CN117402286A - Modified acrylic resin, preparation method thereof, powder coating and application - Google Patents
Modified acrylic resin, preparation method thereof, powder coating and application Download PDFInfo
- Publication number
- CN117402286A CN117402286A CN202311713151.7A CN202311713151A CN117402286A CN 117402286 A CN117402286 A CN 117402286A CN 202311713151 A CN202311713151 A CN 202311713151A CN 117402286 A CN117402286 A CN 117402286A
- Authority
- CN
- China
- Prior art keywords
- acrylic resin
- nano
- modified
- filler
- modified acrylic
- 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.)
- Granted
Links
- 239000004925 Acrylic resin Substances 0.000 title claims abstract description 80
- 229920000178 Acrylic resin Polymers 0.000 title claims abstract description 80
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 238000000576 coating method Methods 0.000 title claims abstract description 37
- 239000011248 coating agent Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 239000000843 powder Substances 0.000 title claims abstract description 28
- 239000000945 filler Substances 0.000 claims abstract description 71
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 28
- 239000000178 monomer Substances 0.000 claims abstract description 25
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 claims abstract description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 23
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 19
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000012986 chain transfer agent Substances 0.000 claims abstract description 17
- 239000003999 initiator Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 239000003960 organic solvent Substances 0.000 claims abstract description 16
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 15
- 150000001875 compounds Chemical class 0.000 claims abstract description 12
- 239000011787 zinc oxide Substances 0.000 claims abstract description 11
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 10
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 10
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims abstract description 9
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims abstract description 9
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims abstract description 9
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000004048 modification Effects 0.000 claims description 14
- 238000012986 modification Methods 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 9
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 6
- 229910000077 silane Inorganic materials 0.000 claims description 6
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims description 5
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 4
- NLSFWPFWEPGCJJ-UHFFFAOYSA-N 2-methylprop-2-enoyloxysilicon Chemical compound CC(=C)C(=O)O[Si] NLSFWPFWEPGCJJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000004593 Epoxy Substances 0.000 claims description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 4
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims description 4
- WNAHIZMDSQCWRP-UHFFFAOYSA-N dodecane-1-thiol Chemical compound CCCCCCCCCCCCS WNAHIZMDSQCWRP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052717 sulfur Inorganic materials 0.000 claims description 4
- 239000011593 sulfur Substances 0.000 claims description 4
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical compound [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 claims description 4
- QEQBMZQFDDDTPN-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy benzenecarboperoxoate Chemical compound CC(C)(C)OOOC(=O)C1=CC=CC=C1 QEQBMZQFDDDTPN-UHFFFAOYSA-N 0.000 claims description 3
- CFVWNXQPGQOHRJ-UHFFFAOYSA-N 2-methylpropyl prop-2-enoate Chemical compound CC(C)COC(=O)C=C CFVWNXQPGQOHRJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- XYLMUPLGERFSHI-UHFFFAOYSA-N alpha-Methylstyrene Chemical class CC(=C)C1=CC=CC=C1 XYLMUPLGERFSHI-UHFFFAOYSA-N 0.000 claims description 2
- 239000008393 encapsulating agent Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 230000032683 aging Effects 0.000 abstract description 16
- 238000002834 transmittance Methods 0.000 abstract description 15
- 239000005022 packaging material Substances 0.000 abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 46
- 230000000052 comparative effect Effects 0.000 description 20
- 238000012360 testing method Methods 0.000 description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 18
- 238000005406 washing Methods 0.000 description 17
- 239000000047 product Substances 0.000 description 16
- 238000003756 stirring Methods 0.000 description 15
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 14
- 239000002131 composite material Substances 0.000 description 13
- 239000003929 acidic solution Substances 0.000 description 11
- 235000019441 ethanol Nutrition 0.000 description 11
- 239000004611 light stabiliser Substances 0.000 description 11
- 239000000243 solution Substances 0.000 description 11
- 238000006460 hydrolysis reaction Methods 0.000 description 10
- 239000003795 chemical substances by application Substances 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 239000002253 acid Substances 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 8
- 239000000413 hydrolysate Substances 0.000 description 7
- 239000011259 mixed solution Substances 0.000 description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- -1 benzophenone compound Chemical class 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 6
- TVIDDXQYHWJXFK-UHFFFAOYSA-N dodecanedioic acid Chemical compound OC(=O)CCCCCCCCCCC(O)=O TVIDDXQYHWJXFK-UHFFFAOYSA-N 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000011812 mixed powder Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 239000003963 antioxidant agent Substances 0.000 description 5
- 230000003078 antioxidant effect Effects 0.000 description 5
- 239000003365 glass fiber Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- ISAOCJYIOMOJEB-UHFFFAOYSA-N benzoin Chemical compound C=1C=CC=CC=1C(O)C(=O)C1=CC=CC=C1 ISAOCJYIOMOJEB-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 238000004821 distillation Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000004744 fabric Substances 0.000 description 4
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 4
- 239000011256 inorganic filler Substances 0.000 description 4
