CN106164100B - Emulsion resin composition and its manufacturing method - Google Patents
Emulsion resin composition and its manufacturing method Download PDFInfo
- Publication number
- CN106164100B CN106164100B CN201580017755.5A CN201580017755A CN106164100B CN 106164100 B CN106164100 B CN 106164100B CN 201580017755 A CN201580017755 A CN 201580017755A CN 106164100 B CN106164100 B CN 106164100B
- Authority
- CN
- China
- Prior art keywords
- lotion
- containing polymer
- compound
- monomer
- emulsifier
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000000839 emulsion Substances 0.000 title claims abstract description 65
- 239000011342 resin composition Substances 0.000 title claims abstract description 58
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- 229920000642 polymer Polymers 0.000 claims abstract description 106
- 239000006210 lotion Substances 0.000 claims abstract description 103
- 239000000178 monomer Substances 0.000 claims abstract description 71
- 239000002245 particle Substances 0.000 claims abstract description 63
- 150000001875 compounds Chemical class 0.000 claims abstract description 60
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 60
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 59
- 238000007720 emulsion polymerization reaction Methods 0.000 claims abstract description 38
- 239000003505 polymerization initiator Substances 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 26
- 238000009835 boiling Methods 0.000 claims abstract description 23
- 238000006116 polymerization reaction Methods 0.000 claims description 22
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical class OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 13
- 239000011248 coating agent Substances 0.000 claims description 12
- 238000000576 coating method Methods 0.000 claims description 12
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 7
- 125000005250 alkyl acrylate group Chemical group 0.000 claims description 6
- 150000002148 esters Chemical class 0.000 claims description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 6
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 claims description 5
- 239000002738 chelating agent Substances 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 238000007334 copolymerization reaction Methods 0.000 claims description 3
- 239000000306 component Substances 0.000 claims 1
- 239000008187 granular material Substances 0.000 claims 1
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 133
- -1 (methyl) methyl Chemical group 0.000 description 44
- 239000011347 resin Substances 0.000 description 28
- 229920005989 resin Polymers 0.000 description 28
- 239000000203 mixture Substances 0.000 description 25
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 22
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 14
- 238000004945 emulsification Methods 0.000 description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 239000004615 ingredient Substances 0.000 description 12
- 239000007788 liquid Substances 0.000 description 12
- 235000011187 glycerol Nutrition 0.000 description 11
- JRKICGRDRMAZLK-UHFFFAOYSA-L persulfate group Chemical group S(=O)(=O)([O-])OOS(=O)(=O)[O-] JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 11
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 9
- 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 description 9
- 239000000908 ammonium hydroxide Substances 0.000 description 9
- 239000007864 aqueous solution Substances 0.000 description 9
- 238000003756 stirring Methods 0.000 description 9
- 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 description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 8
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 8
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 8
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 8
- BAPJBEWLBFYGME-UHFFFAOYSA-N acrylic acid methyl ester Natural products COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 8
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 description 8
- 210000000481 breast Anatomy 0.000 description 7
- 239000004816 latex Substances 0.000 description 7
- 229920000126 latex Polymers 0.000 description 7
- 239000003755 preservative agent Substances 0.000 description 7
- 230000002335 preservative effect Effects 0.000 description 7
- 239000002562 thickening agent Substances 0.000 description 7
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 6
- 239000002518 antifoaming agent Substances 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- XWGJFPHUCFXLBL-UHFFFAOYSA-M rongalite Chemical compound [Na+].OCS([O-])=O XWGJFPHUCFXLBL-UHFFFAOYSA-M 0.000 description 6
- 239000000080 wetting agent Substances 0.000 description 6
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 5
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 5
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 230000009477 glass transition Effects 0.000 description 5
- 239000003999 initiator Substances 0.000 description 5
- 239000012299 nitrogen atmosphere Substances 0.000 description 5
- 239000012875 nonionic emulsifier Substances 0.000 description 5
- 238000010992 reflux Methods 0.000 description 5
- 239000001836 Dioctyl sodium sulphosuccinate Substances 0.000 description 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 4
- 239000005977 Ethylene Substances 0.000 description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 150000005215 alkyl ethers Chemical class 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000003431 cross linking reagent Substances 0.000 description 4
- 235000014113 dietary fatty acids Nutrition 0.000 description 4
- 235000019329 dioctyl sodium sulphosuccinate Nutrition 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 239000000194 fatty acid Substances 0.000 description 4
- 229930195729 fatty acid Natural products 0.000 description 4
- 230000000873 masking effect Effects 0.000 description 4
- 229910021645 metal ion Inorganic materials 0.000 description 4
- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical compound [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 description 4
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L sodium sulphate Substances [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 4
- 235000011152 sodium sulphate Nutrition 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 3
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium peroxydisulfate Substances [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 3
- VAZSKTXWXKYQJF-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)OOS([O-])=O VAZSKTXWXKYQJF-UHFFFAOYSA-N 0.000 description 3
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 3
- 150000003863 ammonium salts Chemical class 0.000 description 3
- 150000001450 anions Chemical class 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- XDSGMUJLZDSCPA-UHFFFAOYSA-N diazanium;phenoxybenzene;sulfate Chemical compound [NH4+].[NH4+].[O-]S([O-])(=O)=O.C=1C=CC=CC=1OC1=CC=CC=C1 XDSGMUJLZDSCPA-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- YPHQUSNPXDGUHL-UHFFFAOYSA-N n-methylprop-2-enamide Chemical compound CNC(=O)C=C YPHQUSNPXDGUHL-UHFFFAOYSA-N 0.000 description 3
- 238000010422 painting Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000012966 redox initiator Substances 0.000 description 3
- GRWFGVWFFZKLTI-IUCAKERBSA-N (-)-α-pinene Chemical compound CC1=CC[C@@H]2C(C)(C)[C@H]1C2 GRWFGVWFFZKLTI-IUCAKERBSA-N 0.000 description 2
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 2
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 2
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 2
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 2
- 150000008065 acid anhydrides Chemical class 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000001721 carbon Chemical group 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 229960001484 edetic acid Drugs 0.000 description 2
- 230000001804 emulsifying effect Effects 0.000 description 2
- 125000003700 epoxy group Chemical group 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 230000002687 intercalation Effects 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229940043265 methyl isobutyl ketone Drugs 0.000 description 2
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 2
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 2
- 150000002978 peroxides Chemical class 0.000 description 2
- 229920001568 phenolic resin Polymers 0.000 description 2
- 239000005011 phenolic resin Substances 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 2
- 159000000000 sodium salts Chemical class 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 150000003505 terpenes Chemical class 0.000 description 2
- 235000007586 terpenes Nutrition 0.000 description 2
- OMDQUFIYNPYJFM-XKDAHURESA-N (2r,3r,4s,5r,6s)-2-(hydroxymethyl)-6-[[(2r,3s,4r,5s,6r)-4,5,6-trihydroxy-3-[(2s,3s,4s,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxyoxan-2-yl]methoxy]oxane-3,4,5-triol Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@@H]1OC[C@@H]1[C@@H](O[C@H]2[C@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O)[C@H](O)[C@H](O)[C@H](O)O1 OMDQUFIYNPYJFM-XKDAHURESA-N 0.000 description 1
- PSGCQDPCAWOCSH-UHFFFAOYSA-N (4,7,7-trimethyl-3-bicyclo[2.2.1]heptanyl) prop-2-enoate Chemical compound C1CC2(C)C(OC(=O)C=C)CC1C2(C)C PSGCQDPCAWOCSH-UHFFFAOYSA-N 0.000 description 1
