CN113637366A - A kind of preparation method of silica aerogel modified styrene-acrylic thermal insulation coating - Google Patents
A kind of preparation method of silica aerogel modified styrene-acrylic thermal insulation coating Download PDFInfo
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- CN113637366A CN113637366A CN202111050975.1A CN202111050975A CN113637366A CN 113637366 A CN113637366 A CN 113637366A CN 202111050975 A CN202111050975 A CN 202111050975A CN 113637366 A CN113637366 A CN 113637366A
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- styrene
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 137
- 239000004965 Silica aerogel Substances 0.000 title claims abstract description 105
- 239000011248 coating agent Substances 0.000 title claims abstract description 52
- 238000000576 coating method Methods 0.000 title claims abstract description 52
- 229920001909 styrene-acrylic polymer Polymers 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 238000009413 insulation Methods 0.000 title claims abstract description 26
- 239000000839 emulsion Substances 0.000 claims abstract description 85
- 238000003756 stirring Methods 0.000 claims abstract description 83
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 45
- 239000003999 initiator Substances 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000000178 monomer Substances 0.000 claims abstract description 21
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 18
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims abstract description 10
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims abstract description 10
- 235000017557 sodium bicarbonate Nutrition 0.000 claims abstract description 10
- 239000003973 paint Substances 0.000 claims abstract description 5
- JYYOBHFYCIDXHH-UHFFFAOYSA-N carbonic acid;hydrate Chemical compound O.OC(O)=O JYYOBHFYCIDXHH-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims description 119
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 72
- 230000002209 hydrophobic effect Effects 0.000 claims description 70
- 239000000843 powder Substances 0.000 claims description 57
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 36
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 36
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 36
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 36
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 36
- 238000006243 chemical reaction Methods 0.000 claims description 17
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 9
- 239000004677 Nylon Substances 0.000 claims description 9
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical group [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 9
- 229920001778 nylon Polymers 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims 1
- 239000000463 material Substances 0.000 claims 1
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims 1
- 239000004964 aerogel Substances 0.000 abstract description 15
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 15
- 238000001816 cooling Methods 0.000 abstract description 9
- 238000001914 filtration Methods 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 description 7
- 238000011065 in-situ storage Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000013329 compounding Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000000758 substrate Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 2
- 239000012774 insulation material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- FEIQOMCWGDNMHM-UHFFFAOYSA-N 5-phenylpenta-2,4-dienoic acid Chemical compound OC(=O)C=CC=CC1=CC=CC=C1 FEIQOMCWGDNMHM-UHFFFAOYSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000011527 polyurethane coating Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
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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
- 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
- C09D125/08—Copolymers of styrene
- C09D125/14—Copolymers of styrene with unsaturated esters
-
- 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
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
-
- 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
- C08F212/00—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
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
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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
- 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
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
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- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention belongs to the technical field of water-based paint production, and the specific technical scheme is as follows: a preparation method of a silica aerogel modified styrene-acrylic heat insulation coating comprises the following specific steps: firstly, adding silicon dioxide aerogel into a first emulsifier and a second emulsifier, and uniformly stirring to form a modified emulsifier; adding the modified emulsifier, the mixed monomer, water and sodium bicarbonate into a flask, and uniformly stirring to obtain a pre-emulsion; dissolving potassium persulfate in water to form an initiator solution, and adding the initiator solution into the pre-emulsion to react to obtain a seed emulsion; fifthly, dropwise adding the residual pre-emulsion and the initiator solution into the seed emulsion until the dripping is finished, stopping stirring and heating, and naturally cooling; and seventhly, filtering and adjusting the pH value of the emulsion to obtain the final heat-insulating coating.
Description
Technical Field
The invention belongs to the technical field of water-based paint production, and particularly relates to a preparation method of a silica aerogel modified styrene-acrylic heat-insulating paint.
