CN117186750B - Water-based vacuum aluminizing finishing varnish and preparation method thereof - Google Patents
Water-based vacuum aluminizing finishing varnish and preparation method thereof Download PDFInfo
- Publication number
- CN117186750B CN117186750B CN202311166367.6A CN202311166367A CN117186750B CN 117186750 B CN117186750 B CN 117186750B CN 202311166367 A CN202311166367 A CN 202311166367A CN 117186750 B CN117186750 B CN 117186750B
- Authority
- CN
- China
- Prior art keywords
- stirring
- parts
- component
- minutes
- aqueous
- 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.)
- Active
Links
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 239000002966 varnish Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 40
- 238000005269 aluminizing Methods 0.000 title claims abstract description 25
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000008367 deionised water Substances 0.000 claims abstract description 33
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 33
- 239000002318 adhesion promoter Substances 0.000 claims abstract description 31
- 239000002994 raw material Substances 0.000 claims abstract description 26
- 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 19
- 239000006097 ultraviolet radiation absorber Substances 0.000 claims abstract description 19
- -1 alcohol ester Chemical class 0.000 claims abstract description 17
- 239000002562 thickening agent Substances 0.000 claims abstract description 17
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- 239000012948 isocyanate Substances 0.000 claims abstract description 11
- 150000002513 isocyanates Chemical class 0.000 claims abstract description 11
- 239000000080 wetting agent Substances 0.000 claims abstract description 7
- 239000013530 defoamer Substances 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 138
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 36
- 239000000243 solution Substances 0.000 claims description 36
- 239000011259 mixed solution Substances 0.000 claims description 33
- 239000000203 mixture Substances 0.000 claims description 33
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 28
- 238000007747 plating Methods 0.000 claims description 25
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 239000006185 dispersion Substances 0.000 claims description 20
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 19
- 229910052782 aluminium Inorganic materials 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 18
- FMGBDYLOANULLW-UHFFFAOYSA-N 3-isocyanatopropyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)CCCN=C=O FMGBDYLOANULLW-UHFFFAOYSA-N 0.000 claims description 17
- CUNWUEBNSZSNRX-RKGWDQTMSA-N (2r,3r,4r,5s)-hexane-1,2,3,4,5,6-hexol;(z)-octadec-9-enoic acid Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO.OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO.CCCCCCCC\C=C/CCCCCCCC(O)=O.CCCCCCCC\C=C/CCCCCCCC(O)=O.CCCCCCCC\C=C/CCCCCCCC(O)=O CUNWUEBNSZSNRX-RKGWDQTMSA-N 0.000 claims description 16
- 229960005078 sorbitan sesquioleate Drugs 0.000 claims description 16
- 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 claims description 14
- QZPSOSOOLFHYRR-UHFFFAOYSA-N 3-hydroxypropyl prop-2-enoate Chemical compound OCCCOC(=O)C=C QZPSOSOOLFHYRR-UHFFFAOYSA-N 0.000 claims description 14
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 14
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 14
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 14
- SVWKIGRDISDRLO-UHFFFAOYSA-N 4-(oxiran-2-ylmethoxy)-9h-carbazole Chemical compound C=1C=CC=2NC3=CC=CC=C3C=2C=1OCC1CO1 SVWKIGRDISDRLO-UHFFFAOYSA-N 0.000 claims description 13
- 238000001704 evaporation Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 230000002745 absorbent Effects 0.000 claims description 12
- 239000002250 absorbent Substances 0.000 claims description 12
- 239000012065 filter cake Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 239000004814 polyurethane Substances 0.000 claims description 12
- 239000000376 reactant Substances 0.000 claims description 12
- 238000005303 weighing Methods 0.000 claims description 12
- 229920002635 polyurethane Polymers 0.000 claims description 11
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 claims description 10
- 229920002125 Sokalan® Polymers 0.000 claims description 10
- 238000001723 curing Methods 0.000 claims description 10
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 10
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 10
- 239000004584 polyacrylic acid Substances 0.000 claims description 10
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 claims description 10
- ZXDDPOHVAMWLBH-UHFFFAOYSA-N 2,4-Dihydroxybenzophenone Chemical compound OC1=CC(O)=CC=C1C(=O)C1=CC=CC=C1 ZXDDPOHVAMWLBH-UHFFFAOYSA-N 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 235000019441 ethanol Nutrition 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- UEEJHVSXFDXPFK-UHFFFAOYSA-O N-dimethylethanolamine Chemical compound C[NH+](C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-O 0.000 claims description 4
- 239000002518 antifoaming agent Substances 0.000 claims description 4
- 239000000758 substrate Substances 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 abstract description 11
- 239000007921 spray Substances 0.000 abstract description 10
- 230000032683 aging Effects 0.000 abstract description 9
- 239000000853 adhesive Substances 0.000 abstract description 7
- 230000001070 adhesive effect Effects 0.000 abstract description 7
- 230000000052 comparative effect Effects 0.000 description 17
- 239000003973 paint Substances 0.000 description 14
- 230000008859 change Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- HMUNWXXNJPVALC-UHFFFAOYSA-N 1-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C(CN1CC2=C(CC1)NN=N2)=O HMUNWXXNJPVALC-UHFFFAOYSA-N 0.000 description 2
- WZFUQSJFWNHZHM-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC(=O)N1CC2=C(CC1)NN=N2 WZFUQSJFWNHZHM-UHFFFAOYSA-N 0.000 description 2
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 2
- 238000003848 UV Light-Curing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 1
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical compound C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention provides a water-based vacuum aluminizing finishing varnish which is prepared from a component A and a component B in a mass ratio of 4:1; the component A consists of the following raw materials in parts by weight: 70-80 parts of aqueous acrylic acid dispersoid, 3-4 parts of alcohol ester, 0.1-0.5 part of base material wetting agent, 2-3 parts of adhesion promoter, 1-2 parts of thickener, 0.1-0.5 part of defoamer, 1-2 parts of ultraviolet absorber and 10-20 parts of deionized water; the component B consists of the following raw materials in parts by weight: 30-60 parts of isocyanate curing agent and 40-60 parts of propylene glycol monomethyl ether acetate. The invention also provides a preparation method of the water-based vacuum aluminizing finishing varnish. The aqueous vacuum aluminizing finishing varnish provided by the invention has good adhesive force, water resistance, salt spray resistance, aging resistance and moist heat resistance.
Description
Technical Field
The invention relates to a water-based vacuum aluminizing finishing varnish and a preparation method thereof.
Background
With the popularization of electric vehicles, the application of luminous products on electric vehicles is increasing, and luminous vehicle logos are one of the luminous vehicle logos. Most manufacturers usually adopt a vacuum aluminizing method to manufacture the car logo, and after the vacuum aluminizing, a finishing varnish is generally required to be coated on an aluminized layer. The traditional finishing protective varnish used in the vacuum aluminizing process of the automobile logo is mostly oily PU or oily UV paint, and the paint has higher VOC and serious environmental pollution.