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 description 1
- GDSOZVZXVXTJMI-SNAWJCMRSA-N (e)-1-methylbut-1-ene-1,2,4-tricarboxylic acid Chemical compound OC(=O)C(/C)=C(C(O)=O)\CCC(O)=O GDSOZVZXVXTJMI-SNAWJCMRSA-N 0.000 description 1
- CPKVUHPKYQGHMW-UHFFFAOYSA-N 1-ethenylpyrrolidin-2-one;molecular iodine Chemical class II.C=CN1CCCC1=O CPKVUHPKYQGHMW-UHFFFAOYSA-N 0.000 description 1
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 1
- 125000000954 2-hydroxyethyl group Chemical group [H]C([*])([H])C([H])([H])O[H] 0.000 description 1
- MUZDXNQOSGWMJJ-UHFFFAOYSA-N 2-methylprop-2-enoic acid;prop-2-enoic acid Chemical compound OC(=O)C=C.CC(=C)C(O)=O MUZDXNQOSGWMJJ-UHFFFAOYSA-N 0.000 description 1
- FRIBMENBGGCKPD-UHFFFAOYSA-N 3-(2,3-dimethoxyphenyl)prop-2-enal Chemical compound COC1=CC=CC(C=CC=O)=C1OC FRIBMENBGGCKPD-UHFFFAOYSA-N 0.000 description 1
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- NOWKCMXCCJGMRR-UHFFFAOYSA-N Aziridine Chemical compound C1CN1 NOWKCMXCCJGMRR-UHFFFAOYSA-N 0.000 description 1
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- 229920002799 BoPET Polymers 0.000 description 1
- KXDHJXZQYSOELW-UHFFFAOYSA-M Carbamate Chemical compound NC([O-])=O KXDHJXZQYSOELW-UHFFFAOYSA-M 0.000 description 1
- KXDHJXZQYSOELW-UHFFFAOYSA-N Carbamic acid Chemical compound NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 244000168525 Croton tiglium Species 0.000 description 1
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 description 1
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- 229920000926 Galactomannan Polymers 0.000 description 1
- 244000043261 Hevea brasiliensis Species 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 1
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 description 1
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- 241001597008 Nomeidae Species 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229920000153 Povidone-iodine Chemical class 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000005708 Sodium hypochlorite Chemical class 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- ZUQAPLKKNAQJAU-UHFFFAOYSA-N acetylenediol Chemical compound OC#CO ZUQAPLKKNAQJAU-UHFFFAOYSA-N 0.000 description 1
- 239000000159 acid neutralizing agent Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 125000005370 alkoxysilyl group Chemical group 0.000 description 1
- 150000008051 alkyl sulfates Chemical class 0.000 description 1
- XYLMUPLGERFSHI-UHFFFAOYSA-N alpha-Methylstyrene Chemical compound CC(=C)C1=CC=CC=C1 XYLMUPLGERFSHI-UHFFFAOYSA-N 0.000 description 1
- MVNCAPSFBDBCGF-UHFFFAOYSA-N alpha-pinene Natural products CC1=CCC23C1CC2C3(C)C MVNCAPSFBDBCGF-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229940045719 antineoplastic alkylating agent nitrosoureas Drugs 0.000 description 1
- 239000013556 antirust agent Substances 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 229960000686 benzalkonium chloride Drugs 0.000 description 1
- UREZNYTWGJKWBI-UHFFFAOYSA-M benzethonium chloride Chemical class [Cl-].C1=CC(C(C)(C)CC(C)(C)C)=CC=C1OCCOCC[N+](C)(C)CC1=CC=CC=C1 UREZNYTWGJKWBI-UHFFFAOYSA-M 0.000 description 1
- 229960001950 benzethonium chloride Drugs 0.000 description 1
- 235000019400 benzoyl peroxide Nutrition 0.000 description 1
- CADWTSSKOVRVJC-UHFFFAOYSA-N benzyl(dimethyl)azanium;chloride Chemical class [Cl-].C[NH+](C)CC1=CC=CC=C1 CADWTSSKOVRVJC-UHFFFAOYSA-N 0.000 description 1
- 229930006722 beta-pinene Natural products 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- IAQRGUVFOMOMEM-UHFFFAOYSA-N but-2-ene Chemical group CC=CC IAQRGUVFOMOMEM-UHFFFAOYSA-N 0.000 description 1
- 239000004359 castor oil Substances 0.000 description 1
- 235000019438 castor oil Nutrition 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- SFZULDYEOVSIKM-UHFFFAOYSA-N chembl321317 Chemical compound C1=CC(C(=N)NO)=CC=C1C1=CC=C(C=2C=CC(=CC=2)C(=N)NO)O1 SFZULDYEOVSIKM-UHFFFAOYSA-N 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 150000003983 crown ethers Chemical class 0.000 description 1
- 125000005594 diketone group Chemical group 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 description 1
- 238000002296 dynamic light scattering Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 1
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 125000004029 hydroxymethyl group Chemical group [H]OC([H])([H])* 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- ZLTPDFXIESTBQG-UHFFFAOYSA-N isothiazole Chemical compound C=1C=NSC=1 ZLTPDFXIESTBQG-UHFFFAOYSA-N 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- OMNKZBIFPJNNIO-UHFFFAOYSA-N n-(2-methyl-4-oxopentan-2-yl)prop-2-enamide Chemical compound CC(=O)CC(C)(C)NC(=O)C=C OMNKZBIFPJNNIO-UHFFFAOYSA-N 0.000 description 1
- 229920003052 natural elastomer Polymers 0.000 description 1
- 229920001194 natural rubber Polymers 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 150000002923 oximes Chemical class 0.000 description 1
- RPQRDASANLAFCM-UHFFFAOYSA-N oxiran-2-ylmethyl prop-2-enoate Chemical compound C=CC(=O)OCC1CO1 RPQRDASANLAFCM-UHFFFAOYSA-N 0.000 description 1
- 239000006174 pH buffer Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 125000003367 polycyclic group Chemical group 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000004848 polyfunctional curative Substances 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 235000019394 potassium persulphate Nutrition 0.000 description 1
- 229960001621 povidone-iodine Drugs 0.000 description 1
- 229940080818 propionamide Drugs 0.000 description 1
- GRWFGVWFFZKLTI-UHFFFAOYSA-N rac-alpha-Pinene Natural products CC1=CCC2C(C)(C)C1C2 GRWFGVWFFZKLTI-UHFFFAOYSA-N 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 150000003349 semicarbazides Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 description 1
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical class [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 1
- 229960005076 sodium hypochlorite Drugs 0.000 description 1
- 235000010262 sodium metabisulphite Nutrition 0.000 description 1
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 1
- 235000019345 sodium thiosulphate Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000012430 stability testing Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- WVSZBAHKLHXQFN-UHFFFAOYSA-N tetrahydrate;dihydrochloride Chemical class O.O.O.O.Cl.Cl WVSZBAHKLHXQFN-UHFFFAOYSA-N 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 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
- 239000002699 waste material Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- WTARULDDTDQWMU-UHFFFAOYSA-N β-pinene Chemical compound C1C2C(C)(C)C1CCC2=C WTARULDDTDQWMU-UHFFFAOYSA-N 0.000 description 1
- DGVVWUTYPXICAM-UHFFFAOYSA-N β‐Mercaptoethanol Chemical compound OCCS DGVVWUTYPXICAM-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
-
- 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
- C09D5/02—Emulsion paints including aerosols
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/66—Additives characterised by particle size
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
-
- 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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1808—C8-(meth)acrylate, e.g. isooctyl (meth)acrylate or 2-ethylhexyl (meth)acrylate
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Materials Engineering (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Dispersion Chemistry (AREA)
- Polymerisation Methods In General (AREA)
- Paints Or Removers (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The object of the present invention is to provide can be synthesized by easy method, nonvolatile component is high, and can form fine and close envelope, the excellent emulsion resin composition for including the lotion containing polymer of mechanical stability because viscosity is low.A kind of emulsion resin composition, it includes：Lotion containing polymer, it is so that monomer is carried out made of emulsion polymerization using emulsifier, water and polymerization initiator in the presence of boiling point is 80 DEG C or more of nonionic water soluble compound (except emulsifier) to be somebody's turn to do the lotion containing polymer；And neutralizer, the nonionic water soluble compound that above-mentioned boiling point is 80 DEG C or more is the compound not being copolymerized with monomer, shared by the particle entirety of the above-mentioned lotion containing polymer, grain size is that the ratio shared by 0.05 μm of small particle particle less than 0.6 μm is 2~75 volume %, ratio shared by 5 μm of 0.6 μm of grain size or more big particle below is 25~98 volume %, also, the average grain diameter (D50 average grain diameters) of the lotion entirety containing polymer is 0.2 μm~2 μm.
Description
Technical field
The present invention relates to emulsion resin composition and its manufacturing methods.
Background technology
In the past, various resin combinations had been used in coating, sticker.Being matched with the resin of the resin combination can enumerate
Such as natural rubber, synthetic rubber, carbamate resins, polyester resin, styrene resin and acrylic resin and it
Mixture, wherein from cost, durability, physical property etc. consider, be widely used for styrene resin, acrylic acid series tree
Fat.