Background
The water-based heat insulation coating has the characteristics of high film-forming density, good heat insulation performance, no toxicity, no odor and the like, and is a development direction of heat insulation materials with great significance. Therefore, the research and preparation of the water-based heat-insulating coating which is light, thin, high-efficiency, heat-insulating, convenient to construct and environment-friendly has great significance. The water-based heat insulation coating is generally formed by compounding a water-based coating and a heat insulation functional component, wherein the water-based coating comprises a styrene-acrylic coating, a water-based polyurethane coating and the like. The styrene-acrylic coating is prepared from styrene-acrylic acid (ester) copolymer emulsion, has good weather resistance, water resistance, alkali resistance, chalking resistance and stain resistance, has good adhesive force with cement and good scrubbing resistance, can be used for parts with larger humidity, and is a main variety of the current interior wall coating in China. The silica aerogel has excellent heat insulation performance, good thermal stability, excellent sound insulation performance and the like, and is an environment-friendly building material with the best heat insulation performance in all the heat insulation solid materials at present. The silica aerogel is introduced into the styrene-acrylic coating, so that the heat insulation performance of the styrene-acrylic coating can be improved. Wanghui et al added silica aerogel in the preparation process of styrene-acrylic coating to obtain silica modified styrene-acrylic coating, firstly modified the surface of silica aerogel by silane coupling agent, then mixed with emulsifier and water and stirred uniformly, and then added reaction monomer to carry out the following preparation process, and the heat insulation performance of styrene-acrylic coating obtained by the method is improved to a certain extent.
Most of the silica aerogels obtained by the currently reported preparation methods for preparing silica aerogels are hydrophobic silica aerogels, and the specific surface areas of the hydrophobic silica aerogels prepared by the methods disclosed in patent patents CN109850909A and CN108017062A are 980m respectively2G and 886m2(ii) in terms of/g. The hydrophobic silica aerogel can not be uniformly dispersed in the waterborne styrene-acrylic coating, so that the hydrophobic silica aerogel can not be directly and uniformly dispersed in the styrene-acrylic coating, if the hydrophobic silica aerogel is subjected to surface modification or calcined at a certain temperature, the hydrophilicity of the hydrophobic silica aerogel can be improved, and the dispersibility of the hydrophobic silica aerogel in the styrene-acrylic coating is further improved. Therefore, aiming at the problems, the invention discloses a preparation method of silica aerogel in-situ modified styrene-acrylic coating, which is obtained by introducing hydrophobic silica aerogel and styrene-acrylic coating preparation raw materials into a styrene-acrylic coating preparation process in an in-situ compounding manner.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention discloses a preparation method for obtaining a silica aerogel in-situ modified styrene-acrylic coating by introducing hydrophobic silica aerogel and styrene-acrylic coating preparation raw materials into a styrene-acrylic coating preparation process in an in-situ compounding manner.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a preparation method of a silica aerogel modified styrene-acrylic heat insulation coating comprises the following specific steps:
firstly, adding silicon dioxide aerogel into a first emulsifier, uniformly stirring at 25-50 ℃ to form a first mixture, adding a second emulsifier into the mixture, and uniformly stirring to form a modified emulsifier.
Secondly, adding hydrophobic silica aerogel powder into at least one of styrene, ethyl acrylate, butyl acrylate and acrylic acid;
if hydrophobic silica aerogel powder is added into styrene, the mass ratio of the hydrophobic silica aerogel powder to the styrene is 0.5:100-10:100, and the mixture is uniformly stirred at the temperature of 25-50 ℃ to form a styrene mixture;
if the hydrophobic silica aerogel powder is added into the ethyl acrylate, the mass ratio of the hydrophobic silica aerogel powder to the ethyl acrylate is 0.5:100-10:100, and the mixture is uniformly stirred at the temperature of 25-50 ℃ to form an ethyl acrylate mixture;
if hydrophobic silica aerogel powder is added into butyl acrylate, the mass ratio of the hydrophobic silica aerogel powder to the butyl acrylate is 0.5:100-10:100, and the mixture is uniformly stirred at the temperature of 25-50 ℃ to form a butyl acrylate mixture;
if the hydrophobic silica aerogel powder is added into the acrylic acid, the mass ratio of the hydrophobic silica aerogel powder to the acrylic acid is 0.5:100-10:100, and the mixture is uniformly stirred at the temperature of 25-50 ℃ to form an acrylic acid mixture;
stirring styrene or its mixture, ethyl acrylate or its mixture, butyl acrylate or its mixture, and acrylic acid or its mixture at 30-50 deg.C to obtain mixed monomer. Wherein, the mixed monomer comprises at least one mixture containing silica aerogel.
