CN111019465B - Preparation process of organic-inorganic composite water-based acrylic acid anticorrosive paint - Google Patents
Preparation process of organic-inorganic composite water-based acrylic acid anticorrosive paint Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D143/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing boron, silicon, phosphorus, selenium, tellurium, or a metal; Coating compositions based on derivatives of such polymers
- C09D143/04—Homopolymers or copolymers of monomers containing silicon
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- C09D125/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Coating compositions based on derivatives of such polymers
- C09D125/02—Homopolymers or copolymers of hydrocarbons
- C09D125/04—Homopolymers or copolymers of styrene
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
- C09D5/082—Anti-corrosive paints characterised by the anti-corrosive pigment
- C09D5/084—Inorganic compounds
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/328—Phosphates of heavy metals
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Abstract
A preparation process of an organic-inorganic composite water-based acrylic anticorrosive paint relates to the technical field of production of anticorrosive paints. According to the invention, organic silicon modified acrylic resin and silica sol modified zinc phosphate are mixed, under the action of a coupling agent Coatosil MP 200, a uniform cross-linking structure is formed between organic resin and inorganic antirust pigment by virtue of the polycondensation effect of silicon hydroxyl, and by introducing methyl trimethoxy silane, octyl trimethoxy silane and phenyl trimethoxy silane into linear silica sol, the hydrogen bond interaction force on the surface of modified zinc phosphate particles is weakened, and the dispersibility of the modified zinc phosphate particles is improved.
Description
Technical Field
The invention relates to the technical field of production of anticorrosive coatings.
Background
The water-based acrylic paint has the advantages of high film-forming quality, simple preparation process and the like, so the water-based acrylic paint is widely applied to various metal anti-corrosion finish paints and medium paints. However, the film forming property of the single-component water-based acrylic resin is poor, and the particles are easy to form gaps during fusion, so that various antirust pigments are generally required to be matched, and better shielding and passivation properties are provided. The zinc phosphate is a preferred variety for replacing harmful pigments in the coating industry due to the environmental protection, no toxicity, good antirust effect and the like. However, the conventional zinc phosphate powder has an amorphous surface due to uncontrollable crystallization process, and hydrogen bonds existing between particles are easy to agglomerate, and meanwhile, the conventional zinc phosphate powder and acrylic resin lack chemical bonds to form a unified whole, so that the optimal corrosion resistance is difficult to exert.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation process of an organic-inorganic composite water-based acrylic anticorrosive paint.
The technical scheme of the invention is as follows: mixing and grinding 100 parts by mass of water-based organic silicon modified acrylic resin with the solid content of 50wt%, 5-18 parts by mass of silica sol modified zinc phosphate antirust pigment, 1-3 parts by mass of Coatosil MP 200 as a coupling agent, 0.5-2 parts by mass of PU thickener Acrysol RM-8W, 0.1-0.5 part by mass of defoaming agent, 2 parts by mass of 15wt% sodium nitrite aqueous solution and 1-4 parts by mass of alcohol ester twelve in a three-roll grinder for 2 hours, filtering with 300-mesh filter cloth, and taking the filtrate to obtain the organic-inorganic composite water-based acrylic acid anticorrosive paint.
According to the invention, the organic silicon modified acrylic resin and the silica sol modified zinc phosphate antirust pigment are mixed, and under the action of a coupling agent Coatosil MP 200, a uniform cross-linking structure is formed between the organic resin and the inorganic antirust pigment by virtue of the polycondensation effect of silicon hydroxyl, and the organic resin and the inorganic antirust pigment form a uniform composite structure.
Further, the defoaming agent is one of BYK 024, TEGO Foamex 1488 and Dow burning DC 65. The three defoaming agents are all organic silicon type defoaming agents, have the characteristics of small using amount, high defoaming efficiency and the like, and have better compatibility with organic silicon modified waterborne acrylic resin.
The water-based organic silicon modified acrylic resin is prepared by mixing 30-40 parts by mass of styrene, 30-40 parts by mass of butyl acrylate, 1-5 parts by mass of ethyl acrylate, 1-5 parts by mass of glycidyl methacrylate, 0.5-2 parts by mass of acrylic acid and 1-5 parts by mass of silane with a double bond structure, and then preparing the water-based organic silicon modified acrylic resin with the solid content of 50wt% by a seed semi-continuous emulsion polymerization method by taking 1.8 parts by mass of sodium dodecyl sulfate and 0.9 part by mass of Solvay Abex2515 as emulsifiers and 0.8 part by mass of ammonium persulfate as initiators.