The patent with the application number of CN201711452789.4 discloses an aqueous UV curing vacuum plating primer, a preparation method and a plating method thereof, wherein the aqueous UV curing vacuum plating primer comprises the following components in parts by mass: 10-60 parts of aqueous polyurethane acrylate, 5-30 parts of aqueous acrylate, 2.5-15 parts of trimethylolpropane triacrylate, 0.1-1.5 parts of flatting agent, 1-8 parts of photoinitiator, 8-20 parts of cosolvent and 40-70 parts of water. Although the patent belongs to environment-friendly water paint, the patent has the problem of unsatisfactory salt spray resistance and aging resistance.
Disclosure of Invention
The invention aims to solve the technical problem of providing a water-based vacuum aluminum plating finishing varnish which has better adhesive force, water resistance, salt spray resistance, aging resistance and moist heat resistance.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a water-based vacuum aluminizing finishing varnish is prepared from a component A and a component B in a mass ratio of 4:1; the component A consists of the following raw materials in parts by weight: 70-80 parts of aqueous acrylic acid dispersoid, 3-4 parts of alcohol ester, 0.1-0.5 part of base material wetting agent, 2-3 parts of adhesion promoter, 1-2 parts of thickener, 0.1-0.5 part of defoamer, 1-2 parts of ultraviolet absorber and 10-20 parts of deionized water; the component B consists of the following raw materials in parts by weight: 30-60 parts of isocyanate curing agent and 40-60 parts of propylene glycol monomethyl ether acetate.
Further, the preparation steps of the aqueous acrylic dispersion of the present invention are as follows:
mixing methyl methacrylate, hydroxypropyl acrylate, butyl acrylate, methacrylic acid, sorbitan sesquioleate, azodiisobutyronitrile and isopropanol, stirring for 30 minutes to obtain a mixed solution, adding 1/4 weight of the mixed solution into a reaction bottle, heating to 75 ℃, stirring for reacting for 20-40 minutes, then dripping the rest mixed solution into the reaction bottle, keeping the temperature after dripping, stirring for reacting for 2-3 hours, reducing the temperature to 50 ℃ after evaporating the solvent under reduced pressure, adding N, N-dimethylethanolamine and deionized water into the reaction bottle, stirring for 20-40 minutes, and cooling to room temperature to obtain the aqueous acrylic acid dispersion.
Further, in the preparation step of the aqueous acrylic dispersion, the mass ratio of methyl methacrylate, hydroxypropyl acrylate, butyl acrylate, methacrylic acid, sorbitan sesquioleate, azodiisobutyronitrile, isopropanol, N-dimethylethanolamine and deionized water is 30:30:10:3:2:2.5:45:5:80.
Further, the substrate wetting agent is polyacrylic acid copolymer potassium salt, the thickening agent is polyurethane thickening agent, the defoaming agent is polydimethylsiloxane, and the isocyanate curing agent is HDI.
Further, the preparation steps of the adhesion promoter disclosed by the invention are as follows:
adding 4-glycidoxy carbazole into tetrahydrofuran under the protection of nitrogen, stirring for 10 minutes to obtain a mixed solution, heating to 55 ℃, then dropwise adding 3-isocyanatopropyl trimethoxy silane into the mixed solution, carrying out heat preservation, stirring, reacting for 2-3 hours, and then decompressing and evaporating the tetrahydrofuran to obtain the adhesion promoter.
Further, in the preparation step of the adhesion promoter, the proportion of 4-glycidoxycarbazole, tetrahydrofuran and 3-isocyanatopropyl trimethoxysilane is 5mmol:6mL:5mmol.
Further, the preparation steps of the ultraviolet absorber are as follows:
adding yttrium nitrate into absolute ethyl alcohol, stirring until the mixture is uniform to obtain a first solution, adding 2, 4-dihydroxybenzophenone into absolute ethyl alcohol, stirring until the mixture is uniform to obtain a second solution, dripping the first solution into the second solution, stirring for 30 minutes, adjusting the pH value to 6, continuously stirring for 3-4 hours to obtain a reactant, standing the reactant at room temperature for 12 hours, performing suction filtration to obtain a filter cake, washing the filter cake with deionized water and absolute ethyl alcohol for 3 times respectively, and then performing vacuum drying at 60 ℃ until the weight is constant to obtain the ultraviolet absorbent.
Further, in the preparation step of the ultraviolet absorbent, the concentration of the solution A is 0.2mmol/mL, the concentration of the solution B is 0.2mmol/mL, and the volume ratio of the solution A to the solution B is 1:3.
The invention aims to provide a preparation method of the water-based vacuum aluminum plating finishing varnish.
In order to solve the technical problems, the technical scheme is as follows:
a preparation method of an aqueous vacuum aluminizing finishing varnish comprises the following steps:
s1, weighing the raw materials of the component A according to parts by weight, sequentially adding aqueous acrylic acid dispersoid and deionized water into a stirring kettle, and stirring for 5-10 minutes to obtain a mixture I;
s2, adding the adhesion promoter into the first mixture obtained in the step S1, and stirring for 5-10 minutes to obtain a second mixture;
s3, sequentially adding a substrate wetting agent, a defoaming agent, an ultraviolet absorber and a thickening agent into the mixture II obtained in the step S2, and stirring for 10-15 minutes to obtain a component A;
s4, weighing the raw materials of the component B according to the parts by weight, sequentially adding an isocyanate curing agent and propylene glycol monomethyl ether acetate into a stirring kettle, and stirring for 5 minutes at one stage and stirring for 10 minutes at the second stage to obtain the component B;
s5, uniformly mixing the component A and the component B according to the mass ratio of 4:1 to obtain the water-based vacuum aluminizing finishing varnish.
Further, in the steps S1 and S2, the stirring speed is 300-600 rpm; in the step S3, the stirring speed is 900-1200 rpm; in the step S4, the stirring speed in the first-stage stirring is 300-600 rpm, and the stirring speed in the second-stage stirring is 600-700 rpm.
Compared with the prior art, the invention has the following beneficial effects:
1) The aqueous acrylic dispersion used in the invention is prepared by combining sorbitan sesquioleate and the like with acrylic acid monomers, and can effectively improve the hardness and the moist heat resistance of the aqueous vacuum aluminum plating finishing varnish.
2) The adhesion promoter used in the invention is synthesized by 4-glycidoxy carbazole and 3-isocyanatopropyl trimethoxy silane, can effectively improve the adhesion, water resistance and salt fog resistance of the water-based vacuum aluminum plating finishing varnish, and is not easy to cause the undercut color of an aluminum plating layer.
3) The ultraviolet absorbent used in the invention is prepared by coordination of yttrium nitrate and 2, 4-dihydroxybenzophenone, has excellent ultraviolet absorption capacity, and can effectively improve the aging resistance of the aqueous vacuum aluminizing finishing varnish.
