CN110724226B - Acrylate polymer emulsion and application thereof in preparation of silicate coating - Google Patents

Acrylate polymer emulsion and application thereof in preparation of silicate coating Download PDF

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CN110724226B
CN110724226B CN201911036323.5A CN201911036323A CN110724226B CN 110724226 B CN110724226 B CN 110724226B CN 201911036323 A CN201911036323 A CN 201911036323A CN 110724226 B CN110724226 B CN 110724226B
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silicate
polymer emulsion
acrylate
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CN110724226A (en
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陈爱民
张信
魏金晶
区英强
林杰生
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Guangdong Carpoly Science & Technology Material Co ltd
Zhejiang University of Technology ZJUT
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Guangdong Carpoly Science & Technology Material Co ltd
Zhejiang University of Technology ZJUT
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10—Esters
    • C08F220/12—Esters of monohydric alcohols or phenols
    • C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00—Processes of polymerisation
    • C08F2/12—Polymerisation in non-solvents
    • C08F2/16—Aqueous medium
    • C08F2/22—Emulsion polymerisation
    • C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
    • C08F2/26—Emulsion polymerisation with the aid of emulsifying agents anionic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00—Processes of polymerisation
    • C08F2/12—Polymerisation in non-solvents
    • C08F2/16—Aqueous medium
    • C08F2/22—Emulsion polymerisation
    • C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
    • C08F2/30—Emulsion polymerisation with the aid of emulsifying agents non-ionic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10—Esters
    • C08F220/12—Esters of monohydric alcohols or phenols
    • C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
    • C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
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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
    • C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
    • 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
    • C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
    • C09D1/02—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances alkali metal silicates
    • C09D1/04—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances alkali metal silicates with organic additives
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/65—Additives macromolecular

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Abstract

The invention discloses an acrylate polymer emulsion and application thereof in preparing silicate paint, wherein the emulsion is prepared from the following raw materials in parts by mass: 10-20% of methacrylate monomer, 10-20% of acrylate monomer, 1-3% of functional monomer, 0.1-0.3% of initiator, 0.5-1.0% of anionic emulsifier, 0.7-1.5% of nonionic emulsifier and the balance of water, wherein the total addition amount is 100%; the water absorption of the emulsion film of the dried acrylate polymer emulsion is stabilized at about 5 percent, the pyrolysis temperature is 357.40 ℃, the emulsion film is suitable for paint decoration, and the surface drying time of the film of the prepared silicate inorganic paint is less than 1 h. The silicate inorganic paint prepared by the invention has normal appearance without peculiar smell, the hardness is kept at 3H or above, the adhesive force reaches the first level, no obstacle exists when the paint is coated for two times in the construction process, and the comprehensive performance is good.

Description

Acrylate polymer emulsion and application thereof in preparation of silicate coating
(I) technical field
The invention belongs to the building coating industry, relates to an interior wall coating used for interior decoration, and particularly relates to an acrylate polymer emulsion modified general silicate inorganic coating.
(II) technical background
With the continuous development of society, the living standard of people is continuously improved, the performance is excellent, the environment is friendly, and the requirements of people on decoration articles are increased due to diversified trends of no toxicity, no harm and the like. The polyurethane coating prepared by the bear weiwei inventor in the patent of 'epoxy resin cured precoating anticorrosive coating polyurethane and preparation method thereof' has certain corrosion resistance, but has the defects of easy aging, easy combustion and the like, and has certain influence on the air quality. Meanwhile, the organic latex paint can mildew in a humid environment, and the VOC content is high. The inorganic silicate coating takes inorganic silicate as a main film forming substance, has the advantages of high temperature resistance, weather resistance, no pollution, low VOC, rich raw materials and the like, and meets the requirements of the existing market on the performance and environmental protection of the inorganic coating. However, the common inorganic paint has the defects of long coating drying time, easy cracking and the like, which not only affects the construction performance of the paint, but also has certain influence on the appearance of the paint, thereby causing inconvenience for users. The acrylate polymer emulsion has the advantages of strong water resistance, good temperature resistance, low volatility and the like, is suitable for coating decoration, can shorten the surface drying time of the coating while meeting the market demand after modifying the silicate inorganic coating, and improves the friction resistance, the thermal stability and the brushing performance.
Therefore, the invention provides a polyacrylate emulsion modified silicate water-based interior wall coating, which is simple in preparation method, has the advantages of no toxicity, low VOC content, better flame retardance, better adhesive force than pure inorganic silicate coatings, shorter surface drying time, coating film hardness of 3H or above and the like, can effectively improve the performance of the coating, is suitable for coating decoration, meets the requirement of low VOC content, and has good industrial application.
Disclosure of the invention
Aiming at the problems, the invention aims to provide an acrylate polymer emulsion, a preparation method and application thereof in preparing silicate inorganic coating, wherein the emulsion has strong water resistance, good temperature resistance and low volatility, is suitable for coating decoration, meets the requirement of low VOC content, and simultaneously improves the defects of pure inorganic coating. The silicate inorganic coating prepared by the invention is nontoxic, has low VOC content, better flame retardance, better adhesive force than pure inorganic silicate coating, shorter surface drying time, normal coating appearance and no obstacle when coated for two times in construction, has the hardness of 3H or more, is an environment-friendly and easily-decorated silicate inorganic coating, and also meets the requirements of the current market on the performance and the environment protection of the inorganic coating.
The technical scheme adopted by the invention is as follows:
the invention provides an acrylate polymer emulsion, which is prepared from the following raw materials in parts by mass: 10 to 20 percent of methacrylate monomer, 10 to 20 percent of acrylate monomer, 0.5 to 3 percent of functional monomer, 0.1 to 0.3 percent of initiator, 0.5 to 1.5 percent of anionic emulsifier, 0.5 to 1.5 percent of nonionic emulsifier and the balance of water, wherein the total feeding amount is 100 percent; the anionic emulsifier is one of special alkyl alcohol polyether sulfate ES-430S or branched alkyl alcohol polyether sulfate ES-730, preferably ES-730; the non-ionic emulsifier is one of alkyl polyglycoside or Alcohol Ether Glycoside (AEG), preferably alcohol ether glycoside; the functional monomer is one or more of acrylamide or N, N-diethylacrylamide, preferably N, N-diethylacrylamide; the initiator is one of potassium persulfate or ammonium persulfate, preferably potassium persulfate; the methacrylate monomer is one of methyl methacrylate, ethyl methacrylate, propyl methacrylate, butyl methacrylate, n-octyl methacrylate or isooctyl methacrylate, preferably methyl methacrylate; the acrylate is one of ethyl acrylate, propyl acrylate, butyl acrylate or isooctyl acrylate, and butyl acrylate is preferred.
Further, the acrylate polymer emulsion is prepared from the following raw materials in parts by mass: 10-20% of methacrylate monomer, 10-20% of acrylate monomer, 1-2.5% of functional monomer, 0.1-0.25% of initiator, 0.7-1.0% of anionic emulsifier, 0.7-1.2% of nonionic emulsifier and the balance of water, wherein the total addition amount is 100%.
More preferably, the acrylate polymer emulsion is prepared from the following raw materials in parts by mass: 13 to 15 percent of methacrylate monomer, 13 to 15 percent of acrylate monomer, 1 to 2.5 percent of functional monomer, 0.1 to 0.25 percent of initiator, 0.7 to 1.0 percent of anionic emulsifier, 0.7 to 1.2 percent of nonionic emulsifier and the balance of water, wherein the total feeding amount is 100 percent.
Most preferably, the acrylate polymer emulsion is prepared from the following raw materials in parts by mass: 13-15% of methyl methacrylate, 13-15% of butyl acrylate, 1-2.5% of N, N-diethyl acrylamide, 0.1-0.25% of potassium persulfate, 0.7-1.2% of branched alkyl alcohol polyether sulfate ES-7300.7%, 0.7-1.2% of alcohol ether glycoside and the balance of water, wherein the total feeding amount is 100%.
The invention also provides a preparation method of the acrylate polymer emulsion, which comprises the following steps: firstly, mixing an anionic emulsifier, a nonionic emulsifier and part of water according to the formula amount, stirring, heating to 70-85 ℃ in a water bath, respectively dripping 10-30% of acrylate monomer according to the formula amount, 10-30% of methacrylate monomer according to the formula amount, 10-30% of functional monomer according to the formula amount, 10-30% of initiator according to the formula amount and part of water according to the formula amount within 15min, and continuously preserving heat for 10-30min after dripping is finished; then dropwise adding the water, the initiator, the acrylate monomer, the methacrylate monomer and the functional monomer in the rest formula amount within 2.0-4.0h, heating to 90 ℃ after dropwise adding, and continuously preserving heat for 30-50 min; cooling to 40 ℃, filtering and discharging, and taking the filtrate to obtain the acrylic ester polymer emulsion.
The invention also provides an application of the acrylate polymer emulsion in preparation of silicate inorganic paint.
