CN108795208A - The preparation method of extinguishing waterborn hud typed acrylic resin coating and paint - Google Patents
The preparation method of extinguishing waterborn hud typed acrylic resin coating and paint Download PDFInfo
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- CN108795208A CN108795208A CN201810773980.7A CN201810773980A CN108795208A CN 108795208 A CN108795208 A CN 108795208A CN 201810773980 A CN201810773980 A CN 201810773980A CN 108795208 A CN108795208 A CN 108795208A
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- 238000000576 coating method Methods 0.000 title claims abstract description 47
- 239000011248 coating agent Substances 0.000 title claims abstract description 46
- 239000003973 paint Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 43
- 239000004925 Acrylic resin Substances 0.000 title claims abstract description 37
- 229920000178 Acrylic resin Polymers 0.000 title claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000003063 flame retardant Substances 0.000 claims abstract description 39
- 239000000178 monomer Substances 0.000 claims abstract description 36
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 34
- 238000010792 warming Methods 0.000 claims abstract description 31
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 25
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000006210 lotion Substances 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 230000035484 reaction time Effects 0.000 claims abstract description 16
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000011347 resin Substances 0.000 claims abstract description 12
- 229920005989 resin Polymers 0.000 claims abstract description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 8
- 238000004945 emulsification Methods 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 239000011258 core-shell material Substances 0.000 claims abstract description 7
- 239000003999 initiator Substances 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims description 26
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 15
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 15
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 14
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 claims description 14
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 14
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 12
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 12
- 238000002485 combustion reaction Methods 0.000 claims description 10
- LIWAQLJGPBVORC-UHFFFAOYSA-N ethylmethylamine Chemical compound CCNC LIWAQLJGPBVORC-UHFFFAOYSA-N 0.000 claims description 10
- GJAWHXHKYYXBSV-UHFFFAOYSA-N quinolinic acid Chemical class OC(=O)C1=CC=CN=C1C(O)=O GJAWHXHKYYXBSV-UHFFFAOYSA-N 0.000 claims description 9
- CYEJMVLDXAUOPN-UHFFFAOYSA-N 2-dodecylphenol Chemical compound CCCCCCCCCCCCC1=CC=CC=C1O CYEJMVLDXAUOPN-UHFFFAOYSA-N 0.000 claims description 8
- RGDDVTHQUAQTIE-UHFFFAOYSA-N 2-pentadecylphenol Chemical compound CCCCCCCCCCCCCCCC1=CC=CC=C1O RGDDVTHQUAQTIE-UHFFFAOYSA-N 0.000 claims description 8
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 claims description 8
- RDBMUARQWLPMNW-UHFFFAOYSA-N phosphanylmethanol Chemical compound OCP RDBMUARQWLPMNW-UHFFFAOYSA-N 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- DBVJJBKOTRCVKF-UHFFFAOYSA-N Etidronic acid Chemical compound OP(=O)(O)C(O)(C)P(O)(O)=O DBVJJBKOTRCVKF-UHFFFAOYSA-N 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- OMOVVBIIQSXZSZ-UHFFFAOYSA-N [6-(4-acetyloxy-5,9a-dimethyl-2,7-dioxo-4,5a,6,9-tetrahydro-3h-pyrano[3,4-b]oxepin-5-yl)-5-formyloxy-3-(furan-3-yl)-3a-methyl-7-methylidene-1a,2,3,4,5,6-hexahydroindeno[1,7a-b]oxiren-4-yl] 2-hydroxy-3-methylpentanoate Chemical compound CC12C(OC(=O)C(O)C(C)CC)C(OC=O)C(C3(C)C(CC(=O)OC4(C)COC(=O)CC43)OC(C)=O)C(=C)C32OC3CC1C=1C=COC=1 OMOVVBIIQSXZSZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 6
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 6
- 235000019394 potassium persulphate Nutrition 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- IRXSLJNXXZKURP-UHFFFAOYSA-N fluorenylmethyloxycarbonyl chloride Chemical class C1=CC=C2C(COC(=O)Cl)C3=CC=CC=C3C2=C1 IRXSLJNXXZKURP-UHFFFAOYSA-N 0.000 claims description 5
- KLUDQUOLAFVLOL-UHFFFAOYSA-N acetyl propanoate Chemical compound CCC(=O)OC(C)=O KLUDQUOLAFVLOL-UHFFFAOYSA-N 0.000 claims description 4
- -1 oxygroup amine Chemical class 0.000 claims description 4
- HDMGAZBPFLDBCX-UHFFFAOYSA-M potassium;sulfooxy sulfate Chemical compound [K+].OS(=O)(=O)OOS([O-])(=O)=O HDMGAZBPFLDBCX-UHFFFAOYSA-M 0.000 claims description 4
- YAQLSKVCTLCIIE-UHFFFAOYSA-M 2-bromobutanoate Chemical compound CCC(Br)C([O-])=O YAQLSKVCTLCIIE-UHFFFAOYSA-M 0.000 claims description 3
- 150000008361 aminoacetonitriles Chemical class 0.000 claims description 3
- BSRDNMMLQYNQQD-UHFFFAOYSA-N iminodiacetonitrile Chemical compound N#CCNCC#N BSRDNMMLQYNQQD-UHFFFAOYSA-N 0.000 claims description 3
- 239000013067 intermediate product Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims 1
- 150000001336 alkenes Chemical class 0.000 claims 1
- 210000000481 breast Anatomy 0.000 claims 1
- 230000006837 decompression Effects 0.000 claims 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims 1
- 230000001590 oxidative effect Effects 0.000 claims 1
- 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 abstract description 8
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000839 emulsion Substances 0.000 description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 10
- 229910052760 oxygen Inorganic materials 0.000 description 10
- 239000001301 oxygen Substances 0.000 description 10
- 238000004090 dissolution Methods 0.000 description 8
- 239000012757 flame retardant agent Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 6
- 239000010985 leather Substances 0.000 description 6
- 238000003786 synthesis reaction Methods 0.000 description 6
- 150000001450 anions Chemical class 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 238000013019 agitation Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- NUXCOKIYARRTDC-UHFFFAOYSA-N o-ethylhydroxylamine;hydron;chloride Chemical compound Cl.CCON NUXCOKIYARRTDC-UHFFFAOYSA-N 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- CSIFGMFVGDBOQC-UHFFFAOYSA-N 3-iminobutanenitrile Chemical compound CC(=N)CC#N CSIFGMFVGDBOQC-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 150000001447 alkali salts Chemical class 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 description 2
- 125000001841 imino group Chemical group [H]N=* 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 150000002825 nitriles Chemical class 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 230000000979 retarding effect Effects 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-N sodium;hydron;carbonate Chemical compound [Na+].OC(O)=O UIIMBOGNXHQVGW-UHFFFAOYSA-N 0.000 description 2