4) The water-based vacuum aluminizing finishing varnish prepared by the invention belongs to water-based paint, contains few solvents, does not damage the surface of a product due to solvent problems, has better product performance, has lower VOC content and is more environment-friendly, in addition, a customer can select a normal-temperature self-drying process or a low-temperature baking process according to the process of the customer, the production time and the production cost can be saved, and the purposes of energy conservation and emission reduction are achieved.
Detailed Description
The present invention will be described in detail with reference to specific examples, wherein the exemplary embodiments of the present invention and the descriptions thereof are provided for the purpose of illustrating the present invention, but are not to be construed as limiting the present invention.
Example 1
The aqueous vacuum aluminizing finishing varnish is prepared from a component A and a component B in a mass ratio of 4:1; the component A consists of the following raw materials in parts by weight: 75 parts of aqueous acrylic acid dispersoid, 3.5 parts of alcohol ester, 0.4 part of polyacrylic acid copolymer potassium salt, 2.5 parts of adhesion promoter, 1.5 parts of polyurethane thickener, 0.3 part of polydimethylsiloxane, 1.6 parts of ultraviolet absorbent and 15 parts of deionized water; the component B consists of the following raw materials in parts by weight: 45 parts of HDI and 50 parts of propylene glycol monomethyl ether acetate.
The preparation steps of the aqueous acrylic dispersion are as follows:
mixing and stirring methyl methacrylate, hydroxypropyl acrylate, butyl acrylate, methacrylic acid, sorbitan sesquioleate, azodiisobutyronitrile and isopropanol for 30 minutes to obtain a mixed solution, adding 1/4 weight of the mixed solution into a reaction bottle, heating to 75 ℃, stirring and reacting for 30 minutes, then adding the rest of the mixed solution into the reaction bottle, keeping the temperature and stirring after dripping for 2.5 hours, reducing the temperature to 50 ℃ after evaporating the solvent under reduced pressure, adding N, N-dimethylethanolamine and deionized water into the reaction bottle, stirring for 30 minutes, and cooling to room temperature to obtain the aqueous acrylic acid dispersoid, wherein the mass ratio of the methyl methacrylate, the hydroxypropyl acrylate, the butyl acrylate, the methacrylic acid, the sorbitan sesquioleate, the azodiisobutyronitrile, the isopropanol, the N, N-dimethylethanolamine and the deionized water is 30:30:10:3:2:2.5:45:5:80.
The preparation steps of the adhesion promoter are as follows:
adding 4-glycidoxycarbazole into tetrahydrofuran under the protection of nitrogen, stirring for 10 minutes to obtain a mixed solution, heating to 55 ℃, then dropwise adding 3-isocyanatopropyl trimethoxy silane into the mixed solution, carrying out heat preservation, stirring, reacting for 2.5 hours, and then decompressing and evaporating to remove tetrahydrofuran to obtain the adhesion promoter, wherein the ratio of 4-glycidoxycarbazole to tetrahydrofuran to 3-isocyanatopropyl trimethoxy silane is 5mmol to 6mL to 5mmol.
The ultraviolet absorber is prepared by the following steps:
adding yttrium nitrate into absolute ethyl alcohol, stirring until the solution is uniformly mixed to obtain a solution A with the concentration of 0.2mmol/mL, adding 2, 4-dihydroxybenzophenone into absolute ethyl alcohol, stirring until the solution B with the concentration of 0.2mmol/mL is uniformly mixed, dripping the solution A into the solution B according to the volume ratio of 1:3, stirring for 30 minutes, regulating the pH value to 6, continuously stirring for 3.5 hours to obtain a reactant, standing the reactant at room temperature for 12 hours, filtering to obtain a filter cake, washing the filter cake with deionized water and absolute ethyl alcohol for 3 times respectively, and then vacuum-drying at 60 ℃ until the weight is constant to obtain the ultraviolet absorbent.
The preparation method of example 1 comprises the following steps:
s1, weighing the raw materials of the component A according to parts by weight, sequentially adding aqueous acrylic acid dispersoid and deionized water into a stirring kettle, and stirring for 6 minutes at a stirring speed of 500 revolutions per minute to obtain a mixture I;
s2, adding the adhesion promoter into the first mixture obtained in the step S1, and stirring for 6 minutes at a stirring speed of 500 revolutions per minute to obtain a second mixture;
s3, sequentially adding the potassium salt of the polyacrylic acid copolymer, the polydimethylsiloxane, the ultraviolet absorber and the polyurethane thickener into the mixture II obtained in the step S2, and stirring for 11 minutes at the stirring speed of 1100 revolutions per minute to obtain a component A;
s4, weighing the raw materials of the component B according to parts by weight, sequentially adding an isocyanate curing agent and propylene glycol monomethyl ether acetate into a stirring kettle, and stirring for 5 minutes at a first stage at a stirring speed of 500 rpm, and stirring for 10 minutes at a second stage at a stirring speed of 700 rpm to obtain the component B;
s5, uniformly mixing the component A and the component B according to the mass ratio of 4:1 to obtain the water-based vacuum aluminizing finishing varnish.
Example 2
The aqueous vacuum aluminizing finishing varnish is prepared from a component A and a component B in a mass ratio of 4:1; the component A consists of the following raw materials in parts by weight: 70 parts of aqueous acrylic acid dispersoid, twelve 4 parts of alcohol ester, 0.3 part of polyacrylic acid copolymer potassium salt, 2.1 parts of adhesion promoter, 2 parts of polyurethane thickener, 0.1 part of polydimethylsiloxane, 1.4 parts of ultraviolet absorber and 10 parts of deionized water; the component B consists of the following raw materials in parts by weight: 60 parts of HDI and 60 parts of propylene glycol monomethyl ether acetate.
The preparation steps of the aqueous acrylic dispersion are as follows:
mixing and stirring methyl methacrylate, hydroxypropyl acrylate, butyl acrylate, methacrylic acid, sorbitan sesquioleate, azodiisobutyronitrile and isopropanol for 30 minutes to obtain a mixed solution, adding 1/4 weight of the mixed solution into a reaction bottle, heating to 75 ℃, stirring and reacting for 40 minutes, then adding the rest of the mixed solution into the reaction bottle, keeping the temperature and stirring after dripping for 3 hours, reducing the temperature to 50 ℃ after evaporating the solvent under reduced pressure, adding N, N-dimethylethanolamine and deionized water into the reaction bottle, stirring for 40 minutes, and cooling to room temperature to obtain the aqueous acrylic acid dispersoid, wherein the mass ratio of methyl methacrylate, hydroxypropyl acrylate, butyl acrylate, methacrylic acid, sorbitan sesquioleate, azodiisobutyronitrile, isopropanol, N-dimethylethanolamine and deionized water is 30:30:10:3:2:2.5:45:5:80.
