CN117210058A - Water-based ink-regulating oil and preparation method and application thereof - Google Patents
Water-based ink-regulating oil and preparation method and application thereof Download PDFInfo
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- CN117210058A CN117210058A CN202311064755.3A CN202311064755A CN117210058A CN 117210058 A CN117210058 A CN 117210058A CN 202311064755 A CN202311064755 A CN 202311064755A CN 117210058 A CN117210058 A CN 117210058A
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 39
- 239000004925 Acrylic resin Substances 0.000 claims abstract description 55
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 55
- 239000010452 phosphate Substances 0.000 claims abstract description 55
- 239000002966 varnish Substances 0.000 claims abstract description 46
- 229920000178 Acrylic resin Polymers 0.000 claims abstract description 42
- 239000000178 monomer Substances 0.000 claims abstract description 39
- -1 phosphate modified acrylate Chemical class 0.000 claims abstract description 33
- 239000002904 solvent Substances 0.000 claims abstract description 25
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 21
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 20
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 19
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 16
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002270 dispersing agent Substances 0.000 claims abstract description 12
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 11
- 229920000570 polyether Polymers 0.000 claims abstract description 11
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 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 6
- 239000002562 thickening agent Substances 0.000 claims abstract description 5
- SEILKFZTLVMHRR-UHFFFAOYSA-N 2-phosphonooxyethyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCOP(O)(O)=O SEILKFZTLVMHRR-UHFFFAOYSA-N 0.000 claims abstract description 4
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims abstract description 4
- 125000005250 alkyl acrylate group Chemical group 0.000 claims abstract description 3
- 239000011521 glass Substances 0.000 claims description 47
- 239000003999 initiator Substances 0.000 claims description 37
- 239000003795 chemical substances by application Substances 0.000 claims description 29
- 238000002156 mixing Methods 0.000 claims description 24
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 15
- 239000011347 resin Substances 0.000 claims description 15
- 229920005989 resin Polymers 0.000 claims description 15
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000001038 titanium pigment Substances 0.000 claims description 9
- 239000002518 antifoaming agent Substances 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 6
- CUVLMZNMSPJDON-UHFFFAOYSA-N 1-(1-butoxypropan-2-yloxy)propan-2-ol Chemical compound CCCCOCC(C)OCC(C)O CUVLMZNMSPJDON-UHFFFAOYSA-N 0.000 claims description 3
- CUDYYMUUJHLCGZ-UHFFFAOYSA-N 2-(2-methoxypropoxy)propan-1-ol Chemical compound COC(C)COC(C)CO CUDYYMUUJHLCGZ-UHFFFAOYSA-N 0.000 claims description 3
- WAEVWDZKMBQDEJ-UHFFFAOYSA-N 2-[2-(2-methoxypropoxy)propoxy]propan-1-ol Chemical compound COC(C)COC(C)COC(C)CO WAEVWDZKMBQDEJ-UHFFFAOYSA-N 0.000 claims description 3
- RNFAKTRFMQEEQE-UHFFFAOYSA-N Tripropylene glycol butyl ether Chemical compound CCCCOC(CC)OC(C)COC(O)CC RNFAKTRFMQEEQE-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000003002 pH adjusting agent Substances 0.000 claims description 2
- GICQWELXXKHZIN-UHFFFAOYSA-N 2-[2-[(2-methylpropan-2-yl)oxy]ethoxy]ethanol Chemical compound CC(C)(C)OCCOCCO GICQWELXXKHZIN-UHFFFAOYSA-N 0.000 claims 1
- 238000005245 sintering Methods 0.000 abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 5
- 238000003756 stirring Methods 0.000 description 53
- 239000000843 powder Substances 0.000 description 42
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 40
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 description 28
- 239000000243 solution Substances 0.000 description 28
- 239000003921 oil Substances 0.000 description 26
- 239000000203 mixture Substances 0.000 description 19
- 239000004408 titanium dioxide Substances 0.000 description 19
- 238000010438 heat treatment Methods 0.000 description 16
- 239000002002 slurry Substances 0.000 description 16
- 238000005303 weighing Methods 0.000 description 14
- 230000004907 flux Effects 0.000 description 13
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 description 11
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 11
- 239000010410 layer Substances 0.000 description 11
- 239000002202 Polyethylene glycol Substances 0.000 description 10
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 10
- 238000001816 cooling Methods 0.000 description 10
- 238000002844 melting Methods 0.000 description 10
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 10
- 229920001223 polyethylene glycol Polymers 0.000 description 10
- 238000007650 screen-printing Methods 0.000 description 10
- 238000005336 cracking Methods 0.000 description 9
- 239000003085 diluting agent Substances 0.000 description 9
- 239000006185 dispersion Substances 0.000 description 9
- 239000007788 liquid Substances 0.000 description 9
- 230000001105 regulatory effect Effects 0.000 description 9
- 230000008719 thickening Effects 0.000 description 9
- CBTVGIZVANVGBH-UHFFFAOYSA-N aminomethyl propanol Chemical compound CC(C)(N)CO CBTVGIZVANVGBH-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 7
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 238000000354 decomposition reaction Methods 0.000 description 7
- 230000008018 melting Effects 0.000 description 7
- 230000003472 neutralizing effect Effects 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 229910052710 silicon Inorganic materials 0.000 description 7
- 239000010703 silicon Substances 0.000 description 7
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 6
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 6
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 description 6
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 description 6
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 description 6
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 description 6
- 238000007639 printing Methods 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- DNEHKUCSURWDGO-UHFFFAOYSA-N aluminum sodium Chemical compound [Na].[Al] DNEHKUCSURWDGO-UHFFFAOYSA-N 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000013530 defoamer Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- VALXVSHDOMUUIC-UHFFFAOYSA-N 2-methylprop-2-enoic acid;phosphoric acid Chemical compound OP(O)(O)=O.CC(=C)C(O)=O VALXVSHDOMUUIC-UHFFFAOYSA-N 0.000 description 3
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 3
- UGZICOVULPINFH-UHFFFAOYSA-N acetic acid;butanoic acid Chemical compound CC(O)=O.CCCC(O)=O UGZICOVULPINFH-UHFFFAOYSA-N 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 239000001768 carboxy methyl cellulose Substances 0.000 description 3
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 3
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000002310 reflectometry Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 238000005496 tempering Methods 0.000 description 3
- 238000009736 wetting Methods 0.000 description 3
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 101100393883 Arabidopsis thaliana XLT2 gene Proteins 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 229920006217 cellulose acetate butyrate Polymers 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- AQEFLFZSWDEAIP-UHFFFAOYSA-N di-tert-butyl ether Chemical compound CC(C)(C)OC(C)(C)C AQEFLFZSWDEAIP-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 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 description 1
