CN115820004A - PH response type water-based aluminum paste and preparation method thereof - Google Patents
PH response type water-based aluminum paste and preparation method thereof Download PDFInfo
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- CN115820004A CN115820004A CN202211651943.1A CN202211651943A CN115820004A CN 115820004 A CN115820004 A CN 115820004A CN 202211651943 A CN202211651943 A CN 202211651943A CN 115820004 A CN115820004 A CN 115820004A
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 124
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 124
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 230000004044 response Effects 0.000 title claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 88
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims abstract description 67
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 60
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 44
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims abstract description 42
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 31
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 31
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 29
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 29
- 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 28
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 27
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000000440 bentonite Substances 0.000 claims abstract description 25
- 229910000278 bentonite Inorganic materials 0.000 claims abstract description 25
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims abstract description 25
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 25
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 20
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 20
- 239000000047 product Substances 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 238000011282 treatment Methods 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 8
- 239000010703 silicon Substances 0.000 claims abstract description 8
- 239000003054 catalyst Substances 0.000 claims abstract description 7
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 53
- 239000000243 solution Substances 0.000 claims description 29
- 239000007864 aqueous solution Substances 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 19
- 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 13
- 229920001661 Chitosan Polymers 0.000 claims description 13
- 238000011276 addition treatment Methods 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 239000000654 additive Substances 0.000 claims description 11
- 230000000996 additive effect Effects 0.000 claims description 11
- 229920001296 polysiloxane Polymers 0.000 claims description 10
- -1 aluminum silver Chemical compound 0.000 claims description 8
- 239000011247 coating layer Substances 0.000 claims description 8
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 7
- CYEJMVLDXAUOPN-UHFFFAOYSA-N 2-dodecylphenol Chemical compound CCCCCCCCCCCCC1=CC=CC=C1O CYEJMVLDXAUOPN-UHFFFAOYSA-N 0.000 claims description 6
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 6
- 229910021529 ammonia Inorganic materials 0.000 claims description 6
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 6
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 6
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 239000007790 solid phase Substances 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 5
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000000576 coating method Methods 0.000 abstract description 19
- 239000011248 coating agent Substances 0.000 abstract description 18
- 239000003973 paint Substances 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 8
- 239000006185 dispersion Substances 0.000 abstract description 3
- 230000000051 modifying effect Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract 2
- 239000012752 auxiliary agent Substances 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000000178 monomer Substances 0.000 description 6
- 239000011347 resin Substances 0.000 description 6
- 229920005989 resin Polymers 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 238000006116 polymerization reaction Methods 0.000 description 4
- 229920000178 Acrylic resin Polymers 0.000 description 3
- 239000004925 Acrylic resin Substances 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000011065 in-situ storage Methods 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 230000005595 deprotonation Effects 0.000 description 2
- 238000010537 deprotonation reaction Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 150000002734 metacrylic acid derivatives Chemical class 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 229920000058 polyacrylate Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 230000005588 protonation Effects 0.000 description 2
- 125000001453 quaternary ammonium group Chemical group 0.000 description 2
- 238000002310 reflectometry Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 125000003342 alkenyl group Chemical group 0.000 description 1
- 238000004873 anchoring Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 238000006757 chemical reactions by type Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical class [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 1
- 150000001845 chromium compounds Chemical class 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005536 corrosion prevention Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 239000008394 flocculating agent Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 150000002903 organophosphorus compounds Chemical class 0.000 description 1
- 229920001558 organosilicon polymer Polymers 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920005990 polystyrene resin Polymers 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- XTUSEBKMEQERQV-UHFFFAOYSA-N propan-2-ol;hydrate Chemical compound O.CC(C)O XTUSEBKMEQERQV-UHFFFAOYSA-N 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Landscapes
- Dental Preparations (AREA)
Abstract
The invention discloses a preparation method of PH response type waterborne aluminum paste, which comprises the following steps: taking an aluminum sheet as a carrier, tetraethoxysilane as a silicon source, isopropanol and water as solvents and ammonia water as a catalyst, reacting at the temperature of 30-80 ℃, centrifugally drying a reaction product to obtain a silicon dioxide coated aluminum sheet, and functionally modifying the aluminum sheet with reactive acrylic acid, acrylamide, vinyl organosilicon and hydroxyapatite to obtain a target product. According to the application method, the oily aluminum paste is subjected to solvent dispersion, auxiliary agent coating treatment and chemical reaction and then is directly applied to the water-based paint, the oily aluminum paste is directly applied to the water-based paint after being treated, the added modified hydroxyapatite is pre-modified by the hydrochloric acid solution and other raw materials, the bentonite lamellar structure and the hydroxyapatite are cooperated, the two synergies, and the oily aluminum paste is added to the raw materials, so that the performance effect of the aluminum paste can be improved.