The preparation steps of the adhesion promoter are as follows:
adding 4-glycidoxycarbazole into tetrahydrofuran under the protection of nitrogen, stirring for 10 minutes to obtain a mixed solution, heating to 55 ℃, then dropwise adding 3-isocyanatopropyl trimethoxy silane into the mixed solution, carrying out heat preservation, stirring, reacting for 3 hours, and then decompressing and evaporating to remove tetrahydrofuran to obtain the adhesion promoter, wherein the ratio of 4-glycidoxycarbazole to tetrahydrofuran to 3-isocyanatopropyl trimethoxy silane is 5mmol to 6mL to 5mmol.
The ultraviolet absorber is prepared by the following steps:
adding yttrium nitrate into absolute ethyl alcohol, stirring until the solution is uniformly mixed to obtain a solution A with the concentration of 0.2mmol/mL, adding 2, 4-dihydroxybenzophenone into absolute ethyl alcohol, stirring until the solution B with the concentration of 0.2mmol/mL is uniformly mixed, dripping the solution A into the solution B according to the volume ratio of 1:3, stirring for 30 minutes, regulating the pH value to 6, continuously stirring for 4 hours to obtain a reactant, standing the reactant at room temperature for 12 hours, filtering to obtain a filter cake, washing the filter cake with deionized water and absolute ethyl alcohol for 3 times respectively, and then vacuum-drying at 60 ℃ until the weight is constant to obtain the ultraviolet absorbent.
The preparation method of example 2 comprises the following steps:
s1, weighing the raw materials of the component A according to parts by weight, sequentially adding aqueous acrylic acid dispersoid and deionized water into a stirring kettle, and stirring for 5 minutes at a stirring speed of 600 revolutions per minute to obtain a mixture I;
s2, adding the adhesion promoter into the first mixture obtained in the step S1, and stirring for 5 minutes at the stirring speed of 600 revolutions per minute to obtain a second mixture;
s3, sequentially adding the potassium salt of the polyacrylic acid copolymer, the polydimethylsiloxane, the ultraviolet absorber and the polyurethane thickener into the mixture II obtained in the step S2, and stirring for 10 minutes at the stirring speed of 1200 revolutions per minute to obtain a component A;
s4, weighing the raw materials of the component B according to parts by weight, sequentially adding an isocyanate curing agent and propylene glycol monomethyl ether acetate into a stirring kettle, and stirring for 5 minutes at a first stage at a stirring speed of 600 rpm, and stirring for 10 minutes at a second stage at a stirring speed of 700 rpm to obtain the component B;
s5, uniformly mixing the component A and the component B according to the mass ratio of 4:1 to obtain the water-based vacuum aluminizing finishing varnish.
Example 3
The aqueous vacuum aluminizing finishing varnish is prepared from a component A and a component B in a mass ratio of 4:1; the component A consists of the following raw materials in parts by weight: 80 parts of aqueous acrylic acid dispersoid, 3 parts of alcohol ester, 0.1 part of polyacrylic acid copolymer potassium salt, 3 parts of adhesion promoter, 1.2 parts of polyurethane thickener, 0.2 part of polydimethylsiloxane, 2 parts of ultraviolet absorber and 14 parts of deionized water; the component B consists of the following raw materials in parts by weight: 30 parts of HDI and 40 parts of propylene glycol monomethyl ether acetate.
The preparation steps of the aqueous acrylic dispersion are as follows:
mixing and stirring methyl methacrylate, hydroxypropyl acrylate, butyl acrylate, methacrylic acid, sorbitan sesquioleate, azodiisobutyronitrile and isopropanol for 30 minutes to obtain a mixed solution, adding 1/4 weight of the mixed solution into a reaction bottle, heating to 75 ℃, stirring and reacting for 20 minutes, then adding the rest of the mixed solution into the reaction bottle, keeping the temperature and stirring after dripping for 2 hours, reducing the temperature to 50 ℃ after evaporating the solvent under reduced pressure, adding N, N-dimethylethanolamine and deionized water into the reaction bottle, stirring for 20 minutes, and cooling to room temperature to obtain the aqueous acrylic acid dispersoid, wherein the mass ratio of methyl methacrylate, hydroxypropyl acrylate, butyl acrylate, methacrylic acid, sorbitan sesquioleate, azodiisobutyronitrile, isopropanol, N-dimethylethanolamine and deionized water is 30:30:10:3:2:2.5:45:5:80.
The preparation steps of the adhesion promoter are as follows:
adding 4-glycidoxycarbazole into tetrahydrofuran under the protection of nitrogen, stirring for 10 minutes to obtain a mixed solution, heating to 55 ℃, then dropwise adding 3-isocyanatopropyl trimethoxy silane into the mixed solution, carrying out heat preservation, stirring, reacting for 2 hours, and then decompressing and evaporating to remove tetrahydrofuran to obtain the adhesion promoter, wherein the ratio of 4-glycidoxycarbazole to tetrahydrofuran to 3-isocyanatopropyl trimethoxy silane is 5mmol to 6mL to 5mmol.
The ultraviolet absorber is prepared by the following steps:
adding yttrium nitrate into absolute ethyl alcohol, stirring until the solution is uniformly mixed to obtain a solution A with the concentration of 0.2mmol/mL, adding 2, 4-dihydroxybenzophenone into absolute ethyl alcohol, stirring until the solution B with the concentration of 0.2mmol/mL is uniformly mixed, dripping the solution A into the solution B according to the volume ratio of 1:3, stirring for 30 minutes, regulating the pH value to 6, continuously stirring for 3 hours to obtain a reactant, standing the reactant at room temperature for 12 hours, filtering to obtain a filter cake, washing the filter cake with deionized water and absolute ethyl alcohol for 3 times respectively, and then vacuum-drying at 60 ℃ until the weight is constant to obtain the ultraviolet absorbent.
The preparation method of example 3 comprises the following steps:
s1, weighing the raw materials of the component A according to parts by weight, sequentially adding aqueous acrylic acid dispersoid and deionized water into a stirring kettle, and stirring for 10 minutes at a stirring speed of 300 revolutions per minute to obtain a mixture I;
s2, adding the adhesion promoter into the first mixture obtained in the step S1, and stirring for 10 minutes at the stirring speed of 300 revolutions per minute to obtain a second mixture;
s3, sequentially adding the potassium salt of the polyacrylic acid copolymer, the polydimethylsiloxane, the ultraviolet absorber and the polyurethane thickener into the mixture II obtained in the step S2, and stirring for 15 minutes at the stirring speed of 900 revolutions per minute to obtain a component A;
s4, weighing the raw materials of the component B according to parts by weight, sequentially adding an isocyanate curing agent and propylene glycol monomethyl ether acetate into a stirring kettle, and stirring for 5 minutes at a first stage at a stirring speed of 300 rpm, and stirring for 10 minutes at a second stage at a stirring speed of 600 rpm to obtain the component B;
s5, uniformly mixing the component A and the component B according to the mass ratio of 4:1 to obtain the water-based vacuum aluminizing finishing varnish.