The invention also provides a silicate inorganic coating prepared from the acrylate polymer emulsion, which comprises the following raw materials in parts by mass: 30-45% of water, 25-40% of pigment and filler, 15-30% of inorganic silicate film-forming base material, 1-5% of acrylate polymer emulsion, 0.5-1.3% of defoaming agent, 0.5-1.3% of dispersing agent, 0.4-1.1% of flatting agent, 0.5-1.0% of thickening agent and 100% of total feeding amount; the pigment and filler is one or more of titanium dioxide, calcined kaolin, heavy calcium carbonate and talcum powder, more preferably the pigment and filler is prepared by mixing the heavy calcium carbonate, the talcum powder, the kaolin and the titanium dioxide in a mass ratio of 1:0.4-0.6:0.3-0.6:1.0-1.2, and preferably the pigment and filler is the heavy calcium carbonate, the talcum powder, the kaolin and the titanium dioxide in a mass ratio of 1: 0.4: 0.36: 1.17; the mesh number of the heavy calcium carbonate is 400-1400, the mesh number of the titanium dioxide is 300-800, the mesh number of the kaolin is 500-1500, and the mesh number of the talcum powder is 500-1500; the inorganic silicate film-forming base material is one or more of alkaline silica sol, potassium silicate and sodium silicate, and preferably the inorganic silicate film-forming base material is a mixture of organic silica sol JN-30, sodium silicate and liquid potassium silicate in a mass ratio of 1:0.1-2: 0.1-2; the modulus of potassium silicate is 2.0-4.0, and the modulus of sodium silicate is 2.0-4.0. The defoaming agent is one of mineral oil defoaming agents CK-231, CK-232 and CK-233; the dispersing agent is one of fatty acid dispersing agents CK-921 or CK-922; the leveling agent is one of organic silicon leveling agents CK-113 or CK-114, and the thickening agent is one of carboxymethyl cellulose or hydroxyethyl cellulose.
Further, the silicate inorganic coating is preferably composed of the following raw materials in parts by mass: 30 to 45 percent of water, 25 to 38 percent of pigment and filler, 15 to 27 percent of inorganic silicate film-forming base material, 1 to 4 percent of acrylate polymer emulsion, 0.5 to 1.2 percent of defoaming agent, 0.5 to 1.2 percent of dispersant, 0.4 to 1.0 percent of flatting agent, 0.5 to 1.0 percent of thickening agent and 100 percent of total feeding amount.
Furthermore, the silicate inorganic coating is preferably composed of the following raw materials in parts by mass: 40-45% of water, 25-28% of pigment and filler, 21-25% of inorganic silicate film-forming base material, 3-4% of acrylate polymer emulsion, 1.1-1.2% of defoaming agent, 1.2-1.3% of dispersing agent, 1.1-1.3% of flatting agent, 1.3-1.5% of thickening agent and 100% of total feeding amount; the pigment and filler is prepared by mixing heavy calcium carbonate, talcum powder, kaolin and titanium dioxide according to the mass ratio of 1:0.4-0.6:0.3-0.6: 1.0-1.2; the inorganic silicate film-forming base material is preferably a mixture of organic silica sol JN-30, sodium silicate and liquid potassium silicate in a mass ratio of 1:0.1-2:0.1-2, more preferably 1:0.977: 0.935; the defoaming agent is a mineral oil defoaming agent CK-231; the dispersing agent is a fatty acid dispersing agent CK-921; the leveling agent is an organic silicon leveling agent CK-113, and the thickening agent is carboxymethyl cellulose.
The preparation method of the silicate inorganic coating comprises the following steps: according to the formula amount, firstly adding water, a dispersing agent and a defoaming agent accounting for 1/2 formula amount into a stirring tank, and stirring for 5-15min at the rotation speed of 600-1500 rpm; then adding the pigment and filler, and stirring for 30-55min at the speed of 1000-; then adding inorganic silicate film-forming base material and acrylate polymer emulsion, and stirring for 15-30min at the rotating speed of 1000-2000 rpm; and finally, adding a thickening agent, a flatting agent and the remaining defoaming agent accounting for 1/2 of the formula amount, stirring for 20-50min at the rotating speed of 900-2500rpm, and discharging to obtain the modified silicate coating.
The molecular formula of the acrylate polymer emulsion is as follows:
Figure BDA0002251603040000041
a. b and c represent the molecular numbers of three monomers of methyl methacrylate, butyl acrylate and N, N-diethylacrylamide required for synthesizing the polymer emulsion respectively.
Compared with the prior art, the invention has the following beneficial effects:
the water absorption of the emulsion film of the dried acrylate polymer emulsion is stabilized at about 5 percent, the pyrolysis temperature is 357.40 ℃, the emulsion film is suitable for paint decoration, and the surface drying time of the film of the prepared silicate inorganic paint is less than 1 h.
The inorganic coating has little pollution, hardly releases volatile gases such as formaldehyde, benzene and the like, and the raw materials for producing the silicate inorganic coating have rich sources, high quality and low price.
The silicate inorganic paint prepared by the invention has normal appearance without peculiar smell, the hardness is kept at 3H or above, the adhesive force reaches the first level, no obstacle exists when the paint is coated for two times in the construction process, and the comprehensive performance is good.
(IV) description of the drawings
FIG. 1: example 1 the acrylate polymer emulsion prepared in step 1 is dried to form a film and then the infrared spectrogram is obtained.
FIG. 2: example 2 thermogravimetry of acrylic ester polymer emulsion after drying and film forming made in step 1, a is acrylic ester polymer emulsion without functional monomer modification, b is acrylic ester polymer emulsion modified by functional monomer.
FIG. 3: example 2 the contact angle of the emulsion prepared in step 1 after drying to form a film is a functional monomer-unmodified acrylate polymer emulsion and b is a functional monomer-modified acrylate polymer emulsion.
FIG. 4: coating film pattern of the silicate inorganic paint obtained in example 1.
(V) detailed description of the preferred embodiments
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto.
The branched alkyl alcohol polyether sulfate (ES-730) and the specific alkyl alcohol polyether sulfate (ES-430S) used in the examples of the present invention were obtained from Shanghai loyal Fine chemical Co., Ltd.
The defoaming agent and the leveling agent in the embodiment of the invention are purchased from Tianjin Gaitan New Material science and technology Limited.
Example 1
1. Acrylate polymer emulsion
The acrylic ester polymer emulsion comprises the following components in percentage by mass: 14.4 percent of methyl methacrylate, 14.4 percent of butyl acrylate, 1.2 percent of N, N-diethyl acrylamide, 0.21 percent of potassium persulfate, 1.2 percent of branched alkyl alcohol polyether sulfate (ES-730), 0.6 percent of Alcohol Ether Glycoside (AEG) and the balance of water, wherein the total feeding amount is 100 percent.
In a 250mL four-necked flask equipped with a reflux condenser, dropping funnel and stirrer, 0.60g of an Alcohol Ether Glycoside (AEG), 1.20g of a branched alkyl alcohol polyether sulfate (ES-730) and 38.20g of deionized water were added, stirred and warmed to 80 ℃ in a water bath. 3.0g of mixed monomer and 3.0g of potassium persulfate (KPS) aqueous solution are respectively dripped within 15min, and the temperature is kept for 15min after the dripping is finished. Then, the rest 27.0g of KPS aqueous solution and 27.0g of mixed monomer are dripped into a four-neck flask within 3.0h, after the dripping is finished, the temperature is raised to 90 ℃, and the temperature is kept for 40 min. The temperature is reduced to 40 ℃, 100g of acrylic ester polymer emulsion is prepared after filtering and discharging, and the infrared spectrum after drying and film forming is shown in figure 1.
Wherein the composition of the mixed monomer is 14.40g of butyl acrylate, 14.40g of methyl methacrylate and 1.2g of N, N-diethylacrylamide; KPS aqueous solution 0.21g potassium persulfate dissolved in 29.79g deionized water.
FIG. 1 is an infrared spectrum of an acrylate polymer emulsion, which can be seen at 2955cm-1And 2873cm-1The absorption peak at (A) is C-H (CH)3，CH2) Characteristic stretching vibration absorption. 1726cm-1Stretching vibration of C ═ O, and stretching vibration peak value of C-O-C in acrylic ester polymer latex film was 1235cm-1And 841cm-1；1142.3cm-1Is the C-H stretching vibration peak; 1449cm-1And 1385cm-1is-CH2Deformation vibration of 3433cm-1The absorption peak at (a) is due to the oscillation of the N-H bond in the amide. As can be seen, the value is 1500--1In the range of (1), there is no stretching vibration of C ═ C. Thus, all monomers were successfully copolymerized with polyacrylate as indicated by FT-IR spectroscopy.
2. Silicate inorganic paint
The silicate inorganic coating comprises the following components in percentage by mass: 42% of water, 28% of pigment and filler, 21% of inorganic silicate film-forming base stock, 4% of acrylate polymer emulsion, 1.2% of defoaming agent, 1.2% of dispersing agent, 1.3% of flatting agent and 1.3% of thickening agent; the pigment and filler is heavy calcium carbonate, talcum powder, kaolin and titanium dioxide in a mass ratio of 1: 0.4: 0.36: 1.17, mixing the inorganic silicate film-forming base material with organic silica sol JN-30, sodium silicate and liquid potassium silicate in a mass ratio of 1:0.977:0.935, wherein the defoaming agent is mineral oil defoaming agent CK-231, the dispersing agent is fatty acid dispersing agent CK-921, the leveling agent is organic silicon leveling agent CK-113, and the thickening agent is hydroxyethyl cellulose.