- VPTUPAVOBUEXMZ-UHFFFAOYSA-N (1-hydroxy-2-phosphonoethyl)phosphonic acid Chemical compound OP(=O)(O)C(O)CP(O)(O)=O VPTUPAVOBUEXMZ-UHFFFAOYSA-N 0.000 description 1
- CCJAYIGMMRQRAO-UHFFFAOYSA-N 2-[4-[(2-hydroxyphenyl)methylideneamino]butyliminomethyl]phenol Chemical compound OC1=CC=CC=C1C=NCCCCN=CC1=CC=CC=C1O CCJAYIGMMRQRAO-UHFFFAOYSA-N 0.000 description 1
- YAQLSKVCTLCIIE-UHFFFAOYSA-N 2-bromobutyric acid Chemical class CCC(Br)C(O)=O YAQLSKVCTLCIIE-UHFFFAOYSA-N 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 206010010356 Congenital anomaly Diseases 0.000 description 1
- 241000167847 Koelreuteria paniculata Species 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- 241000219000 Populus Species 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229920003180 amino resin Polymers 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- QMRMTRCBDHFTIV-UHFFFAOYSA-N butyl prop-2-enoate;prop-2-enenitrile;prop-2-enoic acid Chemical compound C=CC#N.OC(=O)C=C.CCCCOC(=O)C=C QMRMTRCBDHFTIV-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229940074391 gallic acid Drugs 0.000 description 1
- 235000004515 gallic acid Nutrition 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 230000013011 mating Effects 0.000 description 1
- 150000007974 melamines Chemical class 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920001228 polyisocyanate Polymers 0.000 description 1
- 239000005056 polyisocyanate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 235000013618 yogurt Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D151/00—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
- C09D151/003—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to macromolecular compounds obtained by reactions only involving unsaturated carbon-to-carbon bonds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/26—Emulsion polymerisation with the aid of emulsifying agents anionic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/30—Emulsion polymerisation with the aid of emulsifying agents non-ionic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F265/00—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
- C08F265/04—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of esters
- C08F265/06—Polymerisation of acrylate or methacrylate esters on to polymers thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/40—Introducing phosphorus atoms or phosphorus-containing groups
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Paints Or Removers (AREA)
- Graft Or Block Polymers (AREA)
Abstract
The preparation method of extinguishing waterborn hud typed acrylic resin coating and paint, preparation method are：The raw material of following weight proportion is added into reaction vessel：0.3 ~ 0.7 part of 50 ~ 65 parts of water, 0.4 ~ 2.3 part of emulsifier, 0.6 ~ 3.0 part of methacrylic acid and acrylic acid, are warming up to 45 DEG C, stir 40min, and A monomers are added, and emulsification times are 30 ~ 70min；It is warming up to 65 DEG C and starts logical recirculation water, kept the temperature after being warming up to 77 DEG C, 0.3 ~ 0.7 parts by weight of initiator A are added dropwise, time for adding continues 1 ~ 3h, and 2 ~ 4h is reacted after dripping, obtains stratum nucleare lotion；Into gained stratum nucleare lotion simultaneously be added dropwise B monomer, 0.3 ~ 0.4 parts by weight initiator A, time for adding continues 1 ~ 2h, 75 ~ 85 DEG C, which are kept the temperature, after dripping is stirred to react 3h, add 0.6 ~ 1.1 parts by weight of fire retardant crosslinking agent, keep the temperature 75 ~ 95 DEG C of 1 ~ 3h of reaction time, cool to 50 DEG C, 0.3 parts by weight of emulsifier are added, reaction time 30min, add ammonium hydroxide tune pH value to 7 ~ 8, described fire-retardant, the waterproof aqueous core shell acrylic esters resin coating and paint, obtained flame-retardant aqueous core shell acrylic esters resin coating and paint have good anti-flammability.
Description
Technical field
The present invention relates to the preparation method of aqueous core shell acrylic esters resin, especially aqueous flame retardant are hud typed
The preparation method of acrylic resin coating and paint.
Background technology
Coating, in the entitled paint of Chinese tradition.So-called coating be coated in the body surface being protected or decorated, and
The continuous film of firm attachment can be formed with coated article, typically based on resin or oil or lotion, add or do not add face
Material, filler add corresponding additive, the thick liquid being formulated with organic solvent or water.
Founding of New is over 60 years, and along with the development of national economy every profession and trade, the coatings industry mating as its is from one
A extremely unobtrusive small industry gradually develops into the essential important industry of all fields of national economy.By several generations
Struggle hard, pioneer and keep forging ahead, China has become second-biggest-in-the-world coating material production state and country of consumption, enters world's coating industry
The mainstream of development.
Water paint has made good with powdery paints, and the building coating especially based on water paint is total in China's coating
About 38% is accounted in amount.Since its chemical characteristic has difference substantially, water paint and oil paint product to water paint with oil paint
Matter also has prodigious difference, then the outmoded understanding for big branch water paint being set to again in paint industry, is unscientific.
Water paint and oily (property) paint should be listed as in liquid coating two very much not homologous series.
By acrylic resin be applied to leather finishing agent initial stage, people for its water desorplion, heat it is glutinous, cold short, intolerant to molten
The shortcomings of agent, is utilized and connects the macromolecule synthesising technologies such as skill, crosslinking, introduces with progress such as functional group styrene, acrylonitrile
It is modified, meet the insufficient needs of the congenital performance of leather finish, the also research for modern high performance leather establishes basis.
Poplar more must et al. develop self-cross linking type acrylic resin coating finiss in butyl acrylate-acrylonitrile-acrylic acid
In methyl ester emulsions polymerization system, by introducing N hydroxymethyl acrylamide and acrylic acid modified, it is preferable performance ratio can be obtained
Leather finishing agent, can improve leather finishing agent not organic solvent-resistant the problems such as.
Acrylic monomers after phosphorus trichloride carboxylic acid halides, is reacted with polyethylene glycol and be prepared for one kind containing length goldenrain tree generation side et al.