Example 4
The aqueous vacuum aluminizing finishing varnish is prepared from a component A and a component B in a mass ratio of 4:1; the component A consists of the following raw materials in parts by weight: 72 parts of aqueous acrylic dispersion, 3.6 parts of alcohol ester, 0.5 part of polyacrylic acid copolymer potassium salt, 2 parts of adhesion promoter, 1 part of polyurethane thickener, 0.5 part of polydimethylsiloxane, 1 part of ultraviolet absorber and 20 parts of deionized water; the component B consists of the following raw materials in parts by weight: 40 parts of HDI and 45 parts of propylene glycol monomethyl ether acetate.
The preparation steps of the aqueous acrylic dispersion are as follows:
mixing and stirring methyl methacrylate, hydroxypropyl acrylate, butyl acrylate, methacrylic acid, sorbitan sesquioleate, azodiisobutyronitrile and isopropanol for 30 minutes to obtain a mixed solution, adding 1/4 weight of the mixed solution into a reaction bottle, heating to 75 ℃, stirring and reacting for 25 minutes, then adding the rest of the mixed solution into the reaction bottle, keeping the temperature and stirring after dripping for 2.5 hours, reducing the temperature to 50 ℃ after evaporating the solvent under reduced pressure, adding N, N-dimethylethanolamine and deionized water into the reaction bottle, stirring for 25 minutes, and cooling to room temperature to obtain the aqueous acrylic acid dispersoid, wherein the mass ratio of the methyl methacrylate, the hydroxypropyl acrylate, the butyl acrylate, the methacrylic acid, the sorbitan sesquioleate, the azodiisobutyronitrile, the isopropanol, the N, N-dimethylethanolamine and the deionized water is 30:30:10:3:2:2.5:45:5:80.
The preparation steps of the adhesion promoter are as follows:
adding 4-glycidoxycarbazole into tetrahydrofuran under the protection of nitrogen, stirring for 10 minutes to obtain a mixed solution, heating to 55 ℃, then dropwise adding 3-isocyanatopropyl trimethoxy silane into the mixed solution, carrying out heat preservation, stirring, reacting for 2.5 hours, and then decompressing and evaporating to remove tetrahydrofuran to obtain the adhesion promoter, wherein the ratio of 4-glycidoxycarbazole to tetrahydrofuran to 3-isocyanatopropyl trimethoxy silane is 5mmol to 6mL to 5mmol.
The ultraviolet absorber is prepared by the following steps:
adding yttrium nitrate into absolute ethyl alcohol, stirring until the solution is uniformly mixed to obtain a solution A with the concentration of 0.2mmol/mL, adding 2, 4-dihydroxybenzophenone into absolute ethyl alcohol, stirring until the solution B with the concentration of 0.2mmol/mL is uniformly mixed, dripping the solution A into the solution B according to the volume ratio of 1:3, stirring for 30 minutes, regulating the pH value to 6, continuously stirring for 3 hours to obtain a reactant, standing the reactant at room temperature for 12 hours, filtering to obtain a filter cake, washing the filter cake with deionized water and absolute ethyl alcohol for 3 times respectively, and then vacuum-drying at 60 ℃ until the weight is constant to obtain the ultraviolet absorbent.
The preparation method of example 4 comprises the following steps:
s1, weighing the raw materials of the component A according to parts by weight, sequentially adding aqueous acrylic acid dispersoid and deionized water into a stirring kettle, and stirring for 7 minutes at a stirring speed of 400 revolutions per minute to obtain a mixture I;
s2, adding the adhesion promoter into the first mixture obtained in the step S1, and stirring for 7 minutes at a stirring speed of 400 revolutions per minute to obtain a second mixture;
s3, sequentially adding the potassium salt of the polyacrylic acid copolymer, the polydimethylsiloxane, the ultraviolet absorber and the polyurethane thickener into the mixture II obtained in the step S2, and stirring for 12 minutes at a stirring speed of 1000 revolutions per minute to obtain a component A;
s4, weighing the raw materials of the component B according to parts by weight, sequentially adding an isocyanate curing agent and propylene glycol monomethyl ether acetate into a stirring kettle, and stirring for 5 minutes at a first stage at a stirring speed of 400 rpm, and stirring for 10 minutes at a second stage at a stirring speed of 600 rpm to obtain the component B;
s5, uniformly mixing the component A and the component B according to the mass ratio of 4:1 to obtain the water-based vacuum aluminizing finishing varnish.
Reference example 1
The difference from example 1 is that: the preparation steps of the aqueous acrylic dispersion in the A component are as follows:
mixing and stirring methyl methacrylate, hydroxypropyl acrylate, butyl acrylate, methacrylic acid, azodiisobutyronitrile and isopropanol for 30 minutes to obtain a mixed solution, adding 1/4 weight of the mixed solution into a reaction bottle, heating to 75 ℃, stirring and reacting for 40 minutes, then dripping the rest mixed solution into the reaction bottle, keeping the temperature and stirring after dripping for 3 hours, reducing the temperature to 50 ℃ after reducing the pressure and evaporating the solvent, adding N, N-dimethylethanolamine and deionized water into the reaction bottle, stirring for 40 minutes, and cooling to room temperature to obtain an aqueous acrylic dispersion, wherein the mass ratio of the methyl methacrylate, the hydroxypropyl acrylate, the butyl acrylate, the methacrylic acid, the azodiisobutyronitrile, the isopropanol, the N, N-dimethylethanolamine and the deionized water is 30:30:10:3:2.5:45:5:80. Namely, the aqueous acrylic dispersion used in referential example 1 was a general aqueous acrylic dispersion into which sorbitan sesquioleate was not introduced.
Reference example 2
The difference from example 1 is that: the adhesion promoter in the component A is replaced by 3-isocyanatopropyl trimethoxy silane, so that the preparation step of the adhesion promoter is omitted.
Reference example 3
The difference from example 1 is that: the ultraviolet absorbent in the component A is replaced by 2, 4-dihydroxybenzophenone, so that the preparation step of the ultraviolet absorbent is omitted.
Comparative example: example 1 of chinese patent application No. CN 201711452789.4.
Experimental example one: adhesion test
The adhesion grades of the paints of examples 1 to 4, reference example 2 and comparative example to the aluminized layer were respectively determined with reference to the GB/T9286-2021 cross-cut method, and the lower the adhesion grade, the better the adhesion. The test results are shown in table 1:
TABLE 1
| Adhesion (grade) | |
| Example 1 | 0 |
| Example 2 | 0 |
| Example 3 | 0 |
| Example 4 | 0 |
| Reference example 2 | 1 |
| Comparative example | 1 |
As can be seen from Table 1, the adhesion of examples 1-4 of the present invention is higher than that of comparative example, which shows that the aqueous vacuum aluminum plating finishing varnish prepared by the present invention has good adhesion. The composition and preparation steps of reference example 2 are different from those of example 1, and the adhesive force grade of reference example 2 is increased to 1 level compared with example 1, which shows that the adhesive force promoter prepared by the invention has better effect of improving the adhesive force of the aqueous vacuum aluminum plating finishing varnish compared with 3-isocyanatopropyl trimethoxysilane.