Styrene is used as a hard monomer, so that good weather resistance and alkali resistance can be provided for the resin; ethyl acrylate and butyl acrylate are soft monomers, so that good flexibility can be provided for the coating; glycidyl methacrylate can be crosslinked in the film forming process to improve the swelling resistance of the coating; acrylic acid can improve the polymerization stability; the silane with double bonds can introduce reactive Si-OH on the surface of acrylic resin, on one hand, the crosslinking degree of the resin is improved, and on the other hand, the silane can be used as an anchor point for connecting organic and inorganic materials.
In addition, as more substances capable of crosslinking are introduced in the emulsion polymerization process, if the solid content is too high, the polymerization process and the later storage process are easy to generate the phenomenon of system instability, and the solid content is too low to provide enough film-forming substances for the later-formulated coating, the solid content of the selected water-based organic silicon modified acrylic resin is 50 wt%.
The silane with a double bond structure is one of vinyl trimethoxy silane, vinyl triethoxy silane and KH 570. The three types of silane have double bond structures for copolymerization with acrylate monomers and slowly hydrolysable silicon ether structures to ensure emulsion polymerization stability, and the silicon ether bonds are hydrolyzed into silanol after polymerization is completed and used as a connecting bridge between acrylic resin and silica sol modified zinc phosphate.
The preparation process of the silica sol modified zinc phosphate antirust pigment comprises the following steps:
a) mixing 100 parts by mass of absolute ethyl alcohol, 40-60 parts by mass of ethyl orthosilicate, 1-3 parts by mass of silane coupling agent KH 560, 2-5 parts by mass of methyltrimethoxysilane, 2-5 parts by mass of octyltrimethoxysilane and 2-5 parts by mass of phenyltrimethoxysilane at the temperature of 20-40 ℃ to obtain a mixed solution, adjusting the pH value of the mixed solution to 3-4 by using an inorganic acid catalyst, and aging at the temperature of 20-40 ℃ for 48 hours to obtain modified silica sol;
b) uniformly mixing 100 parts by mass of 50wt% ethanol aqueous solution, 15-25 parts by mass of zinc acetate, 1-5 parts by mass of wetting agent, 2-5 parts by mass of modified silica sol and 1-5 parts by mass of hexadecyl trimethyl ammonium bromide, adjusting the pH value to 4-5 by using 85wt% phosphoric acid, stirring and aging for 48 hours, filtering to obtain a solid phase, washing with deionized water, and drying to obtain the silica sol modified zinc phosphate antirust pigment.
According to the invention, linear silica sol is introduced to serve as a crystallization template of zinc phosphate, so that the newly generated zinc phosphate in the solution is directionally crystallized into a sheet structure under the induction of silicon hydroxyl; by grafting the hydrophobic functional group on the surface of the silica sol, the hydrogen bond interaction of the silica sol modified zinc phosphate particles is weakened, and the dispersion performance of the particles is improved.
The beneficial effects are as follows:
1. the silane coupling agent KH 560 is introduced into the linear silica sol, so that the compatibility of the silica sol-zinc phosphate composite particles in the polymer resin is improved.
2. Methyl trimethoxy silane, octyl trimethoxy silane and phenyl trimethoxy silane are introduced into the linear silica sol to weaken the interaction force of hydrogen bonds on the surfaces of the modified zinc phosphate particles and improve the dispersibility of the modified zinc phosphate particles.
3. In the crystallization process of the zinc acetate and the phosphoric acid, modified silica sol is introduced as a template, and the nascent zinc phosphate is induced to directionally crystallize on the surface of the silica sol to form a sheet structure.
4. By introducing cetyl trimethyl ammonium bromide and a wetting agent, the surface tension of water is reduced, and the wetting and the dispersion of zinc phosphate and silica sol are facilitated, so that the aim of reducing the particle size of the pigment is fulfilled.
The inorganic acid catalyst is one of nitric acid, hydrochloric acid and sulfuric acid.
The wetting agent is one of TEGO 4100, BYK 348 and Surfynol 104E.
Drawings
FIG. 1 is a SEM sectional view of a coating layer of the organic-inorganic composite water-based acrylic anticorrosive paint prepared in example 1.