- 229940058020 2-amino-2-methyl-1-propanol Drugs 0.000 description 1
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- HCYAFALTSJYZDH-UHFFFAOYSA-N Desimpramine Chemical compound C1CC2=CC=CC=C2N(CCCNC)C2=CC=CC=C21 HCYAFALTSJYZDH-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- UEEJHVSXFDXPFK-UHFFFAOYSA-O N-dimethylethanolamine Chemical compound C[NH+](C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-O 0.000 description 1
- IAXXETNIOYFMLW-COPLHBTASA-N [(1s,3s,4s)-4,7,7-trimethyl-3-bicyclo[2.2.1]heptanyl] 2-methylprop-2-enoate Chemical compound C1C[C@]2(C)[C@@H](OC(=O)C(=C)C)C[C@H]1C2(C)C IAXXETNIOYFMLW-COPLHBTASA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000001476 alcoholic effect 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
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 235000019400 benzoyl peroxide Nutrition 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 239000012986 chain transfer agent Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
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- 229960003914 desipramine Drugs 0.000 description 1
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- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 238000007499 fusion processing Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229940119545 isobornyl methacrylate Drugs 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
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- 239000000377 silicon dioxide Substances 0.000 description 1
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- 239000007858 starting material Substances 0.000 description 1
- 230000003335 steric effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009974 thixotropic effect Effects 0.000 description 1
Landscapes
- Paints Or Removers (AREA)
Abstract
The invention discloses water-based ink-regulating oil and a preparation method and application thereof, wherein the preparation raw materials comprise the following components in parts by weight: 1 to 10 parts of phosphate modified acrylic resin, 0.5 to 5 parts of thickener, 1 to 2 parts of dispersant and 80 to 95 parts of solvent; the preparation raw materials of the phosphate modified acrylic resin comprise: phosphate functional monomers, methoxypolyethylene glycol acrylate, acrylic acid and acrylate; the phosphate functional monomer comprises at least one of methacrylic acid acyloxyethyl phosphate, ethylene glycol methacrylate phosphate, alkyl acrylate phosphate, allyl polyether phosphate and methacrylic acid polyether phosphate; the weight average molecular weight of the phosphate modified acrylic resin is 5000-100000 MW. The environment-friendly water-based ink varnish prepared from the phosphate modified acrylate resin has low smell, is environment-friendly, has little ash content after high-temperature sintering, has little carbon residue, and has little influence on the color of a glaze layer.
Description
Technical Field
The invention belongs to the technical field of ink, and particularly relates to water-based ink-regulating oil, and a preparation method and application thereof.
Background
The existing photovoltaic glass high-reflection ink is generally prepared from low-melting-point glass powder, titanium dioxide, ink-regulating oil and the like, wherein the content of the powder is up to more than 70%. The ink-regulating oil, also called as scraping plate oil (binder), is an important component of printing ink, and the rheological property, viscosity, drying property, film forming property, printing property and the like of the ink depend on the ink-regulating oil, and is the key of the quality of the ink. The main components of the glass screen printing ink are various organic resins, high boiling point organic solvents and auxiliary agents, and the glass screen printing ink mainly has the functions of mixing powdery low-melting glass powder, titanium pigment and other pigment fillers into paste so as to facilitate screen printing, and the glass powder and the titanium pigment can be temporarily adhered to the surface of a smooth glass product by means of the viscosity of the glass powder and the titanium pigment, and the glass powder and the titanium pigment must be completely volatilized and burnt in the high-temperature decoration firing (firing) process. The sintering process of the high-reflection printing ink for the photovoltaic glass is generally carried out at 680-750 ℃ for 2-6 min, the softening point of the low-melting glass powder for the high-reflection printing ink for the photovoltaic glass is generally between 450-600 ℃, the resin is rapidly decomposed at high temperature during glass tempering, and meanwhile, the low-melting glass powder is melted and softened to replace the resin as a binder to form an enamel body, so that the printing ink is converted from organic bonding to inorganic bonding and firmly bonded with the glass. In order to obtain good sintering properties (high reflection and ink layer compactness) and acid resistance, it is desirable that the resin and the low melting glass frit have good matching properties, i.e., to ensure that the low melting glass frit starts to melt flow when the resin decomposition is completed. Therefore, it is required that the final decomposition temperature of the resin and the softening point of the low melting glass frit are not greatly different; meanwhile, the softening point and crystallization temperature of the low-melting-point glass powder are required to be lower than the sintering temperature, so that the ink can be fully melted, flowed and spread into a compact surface layer during sintering, and the surface layer is crystallized to achieve better reflectivity and weather resistance. The problem of matching between the decomposition temperature of the varnish resin and the melting temperature of the selected low-melting-point glass powder and the temperature of a tempering furnace is required, the varnish cannot be decomposed prematurely, the ink layer is easy to pulverize and fall off due to the fact that the glass powder is not melted in the early decomposition process, the varnish cannot be decomposed too late, organic matters cannot be decomposed completely due to the fact that glass liquid melted by the glass powder covers and wraps the varnish in the late decomposition process, and the colored glaze is coked and blackened. In addition, for the ink with high powder content, the ink-preparing oil resin is also required to have excellent wetting and dispersing ability on powder, so that the surface of the powder is rapidly wetted and wrapped and the powder is quickly opened after penetrating into the powder, the powder dispersing and grinding efficiency is improved, the powder dispersing particle size is small, meanwhile, the agglomeration of the powder can be prevented, and the inorganic powder is easy to settle and delaminate, so that the storage stability and printing adaptability of the ink are affected.
In the prior art, the introduction of the organic silicon can reduce the surface energy and increase the wettability of resin to glass powder and titanium pigment, but the introduction of the organic silicon and styrene can also cause the decomposition temperature of the resin to be increased, so that the white high-reflection glaze layer is easy to cause higher carbon residue after sintering, and the color of the glaze layer is blacker; meanwhile, mass production data show that the introduction of the organic silicon easily causes 'white fog' in the toughening furnace, namely, the organic silicon is gasified to form fumed silica which is adhered to the upper cavity of the toughening furnace and the conveying roller, and the furnace needs to be shut down frequently for cleaning, so that the production efficiency is affected.