Experimental example two: water resistance test
The adhesion grades to the aluminized layer after 10 days of the water resistance test of examples 1 to 4, reference example 2, and comparative example were measured with reference to GB/T5209-1985, respectively, and the test results are shown in Table 2:
TABLE 2
| Adhesion (grade) to aluminized layer after 10 days of water resistance test | |
| Example 1 | 1 |
| Example 2 | 1 |
| Example 3 | 1 |
| Example 4 | 1 |
| Reference example 2 | 2 |
| Comparative example | 2 |
As can be seen from Table 2, the adhesion grades of the water-resistance test on the aluminized layers after 10 days of the water-resistance test of the invention examples 1-4 are lower than those of the comparative examples, which shows that the water-based vacuum aluminized finishing varnish prepared by the invention has better water resistance. The components and preparation steps of reference example 2 are different from those of example 1, and the adhesive force grade of the reference example 2 to an aluminized layer is increased to 2 grade after the water resistance test is carried out for 10 days compared with example 1, which shows that the adhesive force promoter prepared by the invention has better water resistance improving effect on the water-based vacuum aluminized finishing varnish compared with 3-isocyanatopropyl trimethoxysilane.
Experimental example three: salt spray resistance test
The adhesion level to the aluminized layer after 240 hours of salt spray resistance test of examples 1 to 4, reference example 2, and comparative example were measured with reference to GB/T1771-2007, respectively, and the test results are shown in Table 3:
TABLE 3 Table 3
| Adhesion (grade) to aluminized layer after 240 hours of salt spray resistance test | |
| Examples1 | 1 |
| Example 2 | 1 |
| Example 3 | 1 |
| Example 4 | 1 |
| Reference example 2 | 2 |
| Comparative example | 2 |
As can be seen from Table 3, the adhesion grades of the aqueous vacuum aluminum plating finishing varnish prepared by the invention are lower than those of the comparative examples after the salt spray resistance test is carried out for 240 hours in the examples 1-4, so that the aqueous vacuum aluminum plating finishing varnish prepared by the invention has better salt spray resistance. The composition and preparation steps of reference example 2 are different from those of example 1, and the adhesion grade of the reference example 2 to an aluminized layer is increased to 2 grade after salt spray resistance test is carried out for 240 hours compared with example 1, which shows that the adhesion promoter prepared by the invention has better effect of improving the salt spray resistance of the aqueous vacuum aluminized finishing varnish compared with 3-isocyanatopropyl trimethoxysilane.
Experimental example four: hardness test
The hardness of each of examples 1 to 4, reference example 1 and comparative example was measured with reference to GB/T6739-2006, respectively. The test results are shown in table 4:
TABLE 4 Table 4
| Hardness of | |
| Example 1 | 2H |
| Example 2 | 2H |
| Example 3 | 2H |
| Example 4 | 2H |
| Reference example 1 | HB |
| Comparative example | 2H |
As can be seen from Table 4, the hardness of examples 1-4 of the present invention is comparable to that of comparative example, showing that the aqueous vacuum aluminum-plating finishing varnish prepared by the present invention has better hardness. The composition and preparation procedure of reference example 1 were different from those of example 1, and the hardness of reference example 1 was reduced as compared with example 1, indicating that the aqueous acrylic dispersion incorporating sorbitan sesquioleate used in the present invention was effective in improving the hardness of aqueous vacuum aluminum-plating finishing varnish as compared with ordinary aqueous acrylic dispersion.
Experimental example five: test of resistance to moist Heat
The paint film surface changes after 240 hours of the wet heat resistance test were measured for each of examples 1 to 4, reference example 1, and comparative example, respectively, with reference to GB/T1740-2007, under conditions of 60℃and 90% humidity. The test results are shown in table 5:
TABLE 5
| Example 1 | No change on the surface of paint film |
| Example 2 | No change on the surface of paint film |
| Example 3 | No change on the surface of paint film |
| Example 4 | No change on the surface of paint film |
| Reference example 1 | Slight blushing of the paint film surface |
| Comparative example | Slight blushing of the paint film surface |
As can be seen from Table 5, the hardness of examples 1 to 4 of the present invention was measured for 240 hours, and the surface of the paint film was unchanged, which indicates that the aqueous vacuum aluminum-plating finishing varnish prepared by the present invention had a good wet heat resistance. The composition and preparation procedure of reference example 1 were different from those of example 1, and the paint film surface was slightly whitened after 240 hours of wet heat resistance test in reference example 1 compared with example 1, indicating that the aqueous acrylic dispersion incorporating sorbitan sesquioleate used in the present invention was effective in improving the wet heat resistance of aqueous vacuum aluminum plating finishing varnish compared with ordinary aqueous acrylic dispersion.
Experimental example six: aging resistance test
The light loss rates of examples 1 to 4, reference example 3 and comparative example were measured with reference to GB/T1766-2008 and GB/T1865-2009, respectively, and the test instrument was a xenon lamp accelerated aging test chamber with a test time of 2000 hours. The lower the light loss rate, the better the aging resistance, and the test results are shown in table 6:
TABLE 6
As can be seen from Table 6, the light loss rates of the examples 1-4 of the invention are lower than those of the comparative examples, which shows that the aqueous vacuum aluminum plating finishing varnish prepared by the invention has better aging resistance. The composition and preparation procedure of reference example 3 are different from those of example 1, and the light loss rate of reference example 3 is improved compared with that of example 1, which shows that the ultraviolet absorber prepared by the invention has better effect of improving the ageing resistance of the aqueous vacuum aluminizing coating varnish compared with that of 2, 4-dihydroxybenzophenone.
The above embodiments are merely illustrative of the principles of the present invention and its effectiveness, and are not intended to limit the invention. Modifications and variations may be made to the above-described embodiments by those skilled in the art without departing from the spirit and scope of the invention. Accordingly, it is intended that all equivalent modifications and variations of the invention be covered by the claims, which are within the ordinary skill of the art, be within the spirit and scope of the present disclosure.
Claims (9)
1. An aqueous vacuum aluminizing finishing varnish is characterized in that: is prepared from a component A and a component B in a mass ratio of 4:1; the component A consists of the following raw materials in parts by weight: 70-80 parts of aqueous acrylic acid dispersoid, 3-4 parts of alcohol ester, 0.1-0.5 part of base material wetting agent, 2-3 parts of adhesion promoter, 1-2 parts of thickener, 0.1-0.5 part of defoamer, 1-2 parts of ultraviolet absorber and 10-20 parts of deionized water; the component B consists of the following raw materials in parts by weight: 30-60 parts of isocyanate curing agent and 40-60 parts of propylene glycol monomethyl ether acetate;
the preparation steps of the aqueous acrylic dispersion are as follows:
mixing methyl methacrylate, hydroxypropyl acrylate, butyl acrylate, methacrylic acid, sorbitan sesquioleate, azodiisobutyronitrile and isopropanol, stirring for 30 minutes to obtain a mixed solution, adding 1/4 weight of the mixed solution into a reaction bottle, heating to 75 ℃, stirring for reacting for 20-40 minutes, then dripping the rest mixed solution into the reaction bottle, keeping the temperature after dripping, stirring for reacting for 2-3 hours, reducing the temperature to 50 ℃ after evaporating the solvent under reduced pressure, adding N, N-dimethylethanolamine and deionized water into the reaction bottle, stirring for 20-40 minutes, and cooling to room temperature to obtain the aqueous acrylic acid dispersion.