The acrylic acid list polyethylene glycol ester monomer of polarity side group, it is then that the monomer and other acrylate, vinylic chemical compound is total
Poly- to be prepared for emulsion acrylic resin, due to the presence of long, soft polarity side group, which has higher anti-tensile strong
Degree, elongation at break；The solvent resistant and water resistance of coating can be significantly improved for leather finish.Nuclear-shell emulsion polymerization is 80
A kind of new technology that age grows up, it is a kind of completely new resin polymerization technology carried out with particle design principle.Nucleocapsid
Type acrylic emulsions copolymer is coexisted in heterogeneous in emulsion particle by two or more polymer, i.e., a kind of polymer is core
Core, another kind are nucleocapsid, packet emulsion layer again outside shell.The obtained anti-after tack of lotion is good, film-forming temperature is low, best film forming,
Stability and more superior mechanical property, and by select different performance monomer respectively as emulsion particle shell or stratum nucleare from
And make lotion that there is particular characteristic, the problem of nucleocapsid can make previous resin property such as it is soft with it is hard, heat-resisting and cold-resistant the problems such as
It settles one by one, this technology is widely used in the synthesis and study on the modification of acrylic resin.
But emulsified acrylic acid cold coating used at present also increasingly shows its unconquerable disadvantage[7], such as low
It is dry slow, it is difficult to form a film in the case that how wet temperature is；Film easily mildews, easy to pollute, not wear-resisting；Freeze-thaw stability and mechanically stable
Property is bad；The Bearable dry and wet wipe of finishing agent, film forming compactness, planarization and glossiness are bad etc., make coating material performance into
The raising of one step is restricted.
In addition there is the defect that flame retardant property is not high and addition emulsifier is comparatively laborious.
201610506501.6 the present invention relates to a kind of self-flame-retardant acrylic emulsions, it is characterised in that：Described hinders certainly
Combustion type modifying cinepazid emulsion is to utilize the halogen flame retardant type vinyl monomer of response type, lotion can occur with acrylic ester monomer
Copolymerization is fixed on fire-retardant group in resinous molecular structure by chemical bond mode, will not parse and fall off, after synthesis
Acrylic emulsion has and need not in addition add other fire retardants from flame retardant property, when preparing coating and can play lasting anti-flammability
Energy；The present invention also provides a kind of preparation methods of self-flame-retardant acrylic emulsion.Self-flame-retardant propylene yogurt produced by the present invention
Liquid have good adhesive force, water resistance, durability, manufactured film have water resistance, alkali resistance, scrub resistance and persistently from
Flame retardant property is widely used in the anti-flaming dope of indoor and outdoor woodenware, steel construction, building, not only plays decoration function, but also plays protection and make
With
201610645798.4 the present invention relates to the production preparation fields of macromolecule product more particularly to a kind of acrylic resin to hinder
Burning coating material, 12-18 parts of amino resins, 3-6 parts of ethyl acrylates, 3-5 parts of butyl acrylates, 2-10 parts of melamines, 1-2 parts disappear
Infusion, 2-6 part color stuffing, 2-3 parts of acrylic acid, the carboxylic anion aqueous resin of 60~70 parts by weight, 5~10 parts by weight
Waterproof pigment, the auxiliary agent of 7~8 parts by weight, the interfacial adhesion promoting agent of 1~2 parts by weight, 4-8 parts of carbon forming agents, 10~20 weights
Measure the deionized water of part；Interfacial adhesion promoting agent is reacted by metallorganic, polyisocyanates and oligomer containing hydroxyl
It forms.With excellent interfacial adhesion and with good fire-retardant effect between the acrylic resin paint and base material of the present invention
Fruit.
Invention content
The present invention relates to the preparation method of extinguishing waterborn hud typed acrylic resin coating and paint, main conjunctions
It is that crosslinking agent flame retarding function is improved into the anti-flammability of aqueous core shell acrylic esters resin coating and paint at route,
It is exactly flame-retardant modified from the angle progress for being related to chemical materials needed for acrylic resin, simultaneously because current acrylate
Required anion and nonionic collocation raising soda acid salt-stable and mechanical agitation obtain stability in the synthesis of resinoid, by the two
It is combined into one, a kind of novel emulsifier for having anion and nonionic energy concurrently of self-control, the emulsifier can have easy to operate, acid
Alkali salt stability and mechanical agitation obtain the strong advantage of stability.
The preparation method of extinguishing waterborn hud typed acrylic resin coating and paint, preparation method are：
（1）The raw material of following weight proportion is added into reaction vessel：50 ~ 65 parts of water, 0.4 ~ 2.3 part of emulsifier, metering system
Acid 0.6 ~ 3.0 part and 0.3 ~ 0.7 part of acrylic acid is warming up to 45 DEG C, stirs 40min, is added A monomers, and emulsification times are 30 ~
70min；It is warming up to 65 DEG C and starts logical recirculation water, kept the temperature after being warming up to 77 DEG C, be added dropwise 0.3 ~ 0.7 parts by weight of initiator A, when dropwise addition
Between continue 1 ~ 3h, after dripping react 2 ~ 4h, obtain stratum nucleare lotion；
The A monomers be by：2 ~ 7 parts by weight of butyl acrylate, 2 ~ 5 parts by weight of methyl methacrylate, ethyl acrylate 3 ~ 3.5
Parts by weight, 2-4 parts of hydroxy-ethyl acrylate mix；
（2）To step（1）Be added dropwise simultaneously in gained stratum nucleare lotion B monomer, 0.3 ~ 0.4 parts by weight initiator A, time for adding holds
Continuous 1 ~ 2h keeps the temperature 75 ~ 85 DEG C after dripping and is stirred to react 3h, adds 0.6 ~ 1.1 parts by weight of fire retardant crosslinking agent, and heat preservation 75 ~
95 DEG C of 1 ~ 3h of reaction time cool to 50 DEG C, and 0.3 parts by weight of emulsifier are added, and reaction time 30min adds ammonium hydroxide tune pH value to 7
~ 8, obtain described fire-retardant, the waterproof aqueous core shell acrylic esters resin coating and paint；
The B monomer be by：1 ~ 6 parts by weight of butyl acrylate, 3 ~ 7 parts by weight of methyl methacrylate, 3 ~ 5 weight of ethyl acrylate
Amount part, 2-6 parts of hydroxy-ethyl acrylate mix.