On the other hand, it is widely used for emulsion resin for the purpose of environmental protection and cost reduction.By the emulsion-type
In the case that resin is used in the purposes of coating, sticker (hereinafter referred to as masking liquid), the envelope of film, adhering agent layer is formed, but
If not suitably controlling the viscosity of masking liquid in the envelope is formed, it is difficult to obtain smooth and flawless envelope.
For this respect, contain the lotion of polymer using water as decentralized medium, exist as particle.Therefore, it does
Even if dry film is at first sight transparent and uniformly as it can be seen that but being easy to generation gap, be not easy shape between microscopic scale, particle and particle
At the envelope of flawless densification.
Therefore disclose in patent document 1 obtained by using specific reactive emulsifier and agglutinant it is high non-volatile
The method of the lotion containing polymer of ingredient.
In addition the lotion containing polymer that polymer is prepared by 2 stages is disclosed in patent document 2.
In addition the high nonvolatile component Patent Document 3 discloses the amount by adjusting polymerization initiator and emulsifier
The lotion containing polymer.
However, the amount of polymerization initiator, emulsifier is considerably less.Therefore, according to initiator, the measuring accuracy of emulsifier and it is outer
Sight state is easy to change, it is difficult to steady production.In addition, the mechanical stability of lotion is also insufficient.
The different latex particle of grain size (エ マ Le シ ョ Application particle) is mixed and improved in addition, being disclosed in patent document 4
Make film property and the lotion containing polymer of adhesive performance.
Existing technical literature
Patent document
Patent document 1：Japanese Unexamined Patent Publication 5-255411 bulletins
Patent document 2：Japanese Unexamined Patent Application 60-179402 bulletins
Patent document 3：Japanese Unexamined Patent Application 63-234076 bulletins
Patent document 4：Japanese Unexamined Patent Publication 4-320475 bulletins
Invention content
Problems to be solved by the invention
However, the lotion containing polymer of patent document 1 needs to use specific emulsifier, therefore there are the viscous of masking liquid
Property control, adhesive performance the narrow this problem of adjusting range.In addition, there is breast in the lotion containing polymer of patent document 2
The mechanical stability of liquid is insufficient, in addition, the working hour in terms of production is more, manufacturing time is also grown, therefore cost gets higher this problem.
In addition, the lotion containing polymer of patent document 3 since the usage amount of polymerization initiator and emulsifier is considerably less, exists
According to polymerization initiator, emulsifier measuring accuracy and the lotion containing polymer that obtains character variation etc., it is industrial difficult
With steady production, further, low this problem of mechanical stability of lotion.In addition, the breast containing polymer of patent document 4
Liquid needs to manufacture 2 kinds of lotions containing polymer respectively therefore there are the high this problems of production cost.
The object of the present invention is to provide can be synthesized by easy method, nonvolatile component is high, and due to viscosity is low
Fine and close envelope, the excellent emulsion resin composition for including the lotion containing polymer of mechanical stability can be formed.
Means for solving the problems
The emulsion resin composition of the present invention, which is characterized in that be included in the non-ionic water that boiling point is 80 DEG C or more
In the presence of soluble compound (except emulsifier), it will be contained made of monomer polymerization using emulsifier, water and polymerization initiator
The lotion of polymer；The nonionic water soluble compound that above-mentioned boiling point is 80 DEG C or more is the compound not being copolymerized with monomer；
0.05 μm of shared in the particle entirety of the above-mentioned lotion containing polymer, grain size is less than 0.6 μm of small particle particle
Shared ratio is 2~75 volume %, and the ratio shared by 5 μm of 0.6 μm of grain size or more big particle below is 25~98 bodies
Product %, also, the average grain diameter (D50 average grain diameters) of the lotion entirety containing polymer is 0.2 μm~2 μm.
The effect of invention
It is water-soluble by the nonionic for the use of boiling point being 80 DEG C or more for separately including appropriate amount according to the above-mentioned present invention
Property compound and the big particle and small particle particle that synthesize, to can get because small particle particle fills big particle
Between the gap that generates thus per unit volume nonvolatile component it is high, and the emulsion resin composition that viscosity is low.It uses
The envelope of the emulsion resin composition can form the envelope with fine and close surface.In addition, the emulsion resin composition
Also it can get the excellent such effect of mechanical stability.
By the invention it is possible to which providing can be synthesized by easy method, nonvolatile component is high, and due to viscosity is low
Fine and close envelope, the excellent emulsion resin composition for including the lotion containing polymer of mechanical stability can be formed.
Specific implementation mode
Term is defined before the present invention will be described.
The emulsion resin composition of the present invention includes the lotion containing polymer.
The above-mentioned lotion containing polymer, which is characterized in that 0.05 μm shared of grain size or more and small in the particle entirety
Ratio shared by 0.6 μm of small particle particle is 2~75 volume %, 5 μm of 0.6 μm of grain size or more big particle institute below
The ratio accounted for is 25~98 volume %, also, the average grain diameter (D50 average grain diameters) of the lotion entirety containing polymer is 0.2 μ
M~2 μm.
The present invention emulsion resin composition can it is preferable to use in purposes such as coating, stickers.
1. first embodiment
The first embodiment of the emulsion resin composition of the present invention is illustrated.
First embodiment be related to the present invention emulsion resin composition be included in boiling point be 80 DEG C or more it is non-from
In the presence of sub- property water soluble compound (except emulsifier), monomer polymerization is formed using emulsifier, water and polymerization initiator
The lotion containing polymer；The nonionic water soluble compound that above-mentioned boiling point is 80 DEG C or more is the change not being copolymerized with monomer
Close object；0.05 μm of shared in the particle entirety of the above-mentioned lotion containing polymer, grain size is less than 0.6 μm of small particle
Ratio shared by particle is 2~75 volume %, the ratio shared by 5 μm of 0.6 μm of grain size or more big particle below for 25~
98 volume %, also, the average grain diameter (D50 average grain diameters) of the lotion entirety containing polymer is 0.2 μm~2 μm.
The lotion containing polymer can be by being 80 DEG C or more of nonionic water solubility in boiling point in the present invention
In the presence of closing object (except emulsifier), monomer polymerization is obtained using emulsifier, water and polymerization initiator.
First embodiment is not emulsify monomer in advance with emulsifier, and monomer is directly put into emulsion polymerization place
Emulsion polymerization is carried out to obtain the embodiment (direct polymerization method) of the lotion containing polymer.
In emulsion polymerization, using raw materials such as water, monomer, emulsifier, polymerization initiators, but in these raw materials (especially water)
Including micro metal ion.The metal ion can work in emulsion polymerization in terms of the grain size for increasing lotion.This hair
It, will by being above-mentioned effect that 80 DEG C or more of nonionic water soluble compound can inhibit metal ion comprising boiling point in bright
The grain size of lotion containing polymer is adjusted to range appropriate, thus can obtain for high nonvolatile component, low viscosity it is molten
Liquid can form the emulsion resin composition of fine and close envelope.
Boiling point is 80 DEG C or more of nonionic water soluble compound (hereinafter referred to as nonionic water soluble compound)
Reduce the compound of the influence of metal ion, it is however preferred to have the compound of carbonyl, the compound with hydroxyl and chelating agent etc..
In addition, the nonionic water soluble compound that boiling point is 80 DEG C or more is not copolymerized with monomer, it is not emulsifier.So-called emulsifier,
Be if with stirred together with monomer if can form the compound of micella (Micelle).
As nonionic water soluble compound used in the present invention, it preferably is dissolved in water at 25 DEG C, and have
The compound of the boiling point of nonvolatile degree in the polymerization.In addition, nonionic water solubility chemical combination used in the present invention
As long as object has the property for being dissolved in water at 25 DEG C, in an embodiment of the present invention, without the concern for the upper limit of its boiling point.
Compound with carbonyl is preferably ketone, carboxylic acid, acid anhydrides etc..
Ketone can enumerate the diketone such as methyl iso-butyl ketone (MIBK), 2,3- pentanes diketone and 2,4- pentane diketone.
As carboxylic acid, can enumerate such as acetic acid, lactic acid, citric acid.
As acid anhydrides, can enumerate such as acetic anhydride.
As the compound with hydroxyl, can enumerate the water-soluble alcohol such as propyl alcohol, isopropanol, butanol and 2- butanol and
The polyalcohols such as glycol (such as ethylene glycol, propylene glycol, diethylene glycol (DEG) etc.) and glycerine, D-sorbite, pentaerythrite.