- 229910003475 inorganic filler Inorganic materials 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 238000005191 phase separation Methods 0.000 description 4
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 description 4
- WYLMGXULBMHUDT-UHFFFAOYSA-N 2-[4,6-bis(2,4-dimethylphenyl)-1,3,5-triazin-2-yl]-5-[3-(2-ethylhexoxy)-2-hydroxypropoxy]phenol Chemical group OC1=CC(OCC(O)COCC(CC)CCCC)=CC=C1C1=NC(C=2C(=CC(C)=CC=2)C)=NC(C=2C(=CC(C)=CC=2)C)=N1 WYLMGXULBMHUDT-UHFFFAOYSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 108010009736 Protein Hydrolysates Proteins 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000007774 longterm Effects 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000002604 ultrasonography Methods 0.000 description 3
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical compound C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 2
- 229940083957 1,2-butanediol Drugs 0.000 description 2
- CUVLMZNMSPJDON-UHFFFAOYSA-N 1-(1-butoxypropan-2-yloxy)propan-2-ol Chemical compound CCCCOCC(C)OCC(C)O CUVLMZNMSPJDON-UHFFFAOYSA-N 0.000 description 2
- 235000021314 Palmitic acid Nutrition 0.000 description 2
- 244000028419 Styrax benzoin Species 0.000 description 2
- 235000000126 Styrax benzoin Nutrition 0.000 description 2
- 235000008411 Sumatra benzointree Nutrition 0.000 description 2
- 239000012445 acidic reagent Substances 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 229960002130 benzoin Drugs 0.000 description 2
- BMRWNKZVCUKKSR-UHFFFAOYSA-N butane-1,2-diol Chemical compound CCC(O)CO BMRWNKZVCUKKSR-UHFFFAOYSA-N 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 235000019382 gum benzoic Nutrition 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 2
- SSDSCDGVMJFTEQ-UHFFFAOYSA-N octadecyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 SSDSCDGVMJFTEQ-UHFFFAOYSA-N 0.000 description 2
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 2
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 description 2
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical class [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- OUPZKGBUJRBPGC-UHFFFAOYSA-N 1,3,5-tris(oxiran-2-ylmethyl)-1,3,5-triazinane-2,4,6-trione Chemical compound O=C1N(CC2OC2)C(=O)N(CC2OC2)C(=O)N1CC1CO1 OUPZKGBUJRBPGC-UHFFFAOYSA-N 0.000 description 1
- QFGCFKJIPBRJGM-UHFFFAOYSA-N 12-[(2-methylpropan-2-yl)oxy]-12-oxododecanoic acid Chemical compound CC(C)(C)OC(=O)CCCCCCCCCCC(O)=O QFGCFKJIPBRJGM-UHFFFAOYSA-N 0.000 description 1
- MKBBSFGKFMQPPC-UHFFFAOYSA-N 2-propyl-1h-imidazole Chemical compound CCCC1=NC=CN1 MKBBSFGKFMQPPC-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- ACZGCWSMSTYWDQ-UHFFFAOYSA-N 3h-1-benzofuran-2-one Chemical class C1=CC=C2OC(=O)CC2=C1 ACZGCWSMSTYWDQ-UHFFFAOYSA-N 0.000 description 1
- SWZOQAGVRGQLDV-UHFFFAOYSA-N 4-[2-(4-hydroxy-2,2,6,6-tetramethylpiperidin-1-yl)ethoxy]-4-oxobutanoic acid Chemical compound CC1(C)CC(O)CC(C)(C)N1CCOC(=O)CCC(O)=O SWZOQAGVRGQLDV-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000012965 benzophenone Substances 0.000 description 1
- 239000012964 benzotriazole Substances 0.000 description 1
- XITRBUPOXXBIJN-UHFFFAOYSA-N bis(2,2,6,6-tetramethylpiperidin-4-yl) decanedioate Chemical compound C1C(C)(C)NC(C)(C)CC1OC(=O)CCCCCCCCC(=O)OC1CC(C)(C)NC(C)(C)C1 XITRBUPOXXBIJN-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012975 dibutyltin dilaurate Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 1
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229920005570 flexible polymer Polymers 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- YPSLATCYOGSFDU-UHFFFAOYSA-N piperidine;triazine Chemical compound C1CCNCC1.C1=CN=NN=C1 YPSLATCYOGSFDU-UHFFFAOYSA-N 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- FZYCEURIEDTWNS-UHFFFAOYSA-N prop-1-en-2-ylbenzene Chemical compound CC(=C)C1=CC=CC=C1.CC(=C)C1=CC=CC=C1 FZYCEURIEDTWNS-UHFFFAOYSA-N 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229960001860 salicylate Drugs 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 229940047908 strontium chloride hexahydrate Drugs 0.000 description 1
- AMGRXJSJSONEEG-UHFFFAOYSA-L strontium dichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Sr]Cl AMGRXJSJSONEEG-UHFFFAOYSA-L 0.000 description 1
- GJBRNHKUVLOCEB-UHFFFAOYSA-N tert-butyl benzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1 GJBRNHKUVLOCEB-UHFFFAOYSA-N 0.000 description 1
- 150000007970 thio esters Chemical class 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- 238000004383 yellowing Methods 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
- 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
- C08F220/26—Esters containing oxygen in addition to the carboxy oxygen
- C08F220/32—Esters containing oxygen in addition to the carboxy oxygen containing epoxy radicals
- C08F220/325—Esters containing oxygen in addition to the carboxy oxygen containing epoxy radicals containing glycidyl radical, e.g. glycidyl (meth)acrylate
-
- 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
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- 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
- C09D133/14—Homopolymers or copolymers of esters of esters containing halogen, nitrogen, sulfur or oxygen atoms in addition to the carboxy oxygen
-
- 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
- C09D5/03—Powdery paints
-
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Abstract
The invention provides a modified acrylic resin, a preparation method thereof, a powder coating and application thereof, and belongs to the technical field of photovoltaic packaging materials. The method comprises the steps of mixing a monomer, an initiator, a chain transfer agent, a modified nano filler and an organic solvent, and carrying out polymerization reaction to obtain the modified acrylic resin; the monomer is a compound of methyl methacrylate, glycidyl methacrylate, butyl acrylate, styrene and methacrylic acid; the modified nano filler is obtained by modifying inorganic nano filler through a silane coupling agent, the inorganic nano filler is a compound of main filler and a nano strontium titanate auxiliary agent, and the main filler comprises nano silicon dioxide or nano zinc oxide. The inorganic matters and the organic matters in the modified acrylic resin prepared by the method have good compatibility, and the modified acrylic resin has excellent ageing resistance and high light transmittance when being used in a photovoltaic module packaging material.