In summary, developing an aqueous ink-transfer oil with less residual carbon after high-temperature sintering is a difficult problem that researchers in the field need to explore.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems in the prior art described above. Therefore, the invention provides the water-based ink-transfer oil, and the preparation method and application thereof, and the water-based ink-transfer oil is prepared from the phosphate modified acrylic ester resin, so that the water-based ink-transfer oil has low smell, is environment-friendly, has good screen printability, does not block a screen plate, has no screen printing problems such as sawtooth ink overflow and the like, has less ash content after high-temperature sintering, has less carbon residue, and has small influence on the color of a glaze layer.
The second aspect of the invention provides a preparation method of the water-based ink-regulating oil.
The third aspect of the invention also provides a reflective glaze, and the preparation raw materials of the reflective glaze comprise the water-based varnish.
The fourth aspect of the invention also provides an application of the reflective glaze in photovoltaic glass.
According to a first aspect of the invention, an aqueous varnish is provided, which comprises the following raw materials in parts by weight: 1 to 10 parts of phosphate modified acrylic resin, 0.5 to 5 parts of thickener, 1 to 2 parts of dispersant and 80 to 95 parts of solvent;
the preparation raw materials of the phosphate modified acrylic ester resin comprise: phosphate functional monomers, methoxypolyethylene glycol acrylate, acrylic acid and acrylate;
the phosphate functional monomer comprises at least one of methacrylic acid acyloxyethyl phosphate, ethylene glycol methacrylate phosphate, alkyl acrylate phosphate, allyl polyether phosphate and methacrylic acid polyether phosphate;
the weight average molecular weight of the phosphate modified acrylic resin is 5000-100000 MW
The first aspect according to the invention has at least the following advantages:
the phosphate modified acrylic resin is prepared by introducing phosphate functional monomers, methoxy polyethylene glycol acrylic ester and conventional acrylic acid/acrylic ester monomers, and has the advantages of low molecular weight, poor continuous film forming property, high molecular weight, poor wetting and dispersing effects on powder and high decomposition temperature, and the weight average molecular weight of the water soluble acrylic resin is 5000-100000 MW. The environment-friendly water-based ink-regulating oil is low in smell, environment-friendly, good in wetting and dispersing capacity for powder materials such as glass powder and titanium dioxide, stable in storage of the prepared photovoltaic glass ink, good in screen printing performance, free of screen blocking, free of screen printing problems such as sawtooth ink overflow and the like, less in ash content after high-temperature sintering, less in carbon residue, and small in influence on the color of a glaze layer. Meanwhile, the photovoltaic glass ink prepared by the environment-friendly water-based ink-regulating oil has good process adaptability, has lower requirements on temperature and humidity environments between silk-screen printing, can be cleaned by water, and reduces the comprehensive cost for preparing the glass glaze layer of the photovoltaic backboard.
In some embodiments of the invention, the thickener comprises at least one of hydroxypropyl methylcellulose, cellulose acetate butyrate and carboxymethyl cellulose acetate butyrate.
In some embodiments of the invention, the dispersant includes at least one of BYK-180, BYK-182, TEGO750W, TEGO755W, and TEGO 760W.
In some embodiments of the invention, the solvent of the aqueous ink-transfer oil includes at least one of diethylene glycol butyl ether, dipropylene glycol methyl ether, tripropylene glycol methyl ether, dipropylene glycol butyl ether, tripropylene glycol butyl ether, diethylene glycol t-butyl ether, RY305, RY306, RY307, RY308, RY505, and the like.
The solvent is a low-carbon environment-friendly high-boiling point solvent which does not contain benzene rings and does not contain benzene rings, and has lipophilic covalent ether bonds and hydrophilic alcoholic hydroxyl groups on chemical structures, so that the solvent has the characteristics of low surface tension, high boiling point, slow volatilization, low toxicity, low odor, good solubility to resin and good hydrophilicity, can improve ink leveling, eliminate pinholes, small particles and bubbles of a paint film, can also adjust ink drying speed, is favorable for screen printing adaptability, is not easy to block a screen printing plate, and can be cleaned by water.
In some embodiments of the invention, the aqueous varnish preparation raw material further comprises an antifoaming agent and a leveling agent.
In some embodiments of the invention, the defoamer comprises a non-silicon based defoamer.
In some embodiments of the invention, the non-silicon based defoamer includes at least one of BYK1790, BYK-A501, TEGO Foamex 830, TEGO 936, and TEGO 920.
In some embodiments of the invention, the leveling agent comprises a water-oil universal non-silicone leveling agent.
In some embodiments of the present invention, the water-oil universal non-silicone leveling agent includes at least one of BYK358N, BYK N and BYK 381.
In some embodiments of the present invention, the preparation raw materials of the phosphate modified acrylate resin include 1 to 5 parts by weight of phosphate functional monomer, 2 to 5 parts by weight of methoxypolyethylene glycol acrylate, 2 to 5 parts by weight of acrylic acid and 35 to 60 parts by weight of acrylate.
In some embodiments of the invention, the methoxypolyethylene glycol acrylate comprises at least one of methoxypolyethylene glycol (350) acrylate, methoxypolyethylene glycol (400) acrylate, methoxypolyethylene glycol (550) acrylate, and methoxypolyethylene glycol (1000) acrylate.
The methoxy polyethylene glycol acrylate has great amount of ether bond in the molecular chain, so that the resin has raised solubility in the dispersing medium, and the polyether segment is relatively long, so as to stabilize the powder particle via steric effect.
In some embodiments of the invention, the acrylate comprises at least one of methyl methacrylate, butyl acrylate, and hydroxyethyl acrylate.
In some embodiments of the invention, the phosphate modified acrylate resin is prepared from a starting material that further includes an alcohol ether solvent.
In some embodiments of the invention, the alcohol ether solvent comprises at least one of diethylene glycol butyl ether, dipropylene glycol methyl ether, tripropylene glycol methyl ether, dipropylene glycol butyl ether, tripropylene glycol butyl ether, and diethylene glycol t-butyl ether.
In some embodiments of the present invention, the preparation raw materials of the phosphate modified acrylate resin further comprise an initiator and a pH regulator.
In some embodiments of the invention, the initiator comprises at least one of azobisisobutyronitrile, azobisisobutylamidine hydrochloride, benzoyl peroxide, and t-butyl peroxybenzoate.
In some embodiments of the invention, the pH adjuster comprises at least one of ammonia, N-dimethylethanolamine, and 2-amino-2-methyl-1-propanol.