Detailed Description
Firstly, preparing a water-based paint.
Example 1:
1. preparing water-based organic silicon modified acrylic resin:
30kg of styrene, 40kg of butyl acrylate, 1kg of ethyl acrylate, 5kg of glycidyl methacrylate, 0.5kg of acrylic acid and 3kg of vinyl trimethoxy silane are subjected to seed semi-continuous emulsion polymerization by taking 1.8kg of sodium dodecyl sulfate and 0.9kg of Solvay Abex2515 as emulsifiers and 0.8 kg of ammonium persulfate as an initiator to prepare the water-based organic silicon modified acrylic resin with the solid content of 50 wt%.
2. Preparation of silica sol modified zinc phosphate rust-proof pigment:
(1) mixing 100kg of absolute ethyl alcohol, 40kg of ethyl orthosilicate, 1kg of silane coupling agent KH 560, 5kg of silane coupling agent methyltrimethoxysilane, 2kg of silane coupling agent octyltrimethoxysilane and 3kg of silane coupling agent phenyltrimethoxysilane at the temperature of 20-40 ℃, then adjusting the pH value of the mixed solution to 3-4 by using sulfuric acid, and aging for 48 hours at the temperature of 20-40 ℃ to prepare the modified silica sol.
(2) And (2) adding 100kg of 50wt% ethanol aqueous solution, 15kg of zinc acetate, 5kg of TEGO 4100, 2kg of modified silica sol prepared in the step (1) and 1kg of hexadecyl trimethyl ammonium bromide into another reactor, uniformly mixing, adjusting the pH value to 4-5 by using 85wt% phosphoric acid, stirring and aging for 48 hours, filtering, washing by using deionized water, and drying to obtain the silica sol modified zinc phosphate antirust pigment.
3. Preparing an organic-inorganic composite water-based acrylic acid anticorrosive paint:
and (3) adding 100kg of the water-based organic silicon modified acrylic resin, 5kg of the silica sol modified zinc phosphate antirust pigment prepared in the step (2), 1kg of Coatosil MP 200, 0.5kg of PU thickener Acrysol RM-8W, 0.1kg of BYK 024, 2kg of sodium nitrite aqueous solution with the concentration of 15wt% and 1kg of alcohol ester twelve into a three-roll grinder, grinding for 2 hours, then filtering with 300-mesh filter cloth, and filtering to obtain the organic-inorganic composite water-based acrylic acid anticorrosive paint.
Comparative example 1:
1. preparing water-based organic silicon modified acrylic resin:
30kg of styrene, 40kg of butyl acrylate, 1kg of ethyl acrylate, 5kg of glycidyl methacrylate, 0.5kg of acrylic acid and 3kg of vinyl trimethoxy silane are used for preparing the water-based organic silicon modified acrylic resin with the solid content of 50wt% by a seed semi-continuous emulsion polymerization method by taking 1.8kg of sodium dodecyl sulfate, 0.9kg of Solvay Abex2515 as an emulsifier and 0.8 kg of ammonium persulfate as an initiator.
2. Preparing an organic-inorganic composite water-based acrylic acid anticorrosive paint:
100kg of water-based organic silicon modified acrylic resin, 5kg of commercial zinc phosphate antirust pigment, 1kg of Coatosil MP 200, 0.5kg of PU thickener Acrysol RM-8W, 0.1kg of BYK 024, 2kg of sodium nitrite aqueous solution with the concentration of 15wt% and 1kg of alcohol ester twelve are added into a three-roll grinder, the mixture is ground for 2 hours, then the mixture is filtered by 300-mesh filter cloth, and the filtrate is taken to obtain the organic-inorganic composite water-based acrylic acid anticorrosive paint.
Example 2:
1. preparing water-based organic silicon modified acrylic resin:
35kg of styrene, 35kg of butyl acrylate, 4kg of ethyl acrylate, 3kg of glycidyl methacrylate, 1.5kg of acrylic acid, 1kg of vinyltriethoxysilane, 1.8kg of sodium dodecyl sulfate and 0.9kg of Solvay Abex2515 which serve as emulsifying agents and 0.8 kg of ammonium persulfate which serve as initiating agents are subjected to a seed semi-continuous emulsion polymerization method to prepare the water-based organic silicon modified acrylic resin with the solid content of 50 wt%.