Wherein the styrene mixture is formed by adding silicon dioxide aerogel into styrene and uniformly stirring at 25-50 ℃; the ethyl acrylate mixture is formed by adding silicon dioxide aerogel into ethyl acrylate and uniformly stirring at 25-50 ℃; the butyl acrylate mixture is formed by adding silicon dioxide aerogel into butyl acrylate and uniformly stirring at 25-50 ℃; the acrylic acid mixture is formed by adding silica aerogel into acrylic acid and stirring uniformly at 25-50 ℃.
And thirdly, adding the modified emulsifier, the mixed monomer, water and sodium bicarbonate into a 500ml four-neck flask, uniformly stirring at 25-50 ℃ to obtain milky pre-emulsion, and transferring the pre-emulsion into a beaker for later use.
Fourthly, dissolving the potassium persulfate in the water to form an initiator solution.
Placing 1/5 initiator solution into a constant pressure dropping funnel, placing 1/5 pre-emulsion into a 500ml four-neck flask, adding the 1/5 initiator solution into the pre-emulsion under the condition of stirring, heating the four-neck flask by using a constant temperature water bath until the reaction temperature reaches 70-80 ℃, and reacting for 0.5-2h at the reaction temperature to obtain the seed emulsion.
And sixthly, respectively and simultaneously dripping the residual pre-emulsion and the initiator solution into the seed emulsion by using two constant-pressure dropping funnels until the dripping is finished, reacting for 2-4h at the temperature of 70-80 ℃, stopping stirring and heating, and naturally cooling.
And seventhly, filtering the emulsion in the four-neck flask by using a 200-mesh 400-mesh nylon net, removing the gel and the residues, and adjusting the pH value of the emulsion to 7-8 by using ammonia water to obtain the final silicon dioxide aerogel modified styrene-acrylic heat-insulating coating.
Preferably, the first emulsifier is OP-10 emulsifier, and the second emulsifier is sodium dodecyl sulfate.
The silicon dioxide aerogel is hydrophobic silicon dioxide aerogel powder, and in the step one, the mass ratio of the hydrophobic silicon dioxide aerogel powder to the first emulsifier is 1:100-20: 100.
In the second step, in the styrene mixture, the mass ratio of the hydrophobic silica aerogel powder to the styrene is 0.5:100-10: 100; in the ethyl acrylate mixture, the mass ratio of the hydrophobic silica aerogel powder to the ethyl acrylate is 0.5:100-10: 100; in the butyl acrylate mixture, the mass ratio of the hydrophobic silica aerogel powder to the butyl acrylate is 0.5:100-10: 100; in the acrylic acid mixture, the mass ratio of the hydrophobic silica aerogel powder to the acrylic acid is 0.5:100-10: 100.
The mass concentration of the initiator solution was 3.4%.
The mixture ratio of the raw materials is as follows: 250 portions of first emulsifier 200-.
Compared with the prior art, the invention has the following specific beneficial effects: according to the invention, the hydrophobic silica aerogel is introduced into a plurality of raw materials for preparing the coating, and the raw materials and the hydrophobic silica aerogel are compounded, so that the final overall in-situ compounding preparation mode is realized, the aim of regulating and controlling the doping amount of the hydrophobic silica aerogel for a plurality of times is achieved, the high specific surface area and the porosity of the hydrophobic silica aerogel can be well maintained, and the heat insulation performance of the coating can be improved to a greater extent; when the paint is used in the later period, the process of adding heat insulation functional components is omitted, and the engineering efficiency is greatly improved.
Drawings
FIG. 1 is a graph showing a comparison of a comparative sample A (without silica aerogel) and a coating sample B prepared according to the present invention after they are dried on a glass substrate.
FIG. 2 is a graph of the temperature of the backside of comparative sample A and inventive coating sample B over time on a substrate at 120 ℃.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example one
A preparation method of a silica aerogel modified styrene-acrylic heat insulation coating comprises the following specific steps:
step one, adding 2 parts of hydrophobic silica aerogel powder into 200 parts of OP-10 emulsifier, uniformly stirring at 25 ℃ to form a first mixture, adding 60 parts of sodium dodecyl sulfate into the mixture, and uniformly stirring to form the modified emulsifier.
And step two, mixing one or more of a styrene mixture, an ethyl acrylate mixture, a butyl acrylate mixture and an acrylic acid mixture, and uniformly stirring to form a mixed monomer.