In some embodiments of the invention, the preparation raw materials of the phosphate modified acrylate resin comprise, by weight, 1-5 parts of phosphate functional monomer, 2-5 parts of methoxy polyethylene glycol acrylate, 2-5 parts of acrylic acid, 20-30 parts of methyl methacrylate, 10-20 parts of butyl acrylate, 5-10 parts of hydroxyethyl acrylate, 40-60 parts of alcohol ether solvent and 0.1-5 parts of pH regulator.
In some embodiments of the invention, the initiator comprises 0.2 to 2% by weight of the total monomer weight.
In some embodiments of the present invention, the method for preparing a phosphate modified acrylate resin includes: and mixing the preparation raw materials of the phosphate modified acrylate resin.
In some embodiments of the invention, the temperature of the mixing is 70-100 ℃.
In some preferred embodiments of the present invention, the method for preparing the modified phosphate modified acrylate resin comprises: taking about 1/3 of mixed monomer (methyl methacrylate, butyl acrylate, hydroxyethyl acrylate, acrylic acid and a copolymerization function monomer mixture) of an alcohol ether solvent at 70-100 ℃, adding 1/4 of initiator into a four-neck flask, reacting for 15min, dropwise adding the mixture of the rest mixed monomer and 1/2 of initiator into the four-neck flask within 3-4 h, preserving heat for reacting for 3-6 h after dropwise adding, adding the rest 1/4 of initiator, continuously preserving heat for reacting for 1-2 h, cooling to 40-50 ℃, adding a pH regulator, regulating the pH of the system to 8-9, and stirring for reacting for 0.5h to obtain the water-soluble acrylic resin.
The mixture of the copolymerization functional monomers is phosphate functional monomers and methoxy polyethylene glycol acrylate.
According to a second aspect of the present invention, a method for preparing an aqueous varnish is provided, comprising mixing the preparation raw materials of the aqueous varnish.
In some embodiments of the present invention, the method of preparing the aqueous varnish includes mixing the thickener and the solvent, adding the phosphate modified acrylate resin, mixing uniformly, and adding the dispersant, the defoamer, the leveling agent and the neutralizer.
The third aspect of the invention provides a reflective glaze, wherein the preparation raw materials of the reflective glaze comprise the aqueous varnish.
In some embodiments of the present invention, the reflective glaze material further comprises sodium aluminum silicate salt and titanium pigment.
In some embodiments of the invention, the sodium aluminum silicate salt comprises Sipernat 820A of desipramine.
The sodium aluminum silicate salt has high whiteness, can replace part of titanium dioxide to improve the covering power and whiteness of a glaze layer, thereby improving the reflectivity of the white glaze layer, has auxiliary thickening and thixotropic effects, can improve the defects of ink overflow, saw teeth, paste plates and the like in the silk screen printing process of the glaze, has lower cost than the titanium dioxide, and has the effects of improving the whiteness, improving the reflectivity and reducing the cost by replacing part of the titanium dioxide.
In some embodiments of the invention, the reflective glaze is prepared from raw materials further comprising a glass flux, high temperature crack resistance powder, and a diluent.
In some embodiments of the invention, the reflective glaze is prepared from the following raw materials, by weight, 20-30 parts of environment-friendly water-based ink-transfer oil, 3-18 parts of titanium dioxide, 12-41.5 parts of aluminum silicate sodium salt, 55-70 parts of glass flux and 0-10 parts of high-temperature anti-cracking powder.
In some embodiments of the invention, the titanium dioxide comprises rutile titanium dioxide.
The weather resistance of the white high-reflection glaze layer can be ensured under the addition amount.
The titanium dioxide is rutile titanium dioxide prepared by a chlorination method, and silica and alumina are used for inorganic coating treatment. The titanium dioxide prepared by the method has extremely low impurity content, and silicon oxide and aluminum oxide are used for coating treatment, so that lattice defects caused by titanium dioxide under the ultraviolet irradiation condition can be blocked, light activation points on the surface of the titanium dioxide are shielded, and the PID resistance is improved.
In some embodiments of the invention, the glass flux comprises a lead-free cadmium-free environmentally friendly low melting glass frit.
In some embodiments of the invention, the glass fusing agent comprises one of D245, N250, and N255.
The glass flux is lead-free cadmium environment-friendly low-melting-point glass powder, the grain size is preferably 5-10 mu m, the complete melting temperature is preferably 600-670 ℃, the white high-reflection glaze is enabled to be completely melted within a tempering temperature range of 680-720 ℃ in a short time, the melting flow property is better, the titanium pigment can be better coated, and the high adhesive force and the weather resistance of the glaze layer are further ensured.
In some embodiments of the invention, the high temperature crack resistant powder comprises an inorganic ultra-fine powder.
In some embodiments of the invention, the inorganic-based ultrafine powder comprises GT18 high temperature crack resistant powder.
In some embodiments of the invention, the inorganic superfine powder can generate phase change in the structural shape of the material at 220 ℃ and 350 ℃ respectively, the volume is relatively increased, the shrinkage stress impact caused by cooling and solidifying the high-temperature liquid phase material can be improved, the material process mechanics is balanced to prevent shrinkage cracking, and the shock resistance of the white high-reflection glazed glass is improved. Such as An Miwei nm, inc. GT18 high temperature crack resistant powder.
In some embodiments of the present invention, the method of preparing the reflective frit includes: mixing the water-based ink-regulating oil, the titanium pigment, the sodium aluminum silicate, the glass flux and the high-temperature anti-cracking powder.
In some embodiments of the invention, the reflective frit has a fineness of < 10 μm.
According to a fourth aspect of the invention, the use of said reflective glazing in photovoltaic glass is proposed.
Detailed Description
The conception and the technical effects produced by the present invention will be clearly and completely described in conjunction with the embodiments below to fully understand the objects, features and effects of the present invention. It is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and that other embodiments obtained by those skilled in the art without inventive effort are within the scope of the present invention based on the embodiments of the present invention.
Example 1
The phosphate modified acrylic resin and the environment-friendly water-based varnish are prepared in the embodiment.