2. Preparation of silica sol modified zinc phosphate rust-proof pigment:
(1) mixing 100kg of absolute ethyl alcohol, 50kg of ethyl orthosilicate, 2kg of KH 560, 4kg of methyltrimethoxysilane, 3kg of octyltrimethoxysilane and 2kg of phenyltrimethoxysilane at the temperature of 20-40 ℃, adjusting the pH value of the mixed solution to 3-4 by using nitric acid, and aging for 48 hours at the temperature of 20-40 ℃ to obtain the modified silica sol.
(2) And (2) adding 100kg of 50wt% ethanol aqueous solution, 20kg of zinc acetate, 4kg of BYK 348, 3kg of modified silica sol prepared in the step (1) and 2kg of hexadecyl trimethyl ammonium bromide into another reactor, uniformly mixing, adjusting the pH value to 4-5 by using 85wt% phosphoric acid, stirring and aging for 48 hours, filtering, washing by using deionized water, and drying to obtain the silica sol modified zinc phosphate antirust pigment.
3. Preparing an organic-inorganic composite water-based acrylic acid anticorrosive paint:
100kg of water-based organic silicon modified acrylic resin, 10kg of silica sol modified zinc phosphate antirust pigment, 2kg of Coatosil MP 200, 1kg of PU thickening agent Acrysol RM-8W, 0.3kg of TEGO Foamex 1488, 2kg of sodium nitrite aqueous solution with the concentration of 15wt% and 3kg of alcohol ester twelve are added into a three-roll grinder, the mixture is ground for 2 hours, then filtered by 300-mesh filter cloth, and filtered liquid is taken to obtain the organic-inorganic composite water-based acrylic acid anticorrosive paint.
Example 3:
1. preparing water-based organic silicon modified acrylic resin:
40kg of styrene, 30kg of butyl acrylate, 5kg of ethyl acrylate, 1kg of glycidyl methacrylate, 2kg of acrylic acid, 5kg of KH 570, 1.8kg of sodium dodecyl sulfate and 0.9kg of Solvay Abex2515 serving as emulsifiers and 0.8 kg of ammonium persulfate serving as initiators are subjected to a seed semi-continuous emulsion polymerization method to prepare the water-based organic silicon modified acrylic resin with the solid content of 50 wt%.
2. Preparing a silica sol modified zinc phosphate antirust pigment:
(1) mixing 100kg of absolute ethyl alcohol, 60kg of ethyl orthosilicate, 3kg of KH 560, 2kg of methyltrimethoxysilane, 5kg of octyltrimethoxysilane and 5kg of phenyltrimethoxysilane at the temperature of 20-40 ℃, adjusting the pH value of the mixed solution to 3-4 by using hydrochloric acid, and aging for 48 hours at the temperature of 20-40 ℃ to obtain the modified silica sol.
(2) And (2) adding 100kg of 50wt% ethanol aqueous solution, 25kg of zinc acetate, 1kg of Surfynol 104E, 5kg of modified silica sol prepared in the step (1) and 5kg of hexadecyl trimethyl ammonium bromide into another reactor, uniformly mixing, adjusting the pH value to 4-5 by using 85wt% phosphoric acid, stirring and aging for 48 hours, filtering, washing with deionized water, and drying to obtain the silica sol modified zinc phosphate antirust pigment.
3. Preparing an organic-inorganic composite water-based acrylic acid anticorrosive paint:
100kg of water-based organic silicon modified acrylic resin, 18kg of silica sol modified zinc phosphate antirust pigment, 3kg of Coatosil MP 200, 2kg of PU thickening agent Acrysol RM-8W, 0.5kg of Dow corning DC65, 2kg of sodium nitrite aqueous solution with the concentration of 15wt% and 4kg of alcohol ester twelve are added into a three-roll grinder, the mixture is ground for 2 hours, and then filtered by 300-mesh filter cloth, and the filtered solution is taken to obtain the organic-inorganic composite water-based acrylic acid anticorrosive paint.
The coatings prepared in the above examples are uniformly sprayed on a tinplate test plate subjected to surface treatment according to GB/T9271-2008 standard, the tinplate test plate is dried for 7 days at room temperature, the thickness of the dry film is controlled to be 30-50 micrometers, performance tests are respectively carried out after edge sealing, and test results are shown in Table 1.