2. The aqueous vacuum aluminum plating varnish according to claim 1, wherein: in the preparation step of the aqueous acrylic dispersion, the mass ratio of methyl methacrylate, hydroxypropyl acrylate, butyl acrylate, methacrylic acid, sorbitan sesquioleate, azodiisobutyronitrile, isopropanol, N-dimethylethanolamine and deionized water is 30:30:10:3:2:2.5:45:5:80.
3. The aqueous vacuum aluminum plating varnish according to claim 1, wherein: the substrate wetting agent is polyacrylic acid copolymer potassium salt, the thickening agent is polyurethane thickening agent, the defoaming agent is polydimethylsiloxane, and the isocyanate curing agent is HDI.
4. The aqueous vacuum aluminum plating varnish according to claim 1, wherein: the preparation steps of the adhesion promoter are as follows:
adding 4-glycidoxy carbazole into tetrahydrofuran under the protection of nitrogen, stirring for 10 minutes to obtain a mixed solution, heating to 55 ℃, then dropwise adding 3-isocyanatopropyl trimethoxy silane into the mixed solution, carrying out heat preservation, stirring, reacting for 2-3 hours, and then decompressing and evaporating the tetrahydrofuran to obtain the adhesion promoter.
5. The aqueous vacuum aluminum plating varnish according to claim 4, wherein: in the preparation step of the adhesion promoter, the proportion of 4-glycidoxycarbazole, tetrahydrofuran and 3-isocyanatopropyl trimethoxysilane is 5 mmol/6 mL/5 mmol.
6. The aqueous vacuum aluminum plating varnish according to claim 1, wherein: the preparation steps of the ultraviolet absorber are as follows:
adding yttrium nitrate into absolute ethyl alcohol, stirring until the mixture is uniform to obtain a first solution, adding 2, 4-dihydroxybenzophenone into absolute ethyl alcohol, stirring until the mixture is uniform to obtain a second solution, dripping the first solution into the second solution, stirring for 30 minutes, adjusting the pH value to 6, continuously stirring for 3-4 hours to obtain a reactant, standing the reactant at room temperature for 12 hours, performing suction filtration to obtain a filter cake, washing the filter cake with deionized water and absolute ethyl alcohol for 3 times respectively, and then performing vacuum drying at 60 ℃ until the weight is constant to obtain the ultraviolet absorbent.
7. The aqueous vacuum aluminum plating varnish according to claim 6, wherein: in the preparation step of the ultraviolet absorbent, the concentration of the solution A is 0.2mmol/mL, the concentration of the solution B is 0.2mmol/mL, and the volume ratio of the solution A to the solution B is 1:3.
8. The method for preparing the aqueous vacuum aluminum plating finishing varnish according to any one of claims 1 to 7, which is characterized in that: the method comprises the following steps:
s1, weighing the raw materials of the component A according to parts by weight, sequentially adding aqueous acrylic acid dispersoid and deionized water into a stirring kettle, and stirring for 5-10 minutes to obtain a mixture I;
s2, adding the adhesion promoter into the first mixture obtained in the step S1, and stirring for 5-10 minutes to obtain a second mixture;
s3, sequentially adding a substrate wetting agent, a defoaming agent, an ultraviolet absorber and a thickening agent into the mixture II obtained in the step S2, and stirring for 10-15 minutes to obtain a component A;
s4, weighing the raw materials of the component B according to the parts by weight, sequentially adding an isocyanate curing agent and propylene glycol monomethyl ether acetate into a stirring kettle, and stirring for 5 minutes at one stage and stirring for 10 minutes at the second stage to obtain the component B;
s5, uniformly mixing the component A and the component B according to the mass ratio of 4:1 to obtain the water-based vacuum aluminizing finishing varnish.
9. The method for preparing the aqueous vacuum aluminum plating finishing varnish according to claim 8, which is characterized in that: in the steps S1 and S2, the stirring speed is 300-600 rpm; in the step S3, the stirring speed is 900-1200 rpm; in the step S4, the stirring speed in the first-stage stirring is 300-600 rpm, and the stirring speed in the second-stage stirring is 600-700 rpm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311166367.6A CN117186750B (en) | 2023-09-11 | 2023-09-11 | Water-based vacuum aluminizing finishing varnish and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311166367.6A CN117186750B (en) | 2023-09-11 | 2023-09-11 | Water-based vacuum aluminizing finishing varnish and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN117186750A CN117186750A (en) | 2023-12-08 |
| CN117186750B true CN117186750B (en) | 2024-03-15 |
Family
ID=88997441
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311166367.6A Active CN117186750B (en) | 2023-09-11 | 2023-09-11 | Water-based vacuum aluminizing finishing varnish and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117186750B (en) |
Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| USRE33008E (en) * | 1985-04-04 | 1989-08-01 | Alco Chemical Corporation | Acrylic emulsion copolymers for thickening aqueous systems and copolymerizable surfactant monomers for use therein |
| JPH10101544A (en) * | 1996-09-27 | 1998-04-21 | Shiseido Co Ltd | Antioxidant and anti oxidant cosmetic |
| US6053438A (en) * | 1998-10-13 | 2000-04-25 | Eastman Kodak Company | Process for making an ink jet ink |
| WO2003037945A1 (en) * | 2001-10-29 | 2003-05-08 | Kaneka Corporation | Acrylonitrile-containing block copolymer and thermo- plastic resin compositions |
| CN103342955A (en) * | 2013-07-20 | 2013-10-09 | 海洋化工研究院有限公司 | Eradication-resisting and coating-preventing marker paint for fishery vessel |
| CN105199511A (en) * | 2015-09-24 | 2015-12-30 | 维新制漆（深圳）有限公司 | Varnish for stainless steel substrate and preparation method and application of varnish |
| JP2016113561A (en) * | 2014-12-16 | 2016-06-23 | 関西ペイント株式会社 | Aqueous coating composition for coating can |
| CN109679479A (en) * | 2018-12-29 | 2019-04-26 | 东来涂料技术（上海）股份有限公司 | A kind of environment-friendly water-based varnish of high durable acid and alkali-resistance and preparation method thereof |
| CN111234598A (en) * | 2020-02-23 | 2020-06-05 | 湖南七纬科技有限公司 | Alcohol-resistant flame-retardant ink |
| CN113045921A (en) * | 2021-03-17 | 2021-06-29 | 山东七维新材料有限公司 | Coating matching system for CR200J type compound-number motor train unit and coating process thereof |