As chelating agent, can enumerate the ethylenediamine tetra-acetic acid of the amino carboxylic acid for example as organic system sodium salt (hereinafter,
Referred to as EDTA), crown ether etc..
The application method of nonionic water soluble compound when as emulsion polymerization, can be by all pre- of its usage amount
First put into reaction vessel (also referred to as locus of polymerization).Or part of it can be put into locus of polymerization, by remainder with
Monomer puts into locus of polymerization together.Nonionic water soluble compound is preferably put into the starting stage of emulsion polymerization,
Specifically, nonionic water soluble compound puts into locus of polymerization preferably since emulsion polymerization within about 1 hour.Thus
The control of the size distribution of lotion becomes easy.
The usage amount of nonionic water soluble compound relative to 100 parts by weight of monomer mixture, preferably 5ppm~
50000ppm, more preferably 10ppm~20000ppm, further preferably 20ppm~10000ppm.Nonionic water solubility
The usage amount for closing object, relative to 100 parts by weight of monomer mixture, can even more preferably be such as 20ppm~5000ppm,
20ppm~2000ppm, 20ppm~1500ppm, 20ppm~1000ppm, 30ppm~1000ppm, 30ppm~500ppm,
30ppm~400ppm, 30ppm~300ppm, 30ppm~200ppm, 30ppm~100ppm.It is water-soluble by using nonionic
Property compound 5ppm or more, is easily obtained the grain size of preferred range.In addition, if more than 50000ppm then unreacted monomers
It is easy to remain.
If using above-mentioned nonionic water soluble compound, grain size can be obtained as 0.05 μm less than 0.6 μ
Ratio shared by the small particle particle of m is 2~75 volume %, and the ratio shared by 0.6 μm or more 5 μm big particles below is
25~98 volume %, also, the breast containing polymer that the average grain diameter (D50 average grain diameters) of whole region is 0.2 μm~2 μm
Liquid.Particle size determination is the numerical value obtained by dynamic light scattering determination, can be made " Microtrac " etc. by day machine dress (strain)
It measures.
Additionally, it is preferred that the grain size of the lotion containing polymer 0.05 μm less than 0.6 μm of region and 0.6 μm with
Upper 5 μm of regions below are respectively provided at very big (peak), but very big (peak) of the grain size of the lotion containing polymer can also be
0.05 μm or more 5 μm of regions below are 1.
Further the preferably 0.05 μm of grain size less than 0.6 μm of region of the lotion containing polymer is 0.1~0.5
μm, the grain size in 0.6 μm or more 5 μm of regions below is 0.8~2 μm.
About the synthesis of the lotion containing polymer, nonionic water soluble compound is used to synthesize 0.6 μm or more 5 first
μm large-sized lotion (a) containing polymer below, then in the presence of the lotion (a) containing polymer of gained,
Lotion (b) containing polymer of 0.05 μm that monomer progress emulsion polymerization is obtained less than 0.6 μm of small particle
It is not influenced by the type of polymerization initiator and emulsifier, amount substantially, just to fill the gap of the lotion (a) containing polymer
Mode generate.Therefore, by the generation of the lotion (a) containing polymer and the generation of the lotion (b) containing polymer
When, change the composition of the monomer of input, can also change the composition of the polymer of (a) and (b), glass transition temperature (Tg),
Molecular weight can control the fine structure (form) of the dry coating of emulsion resin composition.Furthermore, it is possible to wide according to purposes
The materials such as general selected emulsifier, initiator.
The lotion containing polymer for controlling grain size as described above also can be in the state of maintaining low viscosity, will not
Volatile ingredient is set as 70% or more.
The monomer being used in the present invention is the monomer containing ethylene unsaturated group.
Monomer in the present invention is preferably (methyl) alkyl acrylate and contain carboxylic that the carbon atom number of alkyl is 1~14
The monomer of base.
(methyl) alkyl acrylate can enumerate such as (methyl) methyl acrylate, (methyl) ethyl acrylate, (methyl)
Propyl acrylate, (methyl) isopropyl acrylate, (methyl) butyl acrylate, (methyl) isobutyl acrylate, (methyl) propylene
The own ester of acid, (methyl) 2-ethyl hexyl acrylate, (methyl) 2-EHA, (methyl) decyl acrylate, (methyl) acrylic acid
Acrylate and corresponding methacrylate of the linear chain or branched chains aliphatic alcohol such as dodecyl ester etc..They can individually make
With or be applied in combination a variety of.
In (methyl) alkyl acrylate preferably 100 weight % of monomer mixture used in emulsion polymerization comprising 1~
98.9 weight %.In addition in the case where being used in sticker purposes, preferably 50~99.9 weight %.
Monomer containing carboxyl can enumerate such as acrylic acid, methacrylic acid, maleic anhydride, maleic acid, itaconic acid, crotons
Acid etc..
Contain 0.1~20 in monomer containing the carboxyl preferably 100 weight % of monomer mixture used in emulsion polymerization
Weight %, further preferably 0.2~5 weight %, further preferably 0.2~2 weight %.By containing 0.1~20 weight
Amount %'s makes emulsion polymerization be easy to carry out containing the monomer of carboxyl, and mechanical stability improves, and is easily obtained smooth envelope.
List other than (methyl) alkyl acrylate that carbon atom number as alkyl is 1~14 and the monomer containing carboxyl
Body (hereinafter referred to as other monomers) is, it is preferable to use following monomer.(methyl) acrylic acid 2- hydroxy methacrylates, (methyl) acrylic acid 2-
Hydroxy propyl ester, (methyl) acrylic acid 2- hydroxybutyls, (methyl) acrylic acid 4- hydroxybutyls, polyethylene glycol (methyl) acrylate
Deng the monomer containing alcohol hydroxyl group；The monomer containing epoxy group such as glycidyl acrylate, glycidyl methacrylate；
N- hydroxy alkyls (methyl) acrylamide, N- alkoxyalkyls (methyl) acrylamide, methylolation acrylamide, N- (1,1-
- 3 oxo butyl of dimethyl) (methyl) acrylamide monomer such as acrylamide, Diacetone Acrylamide；Ethylene containing phosphate
The vinyl monomers such as base monomer, vinyl acetate, styrene, butadiene；With methacrylate acetoacetoxyethyl,
Monomer containing alkoxysilyl；Isobornyl acrylate.
Other monomers can be in the 100 weight % of monomer mixture used in emulsion polymerization with 1~98.9 weight %'s
Ratio uses.
Above-mentioned other monomers can use one kind or two or more.
The envelope formed to make the emulsion resin composition by the coating present invention is the envelope of densification, can make to contain
There is the lotion of polymer to be crosslinked.In this case, if monomer uses the monomer with acetoacetoxy groups, in coating
Latex particle self-crosslinking each other in drying process etc..
Emulsifier is ingredient necessary to the emulsion polymerization of monomer in the present invention.Emulsifier can suitably select non-reaction
Property emulsifier, reactive emulsifier use.In addition, emulsifier has non-ionic emulsifier, cationic galactomannan according to ion species
Agent, anion emulsifier, but generally use non-ionic emulsifier, anion emulsifier.In addition reactive emulsifier is tool
There is the emulsifier of ethylene unsaturated group (エ チ レ Application not Eat and base).Furthermore, it is possible to separately coordinate epoxy hardener, nitrogen third
Pyridine curing agent.
Reactive emulsifier can enumerate the ammonium salt or sodium of such as polyoxyalkylene alkenyl ether, polyoxyalkylene alkenyl ether sulfuric ester
Salt, polyoxyethylene -1- (allyloxymethyl) alkyl ether, polyoxyethylene -1- (allyloxymethyl) alkyl ether sulphate
Ammonium salt or sodium salt etc..
Non-ionic emulsifier in non-reacted emulsifier, in addition to using polyoxyethylene alkyl ether as the polyoxyalkylene of representative
Other than the ether type such as the polycyclic phenyl ether of alkyl ether, polyoxyalkylene, it is solid that polyoxyethylene glyceryl ether fatty acid ester, polyoxyethylene can be enumerated
Change Castor Oil Fatty Acid ester, polyoxyethylene trimethylolpropane fatty acid ester, amino acid derivativges, polyglyceryl fatty acid ester, have
Machine silicon systems emulsifier etc..
Anion emulsifier in non-reacted emulsifier is preferably to be modified to above-mentioned non-ionic emulsifier
Sulfuric ester or its ammonium salt or its metal salt etc..
