CN101845124B - Water-based hydrophobic nano-resin, glass thermal insulating coating and preparation method - Google Patents
Water-based hydrophobic nano-resin, glass thermal insulating coating and preparation method Download PDFInfo
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- CN101845124B CN101845124B CN2010101325322A CN201010132532A CN101845124B CN 101845124 B CN101845124 B CN 101845124B CN 2010101325322 A CN2010101325322 A CN 2010101325322A CN 201010132532 A CN201010132532 A CN 201010132532A CN 101845124 B CN101845124 B CN 101845124B
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 46
- 239000011521 glass Substances 0.000 title claims abstract description 38
- 229920005989 resin Polymers 0.000 title claims abstract description 38
- 239000011347 resin Substances 0.000 title claims abstract description 38
- 239000011248 coating agent Substances 0.000 title claims abstract description 37
- 238000000576 coating method Methods 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title abstract description 10
- -1 vinyl siloxane Chemical class 0.000 claims abstract description 38
- 239000000178 monomer Substances 0.000 claims abstract description 37
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 35
- 239000008367 deionised water Substances 0.000 claims abstract description 33
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 32
- 239000003999 initiator Substances 0.000 claims abstract description 26
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 17
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 32
- 238000006243 chemical reaction Methods 0.000 claims description 31
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 17
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- 230000003472 neutralizing effect Effects 0.000 claims description 14
- SKRWFPLZQAAQSU-UHFFFAOYSA-N stibanylidynetin;hydrate Chemical compound O.[Sn].[Sb] SKRWFPLZQAAQSU-UHFFFAOYSA-N 0.000 claims description 14
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 13
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 11
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 9
- 239000013530 defoamer Substances 0.000 claims description 9
- 239000002562 thickening agent Substances 0.000 claims description 9
- 239000004160 Ammonium persulphate Substances 0.000 claims description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 7
- 235000019395 ammonium persulphate Nutrition 0.000 claims description 7
- AGUIILSGLFUTKG-UHFFFAOYSA-N CC(C)O.CC(C)O.CC(C)O.C=C[SiH3] Chemical compound CC(C)O.CC(C)O.CC(C)O.C=C[SiH3] AGUIILSGLFUTKG-UHFFFAOYSA-N 0.000 claims description 6
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 6
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 6
- OWUTVCVPEOXXHD-UHFFFAOYSA-N trimethoxy(prop-1-enyl)silane Chemical compound CO[Si](OC)(OC)C=CC OWUTVCVPEOXXHD-UHFFFAOYSA-N 0.000 claims description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 5
- 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 claims description 5
- JYMITAMFTJDTAE-UHFFFAOYSA-N aluminum zinc oxygen(2-) Chemical compound [O-2].[Al+3].[Zn+2] JYMITAMFTJDTAE-UHFFFAOYSA-N 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- WGRZHLPEQDVPET-UHFFFAOYSA-N 2-methoxyethoxysilane Chemical compound COCCO[SiH3] WGRZHLPEQDVPET-UHFFFAOYSA-N 0.000 claims description 4
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 4
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 claims description 4
- 239000004159 Potassium persulphate Substances 0.000 claims description 4
- QOSMNYMQXIVWKY-UHFFFAOYSA-N Propyl levulinate Chemical compound CCCOC(=O)CCC(C)=O QOSMNYMQXIVWKY-UHFFFAOYSA-N 0.000 claims description 4
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 4
- 239000004141 Sodium laurylsulphate Substances 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 125000004390 alkyl sulfonyl group Chemical group 0.000 claims description 4
- RBIICBLQIHEHJJ-UHFFFAOYSA-N ethenyl(phenoxy)silane Chemical class C(=C)[SiH2]OC1=CC=CC=C1 RBIICBLQIHEHJJ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052738 indium Inorganic materials 0.000 claims description 4
- 239000011858 nanopowder Substances 0.000 claims description 4
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 4
- 235000019394 potassium persulphate Nutrition 0.000 claims description 4
- VVWRJUBEIPHGQF-UHFFFAOYSA-N propan-2-yl n-propan-2-yloxycarbonyliminocarbamate Chemical compound CC(C)OC(=O)N=NC(=O)OC(C)C VVWRJUBEIPHGQF-UHFFFAOYSA-N 0.000 claims description 4
- 229910000077 silane Inorganic materials 0.000 claims description 4
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 4
- GQIUQDDJKHLHTB-UHFFFAOYSA-N trichloro(ethenyl)silane Chemical compound Cl[Si](Cl)(Cl)C=C GQIUQDDJKHLHTB-UHFFFAOYSA-N 0.000 claims description 4
- 239000005050 vinyl trichlorosilane Substances 0.000 claims description 4
- BAPJBEWLBFYGME-UHFFFAOYSA-N acrylic acid methyl ester Natural products COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 3
- 150000008107 benzenesulfonic acids Chemical class 0.000 claims description 3
- 229960002887 deanol Drugs 0.000 claims description 3
- 239000012972 dimethylethanolamine Substances 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 3
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 3
- WYGWHHGCAGTUCH-UHFFFAOYSA-N 2-[(2-cyano-4-methylpentan-2-yl)diazenyl]-2,4-dimethylpentanenitrile Chemical compound CC(C)CC(C)(C#N)N=NC(C)(C#N)CC(C)C WYGWHHGCAGTUCH-UHFFFAOYSA-N 0.000 claims description 2
- CDOUZKKFHVEKRI-UHFFFAOYSA-N 3-bromo-n-[(prop-2-enoylamino)methyl]propanamide Chemical compound BrCCC(=O)NCNC(=O)C=C CDOUZKKFHVEKRI-UHFFFAOYSA-N 0.000 claims description 2
