CN109535811B - Thermal insulation exterior wall putty powder and preparation method thereof - Google Patents
Thermal insulation exterior wall putty powder and preparation method thereof Download PDFInfo
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- CN109535811B CN109535811B CN201910029281.6A CN201910029281A CN109535811B CN 109535811 B CN109535811 B CN 109535811B CN 201910029281 A CN201910029281 A CN 201910029281A CN 109535811 B CN109535811 B CN 109535811B
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Abstract
The invention discloses heat-insulating exterior wall putty powder and a preparation method thereof, belonging to the technical field of building materials. The invention utilizes the good adhesive property of dopamine for grafting, and maintains the internal structure of the hardened putty powder, so that the putty powder forms a hydrated gelled material with strong cohesive force and good flowing property. Utilize capric acid, lauric acid etc. to get into the heat conduction passageway, can absorb or release the heat and reach the heat balance and keep warm, improved the heat preservation effect, fill the hole of putty powder outer wall, improve closely knit degree. The polymethyl vinyl siloxane elastomer and the introduced vinyl form crosslinking, so that the drying shrinkage cracking is reduced, and the mechanical property of the putty powder is improved. The light has a fast propagation speed, and the light can fast penetrate through the putty powder to carry out photo-thermal conversion, so that the light effect and the heat storage and insulation performance of the outer wall are further improved. The invention solves the problem of poor heat preservation and insulation effect of the existing exterior wall putty powder.
Description
Technical Field
The invention belongs to the technical field of building materials, and particularly relates to thermal insulation exterior wall putty powder and a preparation method thereof.
Background
The putty powder is the most commonly used one in building decoration materials, and the main components are talcum powder and glue. The putty is a base material for repairing and leveling wall, and provides a good foundation for next decoration (painting and wallpaper). The putty is divided into an inner wall and an outer wall, and the putty for the outer wall has large adhesiveness, high strength and slightly low environmental protection index because the putty for the outer wall resists wind, wind and sun. The interior wall putty has better comprehensive index, is healthy and environment-friendly, so the interior wall is not externally used, and the exterior wall is not internally used. Typically, the putty is gypsum or cement based so that the surface roughness is easier to bond firmly. However, during construction, a layer of interface agent is coated on the base layer to seal the base layer and improve the adhesion of the wall surface, so that the putty can be better bonded on the base surface. The existing flexible putty powder for external walls is mostly prepared by mixing heavy calcium carbonate, white cement, organic additives and the like, and is mainly used as a leveling material for the external wall surfaces. The quality of exterior wall putty directly influences the decoration and durability of a coating veneer, exterior wall putty or interior wall putty with poor service performance is used externally, and finally, wall surface falling, hollowing and cracking occur soon after the project is delivered and used, and a local or large-area coating loses the original decoration and protection functions, so that the normal use of a building is seriously influenced. The quality requirements of the exterior wall putty in the building engineering are mainly reflected on the indexes of bonding strength, initial cracking resistance, dynamic cracking resistance and the like, and the bonding strength is one of important technical indexes. In the construction, the putty is often incapable of being normally attached to the surface of a wall body due to poor quality of putty products, so that the surface layer of the putty is pulverized or falls off, even peels, and a foaming mark is left after drying. The existing building waterproof material and the existing heat insulation material have single performance, are waterproof, do not preserve heat, are heat-preserving and waterproof, can not be combined with a wall body into a whole for some times, have poor strength and applicability and have high cost. With the rapid development of the building industry, various building coatings emerge like bamboo shoots in the spring after rain, and the consumption requirements of different levels of each level are met. Along with the development of the coating and the continuous improvement of the living standard of people, the requirements of people on the traditional construction method of the coating and the quality of the coating are higher and higher.
At present, most of building heat insulation materials are prepared by jointly acting two products, namely heat insulation paint and products thereof and facing putty, on the surface of a wall body, but the problems of insecure structure, easy peeling and cracking, short service life and the like exist, and safety accidents are often caused by cracking and falling off.
At present, the heat energy in the air is transferred by three ways of conduction, convection and radiation, and the transfer of the radiation heat accounts for more than 90%. In order to slow down or organize the heat transfer, a heat insulation material is required to be arranged on the outer surface of the building, so that the heat insulation performance of the outer wall can be greatly improved in summer, and the heat insulation performance of the wall body can be obviously improved in winter. The traditional heat insulation building materials are all solid plate-shaped and are pasted on the outer side of a wall body of a building, so that the construction is complex, the construction period is long, the cost is high, and unstable factors such as falling from an outer wall easily for a long time and the like can be caused. The liquid heat-insulating putty powder comprises barrier heat-insulating putty powder, reflection heat-insulating putty powder and radiation heat-insulating putty powder. The three kinds of heat insulation putty powder have different heat insulation principles, so that the application occasions are different, and the heat insulation effect is not ideal. Therefore, a new putty powder for heat insulation and preservation of exterior walls is needed to be developed.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the problem of poor heat preservation and insulation effects of the existing exterior wall putty powder, the heat preservation exterior wall putty powder and the preparation method thereof are provided.