Initiator A is any one of ammonium persulfate, potassium peroxydisulfate, potassium hydrogen persulfate；The preparation method of emulsifier is to take
15g triethylene tetramines, 70g water are added in three-necked flask, and ethylene oxide 40g and substance A 1.2 are slowly added to after being warming up to 30 DEG C
~ 2.4g, at 30 DEG C react 2h after, be cooled to 25 DEG C, obtain intermediate product, then be added 15g dodecyl phenol,
Pentadecyl phenol and substance B 0.3g between 1.6g, then 100 DEG C of back flow reaction 1h are increased the temperature to, it is evaporated under reduced pressure out solvent, it is as newborn
Agent；Substance A is any one of 2- bromobutyrates, 9- fluorenylmethyl chloroformates, three boroxane of front three basic ring；Substance B is
Any one of ethoxy amine hydrochloride, methyl ethyl-amine and acetic acid propionic anhydride；The preparation method of fire retardant crosslinking agent is：By hydroxyl
Ethylene-diphosphonic acid 2.1g, tetrakis hydroxymetyl phosphonium sulfuric 2.5g and substance C 1.2g are added in three-necked flask 250ml, are reacted at 70 DEG C
1h, adds formamide 1.5g and 2,3- pyridinedicarboxylic acids 1.6g, reacts 1.5h at 65 DEG C, obtains the fire retardant crosslinking agent；Substance C
For any one of 4,4'- bipyridyls, aminoacetonitriles, iminodiacetonitrile.
Advantage of the invention is that：
（1）Crosslinking agent flame retarding function is improved to the anti-flammability of aqueous core shell acrylic esters resin coating and paint,
It is exactly flame-retardant modified from the angle progress for being related to chemical materials needed for acrylic resin, simultaneously because current acrylate
Required anion and nonionic collocation raising soda acid salt-stable and mechanical agitation obtain stability in the synthesis of resinoid, by the two
It is combined into one, a kind of novel emulsifier for having anion and nonionic energy concurrently of self-control, the emulsifier can have easy to operate, acid
Alkali salt stability and mechanical agitation obtain the strong advantage of stability.
（2）2- bromobutyrates, 9- fluorenylmethyl chloroformates, three boroxane of front three basic ring are as emulsifier synthesis catalytic
Agent, and dodecyl phenol, pentadecyl phenol are improved using ethoxy amine hydrochloride, methyl ethyl-amine and acetic acid propionic anhydride
Synergist；4,4'- bipyridyls, aminoacetonitriles, iminodiacetonitrile are urged as 1-hydroxy ethylidene-1,1-diphosphonic acid, tetrakis hydroxymetyl phosphonium sulfuric
Agent.
（3）The mechanism of the present invention is the film for making acrylic resin form densification using crosslinking agent, while in propylene
Esters of gallic acid resin surface has fire-retardant group, reduces the burning velocity of flame, improves its anti-flammability.
Specific implementation mode
Example 1
The preparation method of extinguishing waterborn hud typed acrylic resin coating and paint, preparation method are：
（1）The raw material of following weight proportion is added into reaction vessel：By 50 parts of water, 0.4 part of emulsifier, methacrylic acid 0.6
0.3 part of part and acrylic acid are added in reaction vessel, are warming up to 45 DEG C, stir 40min, and A monomers are added, and emulsification times are
30min；It is warming up to 65 DEG C and starts logical recirculation water, kept the temperature after being warming up to 77 DEG C, 0.3 parts by weight of ammonium persulfate are added dropwise（It is water-soluble with 5g
Solution）, time for adding continues 1h, reacts 2h after dripping, and obtains stratum nucleare lotion；
The A monomers be by：2 parts by weight of butyl acrylate, 2 parts by weight of methyl methacrylate, 3 parts by weight of ethyl acrylate,
2 parts of hydroxy-ethyl acrylate mixes；
（2）To step（1）In gained stratum nucleare lotion simultaneously be added dropwise B monomer, 0.3 parts by weight ammonium persulfate（With 5g water dissolutions）,
Time for adding continues 1h, and keeping the temperature 75 DEG C after dripping is stirred to react 3h, adds 0.6 parts by weight of fire retardant crosslinking agent, heat preservation 75
DEG C reaction time 1h cools to 50 DEG C, is added 0.3 parts by weight of emulsifier, reaction time 30min, adds ammonium hydroxide tune pH value to 7 ~ 8,
Obtain the hud typed acrylic resin coating of extinguishing waterborn and paint；
The B monomer be by：1 parts by weight of butyl acrylate, 3 parts by weight of methyl methacrylate, 3 parts by weight of ethyl acrylate,
2 parts of hydroxy-ethyl acrylate mixes.
The preparation method of emulsifier is that 15g triethylene tetramines, 70g water is taken to be added in three-necked flask, after being warming up to 30 DEG C
It is slowly added to ethylene oxide 40g and 2- bromobutyrate 1.2g, after reacting 2h at 30 DEG C, 25 DEG C is cooled to, obtains intermediate production
Then object is added pentadecyl phenol and ethoxy amine hydrochloride 0.3g between the dodecyl phenol of 15g, 1.6g, then increases temperature
To 100 DEG C of back flow reaction 1h, it is evaporated under reduced pressure out solvent, as emulsifier；
The preparation method of fire retardant crosslinking agent is：By 1-hydroxy ethylidene-1,1-diphosphonic acid 2.1g, tetrakis hydroxymetyl phosphonium sulfuric 2.5g and 4,4'- connection
Pyridine 1.2g is added in three-necked flask 250ml, reacts 1h at 70 DEG C, adds formamide 1.5g and 2,3- pyridinedicarboxylic acids
1.6g reacts 1.5h at 65 DEG C, obtains the fire retardant crosslinking agent.