Wherein the styrene mixture is a mixture prepared by adding 12.5 parts of hydrophobic silica aerogel powder into 2500 parts of styrene and uniformly stirring at 25 ℃; the ethyl acrylate mixture is a mixture formed by adding 7 parts of hydrophobic silica aerogel powder into 1400 parts of ethyl acrylate and uniformly stirring at 25 ℃; the butyl acrylate mixture is a mixture formed by adding 3.25 parts of hydrophobic silica aerogel powder into 650 parts of butyl acrylate and uniformly stirring at 25 ℃; the acrylic acid mixture was a mixture of 120 parts of acrylic acid with 0.6 part of hydrophobic silica aerogel powder added and stirred uniformly at 25 ℃.
And step three, adding the modified emulsifier, the mixed monomer, 3000 parts of water and 70 parts of sodium bicarbonate into a 500ml four-neck flask, uniformly stirring at 25 ℃ to obtain milky pre-emulsion, and transferring the pre-emulsion into the flask for later use.
And step four, dissolving potassium persulfate in water to form 2000 parts of initiator solution with the mass concentration of 3.4%.
And step five, placing the 1/5 initiator solution in a constant-pressure dropping funnel, placing the 1/5 pre-emulsion in a 500ml four-neck flask, adding the 1/5 initiator solution into the pre-emulsion under the stirring condition, heating the four-neck flask by using a constant-temperature water bath until the reaction temperature reaches 70 ℃, and reacting for 2 hours at the reaction temperature to obtain the seed emulsion.
And step six, respectively and simultaneously dripping the residual pre-emulsion and the initiator solution into the seed emulsion by using two constant-pressure dropping funnels until the dripping is finished, reacting for 4 hours at 70 ℃, stopping stirring and heating, and naturally cooling.
And seventhly, filtering the emulsion in the four-neck flask by using a 200-mesh nylon net, removing gel and residues, and adjusting the pH value of the emulsion to 7 by using ammonia water to obtain the final hydrophobic silica aerogel powder modified styrene-acrylic heat-insulating coating.
The properties of the coating sample prepared by the present invention were compared to those of the comparative sample A, and the thickness of the silica aerogel-modified aqueous polyurethane insulation material sample B in FIG. 2 was 0.4mm, as shown in FIGS. 1 and 2.
Table 1 shows the performance comparison of the silica aerogel modified styrene-acrylic insulating coating sample prepared by the above method and the comparative sample (without silica aerogel) after being dried on a glass substrate:
TABLE 1
Example two
A preparation method of a silica aerogel modified styrene-acrylic heat insulation coating comprises the following specific steps:
step one, adding 50 parts of hydrophobic silica aerogel powder into 250 parts of OP-10 emulsifier, uniformly stirring at 50 ℃ to form a first mixture, adding 85 parts of sodium dodecyl sulfate into the mixture, and uniformly stirring to form the modified emulsifier.
And step two, mixing one or more of a styrene mixture, an ethyl acrylate mixture, a butyl acrylate mixture and an acrylic acid mixture, and uniformly stirring to form a mixed monomer.
Wherein 2800 parts of styrene mixture is a mixture of styrene and 280 parts of hydrophobic silica aerogel powder, which are uniformly stirred at 50 ℃; the ethyl acrylate mixture is a mixture formed by adding 155 parts of hydrophobic silica aerogel powder into 1550 parts of ethyl acrylate and uniformly stirring at 50 ℃; the butyl acrylate mixture is a mixture formed by adding 78 parts of hydrophobic silica aerogel powder into 780 parts of butyl acrylate and uniformly stirring at 50 ℃; the acrylic acid mixture was a mixture obtained by adding 18 parts of hydrophobic silica aerogel powder to 180 parts of acrylic acid and stirring the mixture uniformly at 50 ℃.
And step three, adding the modified emulsifier, the mixed monomer, 3000 parts of water and 86 parts of sodium bicarbonate into a 500ml four-neck flask, uniformly stirring at 50 ℃ to obtain milky pre-emulsion, and transferring the pre-emulsion into the flask for later use.
Step four, dissolving potassium persulfate in water to form 2100 parts of initiator solution with the mass concentration of 3.4%.
And step five, placing the 1/5 initiator solution in a constant-pressure dropping funnel, placing the 1/5 pre-emulsion in a 500ml four-neck flask, adding the 1/5 initiator solution into the pre-emulsion under the stirring condition, heating the four-neck flask by using a constant-temperature water bath until the reaction temperature reaches 80 ℃, and reacting for 0.5h at the reaction temperature to obtain the seed emulsion.