Description
Technical Field
The invention relates to the technical field of aluminum paste, and particularly relates to a pH response type water-based aluminum paste and a preparation method thereof.
Background
Aluminum paste is one of the important metallic pigments, which has been widely used in the paint industry, printing ink and plastic industry because of its high brilliant metallic luster. In the coating aspect, aluminum paste has been used in solvent-based systems. In recent years, with the further development of the coating industry and the enhancement of environmental awareness, regulations for the emission of toxic solvents into the atmosphere environment are becoming stricter, and the production and development of low-pollution, pollution-free and dust-free coating products are receiving high attention. Water is used to replace organic solvent, and water paint is the inevitable trend of paint industry development. More and more factories apply the water paint in China. Aluminum paste is a source of the glittering effect of the coating, and the aluminum paste is required to be used for achieving a good decorative effect. In the furniture industry, the automobile coating industry, the ink industry and the hardware and household appliance industry, a large amount of aluminum pigments of water-based aluminum paste which can be used for water-based coatings are used.
Since the aluminum silver paste reacts with water in the water environment, 2Al +6H 2 O→2Al(OH) 3 +3H 2 Generating H 2 So-called "gassing" leads to problems in all respects. The so-called waterborne aluminum paste on the market is prepared by performing surface modification treatment on the traditional oily aluminum paste. There are two main types, physical protection and chemical protection.
The physical protection method is to wrap a layer of transparent resin on the surface of the aluminum sheet as a protective layer. For example, in-situ polymerization is used to coat a polystyrene resin layer on the surface of an aluminum sheet, but it is known that the bonding force between polystyrene and the aluminum sheet is weak, and the resin is easy to fall off from the surface of the aluminum sheet under the action of high shear, so that the protection effect on the aluminum sheet is lost. And the particle size of the aluminum sheet is relatively large, and the conversion rate of the in-situ polymerization monomer and the resin coating rate by taking the aluminum sheet as a matrix are not too high. The conductivity against high voltage is also poor. The application number 200810207593.3 is coated by epoxy phosphate resin, the phosphate has a strong anchoring effect on an aluminum sheet and strong adsorption capacity, the problem of bonding with the aluminum sheet is solved, but the used matrix is epoxy, the weather resistance of the epoxy and the compatibility with a water-based paint base material have the problems, and the epoxy resin has low molecular weight, has weak capacity of preventing the diffusion of water molecules, and increases the corrosion to aluminum paste.
Chemical protectionThe protection method mainly comprises two types of additive technology and coating technology. The additive technology is mainly characterized in that organic phosphorus compounds such as Stapa series of Eckart and AquasilBP/AN of Siberine (Eckart and Siberine are both suppliers of aluminum sheets in the world) are added, but the stability of the aluminum sheets in water is difficult to really protect due to the addition of small molecular compounds. Another side effect is that the properties of the coating (e.g. drying time, adhesion, humidity resistance) may be affected. The wrapping technique has also gone through two generations. The first generation uses insoluble chromium compounds (such as Eckart Hydrolux), which are also the current representatives of better aluminum flake corrosion prevention performance, but with the increasing awareness of environmental protection, chromates are gradually eliminated due to the carcinogenic toxicity. The second generation is now the more popular SiO 2 Coating, some even on SiO 2 The coating is further modified by organic substances to improve the compatibility with the coating base material and the adhesion, such as the aluminum sheet processing technology of Toyo Japan, the Hydrolan series of Eckart, but the SiO is 2 The coating technology is to add SiO on the basis of the original aluminum sheet 2 The coating layer achieves the effect of protecting the aluminum sheet, and although the comprehensive performances of preventing gas generation, resisting humidity and heat, resisting weather, resisting pipeline circulation and the like are excellent, the SiO film has the advantages of 2 The coating layer will affect the original brightness, flash degree and covering power of the aluminum sheet, agglomeration of the aluminum sheet is easily caused in the treatment process, the manufacturing cost is very high, and the market popularization is difficult.