Example 2
The preparation method of extinguishing waterborn hud typed acrylic resin coating and paint, preparation method are：
（1）The raw material of following weight proportion is added into reaction vessel：By 65 parts of water, 2.3 parts of emulsifier, methacrylic acid 3.0
0.7 part of part and acrylic acid are warming up to 45 DEG C, stir 40min, and A monomers, emulsification times 70min is added；It is warming up to 65 DEG C of beginnings
Logical recirculation water, keeps the temperature after being warming up to 77 DEG C, and 0.7 parts by weight of potassium peroxydisulfate are added dropwise（With 5g water dissolutions）, time for adding continues 3h, drips
4h is reacted after adding, and obtains stratum nucleare lotion；
The A monomers be by：7 parts by weight of butyl acrylate, 5 parts by weight of methyl methacrylate, 3.5 weight of ethyl acrylate
Part, 4 parts of hydroxy-ethyl acrylate mix；
（2）To step（1）In gained stratum nucleare lotion simultaneously be added dropwise B monomer, 0.4 parts by weight potassium peroxydisulfate（With 5g water dissolutions）,
Time for adding continues 2h, and keeping the temperature 85 DEG C after dripping is stirred to react 3h, adds 1.1 parts by weight of fire retardant crosslinking agent, heat preservation 95
DEG C reaction time 3h cools to 50 DEG C, is added 0.3 parts by weight of emulsifier, reaction time 30min, adds ammonium hydroxide tune pH value to 7 ~ 8,
Obtain the hud typed acrylic resin coating of extinguishing waterborn and paint；
The B monomer be by：6 parts by weight of butyl acrylate, 7 parts by weight of methyl methacrylate, 5 parts by weight of ethyl acrylate,
6 parts of hydroxy-ethyl acrylate mixes.
The preparation method of emulsifier is that 15g triethylene tetramines, 70g water is taken to be added in three-necked flask, after being warming up to 30 DEG C
It is slowly added to ethylene oxide 40g and 9- fluorenylmethyl chloroformate 2.4g, after reacting 2h at 30 DEG C, is cooled to 25 DEG C, in obtaining
Between product, pentadecyl phenol and methyl ethyl-amine 0.3g between the dodecyl phenol of 15g, 1.6g is then added, then increase the temperature to
100 DEG C of back flow reaction 1h, are evaporated under reduced pressure out solvent, as emulsifier；
The preparation method of fire retardant crosslinking agent is：By 1-hydroxy ethylidene-1,1-diphosphonic acid 2.1g, tetrakis hydroxymetyl phosphonium sulfuric 2.5g and amino second
Nitrile 1.2g is added in three-necked flask 250ml, reacts 1h at 70 DEG C, adds formamide 1.5g and 2,3- pyridinedicarboxylic acids
1.6g reacts 1.5h at 65 DEG C, obtains the fire retardant crosslinking agent.
Example 3
The preparation method of extinguishing waterborn hud typed acrylic resin coating and paint, preparation method are：
（1）The raw material of following weight proportion is added into reaction vessel：By 57 parts of water, 1.3 parts of emulsifier, methacrylic acid 1.8
0.5 part of part and acrylic acid are warming up to 45 DEG C, stir 40min, and A monomers, emulsification times 50min is added；It is warming up to 65 DEG C of beginnings
Logical recirculation water, keeps the temperature after being warming up to 77 DEG C, and 0.5 parts by weight of potassium hydrogen persulfate are added dropwise（With 5g water dissolutions）, time for adding continues 2h,
3h is reacted after dripping, and obtains stratum nucleare lotion；
The A monomers be by：4.5 parts by weight of butyl acrylate, 3.5 parts by weight of methyl methacrylate, 3.3 weight of ethyl acrylate
Amount part, 3 parts of hydroxy-ethyl acrylate mix；
（2）To step（1）In gained stratum nucleare lotion simultaneously be added dropwise B monomer, 0.3 parts by weight potassium hydrogen persulfate（It is water-soluble with 5g
Solution）, time for adding continues 1.5h, and keeping the temperature 80 DEG C after dripping is stirred to react 3h, adds 0.8 parts by weight of fire retardant crosslinking agent,
85 DEG C of reaction time 2h are kept the temperature, cool to 50 DEG C, 0.3 parts by weight of emulsifier are added, reaction time 30min adds ammonium hydroxide tune pH value
To 7 ~ 8, the hud typed acrylic resin coating of extinguishing waterborn and paint are obtained；
The B monomer be by：3.5 parts by weight of butyl acrylate, 5 parts by weight of methyl methacrylate, 4 weight of ethyl acrylate
Part, 4 parts of hydroxy-ethyl acrylate mix.
The preparation method of emulsifier is that 15g triethylene tetramines, 70g water is taken to be added in three-necked flask, after being warming up to 30 DEG C
It is slowly added to three boroxane 1.8g of ethylene oxide 40g and front three basic ring, after reacting 2h at 30 DEG C, is cooled to 25 DEG C, in obtaining
Between product, pentadecyl phenol and acetic acid propionic anhydride 0.3g between the dodecyl phenol of 15g, 1.6g is then added, then increase temperature
To 100 DEG C of back flow reaction 1h, it is evaporated under reduced pressure out solvent, as emulsifier；
The preparation method of fire retardant crosslinking agent is：By 1-hydroxy ethylidene-1,1-diphosphonic acid 2.1g, tetrakis hydroxymetyl phosphonium sulfuric 2.5g and imino group
Diacetonitrile 1.2g is added in three-necked flask 250ml, reacts 1h at 70 DEG C, adds formamide 1.5g and 2,3- pyridinedicarboxylic acids
1.6g reacts 1.5h at 65 DEG C, obtains the fire retardant crosslinking agent.
Example 4
The preparation method of extinguishing waterborn hud typed acrylic resin coating and paint, preparation method are：
（1）The raw material of following weight proportion is added into reaction vessel：50 parts of water, 2.3 parts of emulsifier, 3.0 parts of methacrylic acid
With 0.3 part of acrylic acid, 45 DEG C are warming up to, stirs 40min, A monomers, emulsification times 40min is added；65 DEG C are warming up to start to lead to
Recirculation water is kept the temperature after being warming up to 77 DEG C, and 0.4 parts by weight of ammonium persulfate are added dropwise（With 5g water dissolutions）, time for adding continues 1.5h, drips
3h is reacted after adding, and obtains stratum nucleare lotion；
The A monomers be by：4 parts by weight of butyl acrylate, 3 parts by weight of methyl methacrylate, 3 parts by weight of ethyl acrylate,
4 parts of hydroxy-ethyl acrylate mixes；
（2）To step（1）In gained stratum nucleare lotion simultaneously be added dropwise B monomer, 0.3 parts by weight ammonium persulfate（With 5g water dissolutions）,
Time for adding continues 1h, and keeping the temperature 75 DEG C after dripping is stirred to react 3h, adds 0.7 parts by weight of fire retardant crosslinking agent, heat preservation 80
DEG C reaction time 2h cools to 50 DEG C, is added 0.3 parts by weight of emulsifier, reaction time 30min, adds ammonium hydroxide tune pH value to 7 ~ 8,
Obtain the hud typed acrylic resin coating of extinguishing waterborn and paint；
The B monomer be by：3 parts by weight of butyl acrylate, 4 parts by weight of methyl methacrylate, 4 parts by weight of ethyl acrylate,
6 parts of hydroxy-ethyl acrylate mixes.