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 2
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 2
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 2
- YQHLDYVWEZKEOX-UHFFFAOYSA-N cumene hydroperoxide Chemical compound OOC(C)(C)C1=CC=CC=C1 YQHLDYVWEZKEOX-UHFFFAOYSA-N 0.000 claims description 2
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims description 2
- 235000019329 dioctyl sodium sulphosuccinate Nutrition 0.000 claims description 2
- MORMPWNLQJTSOT-UHFFFAOYSA-L disodium;4-dodecyl-2-(4-sulfonatophenoxy)benzenesulfonate Chemical compound [Na+].[Na+].CCCCCCCCCCCCC1=CC=C(S([O-])(=O)=O)C(OC=2C=CC(=CC=2)S([O-])(=O)=O)=C1 MORMPWNLQJTSOT-UHFFFAOYSA-L 0.000 claims description 2
- 125000004494 ethyl ester group Chemical group 0.000 claims description 2
- 229910052733 gallium Inorganic materials 0.000 claims description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 2
- QMMOXUPEWRXHJS-UHFFFAOYSA-N pent-2-ene Chemical group CCC=CC QMMOXUPEWRXHJS-UHFFFAOYSA-N 0.000 claims description 2
- PNXMTCDJUBJHQJ-UHFFFAOYSA-N propyl prop-2-enoate Chemical compound CCCOC(=O)C=C PNXMTCDJUBJHQJ-UHFFFAOYSA-N 0.000 claims description 2
- XWGJFPHUCFXLBL-UHFFFAOYSA-M rongalite Chemical compound [Na+].OCS([O-])=O XWGJFPHUCFXLBL-UHFFFAOYSA-M 0.000 claims description 2
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 2
- PODWXQQNRWNDGD-UHFFFAOYSA-L sodium thiosulfate pentahydrate Chemical compound O.O.O.O.O.[Na+].[Na+].[O-]S([S-])(=O)=O PODWXQQNRWNDGD-UHFFFAOYSA-L 0.000 claims description 2
- KZOJQMWTKJDSQJ-UHFFFAOYSA-M sodium;2,3-dibutylnaphthalene-1-sulfonate Chemical compound [Na+].C1=CC=C2C(S([O-])(=O)=O)=C(CCCC)C(CCCC)=CC2=C1 KZOJQMWTKJDSQJ-UHFFFAOYSA-M 0.000 claims description 2
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 claims description 2
- BWYYYTVSBPRQCN-UHFFFAOYSA-M sodium;ethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=C BWYYYTVSBPRQCN-UHFFFAOYSA-M 0.000 claims description 2
- ZESXUEKAXSBANL-UHFFFAOYSA-N trifluoromethyl prop-2-enoate Chemical compound FC(F)(F)OC(=O)C=C ZESXUEKAXSBANL-UHFFFAOYSA-N 0.000 claims description 2
- 238000009413 insulation Methods 0.000 abstract description 24
- 238000002156 mixing Methods 0.000 abstract description 8
- 238000011109 contamination Methods 0.000 abstract description 7
- 230000032683 aging Effects 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 3
- ZYMKZMDQUPCXRP-UHFFFAOYSA-N fluoro prop-2-enoate Chemical compound FOC(=O)C=C ZYMKZMDQUPCXRP-UHFFFAOYSA-N 0.000 abstract 1
- 150000003254 radicals Chemical class 0.000 abstract 1
- 239000000758 substrate Substances 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 39
- 238000005303 weighing Methods 0.000 description 18
- 238000007599 discharging Methods 0.000 description 14
- 239000007788 liquid Substances 0.000 description 14
- 238000003756 stirring Methods 0.000 description 14
- 238000010792 warming Methods 0.000 description 14
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 12
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 description 10
- 239000007864 aqueous solution Substances 0.000 description 9
- 238000001035 drying Methods 0.000 description 8
- 238000010992 reflux Methods 0.000 description 8
- 238000009835 boiling Methods 0.000 description 7
- 238000001132 ultrasonic dispersion Methods 0.000 description 7
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 6
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 6
- 235000017557 sodium bicarbonate Nutrition 0.000 description 6
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 5
- 229910052731 fluorine Inorganic materials 0.000 description 5
- 239000011737 fluorine Substances 0.000 description 5
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 4
- CBTVGIZVANVGBH-UHFFFAOYSA-N aminomethyl propanol Chemical compound CC(C)(N)CO CBTVGIZVANVGBH-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 4
- LDHQCZJRKDOVOX-UHFFFAOYSA-N 2-butenoic acid Chemical group CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910003437 indium oxide Inorganic materials 0.000 description 3
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000003973 paint Substances 0.000 description 3
- 229920005749 polyurethane resin Polymers 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- QTKPMCIBUROOGY-UHFFFAOYSA-N 2,2,2-trifluoroethyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC(F)(F)F QTKPMCIBUROOGY-UHFFFAOYSA-N 0.000 description 2
- 239000000872 buffer Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- GMSCBRSQMRDRCD-UHFFFAOYSA-N dodecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCOC(=O)C(C)=C GMSCBRSQMRDRCD-UHFFFAOYSA-N 0.000 description 2
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 2
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- GILMNGUTRWPWSY-UHFFFAOYSA-N 2-hydroxypropyl prop-2-enoate;2-methylprop-2-enoic acid Chemical compound CC(=C)C(O)=O.CC(O)COC(=O)C=C GILMNGUTRWPWSY-UHFFFAOYSA-N 0.000 description 1
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical group CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 description 1
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical group [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 1
- AOJOEFVRHOZDFN-UHFFFAOYSA-N benzyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC1=CC=CC=C1 AOJOEFVRHOZDFN-UHFFFAOYSA-N 0.000 description 1
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- KBLWLMPSVYBVDK-UHFFFAOYSA-N cyclohexyl prop-2-enoate Chemical compound C=CC(=O)OC1CCCCC1 KBLWLMPSVYBVDK-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000013538 functional additive Substances 0.000 description 1