Disclosure of Invention
In view of the defects of the prior art, the present invention aims to provide a PH-responsive aqueous aluminum paste and a preparation method thereof, so as to solve the problems in the background art.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the invention provides a preparation method of PH response type waterborne aluminum paste, which comprises the following steps:
the method comprises the following steps: taking an aluminum sheet as a carrier, tetraethoxysilane as a silicon source, isopropanol and water as solvents and ammonia water as a catalyst, reacting at 30-80 ℃, and centrifugally drying a reaction product to obtain a silicon dioxide coated aluminum sheet;
step two: reacting the aluminum sheet coated with the silicon dioxide with reactive acrylic acid, acrylamide, vinyl organosilicon and hydroxyapatite at 40-100 ℃ for 1-12 hours to obtain the water-based aluminum silver paste with the coating layer.
Preferably, the mass ratio of the aluminum sheet, the ethyl orthosilicate, the reactive acrylic acid, the acrylamide, the vinyl organosilicon, the isopropanol, the water and the ammonia water is (1-10): (1-2), (1-1.5), (20-30): (50-70) and (0.9-1.8).
One of the selected polymerization reactants is acrylamide, which is mainly used for preparing water-soluble polymers, and the polyacrylamide can be used as an additive for flocculants, thickeners and coating aids. A small amount of acrylamide is used to introduce hydrophilic centers into the lipophilic polymer to improve viscosity, increase softening point and increase solvent resistance of the resin, and may introduce a center for PH response.
One of the polymeric reactants selected for use in the present invention is reactive acrylic acid, including acrylates, methacrylates, and methacrylates. The reactive acrylic acid is a kind of acrylic acid homopolymer or copolymer with different molecular weights, and the substance only slightly reduces the surface tension of the coating and can balance the surface tension difference of the paint film to obtain a truly flat and mirror-like paint film surface. Such substances have a levelling action, which, if the molecular weight is sufficiently high, also has a degassing and defoaming action. The acrylic leveling agent containing a reactive functional group can provide good leveling property without generating haze and without lowering surface hardness, and sometimes can increase surface hardness.
One of the selected polymerization reactants is reactive vinyl organosilicon, and the organosilicon monomer can generate free radical polymerization with the vinyl on the acrylate monomer due to containing active vinyl, so that the organosilicon modified polyacrylate polymer is prepared. The organosilicon monomer containing vinyl is the most organosilicon modified monomer used for modifying polyacrylate at present. The organosilicon monomer containing vinyl comprises side chain vinyl and end ethyleneAn alkenyl group. Organosilicon Polymer and SiO 2 The materials have rich Si-O-Si inorganic structures, and the comprehensive performance is hopeful to be greatly improved when the materials are introduced into acrylic resin due to high strength and good weather resistance. However, when these materials are simply mixed with an aqueous acrylic resin, the desired modifying effect may be lost due to poor compatibility, poor stability, uneven dispersion, and the like. Aiming at the problems, the organic-inorganic nano hybrid resin with stable storage and good coating performance is obtained by compounding organic siloxane, inorganic silica sol, acrylamide and water-based acrylic resin with high content on a nano scale based on a sol-gel method and a blending method.
The material prepared by the invention can control the performance by adjusting the change of pH. The wettability of the material can be changed in situ under the adjustment of pH, and the synthesized copolymer can change the wetting property through protonation and deprotonation under the condition of pH change. In the presence of HCl, the amino group-N (CH) of acrylamide 3 ) 2 Protonation takes place in conjunction with H + A portion of the triamine will be converted to quaternary ammonium (-NH + (CH) 3 ) 2 ) (ii) a Then the NaOH is treated by NaOH aqueous solution, the NaOH can generate neutralization reaction with H + in hydroxyl of the hydroxyapatite, and H + is + Rapidly decreases and becomes almost nonexistent, so-NH + (CH) 3 ) 2 Deprotonation occurs and the quaternary ammonium is converted back to the tertiary amine.
Preferably, the reaction of the silica-coated aluminum sheet is specifically:
mixing aluminum sheet, ethyl orthosilicate, isopropanol and water, stirring for 10-15 minutes, then dripping ammonia water, and continuously stirring and reacting for 1-10 hours at the temperature of 30-80 ℃.
Preferably, the aluminum sheet coated with the silicon dioxide is stirred and refluxed for reaction for 1 to 12 hours in an isopropanol water solution at a temperature of between 40 and 100 ℃;
mixing reactive acrylic acid, acrylamide, vinyl organosilicon and isopropanol, dripping into a silicon dioxide coated aluminum sheet solution, dripping azodiisobutyronitrile, stirring for reacting for 1-12 hours, and performing centrifugal separation to obtain a solid-phase product, namely the target product.