And step six, respectively and simultaneously dripping the residual pre-emulsion and the initiator solution into the seed emulsion by using two constant-pressure dropping funnels until the dripping is finished, reacting for 2 hours at the temperature of 80 ℃, stopping stirring and heating, and naturally cooling.
And seventhly, filtering the emulsion in the four-neck flask by using a 400-mesh nylon net, removing gel and residues, and adjusting the pH value of the emulsion to 8 by using ammonia water to obtain the final silicon dioxide aerogel modified styrene-acrylic heat-insulating coating.
EXAMPLE III
A preparation method of a silica aerogel modified styrene-acrylic heat insulation coating comprises the following specific steps:
step one, adding 23 parts of hydrophobic silica aerogel powder into 230 parts of OP-10 emulsifier, uniformly stirring at 40 ℃ to form a first mixture, adding 72 parts of sodium dodecyl sulfate into the mixture, and uniformly stirring to form the modified emulsifier.
And step two, mixing one or more of a styrene mixture, an ethyl acrylate mixture, a butyl acrylate mixture and an acrylic acid mixture, and uniformly stirring to form a mixed monomer.
Wherein the styrene mixture is a mixture formed by adding 130 parts of hydrophobic silica aerogel powder into 2600 parts of styrene and uniformly stirring at 40 ℃; the ethyl acrylate mixture is a mixture formed by adding 74 parts of hydrophobic silica aerogel powder into 1480 parts of ethyl acrylate and uniformly stirring at 40 ℃; the butyl acrylate mixture is a mixture formed by adding 35 parts of hydrophobic silica aerogel powder into 700 butyl acrylate and uniformly stirring at 40 ℃; the acrylic acid mixture was a mixture of 160 parts of acrylic acid with 8 parts of hydrophobic silica aerogel powder added and stirred uniformly at 40 ℃.
And step three, adding the modified emulsifier, the mixed monomer, 3000 parts of water and 75 parts of sodium bicarbonate into a 500ml four-neck flask, uniformly stirring at 40 ℃ to obtain milky pre-emulsion, and transferring the pre-emulsion into the flask for later use.
Step four, dissolving potassium persulfate in water to form 2050 parts of initiator solution with the mass concentration of 3.4%.
And step five, placing the 1/5 initiator solution in a constant-pressure dropping funnel, placing the 1/5 pre-emulsion in a 500ml four-neck flask, adding the 1/5 initiator solution into the pre-emulsion under the stirring condition, heating the four-neck flask by using a constant-temperature water bath until the reaction temperature reaches 75 ℃, and reacting for 1h at the reaction temperature to obtain the seed emulsion.
And step six, respectively and simultaneously dripping the residual pre-emulsion and the initiator solution into the seed emulsion by using two constant-pressure dropping funnels until the dripping is finished, reacting for 3 hours at 75 ℃, stopping stirring and heating, and naturally cooling.
And seventhly, filtering the emulsion in the four-neck flask by using a 300-mesh nylon net, removing gel and residues, and adjusting the pH value of the emulsion to 7.5 by using ammonia water to obtain the final silicon dioxide aerogel modified styrene-acrylic heat-insulating coating.
Example four
A preparation method of a silica aerogel modified styrene-acrylic heat insulation coating comprises the following specific steps:
step one, adding 22 parts of hydrophobic silica aerogel powder into 220 parts of OP-10 emulsifier, uniformly stirring at 40 ℃ to form a first mixture, adding 75 parts of sodium dodecyl sulfate into the mixture, and uniformly stirring to form the modified emulsifier.
And step two, mixing one or more of a styrene mixture, an ethyl acrylate mixture, a butyl acrylate mixture and an acrylic acid mixture, and uniformly stirring to form a mixed monomer.
Wherein the styrene mixture is a mixture formed by adding 135 parts of hydrophobic silica aerogel powder into 2700 styrene and uniformly stirring at 40 ℃; the ethyl acrylate mixture is a mixture formed by adding 75 parts of hydrophobic silica aerogel powder into 1500 ethyl acrylate and uniformly stirring at 40 ℃; the butyl acrylate mixture is a mixture formed by adding 35 parts of hydrophobic silica aerogel powder into 700 parts of butyl acrylate and uniformly stirring at 40 ℃; the acrylic acid mixture was a mixture obtained by adding 7.5 parts of hydrophobic silica aerogel powder to 150 parts of acrylic acid and stirring the mixture uniformly at 40 ℃.