In order to solve the technical problems, the invention adopts the following technical scheme:
the heat-insulating exterior wall putty powder comprises a putty powder base material, cellulose ether, redispersible rubber powder, polydimethyldiallyl ammonium chloride, a cracking additive, an auxiliary heat-conducting agent and a component crosslinking active agent;
the preparation method of the anti-cracking additive comprises the following steps: taking polyacrylamide according to the mass ratio of 1-4: 10-30, adding N-methyl pyrrolidone, stirring and mixing at 20-25 ℃, adding an activating agent accounting for 50-60% of the mass of the polyacrylamide, stirring and mixing at 30-40 ℃ to obtain a stirring mixture, and taking the stirring mixture according to the mass ratio of 10-15: 2-7, adding reaction raw materials, introducing nitrogen for protection, stirring and mixing at 20-25 ℃, adjusting the pH to 2-3 to obtain a stirring mixture a, and taking the stirring mixture a according to the mass ratio of 3-7: 10-20, adding ethyl acetate, standing, and drying the precipitate to obtain the anti-cracking additive.
The activating agent is: taking 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride according to a mass ratio of 3-7: 2-5: and (1) adding N-hydroxysuccinimide and 1-hydroxybenzotriazole to mix, thus obtaining the compound.
The preparation method of the reaction raw materials comprises the following steps: taking sodium tetraborate according to a mass ratio of 1-3: 0.2-0.5: 20-30, adding sodium bicarbonate and N-methyl pyrrolidone, stirring and mixing to obtain a mixture, and mixing the mixture according to a mass ratio of 20-40: and (3) adding dopamine hydrochloride into the mixture at 1-5 ℃, and stirring and mixing the mixture at 20-30 ℃ to obtain a reaction raw material.
The preparation method of the auxiliary heat conducting agent comprises the following steps: taking graphene oxide according to a mass ratio of 3-7: 10-30, adding deionized water, performing ultrasound to obtain an ultrasound solution, and taking carbon fibers according to a mass ratio of 2-7: 3-5: 10-20, adding corn straws and absolute ethyl alcohol, and performing ultrasonic treatment to obtain ultrasonic liquid a, wherein the ultrasonic liquid is prepared from the following components in a mass ratio of 5-10: 2-7, adding the ultrasonic liquid a, mixing, adding a phase change active agent accounting for 20-40% of the mass of the ultrasonic liquid, oscillating, performing suction filtration, taking suction filtration residues, and performing vacuum drying to obtain the auxiliary heat conducting agent.
The phase change active agent is: mixing 10-20 parts by weight of capric acid, 5-10 parts by weight of lauric acid, 3-7 parts by weight of myristic acid, 2-5 parts by weight of palmitic acid and 10-15 parts by weight of disodium hydrogen phosphate dodecahydrate.
The preparation method of the component crosslinking activator comprises the following steps:
(1) taking 100-130 parts of p-toluic acid, 100-110 parts of hydroquinone, 100-150 parts of methylbenzene and 20-60 parts of carbon tetrachloride, stirring and mixing at 30-50 ℃ to obtain a mixture a, and taking the mixture a according to a mass ratio of 90-120: 1-5, adding a catalyst, introducing nitrogen for protection, stirring and mixing at 50-80 ℃, filtering, washing filter residues, and drying to obtain a dried substance;
(2) taking a dried substance according to a mass ratio of 2-7: 10-15, adding a solvent, adding triethylamine with the mass of 5-10% of that of the dry substance, stirring and mixing at 0-4 ℃ to obtain a mixed solution, and taking acryloyl chloride according to the mass ratio of 2-7: 20-30, stirring and mixing at 0-5 ℃, carrying out suction filtration, washing the filtrate with a sodium bicarbonate solution, carrying out suction filtration, washing the filter residue a with absolute ethyl alcohol, and drying to obtain the component crosslinking activator.
The putty powder for exterior walls insulation according to claim 6, wherein the catalyst in the step (1) is: taking boric acid according to the mass ratio of 3-9: and 2-5, adding sulfuric acid and mixing to obtain the catalyst.
The solvent in the step (2) is as follows: taking tetrahydrofuran according to a mass ratio of 5-10: and 3-5, adding N, N-dimethylformamide and mixing to obtain the finished product.
The putty powder base material comprises: according to the mass parts, 200-300 parts of ordinary portland cement, 20-50 parts of fly ash, 20-40 parts of heavy calcium carbonate, 15-20 parts of quartz powder, 20-40 parts of talcum powder and 30-50 parts of coal gangue are mixed to obtain the cement.
The preparation method comprises the following steps:
s1, mixing 5-10 parts of a cross-linking active agent, 10-15 parts of polymethylvinylsiloxane, 20-30 parts of hydrogen-containing silicone oil, 0.5-1 part of benzoyl peroxide and 70-100 parts of toluene according to parts by weight to obtain a matrix, adding chloroplatinic acid accounting for 1-5% of the matrix, heating to 70-80 ℃, stirring and mixing, carrying out reduced pressure distillation, and drying to obtain a dried substance a;
s2, mixing 200-400 parts of putty powder base material, 20-40 parts of anti-cracking additive, 30-50 parts of auxiliary heat conducting agent, 3-8 parts of dry matter a, 1-4 parts of cellulose ether, 30-40 parts of redispersible rubber powder and 5-10 parts of poly dimethyl diallyl ammonium chloride according to parts by weight to obtain the heat-insulating exterior wall putty powder.
Compared with other methods, the method has the beneficial technical effects that:
(1) the anti-cracking additive prepared by the invention is prepared by ionizing-COOH into-COO in the process of forming hydrate by using polyacrylic acid under the alkali excitation condition of putty powder-In the presence of water, a physical and chemical reaction is generated to form a polymer film and cement gel which are mutually interpenetrated to form a composite matrix phase with a network structure, grafting is carried out by utilizing the better adhesive property of dopamine, sodium borate and sodium bicarbonate are added in the process to form a complex compound to protect dopamine, the complex compound is grafted to a molecular chain of polyacrylic acid, the dopamine has better hydrophilic property, part of water is adsorbed in the network structure in the hydration process, the drying cracking of the hardened putty powder is reduced, the internal structure of the hardened putty powder is maintained, and meanwhile, the hydrated cross-linked network is densified by utilizing the adhesive property of the dopamine, the intermolecular hydrogen bonding effect is enhanced, so that the putty powder forms a hydrated gelled material with strong cohesive force and better flowing property;
(2) the auxiliary heat conducting agent prepared by the invention takes graphene oxide, carbon fiber and corn straw as heat conducting base materials, a bridge structure is formed among the carbon fiber, the graphene oxide and the corn straw by utilizing larger specific surface area and more pores of the graphene and the corn straw, the filling effect on air bag cavities in the graphene is realized, a heat conducting channel is formed, the mechanical property is enhanced, the existence of the carbon fiber enables heat to rapidly pass through the carbon fiber, the influence of air bag cavities is avoided, the heat can rapidly enter the heat conducting channel, carbohydrate in the corn straw has an inhibiting effect on putty powder hydration, a certain water reducing effect is realized, the performance of the putty powder is improved, meanwhile, a phase change active agent is added, capric acid, lauric acid and the like are used for entering the heat conducting channel, the phase change latent heat of the heat conducting agent is utilized, the heat can be absorbed or released in three changes of solid-liquid, solid-solid and liquid-gas to achieve heat balance for heat preservation, the heat preservation effect is improved, calcium carbonate is formed by acid in the phase change activator and a part of hydration products, the pores of the putty powder outer wall are filled, and the compactness is improved;
(3) the added component crosslinking activator takes polymethyl vinyl siloxane elastomer as a main chain, p-toluic acid, acryloyl chloride and the like are added as raw materials to carry out amidation reaction to form a vinyl-terminated crosslinking activator, the vinyl-terminated crosslinking activator, polymethyl vinyl siloxane and hydrogen-containing silicone oil are initiated to form an elastomer with a three-dimensional network structure, on one hand, the silicone chain segments are utilized to reduce the contact surface tension among the components, and the polymethyl vinyl siloxane elastomer and the introduced vinyl are utilized to form crosslinking to ensure the connection of rigid and flexible chain segments, the obtained crosslinking component is utilized to relieve the expansion stress in the hydration process, the shrinkage cracking is reduced, the mechanical property of putty powder is increased, the cracking is prevented, on the other hand, the obtained component crosslinking activator has optical anisotropy, and the crosslinked silicone elastomer is in a liquid crystal state, the light has a fast propagation speed, and the light can fast penetrate through the putty powder to carry out photo-thermal conversion, so that the light effect and the heat storage and insulation performance of the outer wall are further improved.