Preferably, in the first step, the addition amount ratio of deionized water, concentrated ammonia water, ethanol and TEOS is 20ml.
Preferably, in the first step, the stirring reaction time is 1-10h.
Preferably, the weight ratio of the dosage of the silicon dioxide coating and reaction type acrylic acid, acrylamide and vinyl organic silicon is 1:1 to 10:1.
preferably, azobisisobutyronitrile is used in an amount of 0.5 to 3% by weight based on the total weight of the silica-coated aluminum flake.
Preferably, modified hydroxyapatite is further added in the second step, and the addition amount is 5-10% of the total weight of the aluminum sheet coated by the silicon dioxide;
the preparation method of the modified hydroxyapatite comprises the following steps:
s11: adding hydroxyapatite into a hydrochloric acid solution according to a weight ratio of 1:5, stirring and dispersing, then adding 5-10% of lauryl sodium sulfate and 2-5% of carboxymethyl cellulose of the total amount of the hydroxyapatite, stirring uniformly, washing with water, and drying to obtain pretreated hydroxyapatite;
s12: feeding bentonite to 350-400 deg.C, treating for 20-30min, and cooling to room temperature at 3-5 deg.C/min;
s13: adding 1-3 parts of silane coupling agent KH560 into 10-20 parts of deionized water, then adding 2-4 parts of chitosan aqueous solution, uniformly stirring, finally adding 0.2-0.7 part of dodecylphenol, and fully stirring to obtain an addition treatment solution;
s14: and (3) adding the bentonite of the S12 into the addition treatment liquid of the S13, fully stirring, finally adding the pretreated hydroxyapatite, continuously mixing fully, and finally washing and drying to obtain the modified hydroxyapatite.
Preferably, the mass fraction of the hydrochloric acid solution is 2-5%; the mass fraction of the chitosan aqueous solution is 10-20%; the mass ratio of the bentonite of S12 to the additive treatment liquid of S13 to the pretreated hydroxyapatite is 3: (10-15): (5-7).
The invention also provides the waterborne aluminum paste prepared by the preparation method of the PH responsive waterborne aluminum paste.
Compared with the prior art, the invention has the following beneficial effects:
the invention relates to a using method for directly using oily aluminum paste in a water-based paint after solvent dispersion, coating additive treatment and chemical reaction, and a method for directly using the oily aluminum paste in the water-based paint after the oily aluminum paste is treated, wherein the oily aluminum paste is directly applied to the water-based paint through the method.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to specific embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The preparation method of the PH-responsive aqueous aluminum paste of the embodiment includes the following steps:
the method comprises the following steps: taking an aluminum sheet as a carrier, tetraethoxysilane as a silicon source, isopropanol and water as solvents and ammonia water as a catalyst, reacting at the temperature of 30-80 ℃, and centrifugally drying a reaction product to obtain the mesoporous silica coated aluminum sheet;
step two: reacting the aluminum sheet coated by the silicon dioxide with reactive acrylic acid, acrylamide, vinyl organosilicon and hydroxyapatite at the temperature of between 40 and 100 ℃ for 1 to 12 hours to obtain the water-based aluminum silver paste with the coating layer.
The mass ratio of the aluminum sheet, the ethyl orthosilicate, the reactive acrylic acid, the acrylamide, the vinyl silicone, the azobisisobutyronitrile, the isopropanol, the water and the ammonia water in the embodiment is (1-10): (1-2), (1-1.5), (0.1-0.3), (20-30): (50-70) and (0.9-1.8).
The reaction of the aluminum sheet coated with mesoporous silica in this embodiment is specifically as follows:
mixing aluminum sheet, ethyl orthosilicate, isopropanol and water, stirring for 10-15 min, then dripping ammonia water, and continuously stirring and reacting for 1-10h at room temperature.
The silica-coated aluminum sheet of the embodiment is stirred and refluxed for reaction for 1 to 12 hours in an isopropanol aqueous solution at a temperature of between 40 and 100 ℃;
mixing reactive acrylic acid, acrylamide, vinyl organosilicon and isopropanol, dropwise adding the mixture into a silicon dioxide coated aluminum sheet solution, stirring and reacting for 1-12 hours, dropwise adding azodiisobutyronitrile, and performing centrifugal separation to obtain a solid-phase product, namely the target product.
In the first step of this example, the addition ratio of deionized water, concentrated ammonia, ethanol, and TEOS is 20ml.
In the first step of this example, the reaction time is 1-10h.