And step three, adding the modified emulsifier, the mixed monomer, 2900 parts of water and sodium bicarbonate into a 500ml four-neck flask, uniformly stirring at 40 ℃ to obtain milky pre-emulsion, and transferring the pre-emulsion into the flask for later use.
Step four, dissolving potassium persulfate in water to form 2050 parts of initiator solution with the mass concentration of 3.4%.
And step five, placing the 1/5 initiator solution in a constant-pressure dropping funnel, placing the 1/5 pre-emulsion in a 500ml four-neck flask, adding the 1/5 initiator solution into the pre-emulsion under the stirring condition, heating the four-neck flask by using a constant-temperature water bath until the reaction temperature reaches 75 ℃, and reacting for 1h at the reaction temperature to obtain the seed emulsion.
And step six, respectively and simultaneously dripping the residual pre-emulsion and the initiator solution into the seed emulsion by using two constant-pressure dropping funnels until the dripping is finished, reacting for 3 hours at 75 ℃, stopping stirring and heating, and naturally cooling.
And seventhly, filtering the emulsion in the four-neck flask by using a 300-mesh nylon net, removing gel and residues, and adjusting the pH value of the emulsion to 7.5 by using ammonia water to obtain the final silicon dioxide aerogel modified styrene-acrylic heat-insulating coating.
EXAMPLE five
A preparation method of a silica aerogel modified styrene-acrylic heat insulation coating comprises the following specific steps:
step one, adding 0.295g of hydrophobic silica aerogel powder into 2.2g of OP-10 emulsifier, uniformly stirring at 25 ℃, adding 0.75g of sodium dodecyl sulfate, and uniformly stirring at 25 ℃ to form the modified emulsifier.
Step two, adding 2.7g of hydrophobic silica aerogel powder into 27g of styrene, uniformly stirring at 25 ℃ to form a styrene mixture, adding 0.75g of hydrophobic silica aerogel powder into 15g of ethyl acrylate, uniformly stirring at 25 ℃ to form an ethyl acrylate mixture, adding 0.07g of hydrophobic silica aerogel powder into 7g of butyl acrylate, uniformly stirring at 25 ℃ to form a butyl acrylate mixture, adding 0.015g of hydrophobic silica aerogel powder into 1.5g of acrylic acid, uniformly stirring at 25 ℃ to form an acrylic acid mixture, mixing the styrene mixture, the ethyl acrylate mixture, the butyl acrylate mixture and the acrylic acid mixture at 25 ℃, and uniformly stirring to form a mixed monomer.
And step three, adding the modified emulsifier, the mixed monomer, 30g of water and 0.75g of sodium bicarbonate into a 500ml four-neck flask, uniformly stirring at 25 ℃ to obtain milky pre-emulsion, and transferring the pre-emulsion into a beaker for later use.
Step four, 0.7 g of potassium persulfate was dissolved in 20 ml of water to form an initiator solution.
And step five, putting the 1/5 initiator solution into a constant-pressure dropping funnel, putting 1/5 pre-emulsion into a 500-ml four-neck flask, adding the 1/5 initiator solution into the pre-emulsion under the stirring condition, heating to the reaction temperature of 70 ℃ by using a constant-temperature water bath kettle, and reacting for 0.5 hour to obtain the seed emulsion.
And step six, respectively and simultaneously dripping the residual pre-emulsion and the initiator solution into the seed solution by using two constant-pressure dropping funnels until the dripping is finished, then reacting for 2 hours at 70 ℃, stopping stirring and heating, and cooling.
And seventhly, filtering the emulsion by using a 200-mesh nylon net, removing gel and residues, and adjusting the pH =7 of the emulsion by using ammonia water to obtain the final silicon dioxide aerogel modified styrene-acrylic heat-insulating coating.
EXAMPLE six
Step one, 0.295g of hydrophobic silica aerogel powder is added into 22g of OP-10 emulsifier, the mixture is stirred uniformly at 25 ℃, 7.5g of sodium dodecyl sulfate is added, and the mixture is stirred uniformly at 50 ℃ to form the modified emulsifier.