Detailed Description
The activating agent is: taking 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride according to a mass ratio of 3-7: 2-5: and (1) adding N-hydroxysuccinimide and 1-hydroxybenzotriazole to mix, thus obtaining the compound.
The preparation method of the reaction raw materials comprises the following steps: taking sodium tetraborate according to a mass ratio of 1-3: 0.2-0.5: adding sodium bicarbonate and N-methyl pyrrolidone into the mixture 20-30, stirring and mixing for 20-30 min to obtain a mixture, and mixing the mixture according to a mass ratio of 20-40: and (3) adding dopamine hydrochloride into the mixture 1-5, and stirring and mixing the mixture at the temperature of 20-30 ℃ for 20-40 min to obtain a reaction raw material.
The preparation method of the anti-cracking additive comprises the following steps: taking polyacrylamide according to the mass ratio of 1-4: 10-30, adding N-methyl pyrrolidone, stirring and mixing at 20-25 ℃ for 18-24 h, adding an activating agent accounting for 50-60% of the mass of polyacrylamide, stirring and mixing at 30-40 ℃ for 1-3 h to obtain a stirring mixture, and taking the stirring mixture according to the mass ratio of 10-15: 2-7, adding reaction raw materials, introducing nitrogen for protection, stirring and mixing at 20-25 ℃ for 12-18 h, adjusting the pH to 2-3 to obtain a stirring mixture a, and taking the stirring mixture a according to the mass ratio of 3-7: and 10-20, adding ethyl acetate, standing for 40-80 min, and drying the precipitate to obtain the anti-cracking additive.
The phase change active agent is: mixing 10-20 parts by weight of capric acid, 5-10 parts by weight of lauric acid, 3-7 parts by weight of myristic acid, 2-5 parts by weight of palmitic acid and 10-15 parts by weight of disodium hydrogen phosphate dodecahydrate.
The preparation method of the auxiliary heat conducting agent comprises the following steps: taking graphene oxide according to a mass ratio of 3-7: 10-30, adding deionized water, performing ultrasound for 60-90 min to obtain an ultrasound solution, and taking carbon fibers according to a mass ratio of 2-7: 3-5: 10-20, adding corn straws and absolute ethyl alcohol, and carrying out ultrasonic treatment for 30-60 min to obtain ultrasonic liquid a, wherein the ultrasonic liquid is prepared from the following components in a mass ratio of 5-10: 2-7, adding the ultrasonic liquid a, mixing, adding a phase change active agent accounting for 20-40% of the mass of the ultrasonic liquid, oscillating for 30-50 min, carrying out suction filtration, taking suction filtration residues, and carrying out vacuum drying to obtain the auxiliary heat conducting agent.
The catalyst is as follows: taking boric acid according to the mass ratio of 3-9: and 2-5, adding 98% sulfuric acid in parts by weight, and mixing to obtain the catalyst.
The solvent is as follows: taking tetrahydrofuran according to a mass ratio of 5-10: and 3-5, adding N, N-dimethylformamide and mixing to obtain the finished product.
The preparation method of the component crosslinking activator comprises the following steps:
(1) taking 100-130 parts of p-toluic acid, 100-110 parts of hydroquinone, 100-150 parts of methylbenzene and 20-60 parts of carbon tetrachloride, stirring and mixing at 30-50 ℃ for 20-40 min to obtain a mixture a, and taking the mixture a according to a mass ratio of 90-120: 1-5, adding a catalyst, introducing nitrogen for protection, stirring and mixing at 50-80 ℃ for 2-4 hours, filtering, washing filter residues with ethanol with the mass fraction of 60%, and drying to obtain a dried substance;
(2) taking a dried substance according to a mass ratio of 2-7: 10-15, adding a solvent, adding triethylamine with the mass of 5-10% of that of the dry substance, stirring and mixing at 0-4 ℃ for 30-60 min to obtain a mixed solution, and taking acryloyl chloride according to the mass ratio of 2-7: and 20-30, adding the mixed solution, stirring and mixing at 0-5 ℃ for 1-3 h, carrying out suction filtration, washing the filtrate by using a sodium bicarbonate solution with the mass fraction of 5%, carrying out suction filtration, washing and drying the filter residue a by using absolute ethyl alcohol, and thus obtaining the component crosslinking activator.
Putty powder base material: according to the mass parts, 200-300 parts of ordinary portland cement, 20-50 parts of fly ash, 20-40 parts of heavy calcium carbonate, 15-20 parts of quartz powder, 20-40 parts of talcum powder and 30-50 parts of coal gangue are mixed to obtain the cement.
A preparation method of the thermal insulation exterior wall putty powder comprises the following steps:
s1, mixing 5-10 parts of a cross-linking activator, 10-15 parts of polymethylvinylsiloxane, 20-30 parts of hydrogen-containing silicone oil, 0.5-1 part of benzoyl peroxide and 70-100 parts of toluene according to parts by weight to obtain a matrix, adding chloroplatinic acid accounting for 1-5% of the matrix weight, heating to 70-80 ℃, stirring and mixing for 1-4 hours, carrying out reduced pressure distillation, and drying to obtain a dried substance a;
s2, mixing 200-400 parts of putty powder base material, 20-40 parts of anti-cracking additive, 30-50 parts of auxiliary heat conducting agent, 3-8 parts of dry matter a, 1-4 parts of cellulose ether, 30-40 parts of redispersible rubber powder and 5-10 parts of poly dimethyl diallyl ammonium chloride according to parts by weight to obtain the heat-insulating exterior wall putty powder.
The activating agent is: taking 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride according to a mass ratio of 3: 2: 1, adding N-hydroxysuccinimide and 1-hydroxybenzotriazole and mixing to obtain the product.
The preparation method of the reaction raw materials comprises the following steps: taking sodium tetraborate according to the mass ratio of 1: 0.2: 20, adding sodium bicarbonate and N-methylpyrrolidone, stirring and mixing for 20min to obtain a mixture, and mixing the mixture according to a mass ratio of 20: 1 adding dopamine hydrochloride, stirring and mixing for 20min at 20 ℃ to obtain the reaction raw material.
The preparation method of the anti-cracking additive comprises the following steps: taking polyacrylamide according to the mass ratio of 1: 10, adding N-methyl pyrrolidone, stirring and mixing for 18h at 20 ℃, adding an activating agent accounting for 50% of the mass of the polyacrylamide, stirring and mixing for 1h at 30 ℃ to obtain a stirring mixture, and taking the stirring mixture according to the mass ratio of 10: 2, adding reaction raw materials, introducing nitrogen for protection, stirring and mixing at 20 ℃ for 12 hours, adjusting the pH value to 2 to obtain a stirring mixture a, and taking the stirring mixture a according to a mass ratio of 3: 10 adding ethyl acetate, standing for 40min, and drying the precipitate to obtain the anti-cracking additive.
The phase change active agent is: and mixing 10 parts by weight of capric acid, 5 parts by weight of lauric acid, 3 parts by weight of myristic acid, 2 parts by weight of palmitic acid and 10 parts by weight of disodium hydrogen phosphate dodecahydrate.
The preparation method of the auxiliary heat conducting agent comprises the following steps: taking graphene oxide according to a mass ratio of 3: 10, adding deionized water, performing ultrasonic treatment for 60min to obtain ultrasonic liquid, and taking carbon fibers according to a mass ratio of 2: 3: 10, adding corn straws and absolute ethyl alcohol, performing ultrasonic treatment for 30min to obtain ultrasonic liquid a, and taking the ultrasonic liquid according to a mass ratio of 5: 2, adding the ultrasonic liquid a, mixing, adding a phase change active agent accounting for 20% of the mass of the ultrasonic liquid, oscillating for 30min, carrying out suction filtration, taking suction filtration residues, and carrying out vacuum drying to obtain the auxiliary heat conducting agent.
The catalyst is as follows: taking boric acid according to the mass ratio of 3: 2 adding 98% sulfuric acid in parts by mass and mixing to obtain the product.
The solvent is as follows: taking tetrahydrofuran according to a mass ratio of 5: 3 adding N, N-dimethylformamide and mixing to obtain the finished product.
The preparation method of the component crosslinking activator comprises the following steps:
(1) taking 100 parts of p-toluic acid, 100 parts of hydroquinone, 100 parts of methylbenzene and 20 parts of carbon tetrachloride, stirring and mixing for 20min at 30 ℃ to obtain a mixture a, and taking the mixture a according to a mass ratio of 90: 1, adding a catalyst, introducing nitrogen for protection, stirring and mixing at 50 ℃ for 2 hours, filtering, washing filter residues with ethanol with the mass fraction of 60%, and drying to obtain a dried substance;
(2) taking a dried substance according to the mass ratio of 2: 10 adding a solvent, adding triethylamine with the mass of 5% of that of the dry substance, stirring and mixing for 30min at 0 ℃ to obtain a mixed solution, and taking acryloyl chloride according to the mass ratio of 2: 20, adding the mixed solution, stirring and mixing for 1h at 0 ℃, carrying out suction filtration, washing the filtrate by using a sodium bicarbonate solution with the mass fraction of 5%, carrying out suction filtration, washing and drying the filter residue a by using absolute ethyl alcohol, and thus obtaining the component crosslinking activator.