The amount of the silica-coated reactive acrylic acid, acrylamide, and vinyl silicone used in the present example was 1:1 to 10:1.
in the second step of this embodiment, modified hydroxyapatite is further added, and the addition amount is 5 to 10% of the total weight of the aluminum sheet coated with silicon dioxide;
the preparation method of the modified hydroxyapatite comprises the following steps:
s11: adding hydroxyapatite into a hydrochloric acid solution according to a weight ratio of 1:5, stirring and dispersing, then adding 5-10% of lauryl sodium sulfate and 2-5% of carboxymethyl cellulose of the total amount of the hydroxyapatite, stirring uniformly, washing with water, and drying to obtain pretreated hydroxyapatite;
s12: feeding bentonite to 350-400 deg.C, treating for 20-30min, and cooling to room temperature at 3-5 deg.C/min;
s13: adding 1-3 parts of silane coupling agent KH560 into 10-20 parts of deionized water, then adding 2-4 parts of chitosan aqueous solution, uniformly stirring, finally adding 0.2-0.7 part of dodecylphenol, and fully stirring to obtain an addition treatment solution;
s14: and (3) adding the bentonite of the S12 into the addition treatment liquid of the S13, fully stirring, finally adding the pretreated hydroxyapatite, continuously mixing fully, and finally washing and drying to obtain the modified hydroxyapatite.
The mass fraction of the hydrochloric acid solution in the embodiment is 2-5%; the mass fraction of the chitosan aqueous solution is 10-20%; the mass ratio of the bentonite of S12 to the additive treatment liquid of S13 to the pretreated hydroxyapatite is 3: (10-15): (5-7).
The aqueous aluminum paste prepared by the method for preparing PH-responsive aqueous aluminum paste of this example.
Example 1.
The preparation method of the PH-responsive aqueous aluminum paste of the embodiment includes the following steps:
the method comprises the following steps: reacting at 30 ℃ by taking an aluminum sheet as a carrier, tetraethoxysilane as a silicon source, isopropanol and water as solvents and ammonia water as a catalyst, and centrifugally drying a reaction product to obtain a mesoporous silica-coated aluminum sheet;
step two: and reacting the aluminum sheet coated with the silicon dioxide with reactive acrylic acid, acrylamide, vinyl organosilicon and hydroxyapatite at 40 ℃ for 2 hours to obtain the water-based aluminum silver paste with the coating layer.
The mass ratio of the aluminum sheet, the ethyl orthosilicate, the reactive acrylic acid, the acrylamide, the vinyl silicone, the azobisisobutyronitrile, the isopropanol, the water and the ammonia water in the embodiment is 10: 50:0.9.
The reaction of the aluminum sheet coated with mesoporous silica in this embodiment is specifically as follows:
mixing an aluminum sheet, tetraethoxysilane, isopropanol and water, stirring for 10 minutes, then dropwise adding the ammonia water, and continuously stirring at room temperature for reaction for 1 hour.
The aluminum sheet coated with silicon dioxide of the embodiment is stirred and refluxed for reaction for 1 hour at 40 ℃ in an isopropanol aqueous solution;
mixing reactive acrylic acid, acrylamide, vinyl organosilicon and isopropanol, dropwise adding the mixture into a silicon dioxide coated aluminum sheet solution, stirring and reacting for 1 hour, dropwise adding azobisisobutyronitrile, and performing centrifugal separation to obtain a solid-phase product, namely the target product.
In the first step of this example, the addition ratio of deionized water, concentrated ammonia, ethanol, and TEOS is 20ml.
In the first step of this example, the reaction time was 1 hour.
The amount of the silica-coated reactive acrylic acid, the acrylamide, the vinyl silicone, and the azobisisobutyronitrile used in the present example was 1:5:1:0.1.
in the second step of this embodiment, modified hydroxyapatite is further added, and the addition amount is 5% of the total weight of the aluminum sheet coated with silicon dioxide;
the preparation method of the modified hydroxyapatite comprises the following steps:
s11: adding hydroxyapatite into a hydrochloric acid solution according to a weight ratio of 1:5, stirring and dispersing, then adding sodium dodecyl sulfate accounting for 5% of the total weight of the hydroxyapatite and carboxymethyl cellulose accounting for% of the total weight of the hydroxyapatite, stirring uniformly, washing with water, and drying to obtain pretreated hydroxyapatite;
s12: the bentonite is sent to 350 ℃ for treatment for 20min, and then is cooled to the room temperature at the speed of 3 ℃/min;
s13: adding 1 part of silane coupling agent KH560 into 10 parts of deionized water, then adding 2 parts of chitosan aqueous solution, uniformly stirring, finally adding 0.2 part of dodecylphenol, and fully stirring to obtain an addition treatment solution;
s14: and (3) adding the bentonite of the S12 into the addition treatment liquid of the S13, fully stirring, finally adding the pretreated hydroxyapatite, continuously mixing fully, and finally washing and drying to obtain the modified hydroxyapatite.