The preparation method of the phosphate modified acrylic resin comprises the following steps:
s1, weighing 25g of methyl methacrylate, 10g of butyl acrylate, 10g of hydroxyethyl acrylate, 4g of acrylic acid, 2g of allyl polyether phosphate and 4g of methoxy polyethylene glycol (400) acrylic ester, and uniformly mixing to obtain a mixed monomer A;
s2, weighing 0.22g of azodiisobutyl cyanide and dissolving in 5g of propylene glycol methyl ether to obtain an initiator solution B;
s3, adding 15g of propylene glycol methyl ether and 25g of diethylene glycol butyl ether into a four-necked flask, starting stirring and heating to 90 ℃, adding 1/3 of mixed monomer A and 1/4 of initiator solution B into the four-necked flask, reacting for 15min, dropwise adding the mixture of the residual mixed monomer A and 1/2 of initiator solution B into the four-necked flask within 3-4 h, preserving heat and reacting for 5h after dropwise adding, adding the residual 1/4 of initiator solution B, continuing to preserving heat and reacting for 2h, cooling to 40-50 ℃, adding pH regulator N, N-dimethylethanolamine, regulating the pH of the system to 8-9, and stirring and reacting for 0.5h to obtain the water-soluble acrylic resin.
The preparation method of the environment-friendly water-based varnish comprises the following steps:
s4, slowly adding 2g of thickening anti-settling agent carboxymethyl cellulose acetate butyrate CMCAB641-0.2 (Isman) into 89g of solvent under the condition of low-speed stirring, heating at 40-60 ℃, dispersing and stirring for 30-60 min, taking 6g of water-soluble acrylic resin after complete dissolution, adding 2g of dispersing agent TEGO750W and 1g of flatting agent BYK380N after uniform mixing, and adding a proper amount of neutralizing agent AMP95 after uniform transparent liquid is formed, thus obtaining the environment-friendly water-based ink-regulating oil.
Preparation of aqueous white high-reflection glaze:
s5, adding 30g of the environment-friendly water-based varnish into a dispersion cylinder, and starting a mechanical stirrer, wherein the stirring speed is 500-1500 rpm;
s6, sequentially adding 36g of titanium dioxide and 4g of aluminum silicate sodium salt into a dispersing cylinder, and continuing to disperse at a high speed of 500-1500 rpm for 10-90 min to prepare uniform and fine white slurry;
s7, sequentially adding 60g of glass flux and 5g of high-temperature anti-cracking powder into the white slurry, continuing to disperse at a high speed of 500-1500 rpm for 10-90 min, and then adjusting the viscosity to about 60000-100000 mpas by using a diluent according to the requirement;
s8, finally pouring the white ink into a three-roller grinder for ink binding, and detecting the fineness of the ink to ensure that the fineness is less than 10 mu m, thus obtaining the water-based white high-reflection glaze.
Example 2
The phosphate modified acrylic resin and the environment-friendly water-based varnish are prepared in the embodiment.
The preparation method of the phosphate modified acrylic resin comprises the following steps:
s1, weighing and uniformly mixing 20g of methyl methacrylate, 10g of butyl acrylate, 8g of hydroxyethyl acrylate, 4g of acrylic acid, 4g of ethylene glycol methacrylate phosphate and 4g of methoxy polyethylene glycol (350) acrylic ester to obtain a mixed monomer A;
s2, weighing 0.5g of azodiisobutyl cyanide and dissolving in 5g of propylene glycol methyl ether to obtain an initiator solution B;
s3, adding 20g of propylene glycol methyl ether and 25g of diethylene glycol butyl ether into the four-necked flask, starting stirring and heating to 90 ℃, adding 1/3 of mixed monomer A and 1/4 of initiator solution B into the four-necked flask, reacting for 15min, dropwise adding the mixture of the residual mixed monomer A and 1/2 of initiator solution B into the four-necked flask within 3-4 h, preserving heat and reacting for 5h after dropwise adding, adding the residual 1/4 of initiator solution B, continuing to preserving heat and reacting for 2h, cooling to 40-50 ℃, adding pH regulator N, N-dimethylethanolamine, regulating the pH of the system to 8-9, and stirring and reacting for 0.5h to obtain the water-soluble acrylic resin.
The preparation method of the environment-friendly water-based varnish comprises the following steps:
s4, slowly adding 1g of thickening anti-settling agent carboxymethyl cellulose acetate butyrate CMCAB641-0.5 (Isman) into 90g of odor-free environment-friendly solvent under the condition of low-speed stirring, properly heating if necessary, dispersing and stirring for 30-60 min at the temperature of 40-60 ℃, taking 8g of water-soluble acrylic resin, adding 8g of dispersing agent TEGO750W and 0.5g of flatting agent BYK380N after completely dissolving, fully stirring to form uniform transparent liquid, and adding a proper amount of neutralizing agent AMP95 to obtain the environment-friendly water-based varnish.
Preparation of aqueous white high-reflection glaze:
s5, adding 30g of the environment-friendly water-based varnish into a dispersion cylinder, and starting a mechanical stirrer, wherein the stirring speed is 500-1500 rpm;
s6, sequentially adding 32g of titanium dioxide and 8g of aluminum silicate sodium salt into a dispersing cylinder, and continuing to disperse at a high speed of 500-1500 rpm for 10-90 min to prepare uniform and fine white slurry;
s7, sequentially adding 60g of glass flux and 8g of high-temperature anti-cracking powder into the white slurry, continuing to disperse at a high speed of 500-1500 rpm for 10-90 min, and then adjusting the viscosity to about 60000-100000 mpas by using a diluent according to the requirement;
s8, finally pouring the white ink into a three-roller grinder for ink binding, and detecting the fineness of the ink to ensure that the fineness is less than 10 mu m, thus obtaining the water-based white high-reflection glaze.
Example 3
The phosphate modified acrylic resin and the environment-friendly water-based varnish are prepared in the embodiment.
The preparation method of the phosphate modified acrylic resin comprises the following steps:
s1, weighing 30g of methyl methacrylate, 15g of butyl acrylate, 5g of hydroxyethyl acrylate, 5g of acrylic acid, 3g of polyether phosphate methacrylate and 2g of methoxy polyethylene glycol (550) acrylic ester, and uniformly mixing to obtain a mixed monomer A;
s2, weighing 0.6g of azodiisobutyl cyanide and dissolving in 5g of propylene glycol methyl ether to obtain an initiator solution B;
s3, adding 15g of propylene glycol methyl ether and 20g of diethylene glycol butyl ether into a four-neck flask, starting stirring and heating to 90 ℃, adding 1/3 of mixed monomer A and 1/4 of initiator solution B into the four-neck flask, reacting for 15min, dropwise adding the mixture of the residual mixed monomer A and 1/2 of initiator solution B into the four-neck flask within 3-4 h, preserving heat and reacting for 5h after dropwise adding, adding the residual 1/4 of initiator solution B, continuing to preserving heat and reacting for 2h, cooling to 40-50 ℃, adding pH regulator N, N-dimethylethanolamine, regulating the pH of the system to 8-9, and stirring and reacting for 0.5h to obtain the water-soluble acrylic resin.