- 230000005660 hydrophilic surface Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- GOQYKNQRPGWPLP-UHFFFAOYSA-N n-heptadecyl alcohol Natural products CCCCCCCCCCCCCCCCCO GOQYKNQRPGWPLP-UHFFFAOYSA-N 0.000 description 1
- GLDOVTGHNKAZLK-UHFFFAOYSA-N n-octadecyl alcohol Natural products CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- QIWKUEJZZCOPFV-UHFFFAOYSA-N phenyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC1=CC=CC=C1 QIWKUEJZZCOPFV-UHFFFAOYSA-N 0.000 description 1
- 230000021715 photosynthesis, light harvesting Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
Abstract
The invention relates to a thermal insulating coating widely applied to glass substrates, in particular to a water-based hydrophobic nano-resin, a glass thermal insulation coating and a preparation method. The waterborne hydrophobic nano-resin is prepared by mixing and reacting 10 to 40 percent of the solution of vinyl nano-oxide, 0.5 to 4.0 weight percent of emulsifier, 30 to 60 weight percent of acrylate monomer, 5 to 30 weight percent of fluoroacrylate monomer, 3 to 12 weight percent of vinyl siloxane, 0.1 to 4 weight percent of initiator, 0.5 to 2 weight percent of neutralizer and 5 to 30 weight percent of de-ionized water. The method comprises the following steps of: from the standpoint of chemical grafting, first preparing a nano-oxide containing vinyl; then synthesizing the hydrophobic nano-resin by copolymerizing the nano-oxide with a free radical of a fluoro (silicon) acrylic monomer; and finally preparing the hydrophobic glass thermal insulating coating by using the resin. The glass thermal insulating coating has the advantages of high comprehensive performance, thermal insulation, contamination resistance and aging resistance, and wide market prospect in the environmentally-friendly society.
Description
Technical field:
The present invention relates to a kind of thermal insulating coating that is widely used on the glass baseplate, specifically a kind of water-based hydrophobic nano-resin and glass heat-insulating coating and preparation method.
Background technology:
Along with China's rapid growth of economy, environment and energy problem more and more receive publicity.The glass door and window effect of heat insulation of buildings is poor, cause huge energy dissipation, develop the novel energy-conserving product, reduce power load, have very important significance to alleviating China's present stage energy scarcity, for save energy, people have taked various measures to solve the heat-insulating problem of glass of building.At present, main metal coating heat-reflecting glass and the various heat reflection pad pasting of adopting intercepts seeing through of part sunlight on the market, thereby reaches the purpose of heat insulation and heat control.
Nano transparent insulating coating visible light transmissivity height, infrared, ultraviolet shielded rate height can effectively completely cut off solar radiation, can be applicable to occasions such as constructure screen wall glass, automotive glazing, has good energy-saving effect.Because it is easy to use, price is lower, can satisfy popular consumption requirement, thereby market outlook is had an optimistic view of extensively.But, the promotion and application of environment-friendly heat insulating coating have therefore been hindered because traditional aqueous glass heat insulation paint exists easy contamination, easy performance deficiency such as aging.
Conventional aqueous glass heat insulation paint uses water-base resin and nano pulp blend to make, and it has good effect of heat insulation and visible light permeability.Mono-component aqueous urethane commonly used on the market is as base resin, and the outer then interpolation nano-oxide aqueous solution prepares glass heat-insulating coating, but this coating exists following some deficiency: 1, preparation technology is long, and nano-oxide is difficult to disperse in the aqueous solution; 2, because nano-oxide and waterborne polyurethane resin dispersion are the processes of a physical mixed, and nano-oxide density is excessive, and precipitation is separated out easily in coating, and stability in storage is bad; 3, owing to the limitation of waterborne polyurethane resin, the anti-contamination of filming is difficult to be resolved, thereby has brought very big trouble for the cleaning of glass.Therefore inventing a kind of hydrophobic type glass heat-insulating coating seems very urgent.
Summary of the invention:
Purpose of the present invention is exactly the defective at existing glass heat-insulating coating, and a kind of water-based hydrophobic nano-resin and glass heat-insulating coating and preparation method are provided.The present invention has improved every performance of coating, particularly anti-contamination and ageing-resistant performance.
The present invention at first carries out graft modification on nano-oxide, making its hydrophilic surface modification is lipophilic, and the organo-functional group that on its surface grafting, can react, then by vinyl double bond and the copolymerization of fluorine (silicon) acrylic ester monomer, prepared a kind of hydrophobic nano-resin, utilize this resin with the aqueous functional additive compound, prepared a kind of high-performance hydrophobic type glass heat-insulating coating.The innovation of this coating maximum is exactly to have prepared vinyl nano-oxide solution, has selected fluorine, silicon class vinyl monomer with hydrophobic function then for use, has prepared hydrophobic nano-resin.
Technical scheme of the present invention is achieved in that it is that the following materials based on weight hybrid reaction is formed, and wherein proportion of raw materials is as follows:
Vinyl nano-oxide solution 10%-40%, emulsifying agent 0.5-4.0%, acrylate monomer 30-60%, fluorinated monomer monomer 5-30%, vinylsiloxane 3-12%, initiator 0.1-4%, neutralizing agent 0.5-2%, deionized water 5-30%.
The present invention's technical scheme preferably is that the following materials based on weight hybrid reaction is formed, and wherein proportion of raw materials is as follows:
Vinyl nano-oxide solution 20%, emulsifying agent 2%, acrylate monomer 40%, fluorinated monomer monomer 10%, vinylsiloxane 5%, initiator 2%, neutralizing agent 1%, deionized water 20%.
Wherein said vinyl nano-oxide solution is by the silane coupling agent of the nano-powder of nano-oxide solution quality 10-40%, nano oxidized amount 8-30% and balance of deionized water is mixed gets.Described nano-powder is nano-indium stannum oxide, nano antimony tin oxide, nano aluminium oxide zinc or nano zine oxide gallium; Nano indium oxide, tin have good sunlight reflectivity, therefore have good effect of heat insulation, and price is relatively low, so the present invention preferentially select nano indium oxide, nano tin dioxide or its mixture of 1: 1 for use.
Described silane coupling agent is vinyl trimethoxy (oxyethyl group) silane, propenyl Trimethoxy silane, γ-methacryloxy Trimethoxy silane, 3-methacryloxypropyl trimethoxy silane, triple phenoxyl vinyl silanes, vinyl three (2-methoxy ethoxy) silane, the rare acyloxy propyl trimethoxy silicane of γ-methyl-prop, vinyl silane triisopropoxide, 3-(iso-butylene acyl-oxygen) propyl trimethoxy silicane or vinyl trichloro silane.
Described emulsifying agent is a dialkyl benzene sulfonic acids sodium, sodium dibutyl naphthalene sulfonate, the di-isopropyl sodium naphthalene sulfonate, disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate, sodium lauryl sulphate, sodium laurylsulfonate, Sodium dodecylbenzene sulfonate, dioctyl sodium sulfosuccinate, the allyloxy hydroxypropyl azochlorosulfonate acid sodium, alkylamide vinyl sulfonic acid sodium, to polyoxyethylene nonyl phenyl ethene (n=4-40) ether, to in octylphenol polyethylene ethylene oxide (n=9-40) ether one or more, in the synthetic process, adopt negatively charged ion and nonionogenic tenside composite best, preferentially select the composite emulsifying agent of sodium lauryl sulphate and polyoxyethylene octylphenol ether for use.
Described acrylate monomer is (methyl) vinylformic acid, (methyl) methyl acrylate, (methyl) ethyl propenoate, (methyl) butyl acrylate, cyclohexyl acrylate, the vinylformic acid n-propyl, Isooctyl acrylate monomer, (methyl) lauryl acrylate, vinylbenzene, (methyl) vinylformic acid stearyl alcohol ester, lauryl methacrylate, phenyl methacrylate, benzyl methacrylate, acrylamide, (methyl) senecioate-hydroxyl ethyl ester, senecioate-hydroxypropyl acrylate, vinylformic acid-2-hydroxyl-3-phenoxy group propyl ester, in methacrylic acid-β-hydroxypropyl acrylate one or more.
Described fluorinated monomer monomer is (methyl) vinylformic acid trifluoro ethyl ester; (methyl) vinylformic acid hexafluoro butyl ester; (methyl) vinylformic acid perfluoro capryl ethyl ester; vinylformic acid perfluoro hexyl ethyl ester; (methyl) vinylformic acid tetrafluoro propyl ester; the perfluoro capryl propyl acrylate; (methyl) dodecafluorhe-ptylacrylate; N-hydroxyethyl perfluor decoylamide acrylate; methacrylic acid trifluoroacetyl 2-ethoxyethyl acetate; trifluoromethyl acrylate; (methyl) vinylformic acid octafluoro pentyl ester; the perfluoroalkyl methyl acrylate; N-propyl group perfluoro capryl (alkylsulfonyl) amido ethyl propenoate; 2-(N-methyl PFO base alkylsulfonyl) ethyl propylene acid esters; in the perfluoroalkyl methacrylate one or more.
Described vinylsiloxane is vinyl trimethoxy (oxyethyl group) silane, the propenyl Trimethoxy silane, γ-methacryloxy Trimethoxy silane, the 3-methacryloxypropyl trimethoxy silane, the triple phenoxyl vinyl silanes, vinyl three (2-methoxy ethoxy) silane, the rare acyloxy propyl trimethoxy silicane of γ-methyl-prop, vinyl silane triisopropoxide, in 3-(iso-butylene acyl-oxygen) propyl trimethoxy silicane or the vinyl trichloro silane one or more; Initiator is one or more in Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile), dibenzoyl peroxide, Potassium Persulphate, tertbutyl peroxide, ammonium persulphate, ferrous salt, isopropyl benzene hydroperoxide, sodium bisulfite, Sulfothiorine, the rongalite, preferentially selects Potassium Persulphate, ammonium persulphate or Diisopropyl azodicarboxylate for use; Neutralizing agent is ammoniacal liquor, triethylamine or dimethylethanolamine, preferentially selects ammoniacal liquor for use.
The another invention of the present invention is to utilize above-mentioned nano-resin to prepare a kind of glass heat-insulating coating, and it is mixed by following raw materials by weight:
Claim 1 or 2 water-based hydrophobic nano-resin 60%-90%, aqueous promoter 0.5%-5.0%, surplus are deionized water.Wherein said aqueous promoter is water-based defoamer, water-based thickener or its mixture.
The preparation method of water-based hydrophobic nano-resin of the present invention and glass heat-insulating coating thereof, its concrete technology comprises:
(a) preparation of vinyl nano-oxide solution
Nano-oxide is put into baking oven, and drying is 5 hours under 40-50 ℃ of condition, and the nano-oxide adding that drying is good is dissolved with in the aqueous solution of silane coupling agent, and ultra-sonic dispersion 1 hour makes pre-dispersed liquid.The pre-dispersed liquid adding is had in the 500mL round-bottomed flask of reflux exchanger and agitator, system is warmed up to 80-90 ℃ then, middling speed stirs, reaction 24h, and discharging makes vinyl nano-oxide solution.
(b) water-based hydrophobic nano-resin is synthetic
In the four-hole boiling flask that agitator, thermometer, prolong are housed, add bed material (deionized water, nano-oxide solution, emulsifying agent and buffer reagent) stirring and be warming up to 60 ℃, fluorine (silicon) the esters of acrylic acid mix monomer of adding 5%～25% disperses about 5min, be warming up to 80 ℃, the initiator solution that adds 10-30% again prepares seed, insulation reaction, do not begin to drip remaining mix monomer and initiator solution after having obvious the backflow in the reaction flask, the control rate of addition drips off in 2-4h; Insulation reaction 0.5-1h is cooled to room temperature and with about neutralizing agent adjustment pH to 8, filters discharging, promptly gets water-based hydrophobic nano-resin (solid content is 40-55%).Above-mentioned buffer reagent is a sodium bicarbonate, and its consumption is the 0.2-2% of emulsion weight.
(c) preparation of hydrophobic type glass heat-insulating coating
Get above-mentioned a certain amount of hydrophobic nano-resin in container, add the water-based defoamer successively, water-based thickener, neutralizing agent.Put it in the high speed dispersor and disperse, speed is about 650-1200r/min, disperses 20min, promptly gets the hydrophobic type glass heat-insulating coating.
The present invention is in the process of preparation hydrophobic type glass heat-insulating coating, angle from chemical graft, at first prepared the nano-oxide that contains vinyl, utilize this nano-oxide and fluorine (silicon) acrylic ester monomer free-radical polymerized then, the nano-resin that has synthesized a kind of hydrophobic type, the hydrophobic type glass heat-insulating coating that utilized this resins.Traditional on the market aqueous glass heat insulation paint is selected self-cross linking type waterborne polyurethane resin and nano pulp physical mixed usually for use, and stability is good inadequately, and contamination resistance can not get effective improvement.This invention is when guaranteeing the glass heat-insulating coating thermal insulation, nano-oxide has been carried out the grafting processing, inorganic materials and organic materials are linked together well by chemical bond, thereby defectives such as the reunion of inorganic nano material in organic phase, precipitation have been solved, realized compound on Nano grade of inorganic materials and organic materials, select for use fluorine, Si acrylate that it has been carried out modification simultaneously, further improved the anti-contamination and the ageing-resistant performance of glass heat-insulating coating.This glass heat-insulating coating excellent combination property, thermal insulation, anti-contamination, ageing-resistant performance are given prominence to, and have very extensive market prospects in environmental friendliness society.
Embodiment:
Below in conjunction with embodiment the present invention is described further:
Embodiment 1:
(ATO) puts into baking oven with nano antimony tin oxide, and drying is 5 hours under 50 ℃ of conditions, and the 5.00g vinyltrimethoxy silane is mixed with the 75.00g deionized water; Accurately the adding of weighing 20.00g nano antimony tin oxide is dissolved with in the aqueous solution of silane coupling agent, and ultra-sonic dispersion 1 hour makes pre-dispersed liquid.The pre-dispersed liquid adding is had in the 500mL round-bottomed flask of reflux exchanger and agitator, system is warmed up to 90 ℃ then, middling speed stirs, reaction 24h, and discharging makes the vinyl nano-solution.
Accurate weighing 20.8g methyl methacrylate, the 19.5g butyl methacrylate, 21.4g methacrylic acid hexafluoro butyl ester, 1.3g vinylformic acid, the 2.0g vinyltrimethoxy silane mixes.In the four-hole boiling flask that agitator, thermometer, prolong are housed, add 40.00g deionized water, 0.325g Sodium dodecylbenzene sulfonate, 0.975g polyoxyethylene octylphenol ether, 25g vinyl nano antimony tin oxide solution, 0.250g sodium bicarbonate.Weighing 0.682g ammonium persulphate and 15g deionized water mix, and are initiator solution.Stirring is warming up to 60 ℃, adding 13.00g acrylate mixing monomer disperses about 5min and is warming up to 80 ℃, add the 3.136g initiator solution again and prepare seed, insulation reaction, do not begin to drip remaining mix monomer and initiator solution after having obvious the backflow in the reaction flask, the control rate of addition drips off in 3-5h; Insulation reaction 0.5-1h is cooled to room temperature and with about ammoniacal liquor adjustment pH to 8, filters discharging, promptly gets water-based hydrophobic nano-resin.
Get above-mentioned hydrophobic nano-resin 80.00g in container, add 0.50g water-based defoamer W-090,0.45g water-based thickener WT-105A, 0.30g neutralizing agent AMP-95, supply 100g with deionized water, put it in the high speed dispersor and disperse, speed is about 1200r/min, disperse 20min, promptly get the hydrophobic type glass heat-insulating coating.
Embodiment 2:
(ATO) puts into baking oven with nano antimony tin oxide, and drying is 5 hours under 50 ℃ of conditions, and the 7.00g vinyltriethoxysilane is mixed with the 68.00g deionized water; Accurately the adding of weighing 25.00g nano antimony tin oxide is dissolved with in the aqueous solution of silane coupling agent, and ultra-sonic dispersion 1 hour makes pre-dispersed liquid.The pre-dispersed liquid adding is had in the 500mL round-bottomed flask of reflux exchanger and agitator, system is warmed up to 90 ℃ then, middling speed stirs, reaction 24h, and discharging makes the vinyl nano-solution.
Accurate weighing 19.5g methyl methacrylate, the 23.725g butyl methacrylate, the 19.5g trifluoroethyl methacrylate, 1.1g vinylformic acid, the 1.175g vinyltriethoxysilane mixes.In the four-hole boiling flask that agitator, thermometer, prolong are housed, add 42.50g deionized water, 0.26g sodium lauryl sulphate, 1.04g polyoxyethylene octylphenol ether, 30g vinyl nano antimony tin oxide solution, 0.210g sodium bicarbonate.Weighing 0.651g Potassium Persulphate and 15g deionized water mix, and are initiator solution.Stirring is warming up to 60 ℃, adding 16.25g acrylate mixing monomer disperses about 5min and is warming up to 80 ℃, add the 3.913g initiator solution again and prepare seed, insulation reaction, do not begin to drip remaining mix monomer and initiator solution after having obvious the backflow in the reaction flask, the control rate of addition drips off in 3-5h; Insulation reaction 0.5-1h is cooled to room temperature and with about triethylamine adjustment pH to 8, filters discharging, promptly gets water-based hydrophobic nano-resin.
Get above-mentioned hydrophobic nano-resin 75.00g in container, add 0.30g water-based defoamer W-098,0.35g water-based thickener WT-201,0.40g neutralizing agent MA-95, supply 100g with deionized water, put it in the high speed dispersor and disperse, speed is about 1000r/min, disperse 20min, promptly get the hydrophobic type glass heat-insulating coating.
Embodiment 3:
(ITO) puts into baking oven with nano-indium stannum oxide, and drying is 5 hours under 50 ℃ of conditions, and 4.00g γ-methacryloxy Trimethoxy silane is mixed with the 66.00g deionized water; Accurately the adding of weighing 30.00g nano-indium stannum oxide is dissolved with in the aqueous solution of silane coupling agent, and ultra-sonic dispersion 1 hour makes pre-dispersed liquid.The pre-dispersed liquid adding is had in the 500mL round-bottomed flask of reflux exchanger and agitator, system is warmed up to 90 ℃ then, middling speed stirs, reaction 24h, and discharging makes the vinyl nano-solution.
Accurate weighing 13.0g methyl methacrylate, the 24.05g butyl acrylate, 24.00g tetrafluoropropyl propyl ester, the 0.65g glycidyl methacrylate, the 2.975g vinyltrimethoxy silane mixes.In the four-hole boiling flask that agitator, thermometer, prolong are housed, add 47.00g deionized water, 0.265g Sodium dodecylbenzene sulfonate, 0.52g polyoxyethylene octylphenol ether, 20g vinyl nano indium oxide solution of tin, 0.10g sodium bicarbonate.Weighing 0.26g ammonium persulphate and 15.5g deionized water mix, and are initiator solution.Stirring is warming up to 60 ℃, adding 9.75g acrylate mixing monomer disperses about 5min and is warming up to 80 ℃, add the 2.364g initiator solution again and prepare seed, insulation reaction, do not begin to drip remaining mix monomer and initiator solution after having obvious the backflow in the reaction flask, the control rate of addition drips off in 3-5h; Insulation reaction 0.5-1h is cooled to room temperature and with about ammoniacal liquor adjustment pH to 8, filters discharging, promptly gets water-based hydrophobic nano-resin.
Get above-mentioned hydrophobic nano-resin 85.00g in container, add 0.30g water-based defoamer Tego-902W, 0.40g water-based thickener Tego-3000,0.25g neutralizing agent AMP-95, supply 100g with deionized water, put it in the high speed dispersor and disperse, speed is about 800r/min, disperse 20min, promptly get the hydrophobic type glass heat-insulating coating.
Embodiment 4:
(ATO) puts into baking oven with nano antimony tin oxide, and drying is 5 hours under 50 ℃ of conditions, and the 8.00g vinyl silane triisopropoxide is mixed with the 64.00g deionized water; Accurately the adding of weighing 28.00g nano antimony tin oxide is dissolved with in the aqueous solution of silane coupling agent, and ultra-sonic dispersion 1 hour makes pre-dispersed liquid.The pre-dispersed liquid adding is had in the 500mL round-bottomed flask of reflux exchanger and agitator, system is warmed up to 90 ℃ then, middling speed stirs, reaction 24h, and discharging makes the vinyl nano-solution.
Accurate weighing 12.725g methyl methacrylate, the 20.8g butyl methacrylate, 25.785g methacrylic acid ten difluoro heptyl esters, the 0.65g methacrylic acid, the 1.30g lauryl methacrylate(LMA), the 3.525g vinyltrimethoxy silane mixes.In the four-hole boiling flask that agitator, thermometer, prolong are housed, add 35.60g deionized water, 0.26g Sodium dodecylbenzene sulfonate, 0.56g polyoxyethylene octylphenol ether, 20g vinyl nano antimony tin oxide solution, 0.120g sodium bicarbonate.Weighing 0.327g ammonium persulphate and 15.5g deionized water mix, and are initiator solution.Stirring is warming up to 60 ℃, adding 13.00g acrylate mixing monomer disperses about 5min and is warming up to 80 ℃, add the 3.166g initiator solution again and prepare seed, insulation reaction, do not begin to drip remaining mix monomer and initiator solution after having obvious the backflow in the reaction flask, the control rate of addition drips off in 3-5h; Insulation reaction 0.5-1h is cooled to room temperature and with about dimethylethanolamine adjustment pH to 8, filters discharging, promptly gets water-based hydrophobic nano-resin.
Get above-mentioned hydrophobic nano-resin 75.00g in container, add 0.25g water-based defoamer Tego-805,0.30g water-based thickener Tego-3100,0.30g neutralizing agent AMP-95, supply 100g with deionized water, put it in the high speed dispersor and disperse, speed is about 1000r/min, disperse 20min, promptly get the hydrophobic type glass heat-insulating coating.
Embodiment 5:
(AZO) puts into baking oven with nano aluminium oxide zinc, and drying is 5 hours under 50 ℃ of conditions, and the 8.00g vinyl silane triisopropoxide is mixed with the 68.00g deionized water; Accurately the adding of weighing 24.00g nano aluminium oxide zinc is dissolved with in the aqueous solution of silane coupling agent, and ultra-sonic dispersion 1 hour makes pre-dispersed liquid.The pre-dispersed liquid adding is had in the 500mL round-bottomed flask of reflux exchanger and agitator, system is warmed up to 90 ℃ then, middling speed stirs, reaction 24h, and discharging makes the vinyl nano-solution.
Accurate weighing 13.00g methyl methacrylate, the 24.05g butyl methacrylate, the 24.671g trifluoroethyl methacrylate, the 0.325g methacrylic acid, 2.625g propenyl Trimethoxy silane mixes.In the four-hole boiling flask that agitator, thermometer, prolong are housed, add 35.50g deionized water, 0.52g Sodium dodecylbenzene sulfonate, 1.04g polyoxyethylene octylphenol ether, 35g vinyl nano aluminium oxide zinc solution, 0.130g sodium bicarbonate.Weighing 0.228g ammonium persulphate and 15g deionized water mix, and are initiator solution.Stirring is warming up to 60 ℃, adding 16.25g acrylate mixing monomer disperses about 5min and is warming up to 80 ℃, add the 3.807g initiator solution again and prepare seed, insulation reaction, do not begin to drip remaining mix monomer and initiator solution after having obvious the backflow in the reaction flask, the control rate of addition drips off in 3-5h; Insulation reaction 0.5-1h is cooled to room temperature and with about ammoniacal liquor adjustment pH to 8, filters discharging, promptly gets water-based hydrophobic nano-resin.
Get above-mentioned hydrophobic nano-resin 80.00g in container, add 0.25g water-based defoamer BYK-024,0.35g water-based thickener WT-204,0.40g neutralizing agent DMAE, supply 100g with deionized water, put it in the high speed dispersor and disperse, speed is about 800r/min, disperse 20min, promptly get the hydrophobic type glass heat-insulating coating.
Embodiment 6:
(ATO) puts into baking oven with nano antimony tin oxide, and drying is 5 hours under 50 ℃ of conditions, and 9.00g3-(iso-butylene acyl-oxygen) propyl trimethoxy silicane is mixed with the 61.00g deionized water; Accurately the adding of weighing 30.00g nano antimony tin oxide is dissolved with in the aqueous solution of silane coupling agent, and ultra-sonic dispersion 1 hour makes pre-dispersed liquid.The pre-dispersed liquid adding is had in the 500mL round-bottomed flask of reflux exchanger and agitator, system is warmed up to 90 ℃ then, middling speed stirs, reaction 24h, and discharging makes the vinyl nano-solution.
Accurate weighing 15.275g methyl methacrylate, the 20.8g butyl methacrylate, 24.7g methacrylic acid hexafluoro butyl ester, the 0.65g methacrylic acid, the 1.3g glycidyl methacrylate, 2.275g propenyl Trimethoxy silane mixes.In the four-hole boiling flask that agitator, thermometer, prolong are housed, add 54.90g deionized water, 0.36g dialkyl benzene sulfonic acids sodium, 0.72g polyoxyethylene octylphenol ether, 30.00g vinyl nano antimony tin oxide solution, 0.150g sodium bicarbonate.Weighing 0.752g Diisopropyl azodicarboxylate and acrylate monomer mix.Stirring is warming up to 60 ℃, the mixing solutions of adding 13.15g acrylate and initiator disperses about 5min and is warming up to 80 ℃, do not have the mixing solutions that begins to drip remaining acrylate monomer and initiator after obviously refluxing in the reaction flask, the control rate of addition drips off in 3-5h; Insulation reaction 0.5-1h is cooled to room temperature and with about ammoniacal liquor adjustment pH to 8, filters discharging, promptly gets water-based hydrophobic nano-resin.
Get above-mentioned hydrophobic nano-resin 80.00g in container, add 0.35g water-based defoamer BYK-034,0.30g water-based thickener WT-102,0.40g neutralizing agent AMP-95, supply 100g with deionized water, put it in the high speed dispersor and disperse, speed is about 900r/min, disperse 20min, promptly get the hydrophobic type glass heat-insulating coating.
Claims (6)
1. water-based hydrophobic nano-resin, it is that the following weight percentages hybrid reaction is formed, wherein proportion of raw materials is as follows:
Vinyl nano-oxide solution 10%-40%, emulsifying agent 0.5-4.0%, acrylate monomer 30-60%, fluorinated monomer monomer 5-30%, vinylsiloxane 3-12%, initiator 0.1-4%, neutralizing agent 0.5-2%, deionized water 5-30%; Wherein said vinyl nano-oxide solution is to be that the nano-powder of 10-40%, silane coupling agent that the nano-oxide mass percent is 8-30% and balance of deionized water are mixed by the nano-oxide mass percent; Described nano-powder is nano-indium stannum oxide, nano antimony tin oxide, nano aluminium oxide zinc or nano zine oxide gallium; Described silane coupling agent is vinyl trimethoxy (oxyethyl group) silane, propenyl Trimethoxy silane, γ-methacryloxy Trimethoxy silane, 3-methacryloxypropyl trimethoxy silane, triple phenoxyl vinyl silanes, vinyl three (2-methoxy ethoxy) silane, the rare acyloxy propyl trimethoxy silicane of γ-methyl-prop, vinyl silane triisopropoxide, 3-(iso-butylene acyl-oxygen) propyl trimethoxy silicane or vinyl trichloro silane; Described fluorinated monomer monomer is the vinylformic acid trifluoro ethyl ester; vinylformic acid hexafluoro butyl ester; vinylformic acid perfluoro capryl ethyl ester; vinylformic acid perfluoro hexyl ethyl ester; vinylformic acid tetrafluoro propyl ester; the perfluoro capryl propyl acrylate; dodecafluorhe-ptylacrylate; N-hydroxyethyl perfluor decoylamide acrylate; methacrylic acid trifluoroacetyl 2-ethoxyethyl acetate; trifluoromethyl acrylate; vinylformic acid octafluoro pentyl ester; the perfluoroalkyl methyl acrylate; N-propyl group perfluoro capryl (alkylsulfonyl) amido ethyl propenoate; in 2-(N-methyl PFO base alkylsulfonyl) ethyl propylene acid esters or the perfluoroalkyl methacrylate one or more.
2. a kind of water-based hydrophobic nano-resin according to claim 1, it is that the following weight percentages hybrid reaction is formed, wherein proportion of raw materials is as follows:
Vinyl nano-oxide solution 20%, emulsifying agent 2%, acrylate monomer 40%, fluorinated monomer monomer 10%, vinylsiloxane 5%, initiator 2%, neutralizing agent 1%, deionized water 20%.
3. a kind of water-based hydrophobic nano-resin according to claim 1 and 2, wherein said emulsifying agent be dialkyl benzene sulfonic acids sodium, sodium dibutyl naphthalene sulfonate, di-isopropyl sodium naphthalene sulfonate, disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate, sodium lauryl sulphate, sodium laurylsulfonate, Sodium dodecylbenzene sulfonate, dioctyl sodium sulfosuccinate, allyloxy hydroxypropyl azochlorosulfonate acid sodium, alkylamide vinyl sulfonic acid sodium, to the polyoxyethylene nonyl phenyl Vinyl Ether or in the octylphenol polyethylene ethylene oxide ether one or more.
4. a kind of water-based hydrophobic nano-resin according to claim 1 and 2, wherein said vinylsiloxane are vinyl trimethoxy (oxyethyl group) silane, the propenyl Trimethoxy silane, γ-methacryloxy Trimethoxy silane, the 3-methacryloxypropyl trimethoxy silane, the triple phenoxyl vinyl silanes, vinyl three (2-methoxy ethoxy) silane, the rare acyloxy propyl trimethoxy silicane of γ-methyl-prop, vinyl silane triisopropoxide, in 3-(iso-butylene acyl-oxygen) propyl trimethoxy silicane or the vinyl trichloro silane one or more; Initiator is one or more in Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile), dibenzoyl peroxide, Potassium Persulphate, tertbutyl peroxide, ammonium persulphate, ferrous salt, isopropyl benzene hydroperoxide, sodium bisulfite, Sulfothiorine, the rongalite; Neutralizing agent is ammoniacal liquor, triethylamine or dimethylethanolamine.
5. glass heat-insulating coating, it is mixed by following raw materials by weight:
Claim 1 or 2 water-based hydrophobic nano-resin 60%-90%, aqueous promoter 0.5%-5.0%, surplus are deionized water.
6. a kind of glass heat-insulating coating according to claim 5, wherein said aqueous promoter are water-based defoamer, water-based thickener or its mixture.
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