The mass fraction of the hydrochloric acid solution in this example was 2%; the mass fraction of the chitosan aqueous solution is 10%; the mass ratio of the bentonite of S12 to the additive treatment liquid of S13 to the pretreated hydroxyapatite is 3:10:5.
the aqueous aluminum paste prepared by the method for preparing PH-responsive aqueous aluminum paste of this example.
Example 2.
The preparation method of the PH-responsive aqueous aluminum paste of the embodiment includes the following steps:
the method comprises the following steps: taking an aluminum sheet as a carrier, tetraethoxysilane as a silicon source, isopropanol and water as solvents and ammonia water as a catalyst, reacting at 80 ℃, and centrifugally drying a reaction product to obtain the mesoporous silica coated aluminum sheet;
step two: and reacting the aluminum sheet coated with the silicon dioxide with reactive acrylic acid, acrylamide and vinyl organosilicon at 100 ℃ for 12 hours to obtain the water-based aluminum silver paste with the coating layer.
The mass ratio of the aluminum sheet, the ethyl orthosilicate, the reactive acrylic acid, the acrylamide, the vinyl silicone, the isopropanol, the water and the ammonia water in the embodiment is 10:2:1.5:1.5:1.5:30:70:1.8.
The reaction of the aluminum sheet coated with mesoporous silica in this embodiment is specifically:
mixing an aluminum sheet, tetraethoxysilane, isopropanol and water, stirring for 15 minutes, then dropwise adding the ammonia water, and continuously stirring at room temperature for reaction for 10 hours.
The aluminum sheet coated with silicon dioxide of the embodiment is stirred and refluxed for reaction for 12 hours in isopropanol aqueous solution at 100 ℃;
mixing reactive acrylic acid, acrylamide, vinyl organosilicon and isopropanol, dropwise adding the mixture into a silicon dioxide coated aluminum sheet solution, stirring and reacting for 12 hours, and performing centrifugal separation to obtain a solid-phase product, namely a target product.
In the first step of this example, the addition ratio of deionized water, concentrated ammonia, ethanol, and TEOS is 20ml.
In the first step of this example, the reaction time was 10 hours with stirring.
The amount of the silica-coated reactive acrylic acid, acrylamide, and vinyl silicone used in the present example was 1:5:1.
in the second step of this embodiment, modified hydroxyapatite is further added, and the addition amount is 10% of the total weight of the aluminum sheet coated with silica;
the preparation method of the modified hydroxyapatite comprises the following steps:
s11: adding the hydroxyapatite into the hydrochloric acid solution according to the weight ratio of 1:5, stirring and dispersing, then adding sodium dodecyl sulfate accounting for 10 percent of the total amount of the hydroxyapatite and carboxymethyl cellulose accounting for 5 percent of the total amount of the hydroxyapatite, uniformly stirring, washing and drying to obtain pretreated hydroxyapatite;
s12: the bentonite is sent to 400 ℃ for 30min, and then is cooled to the room temperature at the speed of 5 ℃/min;
s13: adding 3 parts of silane coupling agent KH560 into 20 parts of deionized water, then adding 4 parts of chitosan aqueous solution, uniformly stirring, finally adding 0.7 part of dodecylphenol, and fully stirring to obtain an addition treatment solution;
s14: and (3) adding the bentonite of the S12 into the addition treatment liquid of the S13, fully stirring, finally adding the pretreated hydroxyapatite, continuously mixing fully, and finally washing and drying to obtain the modified hydroxyapatite.
The mass fraction of the hydrochloric acid solution in this example was 5%; the mass fraction of the chitosan aqueous solution is 20%; the mass ratio of the bentonite of S12 to the additive treatment liquid of S13 to the pretreated hydroxyapatite is 3:15:7.
the aqueous aluminum paste prepared by the method for preparing PH-responsive aqueous aluminum paste of this example.
Example 3.