| CN113416472A (en) * | 2021-07-30 | 2021-09-21 | 雅图高新材料股份有限公司 | Water-based bi-component epoxy primer for racing helmet and preparation method thereof |
| WO2022117017A1 (en) * | 2020-12-02 | 2022-06-09 | 立邦涂料（中国）有限公司 | Aqueous secondary dispersion containing copolymer p, preparation method therefor, and application thereof |
| CN114874747A (en) * | 2022-05-05 | 2022-08-09 | 安徽斯迈特新材料股份有限公司 | Preparation method of high-temperature-resistant and strong-ultraviolet-resistant MS (Murashige & Skoog) adhesive |
| CN115851062A (en) * | 2022-12-07 | 2023-03-28 | 雅图高新材料股份有限公司 | Acrylic water-based high-adhesion primer and preparation method thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060127351A1 (en) * | 2004-12-14 | 2006-06-15 | Hercules Incorporated | Process for preparing high molar mass polymers |
| CN103613280B (en) * | 2013-11-22 | 2016-05-18 | 福耀玻璃工业集团股份有限公司 | A kind of masking liquid and ultraviolet absorbing glass that is used to form ultraviolet radiation absorption coating |
| JP6702953B2 (en) * | 2014-09-26 | 2020-06-03 | ザ ケマーズ カンパニー エフシー リミテッド ライアビリティ カンパニー | Non-fluorinated monomer and non-fluorinated polymer for surface effect compositions |
-
2023
- 2023-09-11 CN CN202311166367.6A patent/CN117186750B/en active Active
Patent Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| USRE33008E (en) * | 1985-04-04 | 1989-08-01 | Alco Chemical Corporation | Acrylic emulsion copolymers for thickening aqueous systems and copolymerizable surfactant monomers for use therein |
| JPH10101544A (en) * | 1996-09-27 | 1998-04-21 | Shiseido Co Ltd | Antioxidant and anti oxidant cosmetic |
| US6053438A (en) * | 1998-10-13 | 2000-04-25 | Eastman Kodak Company | Process for making an ink jet ink |
| WO2003037945A1 (en) * | 2001-10-29 | 2003-05-08 | Kaneka Corporation | Acrylonitrile-containing block copolymer and thermo- plastic resin compositions |
| CN103342955A (en) * | 2013-07-20 | 2013-10-09 | 海洋化工研究院有限公司 | Eradication-resisting and coating-preventing marker paint for fishery vessel |
| JP2016113561A (en) * | 2014-12-16 | 2016-06-23 | 関西ペイント株式会社 | Aqueous coating composition for coating can |
| CN105199511A (en) * | 2015-09-24 | 2015-12-30 | 维新制漆（深圳）有限公司 | Varnish for stainless steel substrate and preparation method and application of varnish |
| CN109679479A (en) * | 2018-12-29 | 2019-04-26 | 东来涂料技术（上海）股份有限公司 | A kind of environment-friendly water-based varnish of high durable acid and alkali-resistance and preparation method thereof |
| CN111234598A (en) * | 2020-02-23 | 2020-06-05 | 湖南七纬科技有限公司 | Alcohol-resistant flame-retardant ink |
| WO2022117017A1 (en) * | 2020-12-02 | 2022-06-09 | 立邦涂料（中国）有限公司 | Aqueous secondary dispersion containing copolymer p, preparation method therefor, and application thereof |
| CN113045921A (en) * | 2021-03-17 | 2021-06-29 | 山东七维新材料有限公司 | Coating matching system for CR200J type compound-number motor train unit and coating process thereof |
| CN113416472A (en) * | 2021-07-30 | 2021-09-21 | 雅图高新材料股份有限公司 | Water-based bi-component epoxy primer for racing helmet and preparation method thereof |
| CN114874747A (en) * | 2022-05-05 | 2022-08-09 | 安徽斯迈特新材料股份有限公司 | Preparation method of high-temperature-resistant and strong-ultraviolet-resistant MS (Murashige & Skoog) adhesive |
| CN115851062A (en) * | 2022-12-07 | 2023-03-28 | 雅图高新材料股份有限公司 | Acrylic water-based high-adhesion primer and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| RP-HPLC测定卡维地洛片中的杂质D和杂质E;康铁纯等;《药物分析杂志》;第35卷(第10期);1838-1842 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN117186750A (en) | 2023-12-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109337518B (en) | Water-based epoxy resin coating and preparation method thereof | |
| CN114015307B (en) | Single-component water-based acrylic acid strippable paint and preparation method and application thereof | |
| CN111073427A (en) | Dual UV (ultraviolet) curing coating for automotive interior parts, preparation method thereof and paint film formed by dual UV curing coating | |
| CN107936814A (en) | The net taste woodcare paint of high hardness polyurethane that a kind of POSS is modified | |
| CN110283512A (en) | A kind of high richness water varnish composition and preparation method thereof | |
| CN109266142B (en) | Aqueous solvent-free and high-gloss single-component metallic paint without covering and preparation thereof | |
| CN111534216A (en) | Water-soluble triazinyl sulfone polyurethane and application thereof | |
| CN117186750B (en) | Water-based vacuum aluminizing finishing varnish and preparation method thereof | |
| CN112960911A (en) | Silicone oil modified anti-dazzle anti-reflection coating solution, preparation method and application | |
| CN114752268B (en) | Double-curing-surface paint for automobile exterior decoration and preparation method and application thereof | |
| CN111117444B (en) | Water-based polyester-acrylic amino resin hybrid baking paint and preparation method thereof | |
| CN110616034A (en) | Anti-fog UV coating for automobile exterior trimming part and automobile lamp, preparation method of anti-fog UV coating and paint film formed by anti-fog UV coating | |
| CN110511382B (en) | Capsaicin acrylate modified polysiloxane material and preparation method and application thereof | |
| CN113637396A (en) | Single-component acrylic acid modified wrinkle paint and resin preparation method | |
| CN108794683B (en) | Self-repairing acrylic microgel self-emulsifying emulsion and preparation method thereof | |
| CN112626863A (en) | Outdoor curtain manufacturing process | |
| CN115304963B (en) | Initial high-adhesion water-resistant environment-friendly metal coating | |
| CN114380953B (en) | Modified acrylic emulsion for computer heat radiation module water-based baking varnish | |
| CN117186758B (en) | Water-based high-gloss primer-topcoat paint and preparation method thereof | |
| CN112322177A (en) | UV color transparent paint and preparation and coating methods thereof | |
| CN114525075B (en) | Ultra-fast-drying water-based varnish for automobile repair and preparation method thereof | |
| CN114395300B (en) | Water-based noise reduction coating for aluminum plates and preparation method thereof | |
| CN114702894B (en) | Aqueous single-layer UV (ultraviolet) matte black paint | |
| CN114958128B (en) | High-weather-resistance water-based automobile coating and preparation method thereof | |
| CN111454423B (en) | Water-based vacuum plastic and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |