Novel thermal insulation coating
The novel heat-insulating coating addresses poor structural stability and thermal insulation in polyacrylate coatings by using modified hollow glass microspheres and a siloxane-based emulsifier, enhancing particle size and stability for improved wear resistance and thermal performance.
Patent Information
- Application Number
- CN202411491784.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-24
- Publication Date
- 2024-12-31
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
Existing polyacrylate emulsion coatings suffer from poor structural stability, inadequate thermal insulation performance, and insufficient wear resistance due to their small particle size and 'hydrophilic shell, lipophilic core' structure, leading to poor uniformity and surface smoothness during the curing process.
A novel heat-insulating coating is formulated with modified hollow glass microspheres and amphiphilic polyacrylate structure, using a modified emulsifier with a siloxane main chain and hydrophilic and hydrophobic groups to enhance particle size and filling structure, combined with a cross-linking process to improve stability and wear resistance.
The coating achieves improved thermal insulation, wear resistance, and high-temperature oxidation resistance by synergistic cooperation of functional groups in the polyacrylate, hollow glass microspheres, and auxiliary materials, forming a stable and durable emulsion structure.
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Abstract
Description
Technical Field
[0001] The invention relates to the technical field of coating processing, and in particular to a novel heat-insulating coating. Background Art
[0002] Polyacrylate emulsion is a high-performance material widely used in coatings and adhesives. The preparation of polyacrylate emulsion mainly relies on basic emulsion polymerization technology, which improves the environmental friendliness and processing convenience of the product by stably dispersing the polymer in the water phase.
[0003] Among them, polyacrylate emulsion coatings have excellent adhesion and wear resistance, making them suitable for various substrates, including wood, metal and concrete. The good fluidity and self-leveling properties of the emulsion make the construction process smoother and more efficient, reducing construction defects. In recent years, the formulation and performance of polyacrylate emulsions have been continuously improved. For example, the performance of coatings has been improved by introducing nanomaterials. Overall, polyacrylate emulsion coatings have become an indispensable choice in the construction, home and industrial coatings markets due to their environmental friendliness, durability and ease of construction.
[0004] Prior art CN108441010A discloses an exterior wall thermal insulation polyacrylate water-based paint and a preparation method thereof. The thermal insulation polyacrylate water-based paint and the preparation method thereof, in parts by weight, include the following components: 100 parts of modified polyacrylate emulsion, 16-23 parts of vermiculite, 15-28 parts of hollow glass microspheres, 5-9 parts of aluminum oxide, 7-9 parts of polyethylene glycol, 5-8 parts of coupling agent, 3-5 parts of dispersant, 2-4 parts of brightener, 1-2 parts of leveling agent, 2-4 parts of moisture-proof agent, 10-12 parts of filler, 22-34 parts of waterborne polyurethane, and 20-40 parts of water. The exterior wall thermal insulation polyacrylate water-based paint of this application has good thermal insulation effect, high adhesion, and is easy to construct. In addition, the exterior wall thermal insulation paint can maintain stable performance at high and low temperatures, is not easy to crack, and has a long service life.
[0005] In the process of preparing the emulsion, a plurality of polyacrylates are first polymerized to obtain a modified polyacrylate which is then emulsified to obtain a polyacrylate emulsion with a "hydrophilic shell, lipophilic core" structure. However, when this structure is used in various coatings, due to its small particle size and oily inner core, a vacuum effect cannot be achieved, resulting in poor structural stability during the curing process, and the thermal insulation performance needs to be further improved. In addition, the uniformity of the emulsion structure without a certain amount of filling is poor, resulting in the surface smoothness of the coating needing to be further improved during the processing, and the wear resistance also needs to be further improved.
[0006] In view of the technical defects in this aspect, a solution is now proposed. Summary of the invention
[0007] The purpose of the present invention is to provide a novel heat-insulating coating, which is used to solve the technical problems in the prior art that the heat-insulating performance of polyacrylate coatings and the polyacrylate emulsion structure need to be further improved.
[0008] The purpose of the present invention can be achieved by the following technical scheme: a novel heat-insulating coating, comprising the following components in parts by weight: 60-80 parts of polyacrylate emulsion, 6-7 parts of titanium dioxide, 7-8 parts of nano-alumina, 6-8 parts of talc, 2-5 parts of dispersant, 3-5 parts of stabilizer, 2-5 parts of leveling agent and 2-3 parts of anti-sticking agent;
[0009] The dispersant is one or more of polyvinyl alcohol, sodium polyacrylate, and polyvinyl ether; the stabilizer is one or more of isooctyl polyoxyethylene ether, dodecyl polyoxyethylene ether, and fatty alcohol polyoxyethylene ether; the leveling agent is one or more of polydimethylsiloxane, polymethylsiloxane, and polyvinyl siloxane; and the anti-sticking agent is one or more of polyvinyl alcohol, polyethylene glycol, and polypropylene glycol.
[0010] Further, the preparation method of the polyacrylate emulsion comprises the following steps:
[0011] A1. Weigh 10-20 parts of hollow glass microspheres and 30-40 parts of 0.5-2 mol / L sodium hydroxide solution in parts by weight and place them in a reactor. The temperature of the reactor is raised to 60-80° C. and the reaction is kept warm for 1-2 hours. The modified hollow glass microspheres are obtained by post-treatment.
[0012] A2, weighing 30-40 parts of alkyl polyether modified fluorosilicone oil, 5-8 parts of modified emulsifier and 2-3 parts of 3,4-difluorostyrene by weight, adding them into a reaction kettle, stirring at room temperature for 1-2 hours at a stirring rate of 1000-1200 rpm to obtain a reaction precursor solution;
[0013] A3, weigh 30-40 parts of reaction precursor liquid, 20-30 parts of dimethyl sulfoxide, 6-8 parts of 2-methyl-2-acrylic acid-2,3-dihydroxypropyl ester, 3-4 parts of isocyanate methyltrimethoxysilane and 1-2 parts of azobisisobutyl cyanide by weight, add them into a reaction kettle and stir at a stirring rate of 300-400 rpm, raise the temperature of the reaction kettle to 30-50°C, keep the temperature for reaction for 1-3h, and post-treat to obtain an emulsion precursor;
[0014] The reaction equation for synthesizing the emulsion precursor is:
[0015]
[0016] Where:
[0017]
[0018] The reaction principle of synthesizing the emulsion precursor is as follows: under the catalysis of azobisisobutylcyanide, a free radical polymerization reaction occurs between the reactants to obtain an emulsion precursor.
[0019] A4. 10-30 parts of deionized water and 5-8 parts of activated hollow glass microspheres are weighed by weight and added to a reactor. After stirring at a stirring rate of 100-120 rpm for 10-15 minutes at room temperature, the temperature of the reactor is increased to 50-70° C., and the stirring rate is increased to 800-1000 rpm. 40-60 parts of emulsion precursor and 1-3 parts of triethylamine are continuously added thereto. After the reaction is kept warm for 2-3 hours, a polyacrylate emulsion is obtained by post-treatment.
[0020] The reaction equation for synthesizing polyacrylate emulsion is:
[0021]
[0022] Where: Represents the emulsion structure formed by cross-linking of hollow glass microspheres and polyacrylate.
[0023] The reaction principle of synthesizing polyacrylate emulsion is as follows: after the polyacrylate in the emulsion precursor is dispersed in deionized water, under the catalysis of triethylamine, the siloxy groups in the hydrophilic side chains combine with the hydroxyl groups on the surface of the modified hollow glass microspheres to form a coating structure, and part of the water is encapsulated inside the hollow glass microspheres and the organic coating layer, eventually forming emulsion droplets to obtain polyacrylate emulsion.
[0024] Furthermore, in step A1, the post-treatment includes: after the reactor is cooled to room temperature, the reaction liquid is filtered to collect the filter cake, the filter cake is washed with deionized water for 3-5 times, and the filter cake is placed in a drying oven at a temperature of 80°C and vacuum dried until the filter cake has a constant weight to obtain activated hollow glass microspheres; in step A3, the post-treatment includes: after the reactor is cooled to room temperature, the reaction liquid is added to a rotary evaporator with a water bath temperature of 80-100°C, and the vacuum distillation is performed until no liquid is extracted to obtain an emulsion precursor; in step A4, the post-treatment includes: after the reactor is cooled to room temperature, the reaction liquid is placed in a vacuum drying oven at a temperature of 30-40°C, and the vacuum drying is performed until the mass reduction of the reaction liquid is less than 10 mg / min to obtain a polyacrylate emulsion.
[0025] Furthermore, the preparation method of the modified emulsifier is as follows: 20-30 parts of the modified emulsifier precursor, 2-3 parts of 3-isocyanate propylene and 40-60 parts of dimethyl sulfoxide are weighed by weight and added into a reactor, the temperature of the reactor is increased to 50-70°C, the reaction is kept warm for 1-3 hours, and the modified emulsifier is obtained by post-treatment.
[0026] The reaction equation for synthesizing modified emulsifier is:
[0027]
[0028] Where:
[0029] The reaction principle of the synthetic modified emulsifier is: the isocyanate group in 3-isocyanatopropylene undergoes a nucleophilic addition reaction with the hydroxyl group in the modified emulsifier precursor to form a polymer connected by carbamate. In this process, the hydroxyl oxygen atom acts as a nucleophilic reagent to attack the isocyanate carbon atom to generate carbamate, and finally a modified emulsifier is obtained.
[0030] Furthermore, the post-treatment includes: after the reactor is cooled to room temperature, the reaction liquid is added into a rotary evaporator with a water bath temperature of 80-100° C., and the reaction liquid is distilled under reduced pressure until no liquid is extracted to obtain a modified emulsifier.
[0031] Furthermore, the preparation method of the modified emulsifier precursor comprises the following steps:
[0032] B1. Weigh 8-10 parts by weight of phosphated silicone oil, 3-5 parts of hexaphenyldisiloxane, 20-25 parts of 2,4,6,8-tetramethyl-2,4,6,8-tetrakis(3,3,3-trifluoropropyl)cyclotetrasiloxane and 40-50 parts of ether into a reaction kettle, and stir at room temperature for 15-20 minutes to obtain a reaction precursor solution;
[0033] B2, weighing 20-30 parts of the reaction precursor solution and 2-3 parts of 98wt% sulfuric acid solution by weight, adding them into the reaction kettle, and keeping the temperature at room temperature for 8-10 hours to obtain a reaction solution;
[0034] B3. Add solid sodium bicarbonate to the reaction kettle containing the reaction solution until the pH of the reaction solution reaches 7-8, and then perform post-treatment to obtain a modified emulsifier precursor.
[0035] The reaction equation for synthesizing the modified emulsifier precursor is:
[0036]
[0037] Where:
[0038] The reaction principle of the synthetic modified emulsifier precursor is: under the action of concentrated sulfuric acid as an initiator, phosphated silicone oil, hexaphenyldisiloxane and 2,4,6,8-tetramethyl-2,4,6,8-tetra(3,3,3-trifluoropropyl)cyclotetrasiloxane undergo a polycondensation reaction, with hexaphenyldisiloxane serving as a polycondensation agent, phosphated silicone oil and 2,4,6,8-tetramethyl-2,4,6,8-tetra(3,3,3-trifluoropropyl)cyclotetrasiloxane serving as main chain monomer substances, and at the same time, the carbon-oxygen-silicon structure in the side chain undergoes hydrolysis, thereby finally preparing a modified emulsifier precursor.
[0039] Furthermore, in step B3, the post-treatment includes: after the reactor is cooled to room temperature, the reaction liquid is added into a rotary evaporator with a water bath temperature of 80-100° C., and distilled under reduced pressure until no liquid is extracted to obtain a modified emulsifier precursor.
[0040] Furthermore, the preparation method of phosphated silicone oil is as follows: 10-15 parts of chain-extending silicone oil, 2-3 parts of diethyl phosphate, 0.5-0.8 parts of triethylamine and 30-40 parts of dimethyl sulfoxide are weighed by weight and added into a reactor, the temperature of the reactor is increased to 60-80° C., the reaction is kept warm for 1-3 hours, and the phosphated silicone oil is obtained by post-treatment.
[0041] The reaction equation for synthesizing phosphated silicone oil is:
[0042]
[0043] Where:
[0044] The reaction principle of synthesizing phosphated silicone oil is as follows: under weakly alkaline conditions, the hydroxyl group of diethyl phosphate and the epoxy group of the chain-extended silicone oil undergo a ring-opening reaction, and diethyl phosphate and the chain-extended silicone oil are polymerized through ether bonds to prepare phosphated silicone oil.
[0045] Furthermore, the post-treatment includes: after the reactor is cooled to room temperature, the reaction liquid is added into a rotary evaporator with a water bath temperature of 80-100° C., and distilled under reduced pressure until no liquid is produced to obtain phosphated silicone oil.
[0046] Furthermore, the preparation method of the chain-extended silicone oil is as follows: 8-10 parts of amidated silicone oil, 1-2 parts of 2,3-epoxypropionaldehyde, 1-2 parts of 1-acetyl-2-ethyloxirane, 0.1-0.3 parts of γ-alumina and 30-40 parts of dimethyl sulfoxide are weighed by weight and added into a reactor, the temperature of the reactor is increased to 60-80°C, the reaction is kept warm for 2-3 hours, and the chain-extended silicone oil is obtained by post-treatment.
[0047] The reaction equation for synthesizing chain-extended silicone oil is:
[0048]
[0049] Where:
[0050] The reaction principle of synthetic chain-extended silicone oil is as follows: the secondary amine group, aldehyde and ketone with aH in the amidated silicone oil react under acidic conditions, and the imine cation is first generated in the reaction, and then reacts with the enol form of the ketone to form a CC bond to prepare the chain-extended silicone oil.
[0051] Furthermore, the post-treatment includes: after the reactor is cooled to room temperature, the reaction liquid is added into a rotary evaporator with a water bath temperature of 80-100° C., and the reaction liquid is distilled under reduced pressure until no liquid is extracted to obtain the chain-extended silicone oil.
[0052] Furthermore, the preparation method of the amidated silicone oil is as follows: 20-30 parts of modified silicone oil, 5-10 parts of acetic acid, and 75-100 parts of dimethyl sulfoxide are weighed by weight and added to a reactor, stirred at room temperature for 5-10 minutes, the temperature of the reactor is lowered to 0-5°C, 1-2 parts of 1-hydroxybenzotriazole, 1-2 parts of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride and 1-2 parts of N-methylmorphine are added thereto, the reaction is kept warm for 1-2 hours, and the amidated silicone oil is obtained by post-treatment.
[0053] The reaction equation for synthesizing amidated silicone oil is:
[0054]
[0055] Where:
[0056] The reaction principle for synthesizing amidated silicone oil is as follows: the carboxyl group in acetic acid and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride generate active intermediates, and the amino group undergoes nucleophilic attack to generate condensation products. Since the addition intermediate of acid to carbodiimide in the first stage of the reaction is not stable, the addition of acylation catalysts 1-hydroxybenzotriamineazole and N-methylmorphine makes the reaction stable and thorough, and finally the amidated silicone oil is obtained.
[0057] Furthermore, the post-treatment includes: after the reactor is cooled to room temperature, the reaction liquid is added into a rotary evaporator with a water bath temperature of 80-100° C., and the reaction liquid is distilled under reduced pressure until no liquid is produced, thereby obtaining amidated silicone oil.
[0058] Furthermore, the preparation method of the modified silicone oil is as follows: 10-15 parts of functionalized silicone oil, 1-2 parts of trimethylsilyl chloride and 0.3-0.5 parts of triethylamine are weighed by weight and added into a reactor, the temperature of the reactor is increased to 40-60° C., the reaction is kept warm for 1-3 hours, and the modified silicone oil is obtained by post-treatment.
[0059] The reaction equation for synthesizing modified silicone oil is:
[0060]
[0061] Where:
[0062] The reaction principle of synthetic modified silicone oil is: under alkaline conditions, the chlorine group in trimethylchlorosilane and the hydroxyl group in the functionalized silicone oil undergo elimination reaction to form a side chain connected by a carbon-silicon-oxygen structure to obtain modified silicone oil.
[0063] Furthermore, the post-treatment includes: after the reactor is cooled to room temperature, the reaction liquid is added into a rotary evaporator with a water bath temperature of 80-100° C., and the reaction liquid is distilled under reduced pressure until no liquid is produced, thereby obtaining modified silicone oil.
[0064] Furthermore, the preparation method of the functionalized silicone oil is as follows: 8-10 parts by weight of methyl high hydrogen silicone oil, 1-2 parts of allylamine, 2-3 parts of 1,1,1-trifluoro-2-phenyl-3-butene-2-ol and 0.5-1.5 parts of chloroplatinic acid and 40-50 parts of xylene are added into a reactor, the temperature of the reactor is increased to 50-60°C, and the functionalized silicone oil is obtained by post-treatment.
[0065] The reaction equation for synthesizing functionalized silicone oil is:
[0066]
[0067] Where:
[0068] The reaction principle of synthesizing functionalized silicone oil is as follows: under the catalysis of chloroplatinic acid, the silicon-hydrogen bonds in the methyl high hydrogen-containing silicone oil form active intermediates, which undergo silicon-hydrogen addition reactions with allylamine and the secondary double bonds of 1,1,1-trifluoro-2-phenyl-3-butene-2-ol to obtain functionalized silicone oil.
[0069] Furthermore, the post-treatment includes: after the reactor is cooled to room temperature, the reaction liquid is added into a rotary evaporator with a water bath temperature of 80-100° C., and the reaction liquid is distilled under reduced pressure until no liquid is produced, thereby obtaining functionalized silicone oil.
[0070] The present invention has the following beneficial effects:
[0071] 1. In the process of preparing a novel heat-insulating coating, the present invention first prepares a polyacrylate emulsion with modified hollow glass microspheres as carriers and amphiphilic polyacrylate structure as externally modified droplets dispersed therein. Compared with the traditional "hydrophilic in the shell, lipophilic in the core" structure, the droplets in the emulsion prepared by the present invention have a larger particle size and a filling structure inside, which significantly improves the heat-insulating ability and wear resistance of the coating; in the process of preparing the emulsion, the present invention prepares a modified emulsifier, which has a siloxane segment as the main chain and a side chain modified with hydrophobic and hydrophilic groups. By modifying the hydrophilic and hydrophobic groups, the functional The functional groups enable it to participate in the synthesis of polyacrylate chain segments while acting as an emulsifier, and the hydrophilic groups and silane coupling agents can be grafted to cross-link with the surface-modified hollow glass microspheres, forming a structure on the surface of the hollow glass microspheres with the hydrophilic groups as bridges and the siloxane main chain of the modified emulsifier as a coating layer, and there are water layers on the coating layer and the surface of the hollow glass microspheres. After vacuum evaporation, an emulsion structure with hollow glass microspheres as supports and polyacrylate chain segments as coating layers is obtained, wherein the functional groups in the polyacrylate, the hollow glass microspheres and the auxiliary materials cooperate synergistically to obtain a coating that is wear-resistant, high-temperature oxidation-resistant, thermally insulating and corrosion-resistant.
[0072] 2. In the process of preparing a modified emulsifier, the present invention first selects a methyl high hydrogen silicone oil, and through a silylation reaction, a hydrophilic amino group, a hydrophobic and anti-corrosion fluorine group, a wear-resistant and hydrophobic benzene ring structure and a hydroxyl group are modified on the siloxane main chain to obtain a functional silicone oil with an emulsifier prototype; further, by using trimethylchlorosilane to react with the hydroxyl group in the hydrophobic group, the hydrophobicity of the hydrophobic group is improved while protecting the active hydroxyl group; then, by reacting the amino group in the hydrophobic group with acetic acid, a hydrophilic and high temperature resistant amide segment is formed, which significantly improves the high temperature resistance of the hydrophilic group, and the formed secondary amino group provides a functional group basis for further modification; further, by reacting the secondary amino group with aldehydes and ketones to extend the hydrophilic group, an active group epoxy group is introduced into the hydrophilic group, the reactivity of the hydrophilic segment is improved, and diethyl phosphate is further used with the hydrophilic The epoxy group in the water group reacts, and the high-temperature hydrophilicity of the organic segment is further improved by introducing a high-temperature resistant and hydrophilic phosphate group. The hydroxyl group generated by the ring-opening reaction of the epoxy group improves the hydrophilicity of the organic segment and ensures the reaction activity of the hydrophilic segment, providing a basis for further modification. Further, through the catalysis of concentrated sulfuric acid, the phosphated silicone oil and the siloxane substances undergo a polyreaction reaction to enrich the structure of the organic segment, forming a long-chain silicone oil structure with a hydrophobic and wear-resistant group as the end group, while introducing a hydrophobic, high-temperature and corrosion-resistant fluorine group into the side chain. After concentrated sulfuric acid catalytic hydrolysis, the protected hydroxyl group in the hydrophobic group removes the protective structure, thereby improving the activity of the hydrophobic group. Further through modification, carbon-carbon double bonds are introduced into the hydrophilic group and the hydrophobic group, providing a basis for the next step of modification. Through the above steps, a high-temperature resistant, corrosion-resistant and wear-resistant modified emulsifier is finally prepared.
[0073] 3. In the process of preparing the emulsion, the present invention firstly selects to modify the surface of the small-sized hollow glass microspheres, introduces hydroxyl groups on the surface, and enhances the cross-linking ability of the microspheres with organic matter; further, the modified emulsifier undergoes polymerization reaction with the polymer monomer in a mixed solvent to prepare polyacrylate, while further introducing fluorine groups and benzene ring structures into the organic chain segments and further introducing active functional groups hydroxyl groups, the active functional groups hydroxyl groups react with isocyanate in the silane coupling agent, and the silane coupling agent is introduced into the polyacrylate group to obtain an emulsion having Then, the siloxy bonds in the hydrophobic groups act as coupling groups to enhance the compatibility with inorganic auxiliary materials or improve the hydrophobic ability of the chain segments, and the siloxy groups on the silane coupling agent on the hydrophilic groups are cross-linked with the hydroxyl groups on the modified hollow glass microspheres. Further, by vacuum evaporation, an emulsion structure with hollow glass microspheres as the support and polyacrylate segments as the coating layer is obtained, in which the functional groups in the polyacrylate, the hollow glass microspheres and the auxiliary materials cooperate with each other to obtain a wear-resistant, high-temperature oxidation-resistant, thermal-insulating and corrosion-resistant coating. DETAILED DESCRIPTION
[0074] The technical solution of the present invention will be clearly and completely described below in conjunction with the embodiments. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0075] The polyether modified silicone oil Silwet L-77 used in the present invention is purchased from Yisheng Mall, and the product number is 41008ES10;
[0076] The methyl high hydrogen silicone oil used in the present invention is purchased from Anhui Mingyi Silicon Industry Co., Ltd., and the product is MY202 high hydrogen silicone oil;
[0077] The alkyl polyether modified fluorosilicone oil used in the present invention is purchased from Fuzhou Taipuda New Materials Co., Ltd., and the product number is TPD-FS8015;
[0078] The hollow glass microspheres used in the present invention were purchased from Thermo Fisher Scientific, Inc., with a product number of CD9005;
[0079] The polyvinyl alcohol used in the present invention was purchased from Nanjing Reagent, with the product code of C0691870023;
[0080] The polyethylene glycol used in the present invention was purchased from Nanjing Reagent Co., Ltd., with the product code of C0691590323;
[0081] The isooctyl alcohol polyoxyethylene ether used in the present invention was purchased from Element Mall, with the item number being T111874-500mL;
[0082] The polydimethylsiloxane used in the present invention was purchased from Shanghai Titan Technology Co., Ltd. with a product number of 114626BC.
[0083] Example 1
[0084] This embodiment provides a method for preparing a modified emulsifier for preparing acrylic emulsion.
[0085] A1. Preparation of amidated silicone oil
[0086] 12.0 g of methyl high hydrogen silicone oil, 2.4 g of allylamine, 3.6 g of 1,1,1-trifluoro-2-phenyl-3-butene-2-ol, 0.6 g of chloroplatinic acid and 48.0 g of xylene were weighed and added to a reactor. The temperature of the reactor was raised to 50° C. After the reactor was cooled to room temperature, the reaction liquid was added to a rotary evaporator with a water bath temperature of 80° C., and distilled under reduced pressure until no liquid was produced, to obtain 15.8 g of functional silicone oil;
[0087] 14.0 g of functionalized silicone oil, 2.0 g of trimethylsilyl chloride and 0.4 g of triethylamine were weighed and added to a reactor. The temperature of the reactor was raised to 40° C. and the reaction was kept warm for 1 hour. After the reactor was cooled to room temperature, the reaction liquid was added to a rotary evaporator with a water bath temperature of 80° C. and distilled under reduced pressure until no liquid was produced, to obtain 15.6 g of modified silicone oil;
[0088] 14.0 g of modified silicone oil, 4.0 g of acetic acid and 40.0 g of dimethyl sulfoxide were weighed by weight and added to a reactor. The mixture was stirred at room temperature for 5 min. The temperature of the reactor was lowered to 5°C. 0.5 g of 1-hydroxybenzotriazole, 1.0 g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride and 1.0 g of N-methylmorphine were added thereto. The mixture was kept warm for 1 h. After the reactor was cooled to room temperature, the reaction solution was added to a rotary evaporator with a water bath temperature of 80°C and distilled under reduced pressure until no liquid was produced to obtain 17.6 g of amidated silicone oil.
[0089] A2. Preparation of phosphated silicone oil
[0090] 16.0 g of amidated silicone oil, 4.0 g of 2,3-epoxypropionaldehyde, 4.0 g of 1-acetyl-2-ethyloxirane, 0.4 g of γ-alumina and 64.0 g of dimethyl sulfoxide were weighed and added to a reactor, the temperature of the reactor was raised to 60° C., and the reaction was kept warm for 2 hours. After the reactor was cooled to room temperature, the reaction liquid was added to a rotary evaporator with a water bath temperature of 80° C., and the reaction liquid was distilled under reduced pressure until no liquid was produced, to obtain 25.6 g of chain-extended silicone oil;
[0091] 24.0 g of chain-extending silicone oil, 6.0 g of diethyl phosphate, 1.5 g of triethylamine and 64.0 g of dimethyl sulfoxide were weighed by weight and added to a reactor. The temperature of the reactor was raised to 60°C and kept warm for 1 hour. After the reactor was cooled to room temperature, the reaction liquid was added to a rotary evaporator with a water bath temperature of 80°C, and distilled under reduced pressure until no liquid was produced to obtain 28.4 g of phosphated silicone oil.
[0092] A3. Preparation of modified emulsifier
[0093] 25.0 g of phosphated silicone oil, 12.5 g of hexaphenyldisiloxane, 62.5 g of 2,4,6,8-tetramethyl-2,4,6,8-tetrakis(3,3,3-trifluoropropyl)cyclotetrasiloxane and 125.0 g of ether were weighed and added into a reaction kettle, and stirred at room temperature for 15 min to obtain a reaction precursor solution;
[0094] 220.0 g of the reaction precursor solution and 22.0 g of 98 wt % sulfuric acid solution were weighed and added into the reaction kettle, and the mixture was kept at room temperature for 8 h to obtain a reaction solution;
[0095] Solid sodium bicarbonate was added to the reaction kettle containing the reaction solution until the pH of the reaction solution reached 8. After the reaction kettle was cooled to room temperature, the reaction solution was added to a rotary evaporator with a water bath temperature of 80° C. and distilled under reduced pressure until no liquid was produced, to obtain 95.4 g of a modified emulsifier precursor;
[0096] 92.4 g of modified emulsifier precursor, 12.6 g of 3-isocyanate propylene and 201.6 g of dimethyl sulfoxide were weighed by weight and added to the reactor. The temperature of the reactor was raised to 50°C and kept warm for 1 hour. After the reactor was cooled to room temperature, the reaction liquid was added to a rotary evaporator with a water bath temperature of 80°C, and distilled under reduced pressure until no liquid was extracted to obtain 103.5 g of modified emulsifier.
[0097] Example 2
[0098] This embodiment provides a method for preparing a modified emulsifier for preparing acrylic emulsion.
[0099] A1. Preparation of amidated silicone oil
[0100] 12.0 g of methyl high hydrogen silicone oil, 2.4 g of allylamine, 3.6 g of 1,1,1-trifluoro-2-phenyl-3-butene-2-ol, 0.6 g of chloroplatinic acid and 48.0 g of xylene were weighed and added to a reactor. The temperature of the reactor was raised to 60° C. After the reactor was cooled to room temperature, the reaction liquid was added to a rotary evaporator with a water bath temperature of 100° C. and distilled under reduced pressure until no liquid was produced, to obtain 16.2 g of functional silicone oil;
[0101] 15.0 g of functionalized silicone oil, 2.0 g of trimethylsilyl chloride and 0.4 g of triethylamine were weighed and added to a reactor. The temperature of the reactor was raised to 60° C. and the reaction was kept warm for 1 hour. After the reactor was cooled to room temperature, the reaction liquid was added to a rotary evaporator with a water bath temperature of 80° C. and distilled under reduced pressure until no liquid was produced, to obtain 16.4 g of modified silicone oil;
[0102] 15.0 g of modified silicone oil, 5.0 g of acetic acid and 50.0 g of dimethyl sulfoxide were weighed by weight and added to a reactor. The mixture was stirred at room temperature for 5 min. The temperature of the reactor was lowered to 0°C. 1.0 g of 1-hydroxybenzotriazole, 1.0 g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride and 1.0 g of N-methylmorphine were added thereto. The mixture was kept warm for 1 h. After the reactor was cooled to room temperature, the reaction solution was added to a rotary evaporator with a water bath temperature of 80°C and distilled under reduced pressure until no liquid was produced to obtain 19.6 g of amidated silicone oil.
[0103] A2. Preparation of phosphated silicone oil
[0104] 18.0 g of amidated silicone oil, 2.0 g of 2,3-epoxypropionaldehyde, 2.0 g of 1-acetyl-2-ethyloxirane, 0.2 g of γ-alumina and 64.0 g of dimethyl sulfoxide were weighed by weight and added to a reactor. The temperature of the reactor was raised to 80° C. and the reaction was kept warm for 3 hours. After the reactor was cooled to room temperature, the reaction solution was added to a rotary evaporator with a water bath temperature of 100° C. and distilled under reduced pressure until no liquid was produced, to obtain 21.2 g of chain-extended silicone oil;
[0105] 20.0 g of chain-extending silicone oil, 6.0 g of diethyl phosphate, 1.2 g of triethylamine and 64.0 g of dimethyl sulfoxide were weighed by weight and added to a reactor. The temperature of the reactor was raised to 80°C and kept warm for 3 hours. After the reactor was cooled to room temperature, the reaction liquid was added to a rotary evaporator with a water bath temperature of 100°C, and distilled under reduced pressure until no liquid was produced to obtain 25.6 g of phosphated silicone oil.
[0106] A3. Preparation of modified emulsifier
[0107] 24.0 g of phosphated silicone oil, 12.0 g of hexaphenyldisiloxane, 60.0 g of 2,4,6,8-tetramethyl-2,4,6,8-tetrakis(3,3,3-trifluoropropyl)cyclotetrasiloxane and 135.0 g of ether were weighed and added into a reaction kettle, and stirred at room temperature for 20 min to obtain a reaction precursor solution;
[0108] Weigh 230.0 g of the reaction precursor solution and 23.0 g of 98 wt % sulfuric acid solution by weight, add them into the reaction kettle, and keep the temperature at room temperature for 10 hours to obtain a reaction solution;
[0109] Solid sodium bicarbonate was added to the reaction kettle containing the reaction solution until the pH of the reaction solution reached 7. After the reaction kettle was cooled to room temperature, the reaction solution was added to a rotary evaporator with a water bath temperature of 100° C. and distilled under reduced pressure until no liquid was produced, to obtain 93.6 g of a modified emulsifier precursor;
[0110] 90.7 g of modified emulsifier precursor, 11.3 g of 3-isocyanate propylene and 170.0 g of dimethyl sulfoxide were weighed by weight and added to the reactor. The temperature of the reactor was raised to 70°C and kept warm for 3 hours. After the reactor was cooled to room temperature, the reaction liquid was added to a rotary evaporator with a water bath temperature of 100°C, and distilled under reduced pressure until no liquid was extracted to obtain 100.5 g of modified emulsifier.
[0111] Example 3
[0112] This embodiment provides a method for preparing a modified emulsifier for preparing acrylic emulsion.
[0113] A1. Preparation of amidated silicone oil
[0114] 13.4 g of methyl high hydrogen silicone oil, 3.3 g of allylamine, 3.4 g of 1,1,1-trifluoro-2-phenyl-3-butene-2-ol, 1.7 g of chloroplatinic acid and 75.0 g of xylene were weighed and added to a reactor, and the temperature of the reactor was raised to 55° C. After the reactor was cooled to room temperature, the reaction liquid was added to a rotary evaporator with a water bath temperature of 90° C., and distilled under reduced pressure until no liquid was produced, to obtain 18.4 g of functional silicone oil;
[0115] 17.5 g of functionalized silicone oil, 2.5 g of trimethylsilyl chloride and 0.5 g of triethylamine were weighed and added to a reactor. The temperature of the reactor was raised to 50° C. and the reaction was kept warm for 2 h. After the reactor was cooled to room temperature, the reaction liquid was added to a rotary evaporator with a water bath temperature of 90° C. and distilled under reduced pressure until no liquid was produced, to obtain 18.4 g of modified silicone oil;
[0116] 15.0 g of modified silicone oil, 5.0 g of acetic acid and 50.0 g of dimethyl sulfoxide were weighed by weight and added to a reactor. The mixture was stirred at room temperature for 8 min. The temperature of the reactor was lowered to 3°C. 1.0 g of 1-hydroxybenzotriazole, 1.0 g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride and 1.0 g of N-methylmorphine were added thereto. The mixture was kept warm for 2 h. After the reactor was cooled to room temperature, the reaction solution was added to a rotary evaporator with a water bath temperature of 90°C and distilled under reduced pressure until no liquid was produced to obtain 19.6 g of amidated silicone oil.
[0117] A2. Preparation of phosphated silicone oil
[0118] 18.0 g of amidated silicone oil, 4.0 g of 2,3-epoxypropionaldehyde, 4.0 g of 1-acetyl-2-ethyloxirane, 0.4 g of γ-alumina and 70.0 g of dimethyl sulfoxide were weighed and added to a reactor, the reactor temperature was raised to 70°C, and the reaction was kept warm for 3 hours. After the reactor was cooled to room temperature, the reaction liquid was added to a rotary evaporator with a water bath temperature of 90°C, and the reaction liquid was distilled under reduced pressure until no liquid was produced, to obtain 25.3 g of chain-extended silicone oil;
[0119] 24.0 g of chain-extending silicone oil, 4.0 g of diethyl phosphate, 1.2 g of triethylamine and 70.0 g of dimethyl sulfoxide were weighed by weight and added to a reactor. The temperature of the reactor was raised to 70°C and kept warm for 2 hours. After the reactor was cooled to room temperature, the reaction liquid was added to a rotary evaporator with a water bath temperature of 90°C and distilled under reduced pressure until no liquid was produced to obtain 27.6 g of phosphated silicone oil.
[0120] A3. Preparation of modified emulsifier
[0121] 25.0 g of phosphated silicone oil, 12.5 g of hexaphenyldisiloxane, 62.5 g of 2,4,6,8-tetramethyl-2,4,6,8-tetrakis(3,3,3-trifluoropropyl)cyclotetrasiloxane and 125.0 g of ether were weighed and added into a reaction kettle, and stirred at room temperature for 18 min to obtain a reaction precursor solution;
[0122] 220.0 g of the reaction precursor solution and 22.5 g of 98 wt % sulfuric acid solution were weighed and added into the reaction kettle, and the mixture was kept at room temperature for 9 hours to obtain a reaction solution;
[0123] Solid sodium bicarbonate was added to the reaction kettle containing the reaction solution until the pH of the reaction solution was 7. After the reaction kettle was cooled to room temperature, the reaction solution was added to a rotary evaporator with a water bath temperature of 90° C. and distilled under reduced pressure until no liquid was produced to obtain 98.4 g of a modified emulsifier precursor;
[0124] 96.0 g of modified emulsifier precursor, 8.0 g of 3-isocyanate propylene and 180.0 g of dimethyl sulfoxide were weighed by weight and added to the reactor. The temperature of the reactor was raised to 60°C and kept warm for 2 hours. After the reactor was cooled to room temperature, the reaction liquid was added to a rotary evaporator with a water bath temperature of 90°C, and distilled under reduced pressure until no liquid was extracted to obtain 102.5 g of modified emulsifier.
[0125] Example 4
[0126] This embodiment is used to provide a method for preparing a novel thermal insulation coating.
[0127] S1. Preparation of polyacrylate emulsion
[0128] 16.0 g of hollow glass microspheres and 32.0 g of 0.5 mol / L sodium hydroxide solution were weighed and placed in a reactor, the temperature of the reactor was raised to 60° C., and the reaction was kept warm for 1 hour. After the reactor was cooled to room temperature, the reaction liquid was filtered to collect the filter cake, and the filter cake was washed with deionized water for 3 times, and then placed in a drying oven at a temperature of 80° C. and vacuum dried until the filter cake had a constant weight, to obtain 16.5 g of activated hollow glass microspheres;
[0129] 80.0 g of alkyl polyether modified fluorosilicone oil, 15.0 g of modified emulsifier and 3.0 g of 3,4-difluorostyrene were weighed and added into a reaction kettle, and stirred at room temperature for 1 h at a stirring rate of 1000 rpm to obtain 98.4 g of reaction precursor solution;
[0130] 92.0 g of reaction precursor liquid, 60.0 g of dimethyl sulfoxide, 21.0 g of 2-methyl-2-acrylic acid-2,3-dihydroxypropyl ester, 12.0 g of isocyanate methyltrimethoxysilane and 6.0 g of azobisisobutyl cyanide were weighed by weight and added to a reactor and stirred at a stirring rate of 300 rpm. The temperature of the reactor was raised to 30° C. and the reaction was kept warm for 1 hour. After the reactor was cooled to room temperature, the reaction liquid was added to a rotary evaporator with a water bath temperature of 80° C. and distilled under reduced pressure until no liquid was produced, to obtain 123.5 g of an emulsion precursor;
[0131] 60.0 g of deionized water and 15.0 g of activated hollow glass microspheres were weighed by weight and added to a reactor. After stirring at room temperature at a stirring rate of 100 rpm for 10 min, the temperature of the reactor was raised to 50°C, and the stirring rate was increased to 800 rpm. 120.0 g of emulsion precursor and 6.0 g of triethylamine were continued to be added thereto. After the reaction was kept warm for 2 hours, the reactor was cooled to room temperature, and the reaction liquid was placed in a vacuum drying oven at a temperature of 30°C and vacuum dried until the mass reduction of the reaction liquid was less than 10 mg / min, to obtain 130.5 g of polyacrylate emulsion.
[0132] S2. Preparation of thermal insulation coating
[0133] 75.0 g of polyacrylate emulsion, 6.4 g of titanium dioxide, 7.0 g of nano-alumina, 6.4 g of talc, 3.6 g of polyvinyl alcohol, 4.2 g of isooctyl polyoxyethylene ether, 2.4 g of polydimethylsiloxane and 2.4 g of polyethylene glycol were weighed by weight, added into a reaction kettle and mixed evenly, and passed through a 100-mesh sieve to obtain a thermal insulation coating.
[0134] S3, spray paint
[0135] Select a spray gun with a nozzle diameter of 1.4mm, a spraying pressure of 30psi, a distance of 25cm between the spray gun and the substrate, a spray gun movement speed of 30cm / min, and a coating thickness of 20mm. After spraying, place the material in an oven at a temperature of 20°C and a relative humidity of 25% to dry for 2h. After drying, cure it at room temperature for 24h to obtain a material with a surface coated with thermal insulation coating.
[0136] Example 5
[0137] This embodiment is used to provide a method for preparing a novel thermal insulation coating.
[0138] S1. Preparation of polyacrylate emulsion
[0139] 16.0 g of activated hollow glass microspheres and 32.0 g of 0.5 mol / L sodium hydroxide solution were weighed and placed in a reactor, the reactor temperature was raised to 80°C, and the reaction was kept warm for 2 hours. After the reactor was cooled to room temperature, the reaction liquid was filtered to collect the filter cake, and the filter cake was washed with deionized water for 5 times, and then placed in a drying oven at a temperature of 80°C and vacuum dried until the filter cake had a constant weight, to obtain 16.5 g of activated hollow glass microspheres;
[0140] 74.0 g of alkyl polyether modified fluorosilicone oil, 12.0 g of modified emulsifier and 4.0 g of 3,4-difluorostyrene were weighed and added into a reaction kettle, and stirred at room temperature for 2 h at a stirring rate of 1200 rpm to obtain 89.3 g of reaction precursor solution;
[0141] 80.0 g of reaction precursor liquid, 42.0 g of dimethyl sulfoxide, 12.0 g of 2-methyl-2-acrylic acid-2,3-dihydroxypropyl ester, 8.0 g of isocyanate methyltrimethoxysilane and 2.0 g of azobisisobutyl cyanide were weighed by weight and added to a reactor and stirred at a stirring rate of 400 rpm. The temperature of the reactor was raised to 50° C. and the reaction was kept warm for 3 hours. After the reactor was cooled to room temperature, the reaction liquid was added to a rotary evaporator with a water bath temperature of 100° C. and distilled under reduced pressure until no liquid was extracted to obtain 96.8 g of an emulsion precursor;
[0142] 36.0 g of deionized water and 12.0 g of activated hollow glass microspheres were weighed by weight and added to a reactor. After stirring at room temperature at a stirring rate of 120 rpm for 15 min, the temperature of the reactor was raised to 70°C, and the stirring rate was raised to 1000 rpm. 94.0 g of emulsion precursor and 4.0 g of triethylamine were continued to be added thereto. After the reaction was kept warm for 3 hours, the reactor was cooled to room temperature, and the reaction liquid was placed in a vacuum drying oven at a temperature of 40°C and vacuum dried until the mass reduction of the reaction liquid was less than 10 mg / min, to obtain 103.5 g of polyacrylate emulsion.
[0143] S2. Preparation of thermal insulation coating
[0144] Weigh 80.0g of polyacrylate emulsion, 6.4g of titanium dioxide, 7.2g of nano-alumina, 6.4g of talc, 3.6g of polyvinyl alcohol, 4.2g of isooctyl polyoxyethylene ether, 2.4g of polydimethylsiloxane and 2.4g of polyethylene glycol by weight, add them into a reaction kettle and mix evenly, pass through a 100-mesh sieve to obtain a thermal insulation coating.
[0145] S3, spray paint
[0146] Select a spray gun with a nozzle diameter of 1.6mm, a spraying pressure of 40psi, a distance of 30cm between the spray gun and the substrate, a spray gun movement speed of 50cm / min, and a coating thickness of 25mm. After spraying, place the material in an oven at a temperature of 30°C and a relative humidity of 50% to dry for 4 hours. After drying, cure it at room temperature for 24 hours to obtain a material with a surface coated with thermal insulation coating.
[0147] Example 6
[0148] This embodiment is used to provide a method for preparing a novel thermal insulation coating.
[0149] S1. Preparation of polyacrylate emulsion
[0150] 16.0 g of hollow glass microspheres and 36.0 g of 2 mol / L sodium hydroxide solution were weighed and placed in a reactor, the temperature of the reactor was raised to 70° C., and the reaction was kept warm for 1 hour. After the reactor was cooled to room temperature, the reaction liquid was filtered to collect the filter cake, and the filter cake was washed with deionized water for 4 times, and then placed in a drying oven at a temperature of 80° C. and vacuum dried until the filter cake had a constant weight, to obtain 16.4 g of activated hollow glass microspheres;
[0151] 78.0 g of alkyl polyether modified fluorosilicone oil, 16.0 g of modified emulsifier and 6.0 g of 3,4-difluorostyrene were weighed and added to a reaction kettle, and stirred at room temperature for 2 h at a stirring rate of 1100 rpm to obtain 98.3 g of reaction precursor solution;
[0152] 80.0 g of reaction precursor liquid, 48.0 g of dimethyl sulfoxide, 14.0 g of 2-methyl-2-acrylic acid-2,3-dihydroxypropyl ester, 6.0 g of isocyanate methyltrimethoxysilane and 2.4 g of azobisisobutyl cyanide were weighed by weight and added to a reactor and stirred at a stirring rate of 400 rpm. The temperature of the reactor was raised to 40° C. and the reaction was kept warm for 2 h. After the reactor was cooled to room temperature, the reaction liquid was added to a rotary evaporator with a water bath temperature of 90° C. and distilled under reduced pressure until no liquid was extracted to obtain 98.3 g of an emulsion precursor;
[0153] 42.0 g of deionized water and 14.0 g of activated hollow glass microspheres were weighed by weight and added to a reactor. After stirring at room temperature at a stirring rate of 110 rpm for 13 min, the temperature of the reactor was raised to 60°C, and the stirring rate was raised to 900 rpm. 92.0 g of emulsion precursor and 4.0 g of triethylamine were continued to be added thereto. After the reaction was kept warm for 3 hours, the reactor was cooled to room temperature, and the reaction liquid was placed in a vacuum drying oven at a temperature of 35°C and vacuum dried until the mass reduction of the reaction liquid was less than 10 mg / min, to obtain 104.5 g of polyacrylate emulsion.
[0154] S2. Preparation of thermal insulation coating
[0155] Weigh 80.0g of polyacrylate emulsion, 6.4g of titanium dioxide, 7.2g of nano-alumina, 6.4g of talc, 3.6g of polyvinyl alcohol, 4.2g of isooctyl polyoxyethylene ether, 3.6g of polydimethylsiloxane and 2.4g of polyethylene glycol by weight, add them into a reaction kettle and mix evenly, pass through a 100-mesh sieve to obtain a thermal insulation coating.
[0156] S3, spray paint
[0157] Select a spray gun with a nozzle diameter of 1.5mm, a spraying pressure of 35psi, a distance of 28cm between the spray gun and the substrate, a spray gun movement speed of 40cm / min, and a coating thickness of 23mm. After spraying, place the material in an oven at a temperature of 25°C and a relative humidity of 35% to dry for 3h. After drying, cure it at room temperature for 24h to obtain a material with a surface coated with thermal insulation coating.
[0158] Comparative Example 1
[0159] The difference between this comparative example and Example 6 is that in step S1, an equal amount of the modified emulsifier precursor prepared in Example 3 is used to replace the modified emulsifier prepared in Example 3.
[0160] Comparative Example 2
[0161] The difference between this comparative example and Example 6 is that in step S1, an equal amount of polyether-modified silicone oil Silwet L-77 is used to replace the modified emulsifier prepared in Example 3.
[0162] Comparative Example 3
[0163] The difference between this comparative example and Example 6 is that in step S1, ethanol is used to replace the alkyl polyether modified fluorosilicone oil.
[0164] Performance Testing:
[0165] The wear resistance, corrosion resistance, oxidation resistance, and thermal insulation performance of the materials coated with the thermal insulation coatings prepared in Examples 4-6 and Comparative Examples 1-3 were tested:
[0166] The wear resistance of the coating is measured with reference to the standard YY / T 0988.15-2016 “Surgical implant coatings Part 15: Test method for wear resistance of metallic thermal spray coatings”.
[0167] The corrosion resistance of the coating is tested with reference to the standard JB / T 6073-1992 “Laboratory Full Immersion Corrosion Test for Metal Coverings”.
[0168] The antioxidant capacity refers to the standard JB / T 10458-2004 "Technical Conditions for High-temperature Oxidation Resistant Coatings for Mechanical Equipment" to test the state of the coating after high-temperature oxidation treatment at 120°C.
[0169] Thermal insulation performance The thermal conductivity of the sample was measured according to the standard GB / T 10297-2015 "Determination of thermal conductivity of non-metallic solid materials - hot wire method". The specific results are shown in Table 1.
[0170] Table 1-Test data table of each test sample
[0171]
[0172]
[0173] Data Analysis:
[0174] Comparative analysis of the data in Table 1 above shows that the thermal insulation coating prepared by the present invention has a mass loss of only 3.0 mg after 100 cycles of wear and tear, a corrosion rate of only 0.31%, and no powdering, bubbles, shedding, or bottom exposure after 120°C high-temperature oxidation treatment, and a thermal conductivity of only 0.048, and all performances are better than those of the comparative example;
[0175] The invention is described as follows: a modified emulsifier is prepared which has excellent high temperature resistance, corrosion resistance and wear resistance and can be used as a part of a polyacrylate segment, so that the performance of polyacrylate droplets is significantly improved; the silane coupling agent on the hydrophilic segment is cross-linked with the modified hollow glass microspheres, and finally a polyacrylate emulsion with a droplet structure of "lipophilic in the shell and internal filling" is obtained. After being evenly mixed with auxiliary materials, it is sieved to obtain a wear-resistant, high temperature oxidation-resistant, thermal insulating and corrosion-resistant coating.
[0176] The above contents are merely examples and explanations of the structure of the present invention. The technicians in this technical field may make various modifications or additions to the specific embodiments described or replace them in a similar manner. As long as they do not deviate from the structure of the invention or exceed the scope defined by the claims, they should all fall within the protection scope of the present invention.
[0177] In the description of this specification, the description with reference to the terms "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.
[0178] The preferred embodiments of the present invention disclosed above are only used to help explain the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the invention to only specific implementation methods. Obviously, many modifications and changes can be made according to the content of this specification. This specification selects and specifically describes these embodiments in order to better explain the principles and practical applications of the present invention, so that those skilled in the art can understand and use the present invention well. The present invention is limited only by the claims and their full scope and equivalents.
Claims
1. A new type of thermal insulation coating, characterized in that: The invention comprises the following components in parts by weight: 60-80 parts of polyacrylate emulsion, 6-7 parts of titanium dioxide, 7-8 parts of nano-aluminum oxide, 6-8 parts of talc, 2-5 parts of dispersant, 3-5 parts of stabilizer, 2-5 parts of leveling agent and 2-3 parts of anti-sticking agent; The dispersant is one or more of polyvinyl alcohol, sodium polyacrylate, and polyvinyl ether; the stabilizer is one or more of isooctyl polyoxyethylene ether, dodecyl polyoxyethylene ether, and fatty alcohol polyoxyethylene ether; the leveling agent is one or more of polydimethylsiloxane, polymethylsiloxane, and polyvinyl siloxane; and the anti-sticking agent is one or more of polyvinyl alcohol, polyethylene glycol, and polypropylene glycol.
2. A novel heat insulation coating according to claim 1, characterized in that: The preparation method of polyacrylate emulsion comprises the following steps: A1. Weigh 10-20 parts of hollow glass microspheres and 30-40 parts of 0.5-2 mol / L sodium hydroxide solution in parts by weight and place them in a reactor. The temperature of the reactor is raised to 60-80° C. and the reaction is kept warm for 1-2 hours. The modified hollow glass microspheres are obtained by post-treatment. A2, weighing 30-40 parts of alkyl polyether modified fluorosilicone oil, 5-8 parts of modified emulsifier and 2-3 parts of 3,4-difluorostyrene by weight, adding them into a reaction kettle, stirring at room temperature for 1-2 hours at a stirring rate of 1000-1200 rpm to obtain a reaction precursor solution; 30-40 parts of reaction precursor liquid, 20-30 parts of dimethyl sulfoxide, 6-8 parts of 2-methyl-2-acrylic acid-2,3-dihydroxypropyl ester, 3-4 parts of isocyanate methyltrimethoxysilane and 1-2 parts of azobisisobutyl cyanide were weighed and added into a reaction kettle and stirred at a stirring rate of 300-400 rpm. The temperature of the reaction kettle was raised to 30-50° C., and the reaction was kept warm for 1-3 hours, and an emulsion precursor was obtained by post-treatment; A4. Weigh 10-30 parts of deionized water and 5-8 parts of activated hollow glass microspheres by weight and add them to a reactor. Stir at a stirring rate of 100-120 rpm for 10-15 minutes at room temperature. Then, the temperature of the reactor rises to 50-70° C. and the stirring rate rises to 800-1000 rpm. Continue to add 40-60 parts of emulsion precursor and 1-3 parts of triethylamine. After keeping the temperature for reaction for 2-3 hours, post-treat to obtain a polyacrylate emulsion.
3. A novel heat insulation coating according to claim 2, characterized in that: The preparation method of the modified emulsifier is as follows: 20-30 parts of the modified emulsifier precursor, 2-3 parts of 3-isocyanate propylene and 40-60 parts of dimethyl sulfoxide are weighed and added into a reactor, the temperature of the reactor is increased to 50-70° C., the reaction is kept warm for 1-3 hours, and the modified emulsifier is obtained by post-treatment.
4. A novel heat insulation coating according to claim 3, characterized in that: The preparation method of the modified emulsifier precursor comprises the following steps: B1. Weigh 8-10 parts by weight of phosphated silicone oil, 3-5 parts of hexaphenyldisiloxane, 20-25 parts of 2,4,6,8-tetramethyl-2,4,6,8-tetrakis(3,3,3-trifluoropropyl)cyclotetrasiloxane and 40-50 parts of ether into a reaction kettle, and stir at room temperature for 15-20 minutes to obtain a reaction precursor solution; B2, weighing 20-30 parts of the reaction precursor solution and 2-3 parts of 98wt% sulfuric acid solution by weight, adding them into the reaction kettle, and keeping the temperature at room temperature for 8-10 hours to obtain a reaction solution; B3. Add solid sodium bicarbonate to the reaction kettle containing the reaction solution until the pH of the reaction solution reaches 7-8, and then perform post-treatment to obtain a modified emulsifier precursor.
5. A novel heat insulation coating according to claim 4, characterized in that: The preparation method of phosphated silicone oil is as follows: 10-15 parts of chain-extending silicone oil, 2-3 parts of diethyl phosphate, 0.5-0.8 parts of triethylamine and 30-40 parts of dimethyl sulfoxide are weighed by weight and added into a reaction kettle, the temperature of the reaction kettle is increased to 60-80° C., the reaction is kept warm for 1-3 hours, and the phosphated silicone oil is obtained by post-treatment.
6. The novel heat insulation coating according to claim 5 is characterized in that: The preparation method of the chain-extending silicone oil is as follows: 8-10 parts of amidated silicone oil, 1-2 parts of 2,3-epoxypropionaldehyde, 1-2 parts of 1-acetyl-2-ethyloxirane, 0.1-0.3 parts of γ-alumina and 30-40 parts of dimethyl sulfoxide are weighed by weight and added into a reactor, the temperature of the reactor is increased to 60-80°C, the reaction is kept warm for 2-3 hours, and the chain-extending silicone oil is obtained by post-treatment.
7. The novel heat insulation coating according to claim 6 is characterized in that: The preparation method of the amidated silicone oil is as follows: 20-30 parts of modified silicone oil, 5-10 parts of acetic acid and 75-100 parts of dimethyl sulfoxide are weighed by weight and added into a reaction kettle, stirred at room temperature for 5-10 minutes, the temperature of the reaction kettle is lowered to 0-5°C, 1-2 parts of 1-hydroxybenzotriazole, 1-2 parts of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride and 1-2 parts of N-methylmorphine are added thereto, the reaction is kept warm for 1-2 hours, and the amidated silicone oil is obtained by post-treatment.
8. The novel heat insulation coating according to claim 7 is characterized in that: The preparation method of modified silicone oil is as follows: 10-15 parts of functional silicone oil, 1-2 parts of trimethylchlorosilane and 0.3-0.5 parts of triethylamine are weighed by weight and added into a reactor, the temperature of the reactor is increased to 40-60° C., the reaction is kept warm for 1-3 hours, and the modified silicone oil is obtained by post-treatment.
9. The novel heat insulation coating according to claim 8 is characterized in that: The preparation method of the functionalized silicone oil is as follows: 8-10 parts by weight of methyl high hydrogen silicone oil, 1-2 parts of allylamine, 2-3 parts of 1,1,1-trifluoro-2-phenyl-3-butene-2-ol, 0.5-1.5 parts of chloroplatinic acid and 40-50 parts of xylene are added into a reactor, the temperature of the reactor is increased to 50-60°C, and the functionalized silicone oil is obtained by post-treatment.
Citation Information
Patent Citations
Thiadiazolidinone inhibitors of ptpase
CN101421256A
Low-voltage antistatic anti-interference power distribution cabinet and preparation method thereof
CN105837981A
Fluorine-containing hydroxylpolyacrylate aqueous dispersion with high solid content and preparation method and application thereof
CN110256625A
Thermal insulation coating and preparation method thereof
CN111925704A
Hydrophobic fluorine-modified acrylic emulsion as well as preparation method and application thereof
CN111978455A