The preparation method of the PH-responsive aqueous aluminum paste of the embodiment includes the following steps:
the method comprises the following steps: taking an aluminum sheet as a carrier, tetraethoxysilane as a silicon source, isopropanol and water as solvents and ammonia water as a catalyst, reacting at 60 ℃, and centrifugally drying a reaction product to obtain the mesoporous silica coated aluminum sheet;
step two: and reacting the aluminum sheet coated with the silicon dioxide with reactive acrylic acid, acrylamide and vinyl organosilicon at 70 ℃ for 6 hours to obtain the aqueous aluminum silver paste with the coating layer.
The mass ratio of the aluminum sheet, the ethyl orthosilicate, the reactive acrylic acid, the acrylamide, the vinyl silicone, the isopropanol, the water and the ammonia water in the embodiment is 10:1:11:1.2:25:60:1.4.
The reaction of the aluminum sheet coated with mesoporous silica in this embodiment is specifically as follows:
mixing an aluminum sheet, tetraethoxysilane, isopropanol and water, stirring for 12 minutes, then dropwise adding the ammonia water, and continuously stirring at room temperature for reaction for 5 hours.
The silica-coated aluminum sheet of the embodiment is stirred and refluxed for reaction for 6 hours in an isopropanol aqueous solution at 70 ℃;
mixing reactive acrylic acid, acrylamide, vinyl organosilicon and isopropanol, dropwise adding the mixture into a silicon dioxide coated aluminum sheet solution, stirring and reacting for 6 hours, and centrifugally separating to obtain a solid-phase product, namely the target product.
In the first step of this example, the addition ratio of deionized water, concentrated ammonia, ethanol, and TEOS is 20ml.
In the first step of this example, the reaction time was 5 hours with stirring.
The weight ratio of the amount of the silica-coated reactive acrylic acid, the acrylamide and the vinyl silicone in the embodiment is 1:5:1.
in the second step of this embodiment, modified hydroxyapatite is further added, and the addition amount is 7% of the total weight of the aluminum sheet coated with silicon dioxide;
the preparation method of the modified hydroxyapatite comprises the following steps:
s11: adding hydroxyapatite into a hydrochloric acid solution according to a weight ratio of 1:5, stirring and dispersing, then adding sodium dodecyl sulfate accounting for 7% of the total weight of the hydroxyapatite and carboxymethyl cellulose accounting for 3%, stirring uniformly, washing with water, and drying to obtain pretreated hydroxyapatite;
s12: the bentonite is sent to 370 ℃ for treatment for 25min, and then is cooled to the room temperature at the speed of 4 ℃/min;
s13: adding 2 parts of silane coupling agent KH560 into 15 parts of deionized water, then adding 3 parts of chitosan aqueous solution, uniformly stirring, finally adding 0.4 part of dodecylphenol, and fully stirring to obtain an addition treatment solution;
s14: and (3) adding the bentonite of the S12 into the addition treatment liquid of the S13, fully stirring, finally adding the pretreated hydroxyapatite, continuously mixing fully, and finally washing and drying to obtain the modified hydroxyapatite.
The mass fraction of the hydrochloric acid solution in this example was 3.5%; the mass fraction of the chitosan aqueous solution is 15%; the mass ratio of the bentonite of S12 to the additive treatment liquid of S13 to the pretreated hydroxyapatite is 3:12:5.
the aqueous aluminum paste prepared by the method for preparing PH-responsive aqueous aluminum paste of this example.
Comparative example 1.
In contrast to example 3, modified hydroxyapatite was not added.
Comparative example 2.
The difference from example 3 is that no S12 bentonite was added in the preparation of modified hydroxyapatite.
Comparative example 3.
The difference from example 3 is that bentonite is used instead of S12 bentonite.
Comparative example 4.
The difference from example 3 is the preparation method of the additive treatment solution:
adding 1-3 parts of silane coupling agent KH560 into 10-20 parts of deionized water, then adding 2-4 parts of chitosan aqueous solution, and fully stirring to obtain an addition treatment solution.
Comparative example 5.
The difference from example 3 is that the pretreated hydroxyapatite was replaced with hydroxyapatite.