Description
Technical Field
The invention relates to the technical field of photovoltaic packaging materials, in particular to a modified acrylic resin, a preparation method thereof, a powder coating and application thereof.
Background
The lightweight flexible component has great commercial value in the building photovoltaic integration and novel application fields, wherein the lightweight flexible polymer composite front plate is used for replacing inorganic photovoltaic glass, which is a key for realizing the lightweight and flexibility of the photovoltaic component. The invention patent with publication numbers of WO2019006765A1, CN106283677A, CN108695400A and CN108022988A discloses a method for preparing a packaging front plate material for a photovoltaic module based on powder coating hot pressing glass fiber plates, and the commercialized application is partially realized. Compared with the back plate, the front plate has higher weather resistance requirement, so that the development of the transparent front plate with high transparency and excellent weather resistance, aging resistance and ultraviolet cut-off function has important significance for the photovoltaic industry.
The conventional ultraviolet absorber is an organic ultraviolet absorber, such as a benzophenone compound, a salicylate compound, a benzotriazole compound, a triazine compound and the like, is easy to lose efficacy under long-term irradiation of ultraviolet rays, is poor in long-term reliability, is easy to yellow, further influences the light transmittance and the service life of a front plate, reduces the generated energy and even damages a back plate. Therefore, researchers tend to add inorganic ultraviolet absorbers, for example, the patent of the invention with publication number CN109054531a provides a weather-resistant transparent coating and application thereof, the weather resistance of the coating is improved by adding inorganic fillers (such as nano zinc oxide), but the main component of the coating is organic materials, the inorganic fillers are not substantially involved in the curing crosslinking network of the coating, so that the inorganic fillers in the cured coating are easy to separate from the coating in the subsequent use process, the inorganic fillers after phase separation are easy to migrate to the surface of the coating, the ageing resistance and the light transmittance of a front plate in a photovoltaic module are reduced, and the reliability and the stability of the front plate in long-term outdoor use are poor.
Disclosure of Invention
The invention aims to provide a modified acrylic resin, a preparation method thereof, a powder coating and application, wherein inorganic matters and organic matters in the modified acrylic resin prepared by the method have good compatibility, and the modified acrylic resin has excellent ageing resistance and high light transmittance when being used in a photovoltaic module packaging material.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of modified acrylic resin, which comprises the following steps:
mixing a monomer, an initiator, a chain transfer agent, a modified nano filler and an organic solvent, and carrying out polymerization reaction to obtain the modified acrylic resin;
the monomer is a compound of methyl methacrylate, glycidyl methacrylate, butyl acrylate, styrene and methacrylic acid;
the modified nano filler is obtained by modifying inorganic nano filler through a silane coupling agent, the inorganic nano filler is a compound of main filler and a nano strontium titanate auxiliary agent, and the main filler comprises nano silicon dioxide or nano zinc oxide.
Preferably, the mass ratio of the methyl methacrylate, the glycidyl methacrylate, the butyl acrylate, the styrene and the methacrylic acid is 15-20: 15-20: 5-10: 5-10: 0.1-1; the mass ratio of the monomer, the initiator, the chain transfer agent, the modified nano filler and the organic solvent is 105-120: 1-4: 0.1-1: 0.1 to 0.3: 90-100.
Preferably, the nanometer strontium titanate auxiliary agent is an eighteen-surface body strontium titanate nanometer particle, and the granularity of the nanometer strontium titanate auxiliary agent is 100-200 nm; the granularity of the nano silicon dioxide is 20-40 nm; the granularity of the nano zinc oxide is 20-40 nm; the mass ratio of the main filler to the nanometer strontium titanate auxiliary agent is 3-5: 1.
preferably, the silane coupling agent includes one or more of sulfur-containing silane, aminosilane, vinyl silane, epoxy silane, and methacryloxy silane.
Preferably, the mass ratio of the silane coupling agent to the inorganic nano filler is 2-4: 1, a step of; the temperature of the modification treatment is 50-90 ℃ and the time is 2-4 hours.
Preferably, the initiator comprises one or more of di-tert-butyl peroxide, tert-butyl peroxybenzoate and dicumyl peroxide;
the chain transfer agent includes one or more of isobutyl acrylate, dodecyl mercaptan, and alpha-methylstyrene dimer.
Preferably, the temperature of the polymerization reaction is 120-160 ℃ and the time is 1-5 h.
The invention provides the modified acrylic resin prepared by the preparation method.
The invention provides a powder coating, which is prepared from the modified acrylic resin according to the technical scheme.
The invention provides the application of the modified acrylic resin or the powder coating in the photovoltaic module packaging material.
