethylene polyisocyanate with a mass fraction of NCO of 33% and 20 parts by weight of methyl ethyl ketone evenly, add 0.03 parts by weight of N,N-bis(diiminopropyl) isocyanate Propanolamine, obtains the polyphenyl polymethylene polyisocyanate solution containing catalyst;
(3)将步骤(2)的所有含催化剂的多苯基多亚甲基多异氰酸酯溶液升温至75℃,在氮气氛围下,将步骤(1)中的聚醚二醇滴入到异氰酸酯溶液中(滴加的速度为26滴/min),滴加完,继续反应2.5h,得到自制的聚氨酯预聚体;(3) Warm up all the catalyst-containing polyphenyl polymethylene polyisocyanate solutions in step (2) to 75°C, and drop the polyether diol in step (1) into the isocyanate solution under nitrogen atmosphere (the speed of dropping is 26 drops/min), after dropping, continue to react for 2.5h, obtain the self-made polyurethane prepolymer;
(4)在氮气氛围以及75℃下,将2重量份稳定剂Silbk 9020和37重量份古马隆树脂加入85重量份步骤(3)的自制的聚氨酯预聚体中,搅拌2h(搅拌的转速为450r/min),得到分散均匀的体系;(4) under nitrogen atmosphere and 75 DEG C, add 2 parts by weight of stabilizer Silbk 9020 and 37 parts by weight of coumarone resin in the self-made polyurethane prepolymer of 85 parts by weight of step (3), stir for 2h (stirring speed 450r/min), to obtain a uniformly dispersed system;
(5)将步骤(4)的体系降温至37℃,加入175重量份的正戊烷和60重量份的工业400目重晶石粉,搅拌35min(搅拌的转速为450r/min),,得到环保聚氨酯蜂窝胶。(5) Cool the system in step (4) to 37°C, add 175 parts by weight of n-pentane and 60 parts by weight of industrial 400 mesh barite powder, stir for 35 minutes (the rotating speed of stirring is 450r/min), and obtain an environmentally friendly Polyurethane cellular glue.
该环保填充用聚氨酯蜂窝胶粘度3391mPa·s,铝板粘结强度1.8Mpa,剪切强度0.9Mpa,发泡倍率15,燃烧等级B2级,表干固化时间130min。The polyurethane honeycomb adhesive for environmental protection filling has a viscosity of 3391mPa·s, an aluminum plate bond strength of 1.8Mpa, a shear strength of 0.9Mpa, a foaming ratio of 15, a combustion grade of B2, and a surface-dry curing time of 130min.
实施列6Implementation column 6
一种电解门填充用聚氨酯蜂窝胶,通过以下方法制备得到:A kind of polyurethane cellular glue for electrolytic door filling, prepared by the following method:
(1)将40重量份羟值为112三羟甲基丙烷-氧化丙烯聚醚加热到130℃,保温反应75min,使聚醚中的水分充分除去,得到去水的聚醚二元醇;(1) Heating 40 parts by weight of trimethylolpropane-propylene oxide polyether with a hydroxyl value of 112 to 130° C., keeping the temperature for 75 minutes, and fully removing the moisture in the polyether to obtain a dehydrated polyether glycol;
(2)将30重量份的NCO质量分数为32%的多苯基多亚甲基多异氰酸酯和25重量份的甲基异丙基酮搅拌均匀,加入0.05重量份N-乙基吗啉,得到含催化剂的多苯基多亚甲基多异氰酸酯溶液;(2) The NCO mass fraction of 30 parts by weight is 32% polyphenyl polymethylene polyisocyanate and the methyl isopropyl ketone of 25 parts by weight are stirred evenly, add 0.05 parts by weight of N-ethylmorpholine, obtain Catalyst-containing polyphenylpolymethylene polyisocyanate solution;
(3)将步骤(2)的所有含催化剂的多苯基多亚甲基多异氰酸酯溶液升温至67℃,在氮气氛围下,将步骤(1)中的聚醚三元醇滴入到异氰酸酯溶液中(滴加的速度为27滴/min),滴加完后,继续反应3h,得到自制的聚氨酯预聚体;(3) Warm up all the catalyst-containing polyphenyl polymethylene polyisocyanate solutions in step (2) to 67°C, and drop the polyether triol in step (1) into the isocyanate solution under a nitrogen atmosphere (the speed of dropping is 27 drops/min), after dropping, continue reaction 3h, obtain self-made polyurethane prepolymer;
(4)在氮气氛围以及67℃下,加入5重量份稳定剂Silbk 9204和40重量份松香树脂加入80重量份步骤(3)的自制的聚氨酯预聚体中,搅拌1.5h(搅拌的转速为480r/min),得到分散均匀的体系;(4) under nitrogen atmosphere and 67 ℃, add 5 parts by weight of stabilizer Silbk 9204 and 40 parts by weight of rosin resin and add in the self-made polyurethane prepolymer of 80 parts by weight of step (3), stir 1.5h (the rotating speed of stirring is 480r/min), to obtain a uniformly dispersed system;
(5)步骤(4)的体系降温至35℃,加入180重量份的二氯甲烷和50重量份的工业1000目炭黑,搅拌40min(转速为500r/min),得到环保聚氨酯蜂窝胶。(5) The system in step (4) was cooled to 35° C., 180 parts by weight of methylene chloride and 50 parts by weight of industrial 1000 mesh carbon black were added, and stirred for 40 minutes (rotating speed was 500 r/min) to obtain an environmentally friendly polyurethane cellular glue.
该环保填充用聚氨酯蜂窝胶粘度3658mPa·s,铝板粘结强度1.5Mpa,剪切强度0.9Mpa,发泡倍率15,燃烧等级B2级,表干固化时间120min。The polyurethane honeycomb adhesive for environmental protection filling has a viscosity of 3658mPa·s, an aluminum plate bonding strength of 1.5Mpa, a shear strength of 0.9Mpa, a foaming ratio of 15, a combustion grade of B2, and a surface-dry curing time of 120min.
实施列7Implementation column 7
一种电解门填充用聚氨酯蜂窝胶,通过以下方法制备得到:A kind of polyurethane cellular glue for electrolytic door filling, prepared by the following method:
(1)将30重量份羟值为112三羟甲基丙烷-氧化丙烯聚醚加热到140℃,保温反应60min,使聚醚中的水分充分除去,得到去水的聚醚二元醇;(1) heating 30 parts by weight of trimethylolpropane-propylene oxide polyether with a hydroxyl value of 112 to 140° C., and keeping it warm for 60 minutes to fully remove the moisture in the polyether to obtain a dehydrated polyether glycol;
(2)将24重量份的NCO质量分数为31%的多苯基多亚甲基多异氰酸酯、30重量份的乙二醇单乙醚与10重量份二甲苯搅拌均匀,加入0.03重量份二月桂酸二丁基锡,得到含催化剂的多苯基多亚甲基多异氰酸酯溶液;(2) 24 parts by weight of NCO mass fraction is 31% polyphenyl polymethylene polyisocyanate, 30 parts by weight of ethylene glycol monoethyl ether and 10 parts by weight of xylene are stirred evenly, add 0.03 parts by weight of dilauric acid Dibutyltin, obtains the polyphenyl polymethylene polyisocyanate solution containing catalyst;
(3)将步骤(2)的所有含催化剂的多苯基多亚甲基多异氰酸酯溶液升温至72℃,在氮气氛围下,将步骤(1)中的聚醚二醇滴入到异氰酸酯溶液中(滴加的速度位28滴/min),滴加完后,继续反应2.5h,得到自制的聚氨酯预聚体;(3) Warm up all the catalyst-containing polyphenyl polymethylene polyisocyanate solutions in step (2) to 72°C, and drop the polyether diol in step (1) into the isocyanate solution under a nitrogen atmosphere (the speed position of dropping is 28 drops/min), after dropping, continue reaction 2.5h, obtain the self-made polyurethane prepolymer;
(4)在氮气氛围以及72℃下,将4重量份稳定剂B8404和40重量份松香树脂加入100重量份步骤(3)的自制的聚氨酯预聚体中,搅拌1h(搅拌的转速为360r/min),得到分散均匀的体系;(4) under nitrogen atmosphere and 72 DEG C, add 4 parts by weight of stabilizer B8404 and 40 parts by weight of rosin resin in the self-made polyurethane prepolymer of 100 parts by weight of step (3), stir for 1h (the rotating speed of stirring is 360r/ min), to obtain a uniformly dispersed system;
(5)对步骤(4)降温至32℃,加入150重量份的异丁烷和50重量份的工业350目细滑石粉,搅拌40min(搅拌的转速为600r/min),得到环保聚氨酯蜂窝胶。(5) Step (4) is cooled to 32°C, adding 150 parts by weight of isobutane and 50 parts by weight of industrial 350-mesh fine talcum powder, stirring for 40 minutes (the rotating speed of stirring is 600r/min), and an environmentally friendly polyurethane cellular glue is obtained .
该环保填充用聚氨酯蜂窝胶粘度3720mPa·s,铝板粘结强度2.0Mpa,剪切强度0.8Mpa,发泡倍率14,燃烧等级B2级,表干固化时间140min。The polyurethane honeycomb adhesive for environmental protection filling has a viscosity of 3720mPa·s, an aluminum plate bonding strength of 2.0Mpa, a shear strength of 0.8Mpa, a foaming ratio of 14, a combustion grade of B2, and a surface-dry curing time of 140min.
实施列8Implementation Column 8
一种电解门填充用聚氨酯蜂窝胶,通过以下方法制备得到:A kind of polyurethane cellular glue for electrolytic door filling, prepared by the following method:
(1)将30重量份羟值为112三羟甲基丙烷-氧化丙烯聚醚加热到140℃,保温反应75min,使聚醚中的水分充分除去,得到去水的聚醚二元醇;(1) heating 30 parts by weight of trimethylolpropane-propylene oxide polyether with a hydroxyl value of 112 to 140° C., and keeping it warm for 75 minutes to fully remove the moisture in the polyether to obtain a dehydrated polyether glycol;
(2)将20重量份的NCO质量分数为31%的多苯基多亚甲基多异氰酸酯、20重量份的乙二醇单乙醚与20重量份乙酸乙酯搅拌均匀,加入0.05重量份辛酸亚锡,得到含催化剂的多苯基多亚甲基多异氰酸酯溶液;(2) The NCO mass fraction of 20 parts by weight is 31% polyphenyl polymethylene polyisocyanate, the ethylene glycol monoethyl ether of 20 parts by weight and 20 parts by weight of ethyl acetate are stirred evenly, add 0.05 parts by weight of octanoic acid ethylene Tin, obtains the polyphenyl polymethylene polyisocyanate solution containing catalyst;
(3)将步骤(2)的所有含催化剂的多苯基多亚甲基多异氰酸酯溶液升温至68℃,在氮气氛围下,将步骤(1)中的聚醚二醇滴入到异氰酸酯溶液中(滴加的速度为22滴/min),滴加完后,继续反应2.5h,得到自制的聚氨酯预聚体;(3) Warm up all the catalyst-containing polyphenyl polymethylene polyisocyanate solutions in step (2) to 68°C, and drop the polyether diol in step (1) into the isocyanate solution under nitrogen atmosphere (the speed of dropping is 22 drops/min), after dropping, continue reaction 2.5h, obtain self-made polyurethane prepolymer;
(4)在氮气氛围以及68℃下,将4重量份稳定剂B8404和40重量份松香树脂加入90重量份步骤(3)的自制的聚氨酯预聚体中,搅拌2h(搅拌的转速为460r/min),得到分散均匀的体系;(4) under nitrogen atmosphere and 68 ℃, add 4 parts by weight of stabilizer B8404 and 40 parts by weight of rosin resin in the self-made polyurethane prepolymer of 90 parts by weight of step (3), stir for 2h (the rotating speed of stirring is 460r/ min), to obtain a uniformly dispersed system;
(5)将步骤(4)降温至33℃,加入150重量份的正丁烷和50重量份的工业1000目钛白粉,搅拌40min(搅拌的转速为400r/min),得到环保聚氨酯蜂窝胶。(5) Step (4) was cooled to 33° C., 150 parts by weight of n-butane and 50 parts by weight of industrial 1000 mesh titanium dioxide were added, and stirred for 40 minutes (the stirring speed was 400 r/min) to obtain an environmentally friendly polyurethane cellular glue.
该环保填充用聚氨酯蜂窝胶粘度3879mPa·s,铝板粘结强度1.6Mpa,剪切强度1.0Mpa,发泡倍率13,燃烧等级B2级,表干固化时间145min。The polyurethane honeycomb adhesive for environmentally friendly filling has a viscosity of 3879mPa·s, an aluminum plate bonding strength of 1.6Mpa, a shear strength of 1.0Mpa, a foaming ratio of 13, a combustion grade of B2, and a surface-dry curing time of 145min.
本发明的上述实施例仅仅是为清楚地说明本发明所作的举例,而并非是对本发明的实施方式的限定。对于所属领域的普通技术人员来说,在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明权利要求的保护范围之内。The above-mentioned embodiments of the present invention are only examples for clearly illustrating the present invention, rather than limiting the implementation of the present invention. For those of ordinary skill in the art, on the basis of the above description, other changes or changes in different forms can also be made. It is not necessary and impossible to exhaustively list all the implementation manners here. All modifications, equivalent replacements and improvements made within the spirit and principles of the present invention shall be included within the protection scope of the claims of the present invention.
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