It is preferable to use 0.1~5 parts by weight relative to 100 parts by weight of monomer mixture for the usage amount of emulsifier, more preferably
0.5~2 parts by weight.By using 0.1~5 parts by weight, the generation of agglutinator is few, and emulsion intercalation method when emulsion polymerization carries
It is high.
Polymerization initiator can use water-soluble polymerization initiator and water-insoluble polymerization initiator in the present invention, preferably
For water-soluble polymerization initiator.
Water-soluble polymerization initiator is preferably persulfate, water-soluble azo initiator and peroxide.
As water-soluble azo initiator, such as 4 can be enumerated, ammonium salt, 2, the 2 '-azos of the double -4- cyanopentanoic acids of 4 '-azos
Bis- (2- methybutanes amidoxime) the dihydrochloride tetrahydrates of bis- (2- methyl nitrosoureas oxime) dihydrochlorides, 2,2 '-azos, 2,2 '-
Azo bis- { 2- methyl-N- (bis- (the hydroxymethyl) -2- hydroxyethyls of 1,1-)-propionamides } and the bis- (2- methyl-N- of 2,2 '-azos
(2- hydroxyethyls)-propionamide) etc..
As persulfate, can enumerate such as potassium peroxydisulfate, sodium peroxydisulfate, ammonium persulfate.
As polymerization initiator, it is preferably also combined with the initiator (Redox Initiator of polymerization initiator and reducing agent
Agent).It being capable of emulsion polymerization at lower temperatures by using redox initiator.
As the combination of redox initiator, preferably for example as the hydrogen peroxide of peroxide, tertiary butyl hydrogen mistake
Oxide, benzoyl peroxide, cumene hydroperoxide etc. and the rongalite and sodium pyrosulfite etc. as reducing agent
Combination；The combination of the persulfates such as sodium peroxydisulfate and ammonium persulfate and rongalite and sodium thiosulfate etc., aquae hydrogenii dioxidi with it is anti-
The combination of bad hematic acid；Deng.
The usage amount of polymerization initiator relative to 100 parts by weight of monomer mixture, it is preferable to use 0.02~3 parts by weight, more
Preferably 0.1~1 parts by weight.
As the adding method of polymerization initiator, preferably its whole amount is put into reaction vessel, it is poly- to carry out lotion
The method of conjunction；A part for polymerization initiator is put into reaction vessel, remainder is added or is added dropwise by several times and is carried out
The method of emulsion polymerization；The method etc. that the whole amount of polymerization initiator is subjected to gradation addition or dropwise addition and carries out emulsion polymerization.
In addition, by polymerization initiator by several times add or be added dropwise in the case of, can with the mixed state of the lotion containing monomer
It is lower to use polymerization initiator.
The water used in emulsion polymerization is not particularly limited, but in the lotion containing polymer for making high nonvolatile component
In the case of, it is 10~50 weight % or so in the 100 weight % of lotion containing polymer.
When emulsion polymerization, in order to control gained polymer molecular weight, chain-transferring agent can be used.Specifically, excellent
It is selected as mercaptan based compound, thioglycol based compound, β-mercaptopropionic acid based compound etc..
Chain-transferring agent is preferably 0.001~2 parts by weight or so relative to 100 parts by weight of monomer mixture.
In addition can include tackifying resin when emulsion polymerization.Tackifying resin is preferably rosin series resin, terpene system resin, virtue
Fragrant family Petropols, fatty family Petropols etc..
As rosin series resin, such as natural rosin, rosin ester, hydrogenated rosin, hydrogenated wood rosin glycerol ester, polymerization pine can be enumerated
Perfume, newtrex ester, disproportionated rosin, disproportionated rosin ester etc..
As terpene system resin, can enumerate such as α pinene resin, nopinene resin, terpene-phenolic resin, hydrogenation terpene-phenolic resin.
As aromatic system Petropols, such as styrene oligomer, α-methylstyrene/styrol copolymer can be enumerated
Deng.
Tackifying resin is preferably able to be dissolved in monomer, but can also be used as with the tackifier resin emulsion of emulsifier and
It uses.
In addition, when emulsion polymerization, for the raising of emulsion intercalation method or the raising of mechanical stability, can also use
Neutralizer or pH buffer.In addition pH when emulsion polymerization is preferably 2~7, and more preferably 2~6.
The glass transition temperature (Tg) for the polymer that lotion containing polymer is included is according to the combination of monomer, preferably
For 100 DEG C hereinafter, more preferably 50 DEG C or less.In addition in the case of sticker purposes, Tg is preferably 0 DEG C or less.In addition, meter
The method for calculating the Tg of polymer can easily calculate the Tg of homopolymer using the formula of such as FOX.
The emulsion resin composition of the present invention can include above-mentioned lotion and neutralizer containing polymer.As neutralization
Agent can enumerate the alkali compounds such as ammonium hydroxide, sodium hydroxide, potassium hydroxide, water-soluble amine, generally by the lotion containing polymer
PH value is adjusted to 5 or more.In the case where pH value is less than 5, the stability of the latex particle containing polymer is not easy to obtain.PH value
There is no a special upper limit, generally 9 or less Zuo You.
The present invention emulsion resin composition can further coordinate tackifying resin, wetting agent, crosslinking agent, antifoaming agent,
Neutralizer, preservative etc..
Tackifying resin preferably coordinates the tackifier resin emulsion illustrated in epimere.
Wetting agent is the high surfactant of the ability that makes the surface tension of emulsion resin composition reduce, is for example to have
Have and is usually contained in the case of coating masking liquid on the stripping film of organosilicon peeling layer.Wetting agent is preferably such as acetylenediol system
Compound, dioctyl sodium sulphosuccinate, silicon-type emulsifier etc..
Crosslinking agent for can be included with the polymer in the lotion containing polymer reactive functional groups (such as
Hydroxyl, carboxyl, epoxy group etc.) compound of functional group reacted.
As crosslinking agent, it is sub- that such as hydrazide compound, semicarbazide derivative, isocyanates based compound, carbon two can be enumerated
Amine compound, aziridine based compound, epoxy based compound, the metal based compound etc. that complexing can be formed.
The usage amount of crosslinking agent is excellent relative to total 100 parts by weight of polymer included in the lotion containing polymer
It is selected as 0.1~30 parts by weight, more preferably 0.1~10 parts by weight, further preferably 0.1~3 parts by weight.
Antifoaming agent is generally the group for having coordinated inorganic compounds such as mineral oil, polyethers, emulsifier, hydrophobic silica etc.
Close object.The non-ionic emulsifier that mentioned emulsifier mainly can use HLB low.
The corruption of emulsion resin composition in order to prevent can coordinate preservative.As preservative, isothiazole can be enumerated
Quinoline derivant, benzalkonium chloride, benzethonium chloride, sodium hypochlorite, povidone iodine, pyridine thiol derivative, hydrogen peroxide, ethyl alcohol
Deng.
The emulsion resin composition of the present invention can arbitrarily include further various additives etc..Specifically, can lift
Go out the water soluble ingredients such as organic silicon-type resin, antifoaming agent, neutralizer, plasticizer, thickener, colorant, preservative, antirust agent,
The oil-soluble ingredients such as solvent, colorant, hydrophober.
The emulsion resin composition of the present invention can coordinate mentioned component, be filled using being stirred known to homogeneous mixer etc.
It sets to make.
2. second embodiment
Illustrate the second embodiment of the emulsion resin composition of the present invention.
The emulsion resin composition of the present invention, which is characterized in that be included in the non-ionic water that boiling point is 80 DEG C or more
The use of polymerization initiator will include using (methyl) alkyl acrylate as master in the presence of soluble compound (except emulsifier)
The lotion containing monomer of the monomer of ingredient, emulsifier and water carries out the breast containing acrylic acid series polymeric compounds made of emulsion polymerization
Liquid；The nonionic water soluble compound that above-mentioned boiling point is 80 DEG C or more is the compound not being copolymerized with above-mentioned monomer；Contain third
Shared by shared by the particle entirety of the lotion of olefin(e) acid based polymer, 0.05 μm of small particle particle less than 0.6 μm
Ratio is 2~75 volume %, and the ratio shared by 0.6 μm or more 5 μm big particles below is 25~98 volume %, also,
The average grain diameter (D50 average grain diameters) of lotion containing acrylic acid series polymeric compounds is 0.2 μm~2 μm.
Second embodiment is monomer will to be made to be mixed with water, emulsifier for mixing and the pre-emulsification object that makes is put into lotion and gathered
It closes place and carries out emulsion polymerization to obtain the embodiment (pre-emulsifying method) of the lotion containing polymer.