The preparation method of the environment-friendly water-based varnish comprises the following steps:
s4, slowly adding 3g of thickening anti-settling agent hydroxypropyl methylcellulose into 85g of odor-free environment-friendly solvent under the condition of low-speed stirring, heating appropriately if necessary, dispersing and stirring for 30-60 min at the temperature of 40-60 ℃, adding 10g of water-soluble acrylic resin into the mixture after the mixture is completely dissolved, uniformly mixing, adding 1g of dispersing agent TEGO750W,0.1g of defoaming agent TEGO Foamex 830 and 0.9g of flatting agent BYK380N, fully stirring to form uniform transparent liquid, and adding a proper amount of neutralizing agent AMP95 to obtain the environment-friendly water-based ink regulating oil.
Preparation of aqueous white high-reflection glaze:
s5, adding 30g of the environment-friendly water-based varnish into a dispersion cylinder, and starting a mechanical stirrer, wherein the stirring speed is 500-1500 rpm;
s6, sequentially adding 28g of titanium dioxide and 12g of aluminum silicate sodium salt into a dispersing cylinder, and continuing to disperse at a high speed of 500-1500 rpm for 10-90 min to prepare uniform and fine white slurry;
s7, sequentially adding 60g of glass flux and 10g of high-temperature anti-cracking powder into the white slurry, continuing to disperse at a high speed of 500-1500 rpm for 10-90 min, and then adjusting the viscosity to about 60000-100000 mpas by using a diluent according to the requirement;
s8, finally pouring the white ink into a three-roller grinder for ink binding, and detecting the fineness of the ink to ensure that the fineness is less than 10 mu m, thus obtaining the water-based white high-reflection glaze.
Example 4
The phosphate modified acrylic resin and the environment-friendly water-based varnish are prepared in the embodiment.
The preparation method of the phosphate modified acrylic resin comprises the following steps:
s1, weighing and uniformly mixing 20g of methyl methacrylate, 20g of butyl acrylate, 5g of hydroxyethyl acrylate, 5g of acrylic acid, 5g of acyloxy ethyl phosphate methacrylate and 5g of methoxy polyethylene glycol (1000) acrylic ester to obtain a mixed monomer A;
s2, weighing 0.45g of azodiisobutyl cyanide and dissolving in 5g of propylene glycol methyl ether to obtain an initiator solution B;
s3, adding 15g of propylene glycol methyl ether and 20g of diethylene glycol butyl ether into a four-neck flask, starting stirring and heating to 90 ℃, adding 1/3 of mixed monomer A and 1/4 of initiator solution B into the four-neck flask, reacting for 15min, dropwise adding the mixture of the residual mixed monomer A and 1/2 of initiator solution B into the four-neck flask within 3-4 h, preserving heat and reacting for 5h after dropwise adding, adding the residual 1/4 of initiator solution B, continuing to preserving heat and reacting for 2h, cooling to 40-50 ℃, adding pH regulator N, N-dimethylethanolamine, regulating the pH of the system to 8-9, and stirring and reacting for 0.5h to obtain the water-soluble acrylic resin.
The preparation method of the environment-friendly water-based varnish comprises the following steps:
s4, slowly adding 2g of thickening anti-settling agent cellulose acetate butyrate CAB553-0.4 into 88g of odor-removing environment-friendly solvent under the condition of low-speed stirring, heating properly when necessary, dispersing and stirring for 30-60 min at the temperature of 40-60 ℃, adding 10g of water-soluble acrylic resin into the mixture after the mixture is completely dissolved, and fully stirring the mixture to form uniform transparent liquid, thus obtaining the environment-friendly water-based ink-transfer oil.
Preparation of aqueous white high-reflection glaze:
s5, adding 30g of the environment-friendly water-based varnish into a dispersion cylinder, and starting a mechanical stirrer, wherein the stirring speed is 500-1500 rpm;
s6, sequentially adding 24g of titanium dioxide and 16g of sodium aluminum silicate into a dispersing cylinder, and continuing to disperse at a high speed of 500-1500 rpm for 10-90 min to prepare uniform and fine white slurry;
s7, sequentially adding 60g of glass flux and 2g of high-temperature anti-cracking powder into the white slurry, continuing to disperse at a high speed of 500-1500 rpm for 10-90 min, and then adjusting the viscosity to about 60000-100000 mpas by using a diluent according to the requirement;
s8, finally pouring the white ink into a three-roller grinder for ink binding, and detecting the fineness of the ink to ensure that the fineness is less than 10 mu m, thus obtaining the water-based white high-reflection glaze.
Comparative example 1
The comparative example prepares an organosilicon modified water-soluble acrylic resin and an environment-friendly water-based varnish, which comprises the following specific steps:
s1, keeping a reaction kettle clean and anhydrous, adding 40 parts of alcohol ether solvent according to parts by weight, introducing nitrogen into the reaction kettle, keeping the reaction kettle, introducing cooling water into a condensing tube, and heating the alcohol ether solvent to 140 ℃;
s2, taking a dispersing kettle in addition, and sequentially adding 10 parts of tertiary glycidyl ester, 5 parts of hydroxyethyl acrylate, 3 parts of methyl methacrylate, 5 parts of acrylic acid, 10 parts of isobornyl methacrylate, 25 parts of butyl acrylate, 15 parts of styrene, 5 parts of organic silicon monomer, 2 parts of molecular weight regulator (chain transfer agent) and 3.5 parts of initiator according to parts by weight; stirring and mixing uniformly, wherein the stirring rotating speed is 300r/min, and the stirring time is 40min; dripping the mixed solution into the reaction kettle in the step (1) for 6 hours, and controlling the temperature at 140 ℃; after the dripping is finished, preserving heat and reacting for 2 hours, and controlling the temperature at 140 ℃;
s3, adding 0.2 part of initiator into the reaction kettle in the step (1) according to parts by weight, and continuously reacting for 2 hours, wherein the temperature is controlled at 140 ℃;
s4, cooling to 80 ℃, adding 40 parts of alcohol ether solvent according to parts by weight, stirring and mixing uniformly, wherein the stirring speed is 400r/min, and the stirring time is 30min;
s5, dropwise adding a pH regulator with the mass concentration of 10%, adjusting the pH value to 8.0, stirring at the speed of 400r/min and for 20min to obtain the organosilicon modified water-soluble acrylic resin.