Adding water, a dispersing agent and a defoaming agent accounting for 1/2 formula amount into a stirring tank according to the formula amount, stirring for 10min at the rotating speed of 900rpm to mix uniformly, adding a pigment and a filler, stirring for 45min at 2000rpm to stir uniformly, adding an inorganic silicate film-forming base material and the acrylate polymer emulsion prepared in the step 1, stirring for 30min at the rotating speed of 1500rpm to stir uniformly, adding a thickening agent, a leveling agent and the remaining defoaming agent accounting for 1/2 formula amount, stirring for 30min at the rotating speed of 1500rpm, discharging to obtain 77.2g of silicate inorganic coating, and coating the coating on the tinplate, wherein the result is shown in figure 4.
Drying time of the coating: the method comprises the steps of measuring by using a finger touch method in GB/T1728-79(89), starting timing from coating on a board, lightly touching with a finger until the finger is pressed down on the board with proper force, and counting as an off-time when no finger print exists.
Coating hardness: the hardness is measured by scratching the coating film with a hard object on the surface of the paint film by a scratch hardness method of GB/T6739-86; the hardness of the pencil is commonly 13 grades from 6B to 6H, and the pencil can be manually operated and also can be tested by an instrument.
Coating adhesion force: according to a grid cutting method of GB/T9286-88, a grid with the space of 1mm is cut by a cutter in a criss-cross mode, the number of the grids is 5 multiplied by 5, and then the grids are graded according to a rating standard specified in GB/T9286-88, wherein the grade 0 is the best, the grade 5 is the worst, and specifically: the 0-level cutting edge is completely smooth, and no lattice falls off; in level 1, a little coating falls off at the intersection of the cuts, but the cross cutting area is not influenced by more than 5 percent; the coating at the intersection of the cuts and/or along the edges of the cuts falls off in the 2-stage, and the affected cross cutting area is obviously more than 5 percent but not obviously more than 15 percent; the 3-level coating partially or completely falls off in large fragments along the cutting edge and/or on the upper part or the whole of different parts of the grid, and the affected cross cutting area is obviously more than 15 percent but not more than 35 percent; the level 4 coating falls off along the cutting edge in large pieces, and/or some of the pieces fall off partially or completely, and the affected cross cutting area is obviously more than 35 percent, but not more than 65 percent; grade 5 spalled to a degree exceeding grade 4.
Paint contrast ratio (hiding ratio): the inorganic coating is uniformly coated on the surface of an object, and the capability of preventing the color of the substrate from appearing is called hiding power through the absorption, reflection and scattering of the coating to light, which is determined by GB/T1726-79 (89). With the minimum amount of coating (g/m) required to cover a unit area2) The hiding power is indicated.
Material workability: the brushing performance is detected according to the GB/T6753.6-86 standard, and the coating is easy to construct and the obtained coating can be quickly leveled without sagging, wrinkling, shrinkage, bleeding, undercut or yellowing and the like in the process of brushing until a dry coating is formed.
And (3) low-temperature stability of the material: according to the national standard of GB/T9755, a paint sample is filled into a plastic or glass container of about 1L, the container is approximately filled and sealed, the container is placed into a low-temperature box at (-5 +/-2) DEG C, the container is taken out after 18 hours, the container is placed in an environment with the standard temperature of 23 +/-2 ℃ and the relative humidity of 50% +/-5% for 6 hours, after the steps are repeated for three times, the container is opened, the sample is fully stirred, and the phenomena of hard blocks, agglomeration and separation are observed, if not, the low-temperature stability is considered to be good.
The results are shown in Table 1.
Example 2
1. Acrylate polymer emulsion
The acrylic ester polymer emulsion comprises the following components in percentage by mass: 14.25 percent of methyl methacrylate, 14.25 percent of butyl acrylate, 1.5 percent of N, N-diethyl acrylamide, 0.21 percent of potassium persulfate, 0.9 percent of branched alkyl alcohol polyether sulfate (ES-730), 0.9 percent of Alcohol Ether Glycoside (AEG) and the balance of water, wherein the total feeding amount is 100 percent.
In a 250mL four-necked flask equipped with a reflux condenser, dropping funnel and stirrer, 0.90g of an Alcohol Ether Glycoside (AEG), 0.90g of a branched alkyl alcohol polyether sulfate (ES-730) and 38.20g of deionized water were added, stirred and warmed to 80 ℃ in a water bath. 3.0g of mixed monomer and 3.0g of potassium persulfate (KPS) aqueous solution are respectively dripped in 15min, and heat preservation is continued for 15min after the dripping is finished. Then, the rest 27.0g of KPS aqueous solution and 27.0g of mixed monomer are dripped into a four-neck flask within 3.0h, after the dripping is finished, the temperature is raised to 90 ℃, and the temperature is kept for 40 min. Cooling to 40 ℃, filtering and discharging to obtain 100g of acrylic ester polymer emulsion. All monomers were successfully copolymerized with the polyacrylate as indicated by FT-IR spectroscopy.
Wherein the composition of the mixed monomer is 14.25g of butyl acrylate, 14.25g of methyl methacrylate and 1.5g of N, N-diethylacrylamide; the aqueous KPS solution was 0.21g of potassium persulfate dissolved in 29.79g of deionized water.
Under the same conditions, N-diethylacrylamide was removed and supplemented with 0.75g of butyl acrylate and 0.75g of methyl methacrylate, and 100g of an unmodified acrylate polymer emulsion was prepared as a control.
According to the thermogravimetric analysis chart of FIG. 2, the pyrolysis temperature of the acrylate polymer emulsion modified by the functional monomer is 6.37 ℃ higher than that of the unmodified acrylate polymer emulsion. The decomposition temperature of the polymer depends on the heat resistance of various groups, N-diethylacrylamide is introduced, the molecular weight is increased, the structure is complex, the main chain can be protected, and the pyrolysis temperature is increased. Meanwhile, as can be seen from fig. 3, the introduced hydrophobic side chain groups are condensed with each other in water, the contact angle of the latex film is increased by 16.4 degrees, and the hydrophobic property of the polymer is greatly improved.
2. Silicate inorganic paint
The silicate inorganic coating comprises the following components in percentage by mass: 41.50% of water, 27.50% of pigment and filler, 22.20% of inorganic silicate film-forming base material, 3.80% of acrylate polymer emulsion, 1.15% of defoaming agent, 1.25% of dispersing agent, 1.30% of flatting agent and 1.30% of thickening agent; the pigment and filler is heavy calcium carbonate, talcum powder, kaolin and titanium dioxide according to the mass ratio of 1.00: 0.45: 0.38: 1.20, mixing the inorganic silicate film-forming base material with organic silica sol JN-30, sodium silicate and liquid potassium silicate in a mass ratio of 1:0.977:0.935, wherein the defoaming agent is mineral oil defoaming agent CK-231, the dispersing agent is fatty acid dispersing agent CK-921, the leveling agent is organic silicon leveling agent CK-113, and the thickening agent is hydroxyethyl cellulose.
Adding water, a dispersing agent and a defoaming agent accounting for 1/2 formula amount into a stirring tank according to the formula amount, and stirring at the rotating speed of 1200rpm for 5min to uniformly mix the components; adding pigment and filler, and stirring at 1500rpm for 35min to uniformly stir the materials; adding inorganic silicate film-forming base material and the acrylate polymer emulsion prepared in the step 1, and stirring at the rotation speed of 1800rpm for 25min to uniformly stir the materials; and finally, adding a thickening agent, a flatting agent and the remaining defoaming agent accounting for 1/2 of the formula amount, stirring for 35min at the rotating speed of 1200rpm, and discharging to obtain 77.2g of silicate inorganic coating.
The paint properties were measured by the method of example 1 and the results are shown in Table 1.
Example 3
1. Acrylate polymer emulsion
The acrylic ester polymer emulsion comprises the following components in percentage by mass: 14.1 percent of methyl methacrylate, 14.1 percent of butyl acrylate, 1.8 percent of N, N-diethyl acrylamide, 0.21 percent of potassium persulfate, 0.6 percent of branched alkyl alcohol polyether sulfate (ES-730), 1.2 percent of Alcohol Ether Glycoside (AEG) and the balance of water, wherein the total feeding amount is 100 percent.
Adding 1.20g of Alcohol Ether Glycoside (AEG), 0.60g of branched alkyl alcohol polyether sulfate (ES-730) and 38.20g of deionized water into a 250mL four-neck flask provided with a reflux condenser tube, a dropping funnel and a stirrer, stirring and heating to 80 ℃ in a water bath; respectively dripping 3.0g of mixed monomer and 3.0g of potassium persulfate (KPS) aqueous solution within 15min, and keeping the temperature for 15min after dripping; then, the rest 27.0g of KPS aqueous solution and 27.0g of mixed monomer are dripped into a four-neck flask within 3.0h, after the dripping is finished, the temperature is raised to 90 ℃, and the temperature is kept for 40 min. Cooling to 40 ℃, filtering and discharging to obtain 100g of acrylic ester polymer emulsion. All monomers were successfully copolymerized with the polyacrylate as indicated by FT-IR spectroscopy.