The preparation method of emulsifier is that 15g triethylene tetramines, 70g water is taken to be added in three-necked flask, after being warming up to 30 DEG C
It is slowly added to ethylene oxide 40g and 2- bromobutyrate 1.6g, after reacting 2h at 30 DEG C, 25 DEG C is cooled to, obtains intermediate production
Then object is added pentadecyl phenol and ethoxy amine hydrochloride 0.3g between the dodecyl phenol of 15g, 1.6g, then increases temperature
To 100 DEG C of back flow reaction 1h, it is evaporated under reduced pressure out solvent, as emulsifier；
The preparation method of fire retardant crosslinking agent is：By 1-hydroxy ethylidene-1,1-diphosphonic acid 2.1g, tetrakis hydroxymetyl phosphonium sulfuric 2.5g and amino second
Nitrile 1.2g is added in three-necked flask 250ml, reacts 1h at 70 DEG C, adds formamide 1.5g and 2,3- pyridinedicarboxylic acids
1.6g reacts 1.5h at 65 DEG C, obtains the fire retardant crosslinking agent.
Example 5
The preparation method of extinguishing waterborn hud typed acrylic resin coating and paint, preparation method are：
（1）The raw material of following weight proportion is added into reaction vessel：By 65 parts of water, 2.3 parts of emulsifier, methacrylic acid 3.0
0.7 part of part and acrylic acid are warming up to 45 DEG C, stir 40min, and A monomers, emulsification times 70min is added；It is warming up to 65 DEG C of beginnings
Logical recirculation water, keeps the temperature after being warming up to 77 DEG C, and 0.7 parts by weight of potassium peroxydisulfate are added dropwise（With 5g water dissolutions）, time for adding continues 1h, drips
2h is reacted after adding, and obtains stratum nucleare lotion；
The A monomers be by：7 parts by weight of butyl acrylate, 4 parts by weight of methyl methacrylate, 3 parts by weight of ethyl acrylate,
2 parts of hydroxy-ethyl acrylate mixes；
（2）To step（1）In gained stratum nucleare lotion simultaneously be added dropwise B monomer, 0.3 parts by weight potassium peroxydisulfate（With 5g water dissolutions）,
Time for adding continues 1h, and keeping the temperature 75 DEG C after dripping is stirred to react 3h, adds 0.6 parts by weight of fire retardant crosslinking agent, heat preservation 75
DEG C reaction time 1h cools to 50 DEG C, is added 0.3 parts by weight of emulsifier, reaction time 30min, adds ammonium hydroxide tune pH value to 7 ~ 8,
Obtain the hud typed acrylic resin coating of extinguishing waterborn and paint；
The B monomer be by：6 parts by weight of butyl acrylate, 7 parts by weight of methyl methacrylate, 5 parts by weight of ethyl acrylate,
6 parts of hydroxy-ethyl acrylate mixes.
The preparation method of emulsifier is that 15g triethylene tetramines, 70g water is taken to be added in three-necked flask, after being warming up to 30 DEG C
It is slowly added to ethylene oxide 40g and 9- fluorenylmethyl chloroformate 1.6g, after reacting 2h at 30 DEG C, is cooled to 25 DEG C, in obtaining
Between product, pentadecyl phenol and methyl ethyl-amine 0.3g between the dodecyl phenol of 15g, 1.6g is then added, then increase the temperature to
100 DEG C of back flow reaction 1h, are evaporated under reduced pressure out solvent, as emulsifier；
The preparation method of fire retardant crosslinking agent is：By 1-hydroxy ethylidene-1,1-diphosphonic acid 2.1g, tetrakis hydroxymetyl phosphonium sulfuric 2.5g and imino group
Diacetonitrile 1.2g is added in three-necked flask 250ml, reacts 1h at 70 DEG C, adds formamide 1.5g and 2,3- pyridinedicarboxylic acids
1.6g reacts 1.5h at 65 DEG C, obtains the fire retardant crosslinking agent.
Anti-flammability is weighed by oxygen index (OI), flaming combustion time.
1 test performance of table
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | |
| Oxygen index (OI)/% | 29.4 | 29.6 | 30.4 | 29.8 | 29.8 |
| Flaming combustion time/s | 1.1 | 1.6 | 0.8 | 1.2 | 2.1 |
As it can be seen from table 1 the oxygen index (OI) of the hud typed acrylic resin coating of extinguishing waterborn and paint greatly improves, and have
Flame burning time is greatly reduced, and compares the oxygen index (OI) of 201610506501.6 and 201610645798.4 example 1 and have flame
Burning time is respectively 22.6,26.5s and 24.1 and 36.5s.
2 test performance of table（Not plus flame-retardant agent）
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | |
| Oxygen index (OI)/% | 21.6 | 22.7 | 20.4 | 21.2 | 21.7 |
| Flaming combustion time/s | 31.2 | 32.7 | 29.4 | 22.1 | 25.7 |
From table 2 it can be seen that the oxygen of the hud typed acrylic resin coating of flame-retardant agent extinguishing waterborn and paint is not added to refer to
Number is greatly reduced, and flaming combustion time greatly improves.
3 test performance of table（Add flame-retardant agent, does not add substance C）
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | |
| Oxygen index (OI)/% | 25.2 | 24.7 | 26.4 | 25.3 | 27.2 |
| Flaming combustion time/s | 11.2 | 22.7 | 25.4 | 16.1 | 18.2 |
From table 3 it can be seen that plus flame-retardant agent do not add the hud typed acrylic resin coating of extinguishing waterborn when substance C and
The oxygen index (OI) of paint does not add flame-retardant agent to be sharply increased compared to, and flaming combustion time declines to a great extent.