Pre-emulsification object is water and the unseparated degree of lipophilic constituent under static condition, generally, it is preferred to be stirred mixed
It closes until 50% grain size of the latex particle containing monomer is 100 μm or less Zuo You.In addition, so-called " 50% grain size ", refers to body
Median particle diameter (D50 average grain diameters) in product benchmark.
The usage amount of other ingredients is same as the content illustrated in first embodiment.
The manufacturing method of the emulsion resin composition of the present invention is illustrated.
The manufacturing method of emulsion resin composition has following processes (1)~(2).
(1) water-soluble for 80 DEG C or more of nonionic not with the copolymerization of free-radical polymerised unsaturated monomer, boiling point
In the presence of compound (except emulsifier), make free-radical polymerised unsaturated monomer using emulsifier, water and polymerization initiator
Emulsion polymerization is carried out, to obtain the process that grain size is 0.6 μm or more the 5 μm lotions (a) below containing polymer.
Wherein, above-mentioned boiling point be 80 DEG C or more nonionic water soluble compound it is as already described, be not with
The compound of above-mentioned monomer copolymerization.
(2) in the presence of the lotion (a) containing polymer, monomer is made to carry out using emulsifier, water and polymerization initiator
Emulsion polymerization is 0.05 μm of process less than 0.6 μm of the lotion (b) containing polymer to obtain grain size.
The grain moreover, D50 of the above-mentioned lotion containing polymer in the emulsion-based composition obtained in above-mentioned operation is averaged
Diameter is 0.2 μm or more 2 μm hereinafter, also, the emulsion-based composition that is obtained in above-mentioned operation comprising grain size is 0.6 μm or more 5 μm
Lotion (a) below containing polymer and grain size are 0.05 μm less than 0.6 μm of the lotion (b) containing polymer.
In above-mentioned operation (1) and process (2), in the emulsion polymerization of monomer, direct polymerization method or pre-emulsification can be used
Any emulsion polymerization in method, but more preferably pre-emulsifying method.
In addition, the reaction temperature in above-mentioned operation (1) and process (2) is usually 40 DEG C~90 DEG C, preferably 70 DEG C~90
DEG C or so.
The emulsion resin composition of the present invention can be in additive, the sticker etc. in smears, various water paints
With using on the way.
The painting method of emulsion resin composition is not particularly limited, can with brushing machine, comma coater, scrape cutter painting
The previously known painting such as the roll coaters such as cloth machine, gravure coater, slot-die coater, slit coater, curtain coater
Cloth apparatus is carried out with arbitrary coating speed.
It is dry generally to be carried out 30 seconds~5 minutes in room temperature~120 DEG C, tens of seconds are especially often carried out before and after 100 DEG C,
As long as however, not limited to this, the condition of the volatile ingredient in can fully removing the layer of formation.
The thickness of envelope is preferably 5~100 μm, more preferably 10~60 μm.
The emulsion resin composition of the present invention makes easily controllable extensive size distribution, and mechanical stability is excellent to be contained
There is the lotion of polymer.
The emulsion resin composition of the present invention is used preferably as the raw material of coating, bonding agent, sticker etc..That is, this
The emulsion resin composition of invention uses preferably on the base materials such as steel plate, paper, plastics as the coating material for forming envelope.
Embodiment
Hereinafter, the specific embodiment of the present invention is illustrated together with comparative example, but the present invention is not limited to following
Embodiment.In addition, in following embodiments and comparative example, " part " is " parts by weight ", " % " expression " weight % ".In addition, by polyoxy
The repeat number for changing the ethylene oxide of ethylene unit is set as " EO numbers ".
Embodiment 1
It is used in the polymerization for having heating device, blender, reflux cooling device, thermometer, nitrogen ingress pipe and 3 dropwise adding tanks
In container, 45 parts of 45 parts of 2-EHA, the butyl acrylate as monomer, third are added first in the first dropwise adding tank
The mixture of 6 parts of e pioic acid methyl ester, 3 parts of methyl methacrylate, 1 part of acrylic acid.The glass transition temperature found out by FOX formulas
It is -54.3 DEG C.
Next by polymerization with container in a nitrogen atmosphere, 0.1 part of 43 parts of pure water and isopropanol is added. while stirring
0.075 part of 3% persulfate aqueous solution is added as nonvolatile component until 80 DEG C of interior temperature for heating.After 10 minutes, through 4
Monomer mixture is added dropwise from the first dropwise adding tank respectively in hour, and 3% persulfate aqueous solution is added dropwise (as not waving from the second dropwise addition layer
It is 0.225 part to send out ingredient), the mixture of polyoxyethylene alkyl ether sodium sulphate is added dropwise from third dropwise adding tank, carries out emulsion polymerization.Drop
After adding, is kept for 30 minutes at 80 DEG C, interior temperature is then set as 60~65 DEG C through 30 minutes, was divided into every 10 minutes 3 times
Add 0.12 part of 0.1 part of tert-butyl hydroperoxide and rongalite.After further reacting 1 hour while stirring, ammonium hydroxide is used
It neutralizes and pH is made to become 7.5, be filtered, obtain the lotion containing polymer.This contain the lotion of polymer it is non-volatile at
It is divided into 65.1%, viscosity 80mPas.In addition viscosity uses Brookfield viscometer, under conditions of 25 DEG C in #2 rotors/60rpm
It measures (same as below).Nonvolatile component by with electric dry oven at 150 DEG C dry weight after twenty minutes relative to the weight before drying
The weight ratio of amount is found out.
The lotion containing polymer of gained is respectively provided with maximum for 0.21 μm and 1.29 μm in grain size, and 50% grain size is
0.27μm.In the containing ratio of 0.21 μm of grain size 0.05 μm with maximum less than 0.6 μm of small particle particle,
It is 60 volume % in the case that total volume of the latex particle of the lotion containing polymer of gained is set as 100 volume %,
Average grain diameter (D50 average grain diameters) is 0.32 μm.Occupy remaining 40 volume % particle be at 1.29 μm with maximum,
Grain size is 0.6 μm or more 5 μm of big particles below, and the average grain diameter (D50 average grain diameters) in the region is 1.21 μm.Separately
Outside, particle size determination is measured using day machine dress (strain) system " Microtrac ".
The lotion that this is contained to polymer evaluates the mechanical stability (lotus of lotion using Maron mechanical stability testing machines
Weight 15kg, rotating speed 1000rpm, 10 minutes) (same as below), object amount is as a result aggregated relative to 100 weight of lotion containing polymer
Amount part is 0.03 parts by weight.
In 100 parts of the lotion containing polymer of gained, 0.05 part of antifoaming agent is added, as the water-soluble of wetting agent
0.5 part of dioctyl sodium sulphosuccinate, 0.2 part of preservative measure viscosity.As a result being 150mPas (can use thickener
To make the emulsion resin composition of 150mPas or more), further polybasic carboxylic acid system thickener and ammonium hydroxide are added
Mixing dispersion, obtains the emulsion resin composition of 1000mPas.
Embodiment 2
It is used in the polymerization for having heating device, blender, reflux cooling device, thermometer, nitrogen ingress pipe and 3 dropwise adding tanks
In container, 45 parts of 2-EHA, 45 parts of butyl acrylate, methyl acrylate are obtained in the first dropwise adding tank first
6 parts, the mixture of 3 parts of methyl methacrylate, 1 part of acrylic acid.In the mixture, it is further added as water-soluble non-
25 parts of 1 part of the polyoxyethylene alkyl ether sodium sulphate of reactive emulsifier and pure water, are stirred, obtain pre-emulsification object.By upper
Glass transition temperature stating the polymer that the composition of monomer obtains, being found out by FOX formulas is -54.3 DEG C.
Next by polymerization with container in a nitrogen atmosphere, 0.1 part of 18 parts of pure water and isopropanol is added. while stirring
Heating is until 80 DEG C of interior temperature.And add 0.075 part of 3% persulfate aqueous solution as nonvolatile component.After 10 minutes,
Pre-emulsification object was added dropwise from the first dropwise adding tank respectively through 4 hours, 3% persulfate aqueous solution is added dropwise (as not from the second dropwise adding tank
Volatile ingredient is 0.225 part), carry out emulsion polymerization.