Putty powder base material: according to the mass parts, 200 parts of ordinary portland cement, 20 parts of fly ash, 20 parts of heavy calcium carbonate, 15 parts of quartz powder, 20 parts of talcum powder and 30 parts of coal gangue are mixed to obtain the cement.
A preparation method of the thermal insulation exterior wall putty powder comprises the following steps:
s1, mixing 5 parts of a crosslinking activator, 10 parts of polymethylvinylsiloxane, 20 parts of hydrogen-containing silicone oil, 0.5 part of benzoyl peroxide and 70 parts of toluene in parts by mass to obtain a matrix, adding chloroplatinic acid accounting for 1% of the mass of the matrix, heating to 70 ℃, stirring and mixing for 1 hour, and carrying out reduced pressure distillation and drying to obtain a dried substance a;
s2, mixing 200 parts of putty powder base material, 20 parts of anti-cracking additive, 30 parts of auxiliary heat conducting agent, 3 parts of dry matter a, 1 part of cellulose ether, 30 parts of redispersible rubber powder and 5 parts of poly dimethyl diallyl ammonium chloride according to parts by weight to obtain the thermal insulation exterior wall putty powder.
The activating agent is: taking 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride according to a mass ratio of 5: 4: 3 adding N-hydroxysuccinimide and 1-hydroxybenzotriazole and mixing to obtain the product.
The preparation method of the reaction raw materials comprises the following steps: taking sodium tetraborate according to the mass ratio of 2: 0.3: adding sodium bicarbonate and N-methylpyrrolidone into the mixture 25, stirring and mixing the mixture for 25min to obtain a mixture, and mixing the mixture according to a mass ratio of 30: 3 adding dopamine hydrochloride, stirring and mixing for 30min at 25 ℃ to obtain the reaction raw material.
The preparation method of the anti-cracking additive comprises the following steps: taking polyacrylamide according to the mass ratio of 3: 20, adding N-methyl pyrrolidone, stirring and mixing for 21h at 22 ℃, adding an activating agent accounting for 55% of the mass of the polyacrylamide, stirring and mixing for 2h at 35 ℃ to obtain a stirring mixture, and taking the stirring mixture according to the mass ratio of 12: 5, adding reaction raw materials, introducing nitrogen for protection, stirring and mixing for 15 hours at the temperature of 22 ℃, adjusting the pH value to 2.5 to obtain a stirring mixture a, and taking the stirring mixture a according to the mass ratio of 5: 15 adding ethyl acetate, standing for 60min, and drying the precipitate to obtain the anti-cracking additive.
The phase change active agent is: and mixing 15 parts of capric acid, 8 parts of lauric acid, 5 parts of myristic acid, 4 parts of palmitic acid and 12 parts of disodium hydrogen phosphate dodecahydrate in parts by weight.
The preparation method of the auxiliary heat conducting agent comprises the following steps: taking graphene oxide according to a mass ratio of 5: 20, adding deionized water, performing ultrasonic treatment for 75min to obtain ultrasonic liquid, and taking carbon fibers according to a mass ratio of 5: 4: 15, adding corn straws and absolute ethyl alcohol, performing ultrasonic treatment for 45min to obtain ultrasonic liquid a, and taking the ultrasonic liquid according to a mass ratio of 8: and 5, adding the ultrasonic liquid a, mixing, adding a phase change active agent accounting for 30% of the mass of the ultrasonic liquid, oscillating for 40min, performing suction filtration, taking suction filtration residues, and performing vacuum drying to obtain the auxiliary heat conducting agent.
The catalyst is as follows: taking boric acid according to the mass ratio of 6: and 4, adding 98% sulfuric acid in parts by mass, and mixing to obtain the product.
The solvent is as follows: taking tetrahydrofuran according to a mass ratio of 8: 4 adding N, N-dimethylformamide and mixing to obtain the finished product.
The preparation method of the component crosslinking activator comprises the following steps:
(1) taking 115 parts of p-toluic acid, 105 parts of hydroquinone, 125 parts of toluene and 40 parts of carbon tetrachloride, stirring and mixing for 30min at 40 ℃ to obtain a mixture a, and taking the mixture a according to the mass ratio of 105: 3 adding a catalyst, introducing nitrogen for protection, stirring and mixing for 3 hours at 65 ℃, filtering, washing filter residues by using ethanol with the mass fraction of 60%, and drying to obtain a dried substance;
(2) taking a dried substance according to the mass ratio of 5: 12 adding a solvent, adding triethylamine with the mass of 8% of that of the dry substance, stirring and mixing for 45min at the temperature of 2 ℃ to obtain a mixed solution, and taking acryloyl chloride according to the mass ratio of 5: adding the mixed solution 25, stirring and mixing for 2h at 3 ℃, carrying out suction filtration, washing the filtrate by using a sodium bicarbonate solution with the mass fraction of 5%, carrying out suction filtration, washing and drying the filter residue a by using absolute ethyl alcohol, and thus obtaining the component crosslinking activator.
Putty powder base material: and mixing 250 parts of ordinary portland cement, 35 parts of fly ash, 30 parts of heavy calcium carbonate, 18 parts of quartz powder, 30 parts of talcum powder and 40 parts of coal gangue according to parts by weight.
A preparation method of the thermal insulation exterior wall putty powder comprises the following steps:
s1, mixing 8 parts of a crosslinking activator, 12 parts of polymethylvinylsiloxane, 25 parts of hydrogen-containing silicone oil, 0.8 part of benzoyl peroxide and 85 parts of toluene in parts by mass to obtain a matrix, adding chloroplatinic acid with the mass of 3% of the matrix, heating to 75 ℃, stirring and mixing for 2 hours, carrying out reduced pressure distillation, and drying to obtain a dried substance a;
s2, mixing 300 parts of putty powder base material, 30 parts of anti-cracking additive, 40 parts of auxiliary heat conducting agent, 5 parts of dry matter a, 2 parts of cellulose ether, 35 parts of redispersible rubber powder and 8 parts of poly dimethyl diallyl ammonium chloride according to parts by weight to obtain the thermal insulation exterior wall putty powder.
The activating agent is: taking 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride according to a mass ratio of 7: 5: 4 adding N-hydroxysuccinimide and 1-hydroxybenzotriazole and mixing to obtain the product.
The preparation method of the reaction raw materials comprises the following steps: taking sodium tetraborate according to the mass ratio of 3: 0.5: 30, adding sodium bicarbonate and N-methyl pyrrolidone, stirring and mixing for 30min to obtain a mixture, and mixing the mixture according to a mass ratio of 40: 5 adding dopamine hydrochloride, stirring and mixing for 40min at 30 ℃ to obtain the reaction raw material.
The preparation method of the anti-cracking additive comprises the following steps: taking polyacrylamide according to a mass ratio of 4: 30, adding N-methyl pyrrolidone, stirring and mixing for 24 hours at 25 ℃, adding an activating agent accounting for 60 percent of the mass of the polyacrylamide, stirring and mixing for 3 hours at 40 ℃ to obtain a stirring mixture, and taking the stirring mixture according to the mass ratio of 15: 7, adding reaction raw materials, introducing nitrogen for protection, stirring and mixing at 25 ℃ for 18h, adjusting the pH value to 3 to obtain a stirring mixture a, and taking the stirring mixture a according to the mass ratio of 7: and 20, adding ethyl acetate, standing for 80min, and drying the precipitate to obtain the anti-cracking additive.
The phase change active agent is: and (2) mixing 20 parts of capric acid, 10 parts of lauric acid, 7 parts of myristic acid, 5 parts of palmitic acid and 15 parts of disodium hydrogen phosphate dodecahydrate in parts by weight.
The preparation method of the auxiliary heat conducting agent comprises the following steps: taking graphene oxide according to a mass ratio of 7: 30, adding deionized water, performing ultrasonic treatment for 90min to obtain ultrasonic liquid, and taking carbon fibers according to a mass ratio of 7: 5: 20, adding corn straws and absolute ethyl alcohol, performing ultrasonic treatment for 60min to obtain ultrasonic liquid a, and taking the ultrasonic liquid according to a mass ratio of 10: 7 adding the ultrasonic liquid a, mixing, adding a phase change active agent accounting for 40% of the mass of the ultrasonic liquid, oscillating for 50min, performing suction filtration, taking suction filtration residues, and performing vacuum drying to obtain the auxiliary heat conducting agent.
The catalyst is as follows: taking boric acid according to the mass ratio of 9: and 5, adding 98% sulfuric acid in parts by mass, and mixing to obtain the product.
The solvent is as follows: taking tetrahydrofuran according to a mass ratio of 10: and 5, adding N, N-dimethylformamide and mixing to obtain the finished product.