The preparation method of the environment-friendly water-based varnish comprises the following steps:
s6, slowly adding 1g of thickening anti-settling agent hydroxypropyl methyl cellulose into 85g of odor-free environment-friendly solvent under the condition of low-speed stirring, heating appropriately if necessary, dispersing and stirring for 30-60 min at the temperature of 40-60 ℃, adding 10g of the organosilicon modified water-soluble acrylic resin into the mixture after the organosilicon modified water-soluble acrylic resin is completely dissolved, uniformly mixing, adding 2g of dispersing agent TEGO750W,0.1g of defoaming agent TEGO Foamex 830 and 1.9g of flatting agent BYK380N, fully stirring to form uniform transparent liquid, and adding a proper amount of neutralizing agent AMP95 to obtain the environment-friendly water-based ink-regulating oil.
Preparation of aqueous white high-reflection glaze:
s7, adding 30g of the environment-friendly water-based varnish into a dispersion cylinder, and starting a mechanical stirrer at a stirring speed of 500-1500 rpm;
s8, sequentially adding 28g of titanium dioxide and 12g of aluminum silicate sodium salt into a dispersing cylinder, and continuing to disperse at a high speed of 500-1500 rpm for 10-90 min to prepare uniform and fine white slurry;
s9, sequentially adding 60g of glass flux and 10g of high-temperature anti-cracking powder into the white slurry, continuing to disperse at a high speed of 500-1500 rpm for 10-90 min, and then adjusting the viscosity to about 60000-100000 mpas by using a diluent according to the requirement;
s10, finally pouring the white ink into a three-roller grinder for ink pricking, and detecting the fineness of the ink to ensure that the fineness is less than 10 mu m, thus obtaining the water-based white high-reflection glaze.
Comparative example 2
The comparative example prepares an organosilicon modified water-soluble acrylic resin and an environment-friendly water-based varnish, which comprises the following specific steps:
s1, weighing 30g of methyl methacrylate, 15g of styrene, 5g of hydroxyethyl acrylate, 5g of acrylic acid, 3g of polyether phosphate methacrylate and 2g of methoxy polyethylene glycol (550) acrylic ester, and uniformly mixing to obtain a mixed monomer A;
s2, weighing 0.6g of azodiisobutyl cyanide and dissolving in 5g of propylene glycol methyl ether to obtain an initiator solution B;
s3, adding 15g of propylene glycol methyl ether and 20g of diethylene glycol butyl ether into a four-neck flask, starting stirring and heating to 90 ℃, adding 1/3 of mixed monomer A and 1/4 of initiator solution B into the four-neck flask, reacting for 15min, dropwise adding the mixture of the residual mixed monomer A and 1/2 of initiator solution B into the four-neck flask within 3-4 h, preserving heat and reacting for 5h after dropwise adding, adding the residual 1/4 of initiator solution B, continuing to preserving heat and reacting for 2h, cooling to 40-50 ℃, adding pH regulator N, N-dimethylethanolamine, regulating the pH of the system to 8-9, and stirring and reacting for 0.5h to obtain the water-soluble acrylic resin.
The preparation method of the environment-friendly water-based varnish comprises the following steps:
s4, slowly adding 1g of thickening anti-settling agent hydroxypropyl methyl cellulose into 85g of odor-free environment-friendly solvent under the condition of low-speed stirring, heating appropriately if necessary, dispersing and stirring for 30-60 min at the temperature of 40-60 ℃, adding 10g of the organosilicon modified water-soluble acrylic resin into the mixture after the organosilicon modified water-soluble acrylic resin is completely dissolved, uniformly mixing, adding 2g of dispersing agent TEGO750W,0.1g of defoaming agent TEGO Foamex 830 and 1.9g of flatting agent BYK380N, fully stirring to form uniform transparent liquid, and adding a proper amount of neutralizing agent AMP95 to obtain the environment-friendly water-based ink-regulating oil.
Preparation of aqueous white high-reflection glaze:
s5, adding 30g of the environment-friendly water-based varnish into a dispersion cylinder, and starting a mechanical stirrer, wherein the stirring speed is 500-1500 rpm;
s6, sequentially adding 40g of titanium dioxide into a dispersing cylinder, and continuing to disperse at a high speed of 500-1500 rpm for 10-90 min to prepare uniform and fine white slurry;
s7, sequentially adding 60g of glass flux and 2g of high-temperature anti-cracking powder into the white slurry, continuing to disperse at a high speed of 500-1500 rpm for 10-90 min, and then adjusting the viscosity to about 60000-100000 mpas by using a diluent according to the requirement;
s8, finally pouring the white ink into a three-roller grinder for ink binding, and detecting the fineness of the ink to ensure that the fineness is less than 10 mu m, thus obtaining the water-based white high-reflection glaze.
Comparative example 3
The comparative example prepares an organosilicon modified water-soluble acrylic resin and an environment-friendly water-based varnish, which comprises the following specific steps:
s1, weighing 30g of methyl methacrylate, 15g of butyl acrylate, 5g of hydroxyethyl acrylate, 5g of acrylic acid and 2g of methoxy polyethylene glycol (550) acrylic ester, and uniformly mixing to obtain a mixed monomer A;
s2, weighing 0.6g of azodiisobutyl cyanide and dissolving in 5g of propylene glycol methyl ether to obtain an initiator solution B;
s3, adding 15g of propylene glycol methyl ether and 20g of diethylene glycol butyl ether into a four-neck flask, starting stirring and heating to 90 ℃, adding 1/3 of mixed monomer A and 1/4 of initiator solution B into the four-neck flask, reacting for 15min, dropwise adding the mixture of the residual mixed monomer A and 1/2 of initiator solution B into the four-neck flask within 3-4 h, preserving heat and reacting for 5h after dropwise adding, adding the residual 1/4 of initiator solution B, continuing to preserving heat and reacting for 2h, cooling to 40-50 ℃, adding pH regulator N, N-dimethylethanolamine, regulating the pH of the system to 8-9, and stirring and reacting for 0.5h to obtain the water-soluble acrylic resin.
The preparation method of the environment-friendly water-based varnish comprises the following steps:
s4, slowly adding 1g of thickening anti-settling agent hydroxypropyl methyl cellulose into 85g of odor-free environment-friendly solvent under the condition of low-speed stirring, heating appropriately if necessary, dispersing and stirring for 30-60 min at the temperature of 40-60 ℃, adding 10g of the organosilicon modified water-soluble acrylic resin into the mixture after the organosilicon modified water-soluble acrylic resin is completely dissolved, uniformly mixing, adding 2g of dispersing agent TEGO750W,0.1g of defoaming agent TEGO Foamex 830 and 1.9g of flatting agent BYK380N, fully stirring to form uniform transparent liquid, and adding a proper amount of neutralizing agent AMP95 to obtain the environment-friendly water-based ink-regulating oil.