After completion of dropwise addition, is kept for 30 minutes at 80 DEG C, interior temperature is then set as 60~65 DEG C through 30 minutes, every 10 points
Clock is divided into 3 times and adds 0.12 part of 0.1 part of tert-butyl hydroperoxide and rongalite.It is further reacted while stirring 1 hour
Afterwards, being neutralized with ammonium hydroxide becomes 7.5 until pH, is filtered and obtains the lotion containing polymer.This contains the breast of polymer
The nonvolatile component of liquid is 65.2%, viscosity 75mPas.
The lotion containing polymer of gained is respectively provided with maximum for 0.19 μm and 1.60 μm in grain size, and 50% grain size is
0.30μm.In the containing ratio of 0.19 μm of grain size 0.05 μm with maximum less than 0.6 μm of small particle particle,
It is 60 volume % in the case that total volume of the latex particle of the lotion containing polymer of gained is set as 100 volume %,
Average grain diameter (D50 average grain diameters) is 0.20 μm.The particle for occupying remaining 40 volume % be at 1.60 μm have maximum,
Grain size is 0.6 μm or more 5 μm of big particles below, and the average grain diameter (D50 average grain diameters) in the region is 1.37 μm.
In 100 parts of the lotion containing polymer of gained, 0.05 part of antifoaming agent is added, as the water-soluble of wetting agent
0.5 part of dioctyl sodium sulphosuccinate, 0.2 part of preservative measure viscosity, and result, which is 180mPas, (can use thickener
To make the emulsion resin composition of 180mPas or more), further polybasic carboxylic acid system thickener and ammonium hydroxide are added
Add mixing to disperse, obtains the emulsion resin composition of 1000mPas.
Below in embodiment 3~7, viscosity is similarly measured, is all 200mPas or less.
Embodiment 3
The isopropanol used in embodiment 2 is replaced as ethylenediamine tetra-acetic acid, in addition to this, similarly to Example 2 into
It goes and obtains emulsion resin composition.
Embodiment 4
The isopropanol used in embodiment 2 is replaced as glycerine, in addition to this, is performed in the same manner as in Example 2 and obtains
Emulsion resin composition.
Embodiment 5
The polyoxyethylene alkyl ether sodium sulphate used in embodiment 4 is replaced as the polyoxy second as reactive emulsifier
Alkene -1- (allyloxymethyl) alkyl sulfates carry out in addition to this and obtain emulsion-type similarly to Example 4
Resin combination.
Embodiment 6
The polyoxyethylene alkyl ether sodium sulphate used in embodiment 4 is replaced as the polyoxy second as non-reacted emulsifier
Alkene styrenated phenyl ether ammonium sulfate carries out in addition to this and obtains emulsion resin composition similarly to Example 4.
Embodiment 7
The usage amount of the polyoxyethylene styrene phenyl ether ammonium sulfate used in embodiment 6 is altered to 2.0 weight %,
In addition to this, it carries out similarly to Example 6 and obtains emulsion resin composition.
Embodiment 8
It is used in the polymerization for having heating device, blender, reflux cooling device, thermometer, nitrogen ingress pipe and 3 dropwise adding tanks
In container, first by 45 parts of 2-EHA, 45 parts of butyl acrylate, 6 parts of methyl acrylate, methyl methacrylate
3 parts, 1 part of acrylic acid, 5 parts of the rosin series resin " Pine Crystal KE100 " (waste river chemical (strain) system) as tackifying resin
Mixing, tackifying resin is dissolved in monomer, obtains mixture.In the mixture, it is added as water-soluble non-reacted
41 parts of 1 part of the polyoxyethylene styrene phenyl ether ammonium sulfate of emulsifier and pure water, are stirred, and further use homogeneous mixing
Machine obtains the pre-emulsification object that average grain diameter (D50 average grain diameters) is 3 μm.The pre-emulsification object of gained is added to the first dropwise addition
Slot.
Next by polymerization with container in a nitrogen atmosphere, 0.1 part of 18 parts of pure water and glycerine is added, is risen while stirring
Temperature adds 0.075 part of 3% persulfate aqueous solution as nonvolatile component until 80 DEG C of interior temperature.After 10 minutes, through 4
Pre-emulsification object is added dropwise from the first dropwise adding tank respectively in hour, and 3% persulfate aqueous solution is added dropwise (as non-volatile from the second dropwise adding tank
Ingredient is 0.225 part), carry out emulsion polymerization.
After completion of dropwise addition, is kept for 30 minutes at 80 DEG C, interior temperature is then set as 60~65 DEG C through 30 minutes, every 10 points
Clock is divided into 3 times and adds 0.12 part of 0.1 part of tert-butyl hydroperoxide and rongalite.It is further reacted while stirring 1 hour
Afterwards, being neutralized with ammonium hydroxide makes pH become 7.5, is filtered and obtains the lotion containing polymer.This contains the breast of polymer
The nonvolatile component of liquid is 60.2%, viscosity 100mPas.It is similarly tested with embodiment 1 below.
Embodiment 9
It is used in the polymerization for having heating device, blender, reflux cooling device, thermometer, nitrogen ingress pipe and 3 dropwise adding tanks
In container, 45 parts of 2-EHA, 45 parts of butyl acrylate, methyl acrylate are obtained in the first dropwise adding tank first
6 parts, the mixture of 3 parts of methyl methacrylate, 1 part of acrylic acid.In the mixture, it is further added as water-soluble non-
25 parts of 1 part of the polyoxyethylene styrene phenyl ether ammonium sulfate of reactive emulsifier and pure water, are stirred, obtain pre-emulsification
Object.By above-mentioned monomer form the polymer obtained, the glass transition temperature that is found out by FOX formulas be -54.3 DEG C.
Next by polymerization with container in a nitrogen atmosphere, 0.05 part of 18 parts of pure water and glycerine is added. while stirring
Heating is until 80 DEG C of interior temperature.And add 0.075 part of 3% persulfate aqueous solution as nonvolatile component.After 10 minutes,
Pre-emulsification object was added dropwise from the first dropwise adding tank respectively through 4 hours, 3% persulfate aqueous solution is added dropwise (as not from the second dropwise adding tank
0.225 part of volatile ingredient), carry out emulsion polymerization.
After completion of dropwise addition, is kept for 30 minutes at 80 DEG C, interior temperature is then set as 60~65 DEG C through 30 minutes, every 10 points
Clock is divided into 3 times and adds 0.12 part of 0.1 part of tert-butyl hydroperoxide and rongalite.It is further reacted while stirring 1 hour
Afterwards, being neutralized with ammonium hydroxide makes pH become 7.5, is filtered and obtains the lotion containing polymer.This contains the breast of polymer
The nonvolatile component of liquid is 65.1%, viscosity 72mPas.
The lotion containing polymer of gained is respectively provided with maximum for 0.24 μm and 1.20 μm in grain size, and 50% grain size is
1.05μm.In the containing ratio of 0.24 μm of grain size 0.05 μm with maximum less than 0.6 μm of small particle particle,
It is 62 volume % in the case that total volume of the latex particle of the lotion containing polymer of gained is set as 100 volume %,
Average grain diameter (D50 average grain diameters) is 0.34 μm.The particle for occupying remaining 38 volume % be at 1.20 μm have maximum,
Grain size is 0.6 μm or more 5 μm of big particles below, and the average grain diameter (D50 average grain diameters) in the region is 1.30 μm.
In 100 parts of the lotion containing polymer of gained, 0.05 part of antifoaming agent is added, as the water-soluble of wetting agent
0.5 part of dioctyl sodium sulphosuccinate, 0.2 part of preservative measure viscosity, and result, which is 190mPas, (can use thickener
To make the emulsion resin composition of 180mPas or more), further polybasic carboxylic acid system alkalinity thickener and ammonium hydroxide are carried out
Addition mixing dispersion, obtains the emulsion resin composition of 1000mPas.
Embodiment 10
The amount of the glycerine used in embodiment 9 is altered to 0.02 part, in addition to this, carry out similarly to Example 9 and
Obtain emulsion resin composition.
Embodiment 11
The amount of the glycerine used in embodiment 9 is altered to 0.003 part, in addition to this, carry out similarly to Example 9 and
Obtain emulsion resin composition.
Embodiment 12
The amount of the glycerine used in embodiment 9 is altered to 0.15 part, in addition to this, carry out similarly to Example 9 and
Obtain emulsion resin composition.
Embodiment 13
The glycerine used in embodiment 9 is altered to 2,4- pentane diketone, in addition to this, is carried out similarly to Example 9
And obtain emulsion resin composition.