4 test performance of table（Add flame-retardant agent, add substance C, does not add 2,3- pyridinedicarboxylic acids）
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | |
| Oxygen index (OI)/% | 26.3 | 25.8 | 27.1 | 26.1 | 27.3 |
| Flaming combustion time/s | 10.3 | 14.2 | 18.3 | 12.0 | 12.4 |
From table 4, it can be seen that plus flame-retardant agent, plus substance C, and the extinguishing waterborn plus when 2,3- pyridinedicarboxylic acids is hud typed
Acrylic resin coating is compared with the oxygen index (OI) of paint not plus flame-retardant agent is sharply increased, and flaming combustion time is substantially
Decline.
Chemical-resistant reagent stability:Respectively by lotion and 5 % sodium chloride solutions by volume 1:4 ratio mixing, it is close
48h is sealed and stood, its precipitation capacity is observed.
Gel fraction：Measure the percentage of the weight and the weight of theoretical gained lotion of the gel in acrylic resin synthesis.
5 stability of emulsion data of table
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | |
| Chemical-resistant stability | Stablize not stratified | Stablize not stratified | Stablize not stratified | Stablize not stratified | Stablize not stratified |
| Gel filter/% | 1.6 | 2.1 | 1.7 | 1.1 | 0.8 |
As can be found from Table 5, chemical-resistant stability of the invention and gel filter are all relatively good., comparative sample
201610506501.6 the gel filter with 201610645798.4 example 1 is respectively 9.7% and 8.3%.
6 stability of emulsion data of table（Not plus substance A）
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | |
| Chemical-resistant stability | Stablize not stratified | Layering | Stablize not stratified | Layering | Layering |
| Gel filter/% | 7.6 | 5.8 | 6.2 | 4.8 | 6.6 |
As can be found from Table 6, the chemical-resistant stability and gel filter for not adding the present invention of substance A are remarkably decreased.
7 stability of emulsion data of table（Add substance A, does not add substance B）
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | |
| Chemical-resistant stability | Layering | Layering | Layering | Layering | Layering |
| Gel filter/% | 7.7 | 10.3 | 12.7 | 8.6 | 14.3 |
As can be found from Table 7, the present invention does not add the gel of substance B and chemical-resistant stability to be remarkably decreased.
Claims (7)
1. the preparation method of extinguishing waterborn hud typed acrylic resin coating and paint, preparation method are：
（1）The raw material of following weight proportion is added into reaction vessel：By 50 ~ 65 parts of water, 0.4 ~ 2.3 part of emulsifier, methyl-prop
0.3 ~ 0.7 part of mixing of 0.6 ~ 3.0 part of olefin(e) acid and acrylic acid, is warming up to 45 DEG C, stirs 40min, is added A monomers, when emulsification
Between be 30 ~ 70min；It is warming up to 65 DEG C and starts logical recirculation water, kept the temperature after being warming up to 77 DEG C, 0.3 ~ 0.7 weight of initiator A is added dropwise
Part, time for adding continues 1 ~ 3h, and 2 ~ 4h is reacted after dripping, obtains stratum nucleare lotion；
The A monomers be by：2 ~ 7 parts by weight of butyl acrylate, 2 ~ 5 parts by weight of methyl methacrylate, ethyl acrylate 3 ~ 3.5
Parts by weight, 2-4 parts of hydroxy-ethyl acrylate mix；
（2）To step（1）Be added dropwise simultaneously in gained stratum nucleare lotion B monomer, 0.3 ~ 0.4 parts by weight initiator A, time for adding holds
Continuous 1 ~ 2h keeps the temperature 75 ~ 85 DEG C after dripping and is stirred to react 3h, adds 0.6 ~ 1.1 parts by weight of fire retardant crosslinking agent, and heat preservation 75 ~
95 DEG C of 1 ~ 3h of reaction time cool to 50 DEG C, and 0.3 parts by weight of emulsifier are added, and reaction time 30min adds ammonium hydroxide tune pH value to 7
~ 8, obtain described fire-retardant, the waterproof aqueous core shell acrylic esters resin coating and paint；
The B monomer be by：1 ~ 6 parts by weight of butyl acrylate, 3 ~ 7 parts by weight of methyl methacrylate, 3 ~ 5 weight of ethyl acrylate
Amount part, 2-6 parts of hydroxy-ethyl acrylate mix.
2. the preparation method of extinguishing waterborn hud typed the acrylic resin coating and paint as described in right 1, described draws
Send out any one that agent A is ammonium persulfate, potassium peroxydisulfate, potassium hydrogen persulfate.
3. the preparation method of extinguishing waterborn hud typed the acrylic resin coating and paint as described in right 1, the breast
The preparation method of agent is that 15g triethylene tetramines, 70g water is taken to be added in three-necked flask, and ring is slowly added to after being warming up to 30 DEG C
1.2 ~ 2.4g of oxidative ethane 40g and substance A is cooled to 25 DEG C, obtains intermediate product, 15g is then added after reacting 2h at 30 DEG C
Dodecyl phenol, pentadecyl phenol and substance B 0.3g between 1.6g, then increase the temperature to 100 DEG C of back flow reaction 1h, decompression is steamed
Distillate solvent, as emulsifier.
4. the preparation method of extinguishing waterborn hud typed the acrylic resin coating and paint as described in right 3, substance A 2-
Any one of bromobutyrate, 9- fluorenylmethyl chloroformates, three boroxane of front three basic ring.
5. the preparation method of extinguishing waterborn hud typed the acrylic resin coating and paint as described in right 3, substance B is second
Any one of oxygroup amine hydrochlorate, methyl ethyl-amine and acetic acid propionic anhydride.
6. the preparation method of extinguishing waterborn hud typed the acrylic resin coating and paint as described in right 1, the resistance
Combustion property crosslinking agent preparation method be：1-hydroxy ethylidene-1,1-diphosphonic acid 2.1g, tetrakis hydroxymetyl phosphonium sulfuric 2.5g and substance C 1.2g are added
Into three-necked flask 250ml, 1h is reacted at 70 DEG C, adds formamide 1.5g and 2,3- pyridinedicarboxylic acids 1.6g is anti-at 65 DEG C
1.5h is answered, the fire retardant crosslinking agent is obtained.