TABLE 1 results of sample testing
As can be seen from Table 1, the organic-inorganic composite water-based acrylic anticorrosive paint prepared by the method has better coating compactness and can provide better protective capability in humid and salt mist environments.
Claims (6)
1. The preparation process of the organic-inorganic composite water-based acrylic acid anticorrosive paint is characterized by comprising the following steps of: mixing and grinding 100 parts by mass of water-based organic silicon modified acrylic resin with the solid content of 50wt%, 5-18 parts by mass of silica sol modified zinc phosphate antirust pigment, 1-3 parts by mass of Coatosil MP 200, 0.5-2 parts by mass of PU thickener Acrysol RM-8W, 0.1-0.5 part by mass of defoaming agent, 2 parts by mass of sodium nitrite aqueous solution with the concentration of 15wt% and 1-4 parts by mass of alcohol ester twelve in a three-roll grinder for 2 hours, filtering with 300-mesh filter cloth, and taking the filtrate to obtain the organic-inorganic composite water-based acrylic acid anticorrosive paint;
the preparation method of the silica sol modified zinc phosphate antirust pigment comprises the following steps:
a) mixing 100 parts by mass of absolute ethyl alcohol, 40-60 parts by mass of ethyl orthosilicate, 1-3 parts by mass of silane coupling agent KH 560, 2-5 parts by mass of methyltrimethoxysilane, 2-5 parts by mass of octyltrimethoxysilane and 2-5 parts by mass of phenyltrimethoxysilane at the temperature of 20-40 ℃ to obtain a mixed solution, adjusting the pH value of the mixed solution to 3-4 by using an inorganic acid catalyst, and aging at the temperature of 20-40 ℃ for 48 hours to obtain modified silica sol;
b) uniformly mixing 100 parts by mass of 50wt% ethanol aqueous solution, 15-25 parts by mass of zinc acetate, 1-5 parts by mass of wetting agent, 2-5 parts by mass of modified silica sol and 1-5 parts by mass of hexadecyl trimethyl ammonium bromide, adjusting the pH value to 4-5 by using 85wt% phosphoric acid, stirring and aging for 48 hours, filtering to obtain a solid phase, washing with deionized water, and drying to obtain the silica sol modified zinc phosphate antirust pigment.
2. The process of claim 1, wherein the defoaming agent is one of BYK 024, TEGO Foamex 1488, Dow corning DC 65.
3. The process according to claim 1, wherein the aqueous organosilicon modified acrylic resin is prepared by mixing 30-40 parts by mass of styrene, 30-40 parts by mass of butyl acrylate, 1-5 parts by mass of ethyl acrylate, 1-5 parts by mass of glycidyl methacrylate, 0.5-2 parts by mass of acrylic acid and 1-5 parts by mass of silane with a double bond structure, and then carrying out a seed semi-continuous emulsion polymerization method by using 1.8 parts by mass of sodium dodecyl sulfate and 0.9 part by mass of Solvay Abex2515 as emulsifiers and 0.8 part by mass of ammonium persulfate as an initiator to obtain the aqueous organosilicon modified acrylic resin with a solid content of 50 wt%.
4. The process of claim 3, wherein the double-bond silane is one of vinyltrimethoxysilane, vinyltriethoxysilane and KH 570.
5. The process of claim 1, wherein the inorganic acid catalyst is one of nitric acid, hydrochloric acid, and sulfuric acid.
6. The process of claim 1 wherein said wetting agent is one of TEGO 4100, BYK 348, Surfynol 104E.
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| CN116554772A (en) * | 2023-06-07 | 2023-08-08 | 南京中金润恒金属科技股份有限公司 | Salt-fog-resistant metal antirust paint and preparation method thereof |
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| CN104212293B (en) * | 2014-08-27 | 2017-01-11 | 深圳市安品有机硅材料有限公司 | Waterborne acrylic acid antifogging coating and preparation method thereof |
| CN104495776B (en) * | 2014-11-28 | 2016-05-11 | 国家电网公司 | A kind of preparation method of nano-sheet trbasic zinc phosphate |
| CN104629542A (en) * | 2015-02-02 | 2015-05-20 | 芜湖市宝艺游乐科技设备有限公司 | Anti-aging polyethylene powder paint containing silica sol grafted activated meerschaum powder and preparation method thereof |
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