Step two, adding 17g of silica aerogel into 270g of styrene, uniformly stirring at 50 ℃ to form a styrene mixture, adding 15g of silica aerogel into 150g of ethyl acrylate, uniformly stirring at 50 ℃ to form an ethyl acrylate mixture, adding 7g of silica aerogel into 70g of butyl acrylate, uniformly stirring at 50 ℃ to form a butyl acrylate mixture, adding 0.5g of silica aerogel into 15g of acrylic acid, uniformly stirring at 50 ℃ to form an acrylic acid mixture, mixing the styrene mixture, the ethyl acrylate mixture, the butyl acrylate mixture and the acrylic acid mixture at 50 ℃, and uniformly stirring to form a mixed monomer.
And step three, adding the modified emulsifier, the mixed monomer, 300g of water and 7.5g of sodium bicarbonate into a 500ml four-neck flask, uniformly stirring at 50 ℃ to obtain milky pre-emulsion, and transferring the pre-emulsion into a beaker for later use.
Step four, dissolving 7g of potassium persulfate in 200 ml of water to form an initiator solution.
And step five, putting the 1/5 initiator solution into a constant-pressure dropping funnel, putting 1/5 pre-emulsion into a beaker, adding the 1/5 initiator solution into the pre-emulsion under the stirring condition, heating to the reaction temperature of 80 ℃ by using a constant-temperature water bath kettle, and reacting for 2 hours to obtain the seed emulsion.
And step six, respectively and simultaneously dripping the residual pre-emulsion and the initiator solution into the seed solution by using two constant-pressure dropping funnels until the dripping is finished, then reacting for 4 hours at 80 ℃, stopping stirring and heating, and cooling.
And seventhly, filtering the emulsion by using a 200-mesh nylon net, removing gel and residues, and adjusting the pH =8 of the emulsion by using ammonia water to obtain the final silicon dioxide aerogel modified styrene-acrylic heat-insulating coating.
EXAMPLE seven
Step one, 0.295g of hydrophobic silica aerogel powder is added into 4.4g of OP-10 emulsifier and stirred uniformly at 25 ℃, and then 7.5g of sodium dodecyl sulfate is added and stirred uniformly at 35 ℃ to form the modified emulsifier.
Step two, adding 4g of hydrophobic silica aerogel powder into 54g of styrene, uniformly stirring at 35 ℃ to form a styrene mixture, adding 0.3g of hydrophobic silica aerogel powder into 30g of ethyl acrylate, uniformly stirring at 35 ℃ to form an ethyl acrylate mixture, adding 1.4g of hydrophobic silica aerogel powder into 14g of butyl acrylate, uniformly stirring at 35 ℃ to form a butyl acrylate mixture, adding 0.3g of hydrophobic silica aerogel powder into 3g of acrylic acid, uniformly stirring at 35 ℃ to form an acrylic acid mixture, mixing the styrene mixture, the ethyl acrylate mixture, the butyl acrylate mixture and the acrylic acid mixture at 25 ℃, and uniformly stirring to form a mixed monomer.
And step three, adding the modified emulsifier, the mixed monomer, 60g of water and 1.5g of sodium bicarbonate into a 500ml four-neck flask, uniformly stirring at 35 ℃ to obtain milky pre-emulsion, and transferring the pre-emulsion into a beaker for later use.
Step four, 1.4g of potassium persulfate was dissolved in 40 ml of water to form an initiator solution.
And step five, putting the 1/5 initiator solution into a constant-pressure dropping funnel, putting 1/5 pre-emulsion into a 500-ml four-neck flask, adding the 1/5 initiator solution into the pre-emulsion under the stirring condition, heating to the reaction temperature of 75 ℃ by using a constant-temperature water bath kettle, and reacting for 1 hour to obtain the seed emulsion.
And step six, respectively and simultaneously dripping the residual pre-emulsion and the initiator solution into the seed solution by using two constant-pressure dropping funnels until the dripping is finished, then reacting for 3 hours at 75 ℃, stopping stirring and heating, and cooling.
And seventhly, filtering the emulsion by using a 200-mesh nylon net, removing gel and residues, and adjusting the pH of the emulsion to be 7.5 by using ammonia water to obtain the final silicon dioxide aerogel modified styrene-acrylic heat-insulating coating.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principles of the present invention are intended to be included therein.
Claims (6)
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| ZA2022/03084A ZA202203084B (en) | 2021-09-08 | 2022-03-15 | Preparation method of silica aerogel modified styrene acrylic heat-insulating paint |
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