The products of examples 1 to 3 and comparative examples 1 to 5 were subjected to the following performance tests, and the results thereof were as follows
As can be seen from comparative examples 1 to 5 and examples 1 to 3;
the modified hydroxyapatite is added, so that the product still has excellent stability in reflectivity under acid and salt conditions; in the preparation of the modified hydroxyapatite, the bentonite without S12 is not added, the bentonite with S12 is replaced by the bentonite, the performance of the product is obviously poor, meanwhile, the preparation method for adding the treatment solution is different, the pretreated hydroxyapatite is replaced by the hydroxyapatite, the performance of the product tends to be poor, only the modified hydroxyapatite prepared by the method of the invention can have obvious improvement effect on the glossiness and the reflectivity of the product, and meanwhile, the performance stability under the conditions of acid and salt is obvious.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (10)
1. The preparation method of the pH response type waterborne aluminum paste is characterized by comprising the following steps:
the method comprises the following steps: taking an aluminum sheet as a carrier, tetraethoxysilane as a silicon source, isopropanol and water as solvents and ammonia water as a catalyst, reacting at 30-80 ℃, and centrifugally drying a reaction product to obtain a silicon dioxide coated aluminum sheet;
step two: reacting the aluminum sheet coated by the silicon dioxide with reactive acrylic acid, acrylamide, vinyl organosilicon and modified hydroxyapatite at 40-100 ℃ for 1-12 hours to obtain the water-based aluminum silver paste with the coating layer.
2. The method for preparing the PH-responsive aqueous aluminum paste according to claim 1, wherein the mass ratio of the aluminum sheet to the tetraethoxysilane to the reactive acrylic acid to the acrylamide to the vinyl silicone to the isopropanol to the water to the ammonia water is (1-10): (1-2), (1-1.5), (20-30): (50-70) and (0.9-1.8).
3. The method for preparing the pH-responsive aqueous aluminum paste according to claim 1, wherein the reaction of the silica-coated aluminum sheet is specifically as follows:
mixing aluminum sheet, ethyl orthosilicate, isopropanol and water, stirring for 10-15 minutes, then dripping ammonia water, and continuously stirring and reacting for 1-10 hours at the temperature of 30-80 ℃.
4. The method for preparing the PH responsive aqueous aluminum paste according to claim 1, wherein the silica-coated aluminum sheet is stirred and refluxed for 1 to 12 hours at a temperature of between 40 and 100 ℃ in an isopropanol aqueous solution;
mixing reactive acrylic acid, acrylamide, vinyl organosilicon and isopropanol, dripping into a silicon dioxide coated aluminum sheet solution, dripping azodiisobutyronitrile, stirring for reacting for 1-12 hours, and performing centrifugal separation to obtain a solid-phase product, namely the target product.
5. The method for preparing a PH-responsive aqueous aluminum paste according to claim 1, wherein in the first step, the addition amount ratio of deionized water, concentrated ammonia, ethanol and TEOS is 20ml, 2753ml, and the concentration of concentrated ammonia is 28wt.%.
6. The method for preparing a pH responsive aqueous aluminum paste according to claim 1, wherein in the first step, the stirring reaction time is 1-10h.
7. The method for preparing a pH-responsive aqueous aluminum paste according to claim 1, wherein the silicon dioxide-coated and reactive acrylic acid, acrylamide and vinyl silicone are used in an amount by weight ratio of 1:1 to 10:1.
8. the method for preparing the pH response type waterborne aluminum paste according to claim 1, wherein modified hydroxyapatite is further added in the second step, and the addition amount is 5-10% of the total weight of the aluminum sheet coated with the silicon dioxide;
the preparation method of the modified hydroxyapatite comprises the following steps:
s11: adding hydroxyapatite into a hydrochloric acid solution according to a weight ratio of 1:5, stirring and dispersing, then adding sodium dodecyl sulfate accounting for 5-10% of the total weight of the hydroxyapatite and carboxymethyl cellulose accounting for 2-5%, stirring uniformly, washing with water, and drying to obtain pretreated hydroxyapatite;
s12: feeding bentonite to 350-400 deg.C, treating for 20-30min, and cooling to room temperature at 3-5 deg.C/min;
s13: adding 1-3 parts of silane coupling agent KH560 into 10-20 parts of deionized water, then adding 2-4 parts of chitosan aqueous solution, uniformly stirring, finally adding 0.2-0.7 part of dodecylphenol, and fully stirring to obtain an addition treatment solution;
s14: and (3) adding the bentonite of the S12 into the addition treatment liquid of the S13, fully stirring, finally adding the pretreated hydroxyapatite, continuously mixing fully, and finally washing and drying to obtain the modified hydroxyapatite.
9. The method for preparing the pH-responsive aqueous aluminum paste according to claim 8, wherein the hydrochloric acid solution is 2-5% by mass; the mass fraction of the chitosan aqueous solution is 10-20%; the mass ratio of the bentonite of S12 to the additive treatment liquid of S13 to the pretreated hydroxyapatite is 3: (10-15): (5-7).
10. An aqueous aluminum paste prepared according to the method for preparing a PH-responsive aqueous aluminum paste of any one of claims 1-9.
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