The invention provides a preparation method of modified acrylic resin, which comprises the following steps: mixing a monomer, an initiator, a chain transfer agent, a modified nano filler and an organic solvent, and carrying out polymerization reaction to obtain the modified acrylic resin; the monomer is a compound of methyl methacrylate, glycidyl methacrylate, butyl acrylate, styrene and methacrylic acid; the modified nano filler is obtained by modifying inorganic nano filler through a silane coupling agent, the inorganic nano filler is a compound of main filler and a nano strontium titanate auxiliary agent, and the main filler comprises nano silicon dioxide or nano zinc oxide. According to the invention, the inorganic nano filler is modified by the silane coupling agent, and the modified nano filler is added in the acrylic resin synthesis stage, so that the problem of phase separation of the coating prepared based on the acrylic resin in the use process can be effectively solved, and the modified acrylic resin provided by the invention has excellent ageing resistance and high light transmittance when being used in the photovoltaic module packaging material.
Drawings
FIG. 1 is a physical view of a modified acrylic resin prepared in comparative example 4.
Detailed Description
The invention provides a preparation method of modified acrylic resin, which comprises the following steps:
mixing a monomer, an initiator, a chain transfer agent, a modified nano filler and an organic solvent, and carrying out polymerization reaction to obtain the modified acrylic resin;
the monomer is a compound of methyl methacrylate, glycidyl methacrylate, butyl acrylate, styrene and methacrylic acid;
the modified nano filler is obtained by modifying inorganic nano filler through a silane coupling agent, the inorganic nano filler is a compound of main filler and a nano strontium titanate auxiliary agent, and the main filler comprises nano silicon dioxide or nano zinc oxide.
In the present invention, unless otherwise specified, all materials are commercially available or prepared by methods well known to those skilled in the art.
The invention prepares the modified acrylic resin by adopting monomers, an initiator, a chain transfer agent, modified nano fillers and an organic solvent through polymerization reaction, wherein the mass ratio of the monomers, the initiator, the chain transfer agent, the modified nano fillers and the organic solvent is preferably 105-120: 1-4: 0.1-1: 0.1 to 0.3:90 to 100, more preferably 106 to 110: 1-2: 0.3 to 0.5:0.1 to 0.3:95 to 100, more preferably 106.7:1.2:0.4:0.2:100. the following first describes each preparation raw material in detail.
In the invention, the modified nano filler is obtained by modifying inorganic nano filler through a silane coupling agent, the inorganic nano filler is a compound of main filler and a nano strontium titanate auxiliary agent, and the main filler comprises nano silicon dioxide or nano zinc oxide. In the invention, the mass ratio of the silane coupling agent to the inorganic nano filler is preferably 2-4: 1, more preferably 2.5 to 3.5:1, further preferably 3:1. in the invention, the nanometer strontium titanate auxiliary agent is preferably an eighteen-surface body strontium titanate nanometer particle, and the granularity of the nanometer strontium titanate auxiliary agent is preferably 100-200 nm; the granularity of the nano silicon dioxide is preferably 20-40 nm; the granularity of the nano zinc oxide is preferably 20-40 nm; the mass ratio of the main filler to the nanometer strontium titanate auxiliary agent is preferably 3-5: 1, more preferably 3.5 to 4.5:1, further preferably 4:1. according to the invention, the main filler and the nanometer strontium titanate auxiliary agent are compounded for use, so that the weather resistance and the light transmittance of the modified acrylic resin after film formation can be improved.
In the present invention, the silane coupling agent preferably includes one or more of sulfur-containing silane, aminosilane, vinyl silane, epoxysilane and methacryloxy silane, more preferably aminosilane; the sulfur-containing silane preferably comprises bis- [3- (triethoxysilane) -propyl ] -tetrasulfide or bis- [3- (triethoxysilane) -propyl ] -disulfide; the aminosilane preferably comprises gamma-aminopropyl triethoxysilane or N-beta- (aminoethyl) -gamma-aminopropyl trimethoxysilane; the vinyl silane preferably comprises vinyl triethoxysilane or vinyl trimethoxysilane; the epoxysilane is preferably 3-glycidoxypropyl trimethoxysilane; the methacryloxy silane preferably comprises gamma-methacryloxy propyl trimethoxy silane or gamma-methacryloxy propyl triisopropoxy silane. The invention preferably adopts the silane coupling agent of the type to modify the inorganic nano filler, can improve the bonding strength of the acrylic resin and the inorganic nano filler, and can also modify the interface area of the acrylic resin and the inorganic nano filler so as to enhance the bonding strength of the boundary layer of the organic phase and the inorganic phase.
In the present invention, the method for preparing the modified nano-filler by modifying the inorganic nano-filler by using the silane coupling agent preferably comprises the following steps:
mixing a silane coupling agent with an acid solution for hydrolysis reaction to obtain a hydrolysate;
and mixing the hydrolysate with inorganic nano filler for modification treatment to obtain the modified nano filler.
The invention mixes the silane coupling agent and the acid solution to carry out hydrolysis reaction to obtain the hydrolysate. In the present invention, the acidic solution is preferably obtained by mixing an acid reagent, water and ethanol; the acid reagent preferably comprises hydrochloric acid, acetic acid or nitric acid; the volume ratio of water to ethanol is preferably 1:2 to 5, more preferably 1: 3-4; the pH value of the acidic solution is preferably 3-4, more preferably 3.5-4. In the invention, the dosage ratio of the silane coupling agent to the acid solution is preferably 10-20 g:115 to 230mL, more preferably 15g:172.5mL. The invention preferably heats the acid solution to the temperature required by the hydrolysis reaction, and then adds the silane coupling agent to carry out the hydrolysis reaction; the temperature of the hydrolysis reaction is preferably 50-90 ℃, more preferably 70 ℃; the time is preferably 2-4 hours, more preferably 3 hours; the hydrolysis reaction is preferably carried out under ultrasonic and stirring conditions, and the specific conditions of the ultrasonic and stirring are not particularly limited in the present invention. The invention preferably carries out hydrolysis reaction under the conditions, which is favorable for ensuring that the silane coupling agent is fully hydrolyzed and further is convenient for reacting with the inorganic nano filler.
After the hydrolysate is obtained, the hydrolysate is mixed with the inorganic nano filler for modification treatment to obtain the modified nano filler. In the invention, the temperature of the modification treatment is preferably 50-90 ℃, more preferably 70 ℃; the time is preferably 2-4 hours, more preferably 3 hours; the modification treatment is preferably performed under stirring conditions, and the specific conditions of the stirring are not particularly limited in the present invention. After the modification treatment, the obtained product is preferably washed, and the washed product can be stored in an organic solvent for later use or dried for later use as required. In the present invention, the reagent used for washing is preferably water and ethanol in sequence, the water is preferably deionized water, and the ethanol is preferably absolute ethanol.
In the present invention, the initiator preferably includes one or more of di-t-butyl peroxide, t-butyl peroxybenzoate (TBPB) and dicumyl peroxide (DCP), more preferably di-t-butyl peroxide.
In the present invention, the chain transfer agent preferably includes one or more of isobutyl acrylate (IBOA), dodecyl mercaptan, and α -methylstyrene dimer (AMSD), more preferably dodecyl mercaptan.
In the invention, the monomer is a compound of methyl methacrylate, glycidyl methacrylate, butyl acrylate, styrene and methacrylic acid, and the mass ratio of the methyl methacrylate, the glycidyl methacrylate, the butyl acrylate, the styrene and the methacrylic acid is preferably 15-20: 15-20: 5-10: 5-10: 0.1 to 1, more preferably 15 to 17: 18-20: 7-8: 7-8: 0.1 to 0.3.
In the present invention, the organic solvent preferably includes one or more of xylene, propylene glycol methyl ether acetate (PMA) and dipropylene glycol butyl ether (DPnB), and more preferably xylene.
The invention mixes monomer, initiator, chain transfer agent, modified nano filler and organic solvent to carry out polymerization reaction, thus obtaining the modified acrylic resin. The invention preferably heats the organic solvent to 120-160 ℃ (preferably 140 ℃), and then adds the modified nano filler under the stirring condition to obtain modified nano filler dispersion liquid; mixing a monomer, an initiator and a chain transfer agent to obtain a monomer mixed solution; and (3) dropwise adding the monomer mixture into the modified nano filler dispersion liquid to carry out polymerization reaction. In the invention, the dripping time is preferably 1-4 h, more preferably 3h; the dripping is preferably uniform dripping; the system temperature in the dropping process is preferably 130-150 ℃, more preferably 140+/-2 ℃. In the invention, the temperature of the polymerization reaction is preferably 130-150 ℃, more preferably 145 ℃; the polymerization reaction time is preferably 1 to 3 hours, more preferably 1 hour, and is started after the completion of the dropwise addition of the monomer mixture. After the polymerization reaction, the obtained feed liquid is preferably subjected to vacuum reduced pressure distillation, the distillation temperature is preferably 140-200 ℃, more preferably 160-180 ℃, and the modified acrylic resin is obtained after distillation until no solvent drops out.
The invention provides the modified acrylic resin prepared by the preparation method. According to the invention, the inorganic nano filler is modified by the silane coupling agent, and the modified nano filler is added in the acrylic resin synthesis stage, so that the problem of phase separation of the coating prepared based on the acrylic resin in the use process can be effectively solved. Specifically, the inorganic nano filler and the organic resin material cannot be effectively combined, the silane coupling agent contains two groups with different chemical properties, namely groups which are easy to react with inorganic matters and groups which are easy to react with organic matters or generate hydrogen bonds, so that the inorganic nano filler is modified by the silane coupling agent, and the modified nano filler is added in the acrylic resin synthesis stage, so that the interface effect between the inorganic matters and the organic matters, such as physical property, electrical property, thermal property, optical property and the like, can be improved, the two groups have good compatibility, the problem of phase separation of the coating prepared by utilizing the obtained modified acrylic resin in the use process is avoided, and the coating has excellent ageing resistance and high light transmittance when used in the photovoltaic module packaging material.
The invention provides a powder coating, which is prepared from the modified acrylic resin according to the technical scheme. In the invention, the preparation raw materials of the powder coating preferably comprise the following components in parts by weight: 50-90 parts of modified acrylic resin, 10-50 parts of curing agent, 0.05-0.2 part of catalyst, 0-20 parts of antioxidant auxiliary agent, 0-10 parts of surface regulator and 0-20 parts of light stabilizer.
The preparation raw materials of the powder coating comprise, by mass, preferably 50-90 parts of modified acrylic resin, more preferably 60-80 parts, and even more preferably 65-75 parts.
Based on the mass parts of the modified acrylic resin, the preparation raw materials of the powder coating preferably comprise 10-50 parts of curing agent, preferably 18-40 parts, and more preferably 22-30 parts. In the present invention, the curing agent preferably includes one or more of dodecanedioic acid, triglycidyl isocyanurate, and isocyanate, and more preferably, dodecanedioic acid.
Based on the mass parts of the modified acrylic resin, the preparation raw materials of the powder coating preferably comprise 0.05-0.2 part of catalyst, and preferably 0.1-0.15 part of catalyst. In the present invention, the catalyst preferably comprises tetrabutylammonium bromide, dibutyltin dilaurate or 2-propylimidazole, more preferably tetrabutylammonium bromide.
Based on the mass parts of the modified acrylic resin, the preparation raw materials of the powder coating preferably comprise 0-20 parts of antioxidant auxiliary agent, preferably 1-15 parts, and more preferably 5-10 parts. In the invention, the antioxidant auxiliary comprises one or more of beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) octadecyl propionate (antioxidant 1076), benzofuranone derivative and thioester antioxidant.
The preparation raw materials of the powder coating preferably comprise 0-10 parts by weight, preferably 1-8 parts by weight, and more preferably 3-5 parts by weight of a surface regulator based on the mass parts of the modified acrylic resin. In the present invention, the surface conditioner preferably includes benzoin.
The preparation raw materials of the powder coating preferably comprise 0-20 parts, preferably 1-15 parts, and more preferably 5-10 parts of light stabilizer based on the mass parts of the modified acrylic resin. In the present invention, the light stabilizer preferably includes a triazine-based light stabilizer or a hindered amine-based light stabilizer; the triazine light stabilizer is preferably 2- [ 2-hydroxy-4- [3- (2-ethylhexyloxy) -2-hydroxypropoxy ] phenyl ] -4, 6-bis (2, 4-dimethylphenyl) -1,3, 5-triazine (light stabilizer UV-405); the hindered amine light stabilizer is preferably one or more of a high molecular weight triazine-piperidine condensate (light stabilizer 119), tinuvin622 and Tinuvin 770.
The method for preparing the powder coating is not particularly limited, and methods well known to those skilled in the art can be adopted.
The invention provides the application of the modified acrylic resin or the powder coating in the photovoltaic module packaging material. In the present invention, the photovoltaic module is preferably a lightweight photovoltaic module. In the present invention, the encapsulant may be particularly used for the front sheet of the photovoltaic module.
The technical solutions of the present invention will be clearly and completely described in the following in connection with the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The following examples and comparative examples were conducted with the use of the eighteen-face strontium titanate nanoparticles, modified strontium titanate, modified silica, and modified zinc oxide as the products prepared in preparation examples 1 to 4.
Preparation example 1
The preparation method of the decaoctahedral strontium titanate nanoparticle comprises the following steps:
mixing palmitic acid, ethylene glycol and 1, 2-butanediol with water to obtain a composite morphology regulator, wherein the concentration of the palmitic acid in the composite morphology regulator is 0.2wt%, the concentration of the ethylene glycol is 1wt%, and the concentration of the 1, 2-butanediol is 0.2wt%; dropwise adding titanium tetrachloride water solution with the concentration of 0.003g/mL into the composite morphology regulator, wherein the volume ratio of the composite morphology regulator to the titanium tetrachloride water solution is 1:2, stirring for 30min, and cooling with ice water in the stirring process to obtain a mixed solution I;
mixing the mixed solution I, a sodium hydroxide aqueous solution with the concentration of 0.033g/mL and a strontium chloride hexahydrate aqueous solution with the concentration of 0.01g/mL according to the volume ratio of 3:3:1, stirring for 30min to obtain a mixed solution II with the pH value of 14.2;
and heating the mixed solution II to 190 ℃ at a heating rate of 4 ℃/min for hydrothermal reaction for 24 hours, cooling at a cooling rate of 2 ℃/min, centrifuging the substances after the hydrothermal reaction, alternately washing the precipitate with water and ethanol for 3 times, and finally drying at 80 ℃ for 6 hours to obtain the dodecahedral strontium titanate nano particles (granularity is 100-200 nm).
Preparation example 2
The preparation method comprises the following steps:
mixing hydrochloric acid, water and ethanol to obtain an acidic solution, wherein the pH value of the acidic solution is 4, and the volume ratio of the water to the ethanol in the acidic solution is 1:3; heating 100mL of acid solution to 70 ℃, then adding 15g of silane coupling agent KH550, and carrying out hydrolysis reaction for 1h under the conditions of ultrasound and stirring to obtain hydrolysate; adding 5g of the decaoctahedral strontium titanate nanoparticles in preparation example 1 into the hydrolysate, and carrying out modification treatment for 3h under the condition of stirring; after the modification treatment is finished, washing the obtained product with deionized water and absolute ethyl alcohol for 3 times respectively to obtain an absolute ethyl alcohol washing product; and (3) washing a part of the absolute ethyl alcohol washing product with dimethylbenzene, then storing the dimethylbenzene for standby, and drying the rest absolute ethyl alcohol washing product in an oven at 80 ℃ for standby.
Preparation example 3
The preparation of the modified silica comprises the following steps:
mixing hydrochloric acid, water and ethanol to obtain an acidic solution, wherein the pH value of the acidic solution is 4, and the volume ratio of the water to the ethanol in the acidic solution is 9:1; heating 175mL of acid solution to 70 ℃, then adding 15g of silane coupling agent KH570, and carrying out hydrolysis reaction for 1h under the conditions of ultrasound and stirring; adding 5g of nano silicon dioxide (with the granularity of 20-40 nm) into the hydrolysate, and carrying out heat preservation under the stirring condition for modification treatment for 3h; after the modification treatment is finished, washing the obtained product with deionized water and absolute ethyl alcohol for 3 times respectively to obtain an absolute ethyl alcohol washing product; and (3) washing a part of the absolute ethyl alcohol washing product with dimethylbenzene, then storing the dimethylbenzene for standby, and drying the rest absolute ethyl alcohol washing product in an oven at 80 ℃ for standby.
Preparation example 4
The preparation method comprises the following steps:
mixing hydrochloric acid, water and ethanol to obtain an acidic solution, wherein the pH value of the acidic solution is 4, and the volume ratio of the water to the ethanol in the acidic solution is 9:1; heating 175mL of acid solution to 70 ℃, then adding 15g of silane coupling agent KH550, and carrying out hydrolysis reaction for 1h under the conditions of ultrasound and stirring to obtain hydrolysate; adding 5g of nano zinc oxide (with the granularity of 20-40 nm) into the hydrolysate, and carrying out heat preservation under the stirring condition for modification treatment for 3h; after the modification treatment is finished, washing the obtained product with deionized water and absolute ethyl alcohol for 3 times respectively to obtain an absolute ethyl alcohol washing product; and (3) washing a part of the absolute ethyl alcohol washing product with dimethylbenzene, then storing the dimethylbenzene for standby, and drying the rest absolute ethyl alcohol washing product in an oven at 80 ℃ for standby.
Example 1
Heating an organic solvent to 140 ℃, starting a stirring system and a condensing system at the same time, and then adding modified nano filler to obtain modified nano filler dispersion liquid; mixing a monomer, an initiator and a chain transfer agent to obtain a monomer mixed solution;
dripping the monomer mixed solution into the modified nano filler dispersion liquid at a constant speed under the condition of 140+/-2 ℃ for 3 hours, heating to 145 ℃ after dripping, and then carrying out polymerization reaction for 1 hour by heat preservation; and after the polymerization reaction is finished, carrying out vacuum reduced pressure distillation on the obtained feed liquid, and steaming out until no solvent is dropped out, thereby obtaining the modified acrylic resin.
The formulation of the modified acrylic resin in this example is shown in Table 1.
Table 1 formulation of modified acrylic resin in example 1
Example 2
A modified acrylic resin was prepared in the same manner as in example 1 except that modified silica was replaced with modified zinc oxide.
Comparative example 1
An acrylic resin was prepared according to the method of example 1, except that the modified nanofiller was omitted.
Comparative example 2
The acrylic resin prepared in comparative example 1 was mixed with the modified nanofiller of example 1 to obtain a modified acrylic resin.
Comparative example 3
The acrylic resin prepared in comparative example 1 was mixed with the modified nanofiller of example 2 to obtain a modified acrylic resin.
Comparative example 4
Modified acrylic resin was prepared according to the method of example 1, except that the modified nanofiller was replaced with an unmodified nanofiller, i.e., the nanofiller, which was not modified with a silane coupling agent, and a monomer, an initiator, a chain transfer agent, and an organic solvent were directly used to prepare the modified acrylic resin.
FIG. 1 is a physical diagram of a modified acrylic resin prepared in comparative example 4, and shows that the modified acrylic resin prepared directly from a nanofiller, which is not modified with a silane coupling agent, and a monomer, an initiator, a chain transfer agent, and an organic solvent is easily phase-separated.
Test example 1
The appearance of the acrylic resins prepared in examples 1 to 2 and comparative example 1 was observed, and the epoxy value, acid value and solid content were measured, and the results are shown in table 2. As can be seen from Table 2, the modified nanofiller was uniformly incorporated into the resin, the epoxy value of the resin was slightly reduced after the modified nanofiller was added, and the amount of the curing agent was changed.
TABLE 2 test results of acrylic resins prepared in examples 1-2 and comparative example 1
Test example 2
100 parts of acrylic resin (specifically, acrylic resins prepared in examples 1-2 and comparative examples 1-3) are mixed with 0.1 part of catalyst (specifically, tetrabutylammonium bromide) and a proper part of curing agent (specifically, dodecanedioic acid) in parts by weight, wherein the mass ratio of the acrylic resin to the curing agent in example 1 is 100:27.6, the mass ratio of the acrylic resin to the curing agent in example 2 is 100:23, the mass ratio of the acrylic resin to the curing agent in comparative examples 1 to 3 is 100:21.88, and polishing to obtain the powder coating with the granularity of 40-60 mu m.
The appearance of the powder coating was observed and the tilt flowability and gel time were measured using a gel time meter, and the results are shown in table 3. As can be seen from table 3, the gel time of the powder coating after the addition of the modified nanofiller was significantly shortened, and the powder coating prepared with the acrylic resin of examples 1 to 2 was longer and superior in tilting fluidity to the powder coating prepared with the acrylic resin of comparative examples 2 to 3.
TABLE 3 test results for powder coatings
Test example 3
According to parts by weight, 72 parts of acrylic resin (specifically acrylic resin prepared in examples 1-2 and comparative examples 1-3 respectively), 21 parts of curing agent (specifically dodecanedioic acid), 1 part of antioxidant auxiliary agent (specifically antioxidant 1076), 0.085 part of catalyst (specifically tetrabutylammonium bromide), 0.8 part of surface regulator (specifically benzoin) and 1.66 parts of light stabilizer (specifically light stabilizer UV-405) are mixed, melt extruded at 120 ℃, the obtained extrusion material is cooled and crushed to have the granularity of 0.2-1 cm, and then further crushed and classified and screened to obtain the product with the granularity of 30-150 mu mA base material; mixing the matrix material with a dispersing agent (specifically alumina with the granularity of 2-4 mu m, wherein the mass of the dispersing agent is 0.1% of that of the matrix material) to obtain mixed powder; the mixed powder is uniformly scattered on glass fiber cloth (specifically woven glass fiber cloth with gram weight of 100 g/m) by using powder scattering equipment 2 ) Filling glass fiber cloth with mixed powder on the surface into laminating equipment at the powder spraying speed of 4m/min, closing the mold, heating to 130 ℃ to melt the mixed powder, infiltrating the mixed powder into the glass fiber cloth, curing for 30min at 160 ℃ under the pressure of 10MPa, cooling and demolding after curing is finished to obtain the flexible composite material; the content of the mixed powder in the flexible composite material is 55wt%, and the thickness of the flexible composite material is 0.15mm.
The light transmittance of the flexible composite material was tested and the results are shown in table 4. As can be seen from Table 4, the light transmittance of the flexible composite material was improved after the modified nanofiller was added, and the light transmittance of the flexible composite material prepared by the acrylic resin of examples 1 to 2 was better than that of the flexible composite material prepared by the acrylic resin of comparative examples 2 to 3.
Table 4 test results of flexible composites
Test example 4
The acrylic resins prepared in examples 1 to 2 and comparative examples 1 to 3 were subjected to ultraviolet aging test (QUV-B), specifically as follows:
1. the testing method comprises the following steps: GB/T14522-2008.
2. Test conditions: the type of exposure period is specifically shown in table 5.
TABLE 5 ultraviolet aging test conditions
3. Test time: 3000h.
4. Detection equipment: ultraviolet QUV/SPRAY, model: 20-36601-93-SPRAY.
Table 6 shows the results of ultraviolet aging tests of the acrylic resins prepared in examples 1 to 2 and comparative examples 1 to 3, and it is apparent from Table 6 that the total amount of ultraviolet irradiation is 62.45KWh/m 2 When the modified nano filler is not added in the comparative example 1, the yellowing and chromatic aberration change of the acrylic resin prepared by the modified nano filler is maximum, and compared with the light transmittance before the ultraviolet aging test, the light transmittance after the ultraviolet aging test is reduced by 1.1%; the acrylic resin prepared by adding the modified nanofiller in examples 1-2 and comparative examples 1-2 has improved light transmittance after ultraviolet aging test, wherein the acrylic resin prepared in example 1 has the best ultraviolet aging resistance, and the light transmittance after ultraviolet aging test is improved by 0.3% compared with the light transmittance before ultraviolet aging test.
TABLE 6 ultraviolet aging test results of acrylic resins
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (10)
1. The preparation method of the modified acrylic resin is characterized by comprising the following steps:
mixing a monomer, an initiator, a chain transfer agent, a modified nano filler and an organic solvent, and carrying out polymerization reaction to obtain the modified acrylic resin;
the monomer is a compound of methyl methacrylate, glycidyl methacrylate, butyl acrylate, styrene and methacrylic acid;
the modified nano filler is obtained by modifying inorganic nano filler through a silane coupling agent, the inorganic nano filler is a compound of main filler and a nano strontium titanate auxiliary agent, and the main filler comprises nano silicon dioxide or nano zinc oxide.
2. The preparation method of claim 1, wherein the mass ratio of methyl methacrylate, glycidyl methacrylate, butyl acrylate, styrene and methacrylic acid is 15-20: 15-20: 5-10: 5-10: 0.1-1; the mass ratio of the monomer, the initiator, the chain transfer agent, the modified nano filler and the organic solvent is 105-120: 1-4: 0.1-1: 0.1 to 0.3: 90-100.
3. The preparation method of claim 1, wherein the nanometer strontium titanate auxiliary agent is an eighteen-surface body strontium titanate nanometer particle, and the granularity of the nanometer strontium titanate auxiliary agent is 100-200 nm; the granularity of the nano silicon dioxide is 20-40 nm; the granularity of the nano zinc oxide is 20-40 nm; the mass ratio of the main filler to the nanometer strontium titanate auxiliary agent is 3-5: 1.
4. the method of claim 1, wherein the silane coupling agent comprises one or more of sulfur-containing silane, aminosilane, vinyl silane, epoxy silane, and methacryloxy silane.
5. The preparation method according to any one of claims 1 to 4, wherein the mass ratio of the silane coupling agent to the inorganic nanofiller is 2 to 4:1, a step of; the temperature of the modification treatment is 50-90 ℃ and the time is 2-4 hours.
6. The production method according to claim 1 or 2, wherein the initiator comprises one or more of di-t-butyl peroxide, t-butyl peroxybenzoate, and dicumyl peroxide;
the chain transfer agent includes one or more of isobutyl acrylate (IBOA), dodecyl mercaptan, and alpha-methyl styrene dimer.
7. The preparation method according to claim 1, wherein the polymerization reaction is carried out at a temperature of 120-160 ℃ for 1-5 hours.
8. The modified acrylic resin produced by the production method according to any one of claims 1 to 7.
9. A powder coating comprising the modified acrylic resin of claim 8 as a raw material.
10. Use of the modified acrylic resin of claim 8 or the powder coating of claim 9 in a photovoltaic module encapsulant.
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