Wherein the composition of the mixed monomer is 14.10g of butyl acrylate, 14.10g of methyl methacrylate and 1.8g of N, N-diethylacrylamide; the aqueous KPS solution was 0.21g of potassium persulfate dissolved in 29.79g of deionized water.
2. Silicate inorganic paint
The silicate inorganic coating comprises the following components in percentage by mass: 42.50 percent of water, 27.50 percent of pigment and filler, 21.30 percent of inorganic silicate film-forming base material, 3.70 percent of acrylate polymer emulsion, 1.10 percent of defoaming agent, 1.30 percent of dispersing agent, 1.25 percent of flatting agent and 1.35 percent of thickening agent; the pigment and filler is heavy calcium carbonate, talcum powder, kaolin and titanium dioxide according to the mass ratio of 1.00: 0.50: 0.40: 1.15, mixing the inorganic silicate film-forming base material with organic silica sol JN-30, sodium silicate and liquid potassium silicate in a mass ratio of 1:0.977:0.935, wherein the defoaming agent is mineral oil defoaming agent CK-231, the dispersing agent is fatty acid dispersing agent CK-921, the leveling agent is organic silicon leveling agent CK-113, and the thickening agent is hydroxyethyl cellulose.
According to the formula, water, a dispersing agent and a defoaming agent accounting for 1/2 are added into a stirring tank, and the mixture is stirred for 5min at the rotating speed of 1500rpm so as to be uniformly mixed. Adding the pigment filler with the formula amount, and stirring for 55min at 1000rpm to uniformly stir the materials. Adding the inorganic silicate film-forming base material and the acrylate polymer emulsion prepared in the step 1 according to the formula ratio, and stirring at the rotating speed of 1500rpm for 25min to uniformly stir the materials. Adding the thickening agent, the flatting agent and the remaining antifoaming agent accounting for 1/2 of the formula amount, stirring at 1800rpm for 35min, and discharging to obtain 77.2g of silicate inorganic coating.
The paint properties were measured by the method of example 1 and the results are shown in Table 1.
Example 4
1. Acrylate polymer emulsion
The acrylic ester polymer emulsion comprises the following components in percentage by mass: 14.55 percent of methyl methacrylate, 14.55 percent of butyl acrylate, 0.9 percent of N, N-diethyl acrylamide, 0.21 percent of potassium persulfate, 0.72 percent of branched alkyl alcohol polyether sulfate (ES-730), 1.08 percent of Alcohol Ether Glycoside (AEG) and the balance of water, wherein the total feeding amount is 100 percent.
In a 250mL four-necked flask equipped with a reflux condenser, dropping funnel and stirrer, 1.08g of an Alcohol Ether Glycoside (AEG) and 0.72g of a branched alkyl alcohol polyether sulfate (ES-730) and 38.20g of deionized water were added, stirred and warmed to 80 ℃ in a water bath. 3.0g of mixed monomer and 3.0g of potassium persulfate (KPS) aqueous solution are respectively dripped in 15min, and heat preservation is continued for 15min after the dripping is finished. Then, the rest 27.0g of KPS aqueous solution and 27.0g of mixed monomer are dripped into a four-neck flask within 3.0h, after the dripping is finished, the temperature is raised to 90 ℃, and the temperature is kept for 40 min. Cooling to 40 ℃, filtering and discharging to obtain 100g of acrylic ester polymer emulsion. All monomers were successfully copolymerized with polyacrylate as indicated by FT-IR spectroscopy.
Wherein the composition of the mixed monomer is 14.55g of butyl acrylate, 14.55g of methyl methacrylate and 0.90g of N, N-diethylacrylamide; the aqueous KPS solution was 0.21g of potassium persulfate dissolved in 29.79g of deionized water.
2. Silicate inorganic paint
The silicate inorganic coating comprises the following components in percentage by mass: 42.5 percent of water, 27.5 percent of pigment and filler, 21.50 percent of inorganic silicate film-forming base material, 3.50 percent of acrylate polymer emulsion, 1.20 percent of defoaming agent, 1.20 percent of dispersing agent, 1.20 percent of flatting agent and 1.40 percent of thickening agent; the pigment and filler is heavy calcium carbonate, talcum powder, kaolin and titanium dioxide in a mass ratio of 1: 0.50: 0.40: 1.15, mixing the inorganic silicate film-forming base material with organic silica sol JN-30, sodium silicate and liquid potassium silicate in a mass ratio of 1:0.977:0.935, wherein the defoaming agent is mineral oil defoaming agent CK-231, the dispersing agent is fatty acid dispersing agent CK-921, the leveling agent is organic silicon leveling agent CK-113, and the thickening agent is hydroxyethyl cellulose.
According to the formula amount, adding water, a dispersing agent and a defoaming agent accounting for 1/2 formula amount into a stirring tank, and stirring at 600rpm for 15min to uniformly mix. Adding pigment and filler, and stirring at 1800rpm for 45min to stir the materials uniformly. Adding inorganic silicate film-forming base material and the acrylate polymer emulsion prepared in the step 1, and stirring for 15min at the rotating speed of 2000rpm to uniformly stir the materials. Adding the thickening agent, the flatting agent and the remaining antifoaming agent accounting for 1/2 of the formula amount, stirring for 45min at the rotating speed of 1000rpm, and discharging to obtain 77.2g of silicate inorganic coating.
The paint properties were measured by the method of example 1 and the results are shown in Table 1.
Example 5
1. Acrylate polymer emulsion
The acrylic ester polymer emulsion comprises the following components in percentage by mass: 13.95 percent of methyl methacrylate, 13.95 percent of butyl acrylate, 1.2 percent of N, N-diethyl acrylamide, 0.21 percent of potassium persulfate, 1.08 percent of branched alkyl alcohol polyether sulfate (ES-730), 0.72 percent of Alcohol Ether Glycoside (AEG) and the balance of water, wherein the total feeding amount is 100 percent.
In a 250mL four-necked flask equipped with a reflux condenser, dropping funnel and stirrer, 0.72g of an Alcohol Ether Glycoside (AEG), 1.08g of a branched alkyl alcohol polyether sulfate (ES-730) and 38.20g of deionized water were added, stirred and warmed to 80 ℃ in a water bath. 3.0g of mixed monomer and 3.0g of potassium persulfate (KPS) aqueous solution are respectively dripped in 15min, and heat preservation is continued for 15min after the dripping is finished. Then, the rest 27.0g of KPS aqueous solution and 27.0g of mixed monomer are dripped into a four-neck flask within 3.0h, after the dripping is finished, the temperature is raised to 90 ℃, and the temperature is kept for 40 min. Cooling to 40 ℃, filtering and discharging to obtain 100g of acrylic ester polymer emulsion. All monomers were successfully copolymerized with the polyacrylate as indicated by FT-IR spectroscopy.
Wherein the composition of the mixed monomer is 13.95g of butyl acrylate, 13.95g of methyl methacrylate and 2.10g of N, N-diethylacrylamide; the aqueous KPS solution was 0.21g of potassium persulfate dissolved in 29.79g of deionized water.
2. Silicate inorganic paint
The silicate inorganic coating comprises the following components in percentage by mass: 42.2 percent of water, 27.8 percent of pigment and filler, 21.50 percent of inorganic silicate film-forming base material, 3.50 percent of acrylate polymer emulsion, 1.10 percent of defoaming agent, 1.30 percent of dispersing agent, 1.20 percent of flatting agent and 1.40 percent of thickening agent; the pigment and filler is heavy calcium carbonate, talcum powder, kaolin and titanium dioxide in a mass ratio of 1: 0.50: 0.40: 1.15, mixing the inorganic silicate film-forming base material with organic silica sol JN-30, sodium silicate and liquid potassium silicate in a mass ratio of 1:0.977:0.935, wherein the defoaming agent is mineral oil defoaming agent CK-231, the dispersing agent is fatty acid dispersing agent CK-921, the leveling agent is organic silicon leveling agent CK-113, and the thickening agent is hydroxyethyl cellulose.
According to the formula amount, adding water, a dispersing agent and a defoaming agent accounting for 1/2 formula amount into a stirring tank, and stirring at 600rpm for 15min to uniformly mix. Adding pigment and filler, and stirring at 1800rpm for 45min to stir the materials uniformly. Adding inorganic silicate film-forming base material and the acrylate polymer emulsion prepared in the step 1, and stirring for 15min at the rotating speed of 2000rpm to uniformly stir the materials. Adding the thickening agent, the flatting agent and the remaining antifoaming agent accounting for 1/2 of the formula amount, stirring for 45min at the rotating speed of 1000rpm, and discharging to obtain 77.2g of silicate inorganic coating.
The paint properties were measured by the method of example 1 and the results are shown in Table 1.
Example 6
1. Acrylate polymer emulsion
The acrylic ester polymer emulsion comprises the following components in percentage by mass: 14.00 percent of methyl methacrylate, 14.00 percent of butyl acrylate, 2.00 percent of N, N-diethyl acrylamide, 0.21 percent of potassium persulfate, 1.0 percent of branched alkyl alcohol polyether sulfate (ES-730), 0.8 percent of Alcohol Ether Glycoside (AEG) and the balance of water, wherein the total feeding amount is 100 percent.
In a 250mL four-necked flask equipped with a reflux condenser, a dropping funnel and a stirrer, 0.80g of an Alcohol Ether Glycoside (AEG), 1.00g of a branched alkyl alcohol polyether sulfate (ES-730) and 38.20g of deionized water were charged, stirred and warmed to 80 ℃ in a water bath. 3.0g of mixed monomer and 3.0g of potassium persulfate (KPS) aqueous solution are respectively dripped in 15min, and heat preservation is continued for 15min after the dripping is finished. Then, the rest 27.0g of KPS aqueous solution and 27.0g of mixed monomer are dripped into a four-neck flask within 3.0h, after the dripping is finished, the temperature is raised to 90 ℃, and the temperature is kept for 40 min. Cooling to 40 ℃, filtering and discharging to obtain 100g of acrylic ester polymer emulsion. All monomers were successfully copolymerized with the polyacrylate as indicated by FT-IR spectroscopy.
Wherein the composition of the mixed monomer is 14.00g of butyl acrylate, 14.00g of methyl methacrylate and 2.00g of N, N-diethylacrylamide; the aqueous KPS solution was 0.21g of potassium persulfate dissolved in 29.79g of deionized water.
2. Silicate inorganic paint
The silicate inorganic coating comprises the following components in percentage by mass: 42.4 percent of water, 27.6 percent of pigment and filler, 21.80 percent of inorganic silicate film-forming base material, 3.20 percent of acrylate polymer emulsion, 1.10 percent of defoaming agent, 1.30 percent of dispersing agent, 1.20 percent of flatting agent and 1.40 percent of thickening agent; the pigment and filler is heavy calcium carbonate, talcum powder, kaolin and titanium dioxide in a mass ratio of 1: 0.52: 0.42: 1.10, mixing the inorganic silicate film-forming base material with organic silica sol JN-30, sodium silicate and liquid potassium silicate in a mass ratio of 1:0.977:0.935, wherein the defoaming agent is mineral oil defoaming agent CK-231, the dispersing agent is fatty acid dispersing agent CK-921, the leveling agent is organic silicon leveling agent CK-113, and the thickening agent is hydroxyethyl cellulose.
According to the formula amount, adding water, a dispersing agent and a defoaming agent accounting for 1/2 formula amount into a stirring tank, and stirring at 700rpm for 15min to uniformly mix. Adding pigment and filler, and stirring at 1700rpm for 45min to stir the materials uniformly. Adding inorganic silicate film-forming base material and the acrylate polymer emulsion prepared in the step 1, and stirring at the rotating speed of 1500rpm for 15min to uniformly stir the materials. Adding the thickening agent, the flatting agent and the remaining antifoaming agent accounting for 1/2 of the formula amount, stirring for 45min at the rotating speed of 1200rpm, and discharging to obtain 77.2g of silicate paint.
The paint properties were measured by the method of example 1 and the results are shown in Table 2.
Example 7
1. Acrylate polymer emulsion
The acrylic ester polymer emulsion comprises the following components in percentage by mass: 14.2 percent of methyl methacrylate, 14.2 percent of butyl acrylate, 1.6 percent of N, N-diethyl acrylamide, 0.21 percent of potassium persulfate, 0.9 percent of branched alkyl alcohol polyether sulfate (ES-730), 0.9 percent of Alcohol Ether Glycoside (AEG) and the balance of water, wherein the total feeding amount is 100 percent.
In a 250mL four-necked flask equipped with a reflux condenser, dropping funnel and stirrer, 0.90g of an Alcohol Ether Glycoside (AEG), 0.90g of a branched alkyl alcohol polyether sulfate (ES-730) and 38.20g of deionized water were added, stirred and warmed to 80 ℃ in a water bath. 3.0g of mixed monomer and 3.0g of potassium persulfate (KPS) aqueous solution are respectively dripped in 15min, and heat preservation is continued for 15min after the dripping is finished. Then, the rest 27.0g of KPS aqueous solution and 27.0g of mixed monomer are dripped into a four-neck flask within 3.0h, after the dripping is finished, the temperature is raised to 90 ℃, and the temperature is kept for 40 min. Cooling to 40 ℃, filtering and discharging to obtain 100g of acrylic ester polymer emulsion. All monomers were successfully copolymerized with the polyacrylate as indicated by FT-IR spectroscopy.
Wherein the composition of the mixed monomer is 14.20g of butyl acrylate, 14.20g of methyl methacrylate and 1.60g of N, N-diethylacrylamide; the aqueous KPS solution was 0.21g of potassium persulfate dissolved in 29.79g of deionized water.
2. Silicate inorganic paint
The silicate inorganic coating comprises the following components in percentage by mass: 42.6 percent of water, 27.4 percent of pigment and filler, 21.70 percent of inorganic silicate film-forming base material, 3.30 percent of acrylate polymer emulsion, 1.20 percent of defoaming agent, 1.20 percent of dispersing agent, 1.10 percent of flatting agent and 1.50 percent of thickening agent; the pigment and filler is heavy calcium carbonate, talcum powder, kaolin and titanium dioxide in a mass ratio of 1: 0.52: 0.42: 1.10, mixing the inorganic silicate film-forming base material with organic silica sol JN-30, sodium silicate and liquid potassium silicate in a mass ratio of 1:0.977:0.935, wherein the defoaming agent is mineral oil defoaming agent CK-231, the dispersing agent is fatty acid dispersing agent CK-921, the leveling agent is organic silicon leveling agent CK-113, and the thickening agent is hydroxyethyl cellulose.
According to the formula amount, adding water, a dispersing agent and a defoaming agent accounting for 1/2 formula amount into a stirring tank, and stirring at the rotating speed of 800rpm for 15min to uniformly mix. Adding the pigment and filler, and stirring at 1600rpm for 45min to stir the materials uniformly. Adding the inorganic silicate film-forming base material and the acrylate polymer emulsion prepared in the step 1, and stirring for 15min at the rotating speed of 1400rpm to uniformly stir the materials. Adding the thickening agent, the flatting agent and the remaining antifoaming agent accounting for 1/2 of the formula amount, stirring for 45min at the rotating speed of 1300rpm, and discharging to obtain 77.2g of silicate inorganic coating.
The paint properties were measured by the method of example 1 and the results are shown in Table 2.
Example 8
1. Acrylate polymer emulsion
The acrylic ester polymer emulsion comprises the following components in percentage by mass: 14.3 percent of methyl methacrylate, 14.3 percent of butyl acrylate, 1.4 percent of N, N-diethyl acrylamide, 0.21 percent of potassium persulfate, 0.8 percent of branched alkyl alcohol polyether sulfate (ES-730), 1.0 percent of Alcohol Ether Glycoside (AEG) and the balance of water, wherein the total feeding amount is 100 percent.
In a 250mL four-necked flask equipped with a reflux condenser, a dropping funnel and a stirrer, 1.00g of an Alcohol Ether Glycoside (AEG), 0.80g of a branched alkyl alcohol polyether sulfate (ES-730) and 38.20g of deionized water were charged, stirred and warmed to 80 ℃ in a water bath. 3.0g of mixed monomer and 3.0g of potassium persulfate (KPS) aqueous solution are respectively dripped in 15min, and heat preservation is continued for 15min after the dripping is finished. Then, the rest 27.0g of KPS aqueous solution and 27.0g of mixed monomer are dripped into a four-neck flask within 3.0h, after the dripping is finished, the temperature is raised to 90 ℃, and the temperature is kept for 40 min. Cooling to 40 ℃, filtering and discharging to obtain 100g of acrylic ester polymer emulsion. All monomers were successfully copolymerized with polyacrylate as indicated by FT-IR spectroscopy.
Wherein the composition of the mixed monomer is 14.30g of butyl acrylate, 14.30g of methyl methacrylate and 1.40g of N, N-diethylacrylamide; the aqueous KPS solution was 0.21g of potassium persulfate dissolved in 29.79g of deionized water.
2. Silicate inorganic paint
The silicate inorganic coating comprises the following components in percentage by mass: 42.9 percent of water, 27.1 percent of pigment and filler, 21.80 percent of inorganic silicate film-forming base material, 3.20 percent of acrylate polymer emulsion, 1.10 percent of defoaming agent, 1.30 percent of dispersing agent, 1.20 percent of flatting agent and 1.40 percent of thickening agent; the pigment and filler is heavy calcium carbonate, talcum powder, kaolin and titanium dioxide in a mass ratio of 1: 0.52: 0.42: 1.10, mixing the inorganic silicate film-forming base material with organic silica sol JN-30, sodium silicate and liquid potassium silicate in a mass ratio of 1:0.977:0.935, wherein the defoaming agent is mineral oil defoaming agent CK-231, the dispersing agent is fatty acid dispersing agent CK-921, the leveling agent is organic silicon leveling agent CK-113, and the thickening agent is hydroxyethyl cellulose.
According to the formula amount, adding water, a dispersing agent and a defoaming agent accounting for 1/2 formula amount into a stirring tank, and stirring at 900rpm for 15min to uniformly mix. Adding pigment and filler, and stirring at 1400rpm for 45min to stir the materials uniformly. Adding inorganic silicate film-forming base material and the acrylate polymer emulsion prepared in the step 1, and stirring for 15min at the rotating speed of 1200rpm to uniformly stir the materials. Adding the thickening agent, the flatting agent and the remaining antifoaming agent accounting for 1/2 of the formula amount, stirring for 45min at the rotating speed of 1200rpm, and discharging to obtain 77.2g of silicate inorganic coating.
The paint properties were measured by the method of example 1 and the results are shown in Table 2.
Example 9
1. Acrylate polymer emulsion
The acrylic ester polymer emulsion comprises the following components in percentage by mass: 13.9 percent of methyl methacrylate, 13.9 percent of butyl acrylate, 2.2 percent of N, N-diethyl acrylamide, 0.21 percent of potassium persulfate, 0.7 percent of branched alkyl alcohol polyether sulfate (ES-730), 1.1 percent of Alcohol Ether Glycoside (AEG) and the balance of water, wherein the total feeding amount is 100 percent.
In a 250mL four-necked flask equipped with a reflux condenser, dropping funnel and stirrer, 1.10g of an Alcohol Ether Glycoside (AEG) and 0.70g of a branched alkyl alcohol polyether sulfate (ES-730) and 38.20g of deionized water were added, stirred and warmed to 80 ℃ in a water bath. 3.0g of mixed monomer and 3.0g of potassium persulfate (KPS) aqueous solution are respectively dripped in 15min, and heat preservation is continued for 15min after the dripping is finished. Then, the rest 27.0g of KPS aqueous solution and 27.0g of mixed monomer are dripped into a four-neck flask within 3.0h, after the dripping is finished, the temperature is raised to 90 ℃, and the temperature is kept for 40 min. Cooling to 40 ℃, filtering and discharging to obtain 100g of acrylic ester polymer emulsion. All monomers were successfully copolymerized with the polyacrylate as indicated by FT-IR spectroscopy.
Wherein the composition of the mixed monomer is 13.90g of butyl acrylate, 13.90g of methyl methacrylate and 2.20g of N, N-diethylacrylamide; the aqueous KPS solution was 0.21g of potassium persulfate dissolved in 29.79g of deionized water.
2. Silicate inorganic paint
The silicate inorganic coating comprises the following components in percentage by mass: 43.0 percent of water, 27.0 percent of pigment and filler, 21.90 percent of inorganic silicate film-forming binder, 3.10 percent of acrylate polymer emulsion, 1.15 percent of defoaming agent, 1.25 percent of dispersant, 1.25 percent of flatting agent and 1.35 percent of thickening agent; the pigment and filler is heavy calcium carbonate, talcum powder, kaolin and titanium dioxide in a mass ratio of 1: 0.52: 0.42: 1.10, mixing the inorganic silicate film-forming base material with organic silica sol JN-30, sodium silicate and liquid potassium silicate in a mass ratio of 1:0.977:0.935, wherein the defoaming agent is mineral oil defoaming agent CK-231, the dispersing agent is fatty acid dispersing agent CK-921, the leveling agent is organic silicon leveling agent CK-113, and the thickening agent is hydroxyethyl cellulose.
According to the formula amount, adding water, a dispersing agent and a defoaming agent accounting for 1/2 formula amount into a stirring tank, stirring for 15min at the rotating speed of 1000rpm to uniformly mix, adding a pigment and a filler, and stirring for 45min at 1200rpm to uniformly stir materials. Adding inorganic silicate film-forming base material and the acrylate polymer emulsion prepared in the step 1, and stirring for 15min at the rotating speed of 1100rpm to uniformly stir the materials. Adding the thickening agent, the flatting agent and the remaining antifoaming agent accounting for 1/2 of the formula amount, stirring for 45min at the rotating speed of 1100rpm, and discharging to obtain 77.2g of silicate inorganic coating.
The paint properties were measured by the method of example 1 and the results are shown in Table 2.
Comparative example 1: acrylate-free polymer emulsions
1. Silicate inorganic paint
The silicate inorganic coating formula comprises: 43.0 percent of water, 27.0 percent of pigment and filler, 25.0 percent of inorganic silicate film-forming base material, 1.15 percent of defoaming agent, 1.25 percent of dispersing agent, 1.25 percent of flatting agent and 1.35 percent of thickening agent; the pigment and filler is heavy calcium carbonate, talcum powder, kaolin and titanium dioxide in a mass ratio of 1: 0.52: 0.42: 1.10, mixing the inorganic silicate film-forming base material with organic silica sol JN-30, sodium silicate and liquid potassium silicate in a mass ratio of 1:0.977:0.935, wherein the defoaming agent is mineral oil CK-231, the dispersing agent is fatty acid CK-921, the leveling agent is organic silicon CK-113, and the thickening agent is hydroxyethyl cellulose.
According to the formula amount, adding water, a dispersing agent and a defoaming agent accounting for 1/2 formula amount into a stirring tank, stirring for 15min at the rotating speed of 1000rpm to uniformly mix, adding a pigment and a filler, and stirring for 45min at 1200rpm to uniformly stir materials. Adding inorganic silicate film-forming base material, stirring at 1100rpm for 15min to stir the materials uniformly. Adding the thickening agent, the flatting agent and the remaining antifoaming agent accounting for 1/2 of the formula amount, stirring for 45min at the rotating speed of 1100rpm, and discharging to obtain 77.2g of silicate inorganic coating.
The coating properties were measured by the method of example 1 and the results are shown in Table 3.
Example 10: acrylamide as functional monomer
1. Acrylate polymer emulsion
The acrylic ester polymer emulsion comprises the following components in percentage by mass: 13.85% of methyl methacrylate, 13.85% of butyl acrylate, 2.3% of acrylamide, 0.21% of potassium persulfate, 0.7% of branched alkyl alcohol polyether sulfate (ES-730), 1.1% of Alcohol Ether Glycoside (AEG) and the balance of water, wherein the total feeding amount is 100%.
In a 250mL four-necked flask equipped with a reflux condenser, dropping funnel and stirrer, 1.10g of an Alcohol Ether Glycoside (AEG) and 0.70g of a branched alkyl alcohol polyether sulfate (ES-730) and 38.20g of deionized water were added, stirred and warmed to 80 ℃ in a water bath. 3.0g of mixed monomer and 3.0g of potassium persulfate (KPS) aqueous solution are respectively dripped in 15min, and heat preservation is continued for 15min after the dripping is finished. Then, the rest 27.0g of KPS aqueous solution and 27.0g of mixed monomer are dripped into a four-neck flask within 3.0h, after the dripping is finished, the temperature is raised to 90 ℃, and the temperature is kept for 40 min. Cooling to 40 ℃, filtering and discharging to obtain 100g of acrylic ester polymer emulsion. All monomers were successfully copolymerized with the polyacrylate as indicated by FT-IR spectroscopy.
Wherein the composition of the mixed monomer is 13.85g of butyl acrylate, 13.85g of methyl methacrylate and 2.30g of acrylamide; the aqueous KPS solution was 0.21g of potassium persulfate dissolved in 29.79g of deionized water.
2. Silicate inorganic paint
The silicate inorganic coating formula comprises: 43.0 percent of water, 27.0 percent of pigment and filler, 21.90 percent of inorganic silicate film-forming base material, 3.10 percent of acrylate polymer emulsion, 1.15 percent of defoaming agent, 1.25 percent of dispersing agent, 1.25 percent of flatting agent and 1.35 percent of thickening agent; the pigment and filler is heavy calcium carbonate, talcum powder, kaolin and titanium dioxide in a mass ratio of 1: 0.52: 0.42: 1.10, mixing the inorganic silicate film-forming base material with organic silica sol JN-30, sodium silicate and liquid potassium silicate in a mass ratio of 1:0.977:0.935, wherein the defoaming agent is mineral oil CK-231, the dispersing agent is fatty acid CK-921, the leveling agent is organic silicon CK-113, and the thickening agent is hydroxyethyl cellulose.
According to the formula amount, adding water, a dispersing agent and a defoaming agent accounting for 1/2 formula amount into a stirring tank, stirring for 15min at the rotating speed of 1000rpm to uniformly mix, adding a pigment and a filler, and stirring for 45min at 1200rpm to uniformly stir materials. Adding inorganic silicate film-forming base material and the acrylate polymer emulsion prepared in the step 1, and stirring for 15min at the rotating speed of 1100rpm to uniformly stir the materials. Adding the thickening agent, the flatting agent and the remaining antifoaming agent accounting for 1/2 of the formula amount, stirring for 45min at the rotating speed of 1100rpm, and discharging to obtain 77.2g of silicate inorganic coating.
The coating properties were measured by the method of example 1 and the results are shown in Table 3.
Example 11: acrylamide as functional monomer
1. Acrylate polymer emulsion
The acrylic ester polymer emulsion comprises the following components in percentage by mass: 14.1 percent of methyl methacrylate, 14.1 percent of butyl acrylate, 1.8 percent of acrylamide, 0.21 percent of potassium persulfate, 0.6 percent of branched alkyl alcohol polyether sulfate (ES-730), 12 percent of Alcohol Ether Glycoside (AEG) and the balance of water, wherein the total feeding amount is 100 percent.
Adding 1.20g of Alcohol Ether Glycoside (AEG), 0.60g of branched alkyl alcohol polyether sulfate (ES-730) and 38.20g of deionized water into a 250mL four-neck flask provided with a reflux condenser tube, a dropping funnel and a stirrer, stirring and heating to 80 ℃ in a water bath; respectively dripping 3.0g of mixed monomer and 3.0g of potassium persulfate (KPS) aqueous solution within 15min, and keeping the temperature for 15min after dripping; then, the rest 27.0g of KPS aqueous solution and 27.0g of mixed monomer are dripped into a four-neck flask within 3.0h, after the dripping is finished, the temperature is raised to 90 ℃, and the temperature is kept for 40 min. Cooling to 40 ℃, filtering and discharging to obtain 100g of acrylic ester polymer emulsion. All monomers were successfully copolymerized with the polyacrylate as indicated by FT-IR spectroscopy.
Wherein the composition of the mixed monomer is 14.10g of butyl acrylate, 14.10g of methyl methacrylate and 1.8g of acrylamide; the aqueous KPS solution was 0.21g of potassium persulfate dissolved in 29.79g of deionized water.
3. Silicate inorganic paint
The silicate inorganic coating formula comprises: 42.50 percent of water, 27.50 percent of pigment and filler, 21.30 percent of inorganic silicate film-forming base material, 3.70 percent of acrylate polymer emulsion, 1.10 percent of defoaming agent, 1.30 percent of dispersing agent, 1.25 percent of flatting agent and 1.35 percent of thickening agent; the pigment and filler is heavy calcium carbonate, talcum powder, kaolin and titanium dioxide according to the mass ratio of 1.00: 0.50: 0.40: 1.15, the inorganic silicate film-forming base material is a mixture of organic silica sol JN-30, sodium silicate and liquid potassium silicate in a mass ratio of 1:0.977:0.935, the defoaming agent is mineral oil CK-231, the dispersing agent is fatty acid CK-921, the leveling agent is organic silicon CK-113, and the thickening agent is hydroxyethyl cellulose.
According to the formula, water, a dispersing agent and a defoaming agent accounting for 1/2 are added into a stirring tank and stirred for 5min at the rotating speed of 1500rpm, so that the components are uniformly mixed. Adding the pigment filler according to the formula amount, and stirring for 55min at 1000rpm to uniformly stir the materials. Adding the inorganic film-forming base material and the acrylate polymer emulsion prepared in the step 1 according to the formula ratio, and stirring at the rotating speed of 1500rpm for 25min to uniformly stir the materials. Adding the thickening agent, the flatting agent and the remaining antifoaming agent accounting for 1/2 of the formula amount, stirring at 1800rpm for 35min, and discharging to obtain 77.2g of silicate inorganic coating.
The coating properties were measured by the method of example 1 and the results are shown in Table 3.
Example 12 alkyl polyglycoside as non-ionic emulsifier
1. Acrylate polymer emulsion
The acrylic ester polymer emulsion comprises the following components in percentage by mass: 14.1 percent of methyl methacrylate, 14.1 percent of butyl acrylate, 1.8 percent of N, N-diethyl acrylamide, 0.21 percent of potassium persulfate, 0.6 percent of branched alkyl alcohol polyether sulfate (ES-730), 1.2 percent of Alkyl Polyglycoside (APG) and the balance of water, wherein the total feeding amount is 100 percent.
1.20g of Alkyl Polyglycoside (APG), 0.60g of branched alkyl alcohol polyether sulfate (ES-730) and 38.20g of deionized water are added into a 250mL four-neck flask provided with a reflux condenser tube, a dropping funnel and a stirrer, stirred and heated to 80 ℃ in a water bath; respectively dripping 3.0g of mixed monomer and 3.0g of potassium persulfate (KPS) aqueous solution within 15min, and keeping the temperature for 15min after dripping; then, the rest 27.0g of KPS aqueous solution and 27.0g of mixed monomer are dripped into a four-neck flask within 3.0h, after the dripping is finished, the temperature is raised to 90 ℃, and the temperature is kept for 40 min. Cooling to 40 ℃, filtering and discharging to obtain 100g of acrylic ester polymer emulsion. All monomers were successfully copolymerized with the polyacrylate as indicated by FT-IR spectroscopy.
Wherein the composition of the mixed monomer is 14.10g of butyl acrylate, 14.10g of methyl methacrylate and 1.8g of N, N-diethylacrylamide; the aqueous KPS solution was 0.21g of potassium persulfate dissolved in 29.79g of deionized water.
4. Silicate inorganic paint
The silicate inorganic coating formula comprises: 42.50 percent of water, 27.50 percent of pigment and filler, 21.30 percent of inorganic silicate film-forming base material, 3.70 percent of acrylate polymer emulsion, 1.10 percent of defoaming agent, 1.30 percent of dispersing agent, 1.25 percent of flatting agent and 1.35 percent of thickening agent; the pigment and filler is heavy calcium carbonate, talcum powder, kaolin and titanium dioxide according to the mass ratio of 1.00: 0.50: 0.40: 1.15, the inorganic silicate film-forming base material is a mixture of organic silica sol JN-30, sodium silicate and liquid potassium silicate in a mass ratio of 1:0.977:0.935, the defoaming agent is mineral oil CK-231, the dispersing agent is fatty acid CK-921, the leveling agent is organic silicon CK-113, and the thickening agent is hydroxyethyl cellulose.
According to the formula, water, a dispersing agent and a defoaming agent accounting for 1/2 are added into a stirring tank, and the mixture is stirred for 5min at the rotating speed of 1500rpm so as to be uniformly mixed. Adding the pigment filler with the formula amount, and stirring for 55min at 1000rpm to uniformly stir the materials. Adding the inorganic film-forming base material and the acrylate polymer emulsion prepared in the step 1 according to the formula ratio, and stirring at the rotating speed of 1500rpm for 25min to uniformly stir the materials. Adding the thickening agent, the flatting agent and the remaining antifoaming agent accounting for 1/2 of the formula amount, stirring at 1800rpm for 35min, and discharging to obtain 77.2g of silicate inorganic coating.
The coating properties were measured by the method of example 1 and the results are shown in Table 3.
Example 13
1. Acrylate polymer emulsion
The acrylic ester polymer emulsion comprises the following components in percentage by mass: 13.95% of methyl methacrylate, 13.95% of butyl acrylate, 2.1% of acrylamide, 0.21% of Ammonium Persulfate (APS), 1.08% of branched alkyl alcohol polyether sulfate (ES-730), 0.72% of Alcohol Ether Glycoside (AEG) and the balance of water, wherein the total feeding amount is 100%.
In a 250mL four-necked flask equipped with a reflux condenser, dropping funnel and stirrer, 0.72g of an Alcohol Ether Glycoside (AEG), 1.08g of a branched alkyl alcohol polyether sulfate (ES-730) and 38.20g of deionized water were added, stirred and warmed to 80 ℃ in a water bath. 3.0g of mixed monomer and 3.0g of Ammonium Persulfate (APS) aqueous solution are respectively dripped in 15min, and heat preservation is continued for 15min after the dripping is finished. Then, the remaining 27.0g of APS aqueous solution and 27.0g of mixed monomer were added dropwise to the four-necked flask over 3.0 hours, and after the addition was completed, the temperature was raised to 90 ℃ and the temperature was kept for 40 min. Cooling to 40 ℃, filtering and discharging to obtain 100g of acrylic ester polymer emulsion. All monomers were successfully copolymerized with the polyacrylate as indicated by FT-IR spectroscopy.
Wherein the composition of the mixed monomer is 13.95g of butyl acrylate, 13.95g of methyl methacrylate and 2.10g of acrylamide; an aqueous solution of APS, 0.21g of Ammonium Persulfate (APS), was dissolved in 29.79g of deionized water.
2. Silicate inorganic paint
The silicate inorganic coating formula comprises: 42.2 percent of water, 27.8 percent of pigment and filler, 21.50 percent of inorganic silicate film-forming base material, 3.50 percent of acrylate polymer emulsion, 1.10 percent of defoaming agent, 1.30 percent of dispersing agent, 1.20 percent of flatting agent and 1.40 percent of thickening agent; the pigment and filler is heavy calcium carbonate, talcum powder, kaolin and titanium dioxide in a mass ratio of 1: 0.50: 0.40: 1.15, the inorganic silicate film-forming base material is a mixture of organic silica sol JN-30, sodium silicate and liquid potassium silicate in a mass ratio of 1:0.977:0.935, the defoaming agent is mineral oil CK-231, the dispersing agent is fatty acid CK-921, the leveling agent is organic silicon CK-113, and the thickening agent is hydroxyethyl cellulose.
According to the formula amount, adding water, a dispersing agent and a defoaming agent accounting for 1/2 formula amount into a stirring tank, and stirring at 600rpm for 15min to uniformly mix. Adding pigment and filler, and stirring at 1800rpm for 45min to stir the materials uniformly. Adding inorganic silicate film-forming base material and the acrylate polymer emulsion prepared in the step 1, and stirring for 15min at the rotating speed of 2000rpm to uniformly stir the materials. Adding the thickening agent, the flatting agent and the remaining antifoaming agent accounting for 1/2 of the formula amount, stirring for 45min at the rotating speed of 1000rpm, and discharging to obtain 77.2g of silicate inorganic coating.
The coating properties were measured by the method of example 1 and the results are shown in Table 3.
The following table shows the data of the coatings prepared in examples 1 to 9, and according to the data, the inorganic water-based coatings prepared by a system of a proper amount of N, N-diethylacrylamide modified acrylate emulsion and inorganic silicate have better performance.
TABLE 1 Properties of the coatings prepared in examples 1-5
Figure BDA0002251603040000201
TABLE 2 Properties of the coatings prepared in examples 6-9
Figure BDA0002251603040000202
TABLE 3 Properties of the coatings prepared in comparative example 1 and examples 10-13
Figure BDA0002251603040000211
Tables 1-3 show that, when the emulsion is not added, the paint prepared by directly using the inorganic silicate is obviously lower than an organic-inorganic compound system in both adhesive force and hardness, the surface drying time is slightly higher, and the low-temperature stability is poor;
in examples 10 and 11, the functional monomer acrylamide is used to replace N, N-dimethylacrylamide to prepare the acrylate emulsion, and the prepared inorganic silicate coating has lower adhesion and hardness than N, N-dimethylacrylamide, and meets the requirements of low-temperature stability and surface drying time.
Example 12 the acrylate emulsion was prepared by using the nonionic emulsifier Alkyl Polyglycoside (APG) instead of the alcohol ether glycoside, and the prepared inorganic silicate paint had a slightly lower hardness, a lower adhesion, no obstacle at the second pass of painting, and a good low temperature stability.
Example 13 the use of Ammonium Persulfate (APS) instead of the initiator potassium persulfate to prepare the acrylate emulsion resulted in a final formulated inorganic silicate coating with overall better performance, adhesion and hardness slightly lower than the use of potassium persulfate.

Claims (8)

1. The silicate inorganic coating prepared from the acrylate polymer emulsion is characterized by comprising the following raw materials in parts by mass: 30-45% of water, 25-40% of pigment and filler, 15-30% of inorganic silicate film-forming base material, 1-5% of acrylate polymer emulsion, 0.5-1.3% of defoaming agent, 0.5-1.3% of dispersing agent, 0.4-1.25% of flatting agent, 0.5-1.4% of thickening agent and 100% of total feeding amount; the pigment and filler is one or more of titanium dioxide, calcined kaolin, heavy calcium carbonate and talcum powder; the inorganic silicate film-forming base material is one or more of alkaline silica sol, potassium silicate and sodium silicate; the defoaming agent is one of a mineral oil defoaming agent CK-231, a mineral oil defoaming agent CK-232 and a mineral oil defoaming agent CK-233; the dispersing agent is one of fatty acid dispersing agent CK-921 or fatty acid dispersing agent CK-922; the leveling agent is one of an organic silicon leveling agent CK-113 or an organic silicon leveling agent CK-114, and the thickening agent is one of carboxymethyl cellulose or hydroxyethyl cellulose;
the acrylic ester polymer emulsion is prepared from the following raw materials in parts by mass: 10 to 20 percent of methacrylate monomer, 10 to 20 percent of acrylate monomer, 0.5 to 3 percent of functional monomer, 0.1 to 0.5 percent of initiator, 0.5 to 1.5 percent of anionic emulsifier, 0.7 to 1.5 percent of nonionic emulsifier and the balance of water, wherein the total feeding amount is 100 percent; the anionic emulsifier is one of alkyl alcohol polyether sulfate ES-430S or branched alkyl alcohol polyether sulfate ES-730; the non-ionic emulsifier is alcohol ether glucoside; the functional monomer is N, N-diethyl acrylamide; the initiator is one of potassium persulfate or ammonium persulfate; the methacrylate monomer is one of methyl methacrylate, ethyl methacrylate, propyl methacrylate, butyl methacrylate, n-octyl methacrylate or isooctyl methacrylate; the acrylate monomer is one of ethyl acrylate, propyl acrylate, butyl acrylate or isooctyl acrylate.
2. The silicate inorganic paint as claimed in claim 1, wherein the acrylate polymer emulsion is prepared from the following raw materials in percentage by mass: 10-20% of methacrylate monomer, 10-20% of acrylate monomer, 1-2.5% of functional monomer, 0.1-0.25% of initiator, 0.7-1.0% of anionic emulsifier, 0.7-1.2% of nonionic emulsifier and the balance of water, wherein the total addition amount is 100%.
3. The silicate inorganic paint as claimed in claim 1, wherein the acrylate polymer emulsion is prepared from the following raw materials in percentage by mass: 13-15% of methyl methacrylate, 13-15% of butyl acrylate, 1-2.5% of N, N-diethyl acrylamide, 0.1-0.25% of potassium persulfate, 0.7-1.2% of alkyl alcohol polyether sulfate ES-7300.7%, 0.7-1.2% of alcohol ether glycoside and the balance of water, wherein the total feeding amount is 100%.
4. The silicate inorganic paint according to claim 1, wherein the acrylate polymer emulsion is prepared by the following steps: firstly, mixing an anionic emulsifier, a nonionic emulsifier and part of water according to the formula amount, stirring, heating to 70-85 ℃ in a water bath, respectively dripping 10-30% of acrylate monomer according to the formula amount, 10-30% of methacrylate monomer according to the formula amount, 10-30% of functional monomer according to the formula amount, 10-30% of initiator according to the formula amount and part of water according to the formula amount within 15min, and continuously preserving heat for 10-30min after dripping is finished; then dropwise adding the water, the initiator, the acrylate monomer, the methacrylate monomer and the functional monomer in the rest formula amount within 2.0-4.0h, heating to 90 ℃ after dropwise adding, and continuously preserving heat for 30-50 min; cooling to 40 ℃, filtering and discharging, and taking the filtrate to obtain the acrylic ester polymer emulsion.
5. The silicate inorganic paint as claimed in claim 1, wherein the pigment and filler is a mixture of ground calcium carbonate, talc, calcined kaolin and titanium dioxide in a mass ratio of 1:0.4-0.6:0.3-0.6: 1.0-1.2.
6. The silicate inorganic paint as claimed in claim 1, wherein the silicate inorganic paint is prepared from the following raw materials in parts by mass: 30 to 45 percent of water, 25 to 38 percent of pigment and filler, 15 to 27 percent of inorganic silicate film-forming base material, 1 to 4 percent of acrylate polymer emulsion, 0.5 to 1.2 percent of defoaming agent, 0.5 to 1.2 percent of dispersant, 0.4 to 1.0 percent of flatting agent, 0.5 to 1.0 percent of thickening agent and 100 percent of total feeding amount.
7. The silicate inorganic paint as claimed in claim 1, wherein the silicate inorganic paint is prepared from the following raw materials in parts by mass: 40-45% of water, 25-28% of pigment and filler, 21-25% of inorganic silicate film-forming base material, 3-4% of acrylate polymer emulsion, 1.1-1.2% of defoaming agent, 1.2-1.3% of dispersing agent, 1.1-1.25% of flatting agent, 1.3-1.4% of thickening agent and 100% of total feeding amount; the pigment and filler is prepared by mixing heavy calcium carbonate, talcum powder, calcined kaolin and titanium dioxide according to the mass ratio of 1:0.4-0.6:0.3-0.6: 1.0-1.2; the inorganic silicate film-forming base material is formed by mixing organic silica sol JN-30, sodium silicate and liquid potassium silicate in a mass ratio of 1:0.1-2:0.1-2, and the defoaming agent is a mineral oil defoaming agent CK-231; the dispersing agent is a fatty acid dispersing agent CK-921; the leveling agent is an organic silicon leveling agent CK-113, and the thickening agent is carboxymethyl cellulose.
8. The silicate inorganic paint according to claim 1, wherein the silicate inorganic paint is prepared by the following method: according to the formula amount, firstly adding water, a dispersing agent and a defoaming agent accounting for 1/2 formula amount into a stirring tank, and stirring for 5-15min at the rotation speed of 600-1500 rpm; then adding the pigment and filler, and stirring for 30-55min at the speed of 1000-; then adding inorganic silicate film-forming base material and acrylate polymer emulsion, and stirring for 15-30min at the rotating speed of 1000-2000 rpm; and finally, adding a thickening agent, a flatting agent and the remaining defoaming agent accounting for 1/2 of the formula amount, stirring for 20-50min at the rotating speed of 900-2500rpm, and discharging to obtain the modified silicate coating.
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