7. the preparation method of extinguishing waterborn hud typed the acrylic resin coating and paint as described in right 6, substance C 4,
Any one of 4'- bipyridyls, aminoacetonitriles, iminodiacetonitrile.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011369854.9A CN112409877B (en) | 2018-07-15 | 2018-07-15 | Preparation method of flame-retardant water-based core-shell acrylic resin coating |
| CN201810773980.7A CN108795208B (en) | 2018-07-15 | 2018-07-15 | Preparation method of flame-retardant water-based core-shell acrylate resin coating and paint |
| PCT/CN2018/120939 WO2020015289A1 (en) | 2018-07-15 | 2018-12-13 | Flame-retardant, aqueous, core-shell acrylate resin coating and paint preparation method |
| CA3028455A CA3028455A1 (en) | 2018-07-15 | 2018-12-27 | Preparation for acrylate resin coating and paint of flame-retardant, water-proof and water-based core-shell type |
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| CN201810773980.7A CN108795208B (en) | 2018-07-15 | 2018-07-15 | Preparation method of flame-retardant water-based core-shell acrylate resin coating and paint |
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| CN202011369854.9A Division CN112409877B (en) | 2018-07-15 | 2018-07-15 | Preparation method of flame-retardant water-based core-shell acrylic resin coating |
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| CN108795208B CN108795208B (en) | 2020-12-18 |
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| CN201810773980.7A Active CN108795208B (en) | 2018-07-15 | 2018-07-15 | Preparation method of flame-retardant water-based core-shell acrylate resin coating and paint |
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| CN (2) | CN112409877B (en) |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109181458A (en) * | 2018-11-21 | 2019-01-11 | 段瑶瑶 | A kind of preparation method of waterproofness core-shell type aqueous acrylic resin coating and finishing agent |
| CN109468006A (en) * | 2018-11-15 | 2019-03-15 | 段瑶瑶 | A kind of preparation method of the core-shell type aqueous acrylic resin coating of antifriction |
| CN109705681A (en) * | 2018-12-25 | 2019-05-03 | 杨记周 | A kind of new-energy automobile environment-friendly water-based paint and preparation method thereof |
| CN110204989A (en) * | 2019-07-17 | 2019-09-06 | 烟台大学 | The preparation method of the hud typed environment-friendly water-based acrylic resin coating of flame retardant type |
| CN110642982A (en) * | 2019-09-17 | 2020-01-03 | 湖北工业大学 | Preparation method of high-tensile-strength amide benzene ring emulsion polymer with core-shell structure |
| WO2020015289A1 (en) * | 2018-07-15 | 2020-01-23 | 周连惠 | Flame-retardant, aqueous, core-shell acrylate resin coating and paint preparation method |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111794012B (en) * | 2020-06-24 | 2022-04-29 | 杭州华旺新材料科技股份有限公司 | High-strength water-resistant flame-retardant plain colored paper and preparation method thereof |
| CN112646269B (en) * | 2020-12-17 | 2023-04-28 | 安徽强旭塑业科技有限公司 | Environment-friendly high-flame-retardance battery shell and preparation method thereof |
| CN112625173B (en) * | 2020-12-17 | 2021-12-24 | 常熟国和新材料有限公司 | Water-based acrylic resin with good viscosity stability and preparation method thereof |
| JP2024539990A (en) * | 2021-10-26 | 2024-10-31 | スリーエム イノベイティブ プロパティズ カンパニー | Flame retardant pressure sensitive adhesive and method of manufacture |
| CN115160480A (en) * | 2022-02-14 | 2022-10-11 | 上海金狮化工有限公司 | Waterborne acrylic resin for coloring woodware and preparation method thereof |
| CN117024663B (en) * | 2023-08-08 | 2024-05-10 | 南京科工煤炭科学技术研究有限公司 | Acrylate emulsion for core-shell polymer cement and preparation method thereof |
Citations (1)
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| CN102875723A (en) * | 2012-10-26 | 2013-01-16 | 烟台大学 | Preparation method of flame-retardant core-shell-type acrylic resin |
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| JPH0794584B2 (en) * | 1987-01-07 | 1995-10-11 | 日本ペイント株式会社 | Method for producing aqueous dispersion of anionic gel particles |
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| CN105111876B (en) * | 2014-07-27 | 2017-06-13 | 河北晨阳工贸集团有限公司 | Building, the preparation method of the core-shell type aqueous acrylic resin coating of furniture |
| CN108459136A (en) * | 2018-05-29 | 2018-08-28 | 上海福乐医药科技有限公司 | A kind of method of three boroxane content of titration measuring front three basic ring |
| CN112409877B (en) * | 2018-07-15 | 2023-08-01 | 广东省漆色彩新型材料有限公司 | Preparation method of flame-retardant water-based core-shell acrylic resin coating |
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- 2018-07-15 CN CN202011369854.9A patent/CN112409877B/en active Active
- 2018-07-15 CN CN201810773980.7A patent/CN108795208B/en active Active
- 2018-12-13 WO PCT/CN2018/120939 patent/WO2020015289A1/en active Application Filing
- 2018-12-27 CA CA3028455A patent/CA3028455A1/en not_active Abandoned
Patent Citations (1)
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| CN102875723A (en) * | 2012-10-26 | 2013-01-16 | 烟台大学 | Preparation method of flame-retardant core-shell-type acrylic resin |
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| 张大省等: "《图解纤维材料》", 31 August 2015, 中国纺织出版社 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020015289A1 (en) * | 2018-07-15 | 2020-01-23 | 周连惠 | Flame-retardant, aqueous, core-shell acrylate resin coating and paint preparation method |
| CN109468006A (en) * | 2018-11-15 | 2019-03-15 | 段瑶瑶 | A kind of preparation method of the core-shell type aqueous acrylic resin coating of antifriction |
| CN109181458A (en) * | 2018-11-21 | 2019-01-11 | 段瑶瑶 | A kind of preparation method of waterproofness core-shell type aqueous acrylic resin coating and finishing agent |
| CN109705681A (en) * | 2018-12-25 | 2019-05-03 | 杨记周 | A kind of new-energy automobile environment-friendly water-based paint and preparation method thereof |
| CN110204989A (en) * | 2019-07-17 | 2019-09-06 | 烟台大学 | The preparation method of the hud typed environment-friendly water-based acrylic resin coating of flame retardant type |
| CN110642982A (en) * | 2019-09-17 | 2020-01-03 | 湖北工业大学 | Preparation method of high-tensile-strength amide benzene ring emulsion polymer with core-shell structure |
Also Published As
| Publication number | Publication date |
|---|---|
| CA3028455A1 (en) | 2020-01-15 |
| CN108795208B (en) | 2020-12-18 |
| CN112409877A (en) | 2021-02-26 |
| WO2020015289A1 (en) | 2020-01-23 |
| CN112409877B (en) | 2023-08-01 |
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