Embodiment 14
The glycerine used in embodiment 9 is altered to ethylene glycol, in addition to this, carries out and obtains similarly to Example 9
Emulsion resin composition.
Embodiment 15
The glycerine used in embodiment 9 is altered to pentaerythrite, in addition to this, carries out and obtains similarly to Example 9
Obtained emulsion resin composition.
Comparative example 1
It is performed in the same manner as in Example 2 in addition to this without using the isopropanol used in embodiment 2 and obtains lotion
Type resin combination.
Comparative example 2
Hold in the polymerization for having heating device, blender, reflux cooling device, thermometer, nitrogen ingress pipe and dropwise adding tank
In device, the mixture of 132 parts of butyl acrylate, 15 parts of vinyl acetate, 3 parts of acrylic acid is obtained first.
In the mixture, be added 0.5 part of neopelex as water-soluble non-reacted emulsifier with
50 parts of pure water, is stirred, is disperseed with homogeneous mixer, obtains pre-emulsification object.The pre-emulsification object is added to the first dropwise addition
Slot.
Next by polymerization with container in a nitrogen atmosphere, be added 50 parts of pure water, heated up while stirring until interior temperature
80 DEG C, 0.3 part of 0.6% ammonium persulfate aqueous solution is added as nonvolatile component.After 5 minutes, it was added dropwise through 5 hours from first
Pre-emulsification object is added dropwise in slot, has carried out emulsion polymerization.After emulsion polymerization, neutralize so that pH becomes 7.5, being filtered with ammonium hydroxide
And obtain the lotion containing polymer.The nonvolatile component for containing the lotion of polymer is 60.2%, viscosity 90mPa
s。
Comparative example 3
Without using isopropanol used in embodiment 1, in addition to this, carries out similarly to Example 1 and obtain lotion
Type resin combination, agglutinator are very more.
Following evaluations have been carried out to the emulsion resin composition of gained.
By film analysis：The emulsion resin composition of gained is coated on fissility piece, is dried and obtains thickness
50 μm of envelope.Then the PET film of 50 μm of thickness is made to fit in envelope and make sample.The sample is put into 40 DEG C of warm water
And it places 12 hours.Sample is then taken out, multiple light courcess spectral photometric colour measuring meter (SUGA testing machines are used under 23 DEG C of -50% atmosphere
(strain) makes) and measure the L* (lightness) of sample.In addition the smaller then whiteness of the value of L* is lower, therefore can form fine and close quilt
Film.
[table 1]
Claims (6)
1. a kind of emulsion resin composition, it includes：
Lotion containing polymer, the lotion containing polymer be boiling point except emulsifier be 80 DEG C or more it is non-from
In the presence of sub- property water soluble compound, made of so that monomer is carried out emulsion polymerization using emulsifier, water and polymerization initiator, with
And
Neutralizer；
The nonionic water soluble compound that the boiling point is 80 DEG C or more is the compound not being copolymerized with the monomer and is selected from
It is compound with carbonyl, at least one kind of in compound and chelating agent with hydroxyl；
Shared, grain size is 0.05 μm less than 0.6 μm of granule in the particle entirety of the lotion containing polymer
Ratio shared by diameter particle is 2~75 volume %, and the ratio shared by 5 μm of 0.6 μm of grain size or more big particle below is 25
~98 volume %, also, the D50 average grain diameters of the lotion entirety containing polymer are 0.2 μm~2 μm.
2. a kind of emulsion resin composition, it includes：
Lotion containing acrylic acid series polymeric compounds, the lotion containing acrylic acid series polymeric compounds are the boiling points except emulsifier
In the presence of 80 DEG C or more of nonionic water soluble compound, made comprising with (methyl) alkyl acrylate using polymerization initiator
Made of base ester carries out emulsion polymerization for the lotion containing monomer of the monomer of principal component, emulsifier and water, and
Neutralizer；
The nonionic water soluble compound that the boiling point is 80 DEG C or more is the compound not being copolymerized with the monomer and is selected from
It is compound with carbonyl, at least one kind of in compound and chelating agent with hydroxyl；
Shared by the particle entirety of lotion containing acrylic acid series polymeric compounds, grain size is 0.05 μm less than 0.6 μm
Ratio shared by small particle particle is 2~75 volume %, and the ratio shared by big particle that grain size is 0.6 μm~5 μm is 25
~98 volume %, also, the D50 average grain diameters of the lotion containing acrylic acid series polymeric compounds are 0.2 μm or more 2 μm or less.
3. a kind of sticker, it includes emulsion resin compositions as claimed in claim 1 or 2.
4. a kind of coating, it includes emulsion resin compositions as claimed in claim 1 or 2.
5. a kind of coating material, has：Base material and the quilt formed by emulsion resin composition as claimed in claim 1 or 2
Film.
6. a kind of manufacturing method of emulsion resin composition, the emulsion resin composition includes that grain size is 0.6 μm or more 5
μm lotion (a) below containing polymer and grain size are 0.05 μm less than 0.6 μm of the lotion containing polymer
(b), the D50 average grain diameters of the lotion containing polymer be 0.2 μm or more 2 μm hereinafter,
The manufacturing method has following processes：
(1) in the presence of the boiling point except emulsifier is 80 DEG C or more of nonionic water soluble compound, emulsifier, water are used
So that free-radical polymerised unsaturated monomer is carried out emulsion polymerization with polymerization initiator, to obtain grain size be 0.6 μm or more 5 μm with
Under the lotion (a) containing polymer process,
And the nonionic water soluble compound that the boiling point is 80 DEG C or more be not with the free-radical polymerised unsaturation
The compound and at least one kind of in the compound with carbonyl, compound and chelating agent with hydroxyl of monomer copolymerization, with
And
(2) in the presence of the lotion (a) containing polymer, monomer is made to carry out lotion using emulsifier, water and polymerization initiator
Polymerization is 0.05 μm of process less than 0.6 μm of the lotion (b) containing polymer to obtain grain size.
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| JP2014-076377 | 2014-04-02 | ||
| JP2014076377 | 2014-04-02 | ||
| PCT/JP2015/060311 WO2015152318A1 (en) | 2014-04-02 | 2015-04-01 | Emulsion resin composition and method for producing same |
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| JP7439750B2 (en) * | 2018-04-23 | 2024-02-28 | 株式会社レゾナック | Latex and adhesive compositions for adhesive compositions |
| CN112724760B (en) * | 2020-12-29 | 2022-05-10 | 富思特新材料科技发展股份有限公司 | Stain-resistant coating and preparation method and application thereof |
| CN114447523B (en) * | 2021-12-23 | 2024-03-22 | 山东华夏神舟新材料有限公司 | Polyvinylidene fluoride emulsion for lithium ion secondary battery diaphragm and preparation method thereof |
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| CN1408807A (en) * | 2001-09-26 | 2003-04-09 | 日本合成化学工业株式会社 | Method for producing emulsion type adhesive composition |
| CN101974184A (en) * | 2010-09-29 | 2011-02-16 | 苏州凯康化工科技有限公司 | Water-based acrylic emulsion and preparation method and application thereof |
| CN102272168A (en) * | 2009-01-09 | 2011-12-07 | 东洋油墨Sc控股株式会社 | Polymer emulsion and aqueous inkjet recording liquid containing said polymer emulsion |
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| JP2002146275A (en) * | 2000-11-16 | 2002-05-22 | Daicel Chem Ind Ltd | Aqueous coating agent for inorganic building material and aqueous coating material composition for inorganic building material |
| JP2005036189A (en) * | 2003-07-14 | 2005-02-10 | Rohm & Haas Co | Method of aqueous polymerization for preparing aqueous polymer dispersion |
| JP2007224185A (en) * | 2006-02-24 | 2007-09-06 | Toyo Ink Mfg Co Ltd | Foamed sheet with adhesive layer and method for producing the same |
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| CN1408807A (en) * | 2001-09-26 | 2003-04-09 | 日本合成化学工业株式会社 | Method for producing emulsion type adhesive composition |
| CN102272168A (en) * | 2009-01-09 | 2011-12-07 | 东洋油墨Sc控股株式会社 | Polymer emulsion and aqueous inkjet recording liquid containing said polymer emulsion |
| CN101974184A (en) * | 2010-09-29 | 2011-02-16 | 苏州凯康化工科技有限公司 | Water-based acrylic emulsion and preparation method and application thereof |
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| JP2015199955A (en) | 2015-11-12 |
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