Preparation of aqueous white high-reflection glaze:
s5, adding 30g of the environment-friendly water-based varnish into a dispersion cylinder, and starting a mechanical stirrer, wherein the stirring speed is 500-1500 rpm;
s6, sequentially adding 28g of titanium dioxide and 12g of aluminum silicate sodium salt into a dispersing cylinder, and continuing to disperse at a high speed of 500-1500 rpm for 10-90 min to prepare uniform and fine white slurry;
s7, adding 60g of glass flux into the white slurry, continuing to disperse at a high speed of 500-1500 rpm for 10-90 min, and then adjusting the viscosity to about 60000-100000 mpas by using a diluent according to the requirement;
s8, finally pouring the white ink into a three-roller grinder for ink binding, and detecting the fineness of the ink to ensure that the fineness is less than 10 mu m, thus obtaining the water-based white high-reflection glaze.
Comparative example 4
The comparative example prepares an organosilicon modified water-soluble acrylic resin and an environment-friendly water-based varnish, which comprises the following specific steps:
s1, weighing 30g of methyl methacrylate, 15g of butyl acrylate, 5g of hydroxyethyl acrylate, 5g of acrylic acid and 3g of polyether phosphate methacrylate, and uniformly mixing to obtain a mixed monomer A;
s2, weighing 0.6g of azodiisobutyl cyanide and dissolving in 5g of propylene glycol methyl ether to obtain an initiator solution B;
s3, adding 15g of propylene glycol methyl ether and 20g of diethylene glycol butyl ether into a four-neck flask, starting stirring and heating to 90 ℃, adding 1/3 of mixed monomer A and 1/4 of initiator solution B into the four-neck flask, reacting for 15min, dropwise adding the mixture of the residual mixed monomer A and 1/2 of initiator solution B into the four-neck flask within 3-4 h, preserving heat and reacting for 5h after dropwise adding, adding the residual 1/4 of initiator solution B, continuing to preserving heat and reacting for 2h, cooling to 40-50 ℃, adding pH regulator N, N-dimethylethanolamine, regulating the pH of the system to 8-9, and stirring and reacting for 0.5h to obtain the water-soluble acrylic resin.
The preparation method of the environment-friendly water-based varnish comprises the following steps:
s4, slowly adding 1g of thickening anti-settling agent hydroxypropyl methyl cellulose into 85g of odor-free environment-friendly solvent under the condition of low-speed stirring, heating appropriately if necessary, dispersing and stirring for 30-60 min at the temperature of 40-60 ℃, adding 10g of the organosilicon modified water-soluble acrylic resin into the mixture after the organosilicon modified water-soluble acrylic resin is completely dissolved, uniformly mixing, adding 2g of dispersing agent TEGO750W,0.1g of defoaming agent TEGO Foamex 830 and 1.9g of flatting agent BYK380N, fully stirring to form uniform transparent liquid, and adding a proper amount of neutralizing agent AMP95 to obtain the environment-friendly water-based ink-regulating oil.
Preparation of aqueous white high-reflection glaze:
s5, adding 30g of the environment-friendly water-based varnish into a dispersion cylinder, and starting a mechanical stirrer, wherein the stirring speed is 500-1500 rpm;
s6, adding 40g of titanium dioxide into a dispersion cylinder, and continuing to disperse at a high speed of 500-1500 rpm for 10-90 min to prepare uniform and fine white slurry;
s7, adding 60g of glass flux into the white slurry, continuing to disperse at a high speed of 500-1500 rpm for 10-90 min, and then adjusting the viscosity to about 60000-100000 mpas by using a diluent according to the requirement;
s8, finally pouring the white ink into a three-roller grinder for ink binding, and detecting the fineness of the ink to ensure that the fineness is less than 10 mu m, thus obtaining the water-based white high-reflection glaze.
While the embodiments of the present invention have been described in detail, the present invention is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art. Furthermore, embodiments of the invention and features of the embodiments may be combined with each other without conflict.
Claims (10)
1. The water-based varnish is characterized by comprising the following raw materials in parts by weight: 1 to 10 parts of phosphate modified acrylic resin, 0.5 to 5 parts of thickener, 1 to 2 parts of dispersant and 80 to 95 parts of solvent;
the preparation raw materials of the phosphate modified acrylic ester resin comprise: phosphate functional monomers, methoxypolyethylene glycol acrylate, acrylic acid and acrylate;
the phosphate functional monomer comprises at least one of methacrylic acid acyloxyethyl phosphate, ethylene glycol methacrylate phosphate, alkyl acrylate phosphate, allyl polyether phosphate and methacrylic acid polyether phosphate;
the weight average molecular weight of the phosphate modified acrylic resin is 5000-100000 MW.
2. The aqueous varnish as claimed in claim 1, wherein the phosphate modified acrylate resin is prepared from (by weight parts) phosphate functional monomer 1-5, methoxypolyethylene glycol acrylate 2-5, acrylic acid 2-5 and acrylate 35-60.
3. The aqueous varnish of claim 1, wherein the phosphate modified acrylate resin is prepared from a raw material further comprising an alcohol ether solvent; preferably, the alcohol ether solvent comprises at least one of diethylene glycol butyl ether, dipropylene glycol methyl ether, tripropylene glycol methyl ether, dipropylene glycol butyl ether, tripropylene glycol butyl ether and diethylene glycol tert-butyl ether.
4. The phosphate modified acrylate resin of claim 1 wherein the phosphate modified acrylate resin is prepared from a raw material further comprising an initiator and a pH adjuster.
5. The aqueous varnish according to claim 1, wherein the raw materials for preparing the aqueous varnish further comprise an antifoaming agent and a leveling agent.
6. A method of preparing an aqueous varnish as claimed in any one of claims 1 to 5, comprising mixing the preparation materials of the aqueous varnish.
7. The method for producing an aqueous varnish according to claim 6, wherein the mixing temperature is 40 to 60 ℃.
8. A reflective glaze, characterized in that the reflective glaze is prepared from the aqueous varnish according to any one of claims 1 to 5.
9. The reflective glaze according to claim 8, wherein the reflective glaze is further prepared from aluminum silicate sodium salt and titanium pigment.
10. Use of the reflective glazing of claim 8 or 9 in photovoltaic glass.
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