The preparation method of the component crosslinking activator comprises the following steps:
(1) according to the mass parts, 130 parts of p-toluic acid, 110 parts of hydroquinone, 150 parts of toluene and 60 parts of carbon tetrachloride are taken, stirred and mixed for 40min at 50 ℃ to obtain a mixture a, and the mixture a is taken according to the mass ratio of 120: 5 adding a catalyst, introducing nitrogen for protection, stirring and mixing at 80 ℃ for 4h, filtering, washing filter residues with 60% ethanol by mass fraction, and drying to obtain a dried substance;
(2) taking a dried substance according to the mass ratio of 7: 15 adding a solvent, adding triethylamine with the mass percent of that of the dry substance, stirring and mixing for 60min at 4 ℃ to obtain a mixed solution, and taking acryloyl chloride according to the mass ratio of 7: 30, adding the mixed solution, stirring and mixing for 3 hours at the temperature of 5 ℃, carrying out suction filtration, washing the filtrate by using a sodium bicarbonate solution with the mass fraction of 5%, carrying out suction filtration, washing and drying the filter residue a by using absolute ethyl alcohol, and thus obtaining the component crosslinking activator.
Putty powder base material: mixing 300 parts of ordinary portland cement, 50 parts of fly ash, 40 parts of heavy calcium carbonate, 20 parts of quartz powder, 40 parts of talcum powder and 50 parts of coal gangue according to parts by weight.
A preparation method of the thermal insulation exterior wall putty powder comprises the following steps:
s1, mixing 10 parts of a crosslinking activator, 15 parts of polymethylvinylsiloxane, 30 parts of hydrogen-containing silicone oil, 1 part of benzoyl peroxide and 100 parts of toluene in parts by mass to obtain a matrix, adding chloroplatinic acid with the mass of 5% of the matrix, heating to 80 ℃, stirring and mixing for 4 hours, carrying out reduced pressure distillation, and drying to obtain a dried substance a;
s2, mixing 400 parts of putty powder base material, 40 parts of anti-cracking additive, 50 parts of auxiliary heat conducting agent, 8 parts of dry matter a, 4 parts of cellulose ether, 40 parts of redispersible rubber powder and 10 parts of poly dimethyl diallyl ammonium chloride according to parts by weight to obtain the thermal insulation exterior wall putty powder.
Comparative example 1: essentially the same procedure as in example 1 was followed except that the crack preventing additive was absent.
Comparative example 2: the preparation process was substantially the same as that of example 1, except that the auxiliary heat conductive agent was absent.
Comparative example 3: essentially the same procedure as in example 1 was followed except that the component crosslinking activator was absent.
Comparative example 4: the putty powder for heat-insulating exterior walls is produced by a company in Hefei City.
The putty powder for the heat-preservation exterior wall obtained in the examples and the comparative examples is tested according to JG/T229-:
table 1:
| test items | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 |
| Coefficient of thermal conductivity (W/m)2.k） | 0.017 | 0.020 | 0.023 | 0.029 | 0.035 | 0.039 | 0.048 |
| Adhesive Strength (MPa) | 1.27 | 1.23 | 1.25 | 1.12 | 1.09 | 1.05 | 0.98 |
| Heat preservation effect | Continuous heat preservation | Continuous heat preservation | Continuous heat preservation | Continuous heat preservation | Slow decline | Slow decline | Faster decline |
| Flexibility | Does not crack | Does not crack | Does not crack | Does not crack | Does not crack | Cracking of | Cracking of |
In conclusion, the thermal insulation exterior wall putty powder obtained by the invention has good thermal insulation effect, better effect compared with the commercially available product, and is worth popularizing.
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, but rather as the subject matter of the invention is to be construed in all aspects and as broadly as possible, and all changes, equivalents and modifications that fall within the true spirit and scope of the invention are therefore intended to be embraced therein.
Claims (3)
1. The thermal insulation exterior wall putty powder comprises a putty powder base material, cellulose ether, redispersible rubber powder and polydimethyldiallyl ammonium chloride, and is characterized by also comprising an anti-cracking additive, an auxiliary heat-conducting agent and a component crosslinking active agent;
the preparation method of the anti-cracking additive comprises the following steps: taking polyacrylamide according to the mass ratio of 1-4: 10-30, adding N-methyl pyrrolidone, stirring and mixing at 20-25 ℃, adding an activating agent accounting for 50-60% of the mass of the polyacrylamide, stirring and mixing at 30-40 ℃ to obtain a stirring mixture, and taking the stirring mixture according to the mass ratio of 10-15: 2-7, adding reaction raw materials, introducing nitrogen for protection, stirring and mixing at 20-25 ℃, adjusting the pH to 2-3 to obtain a stirring mixture a, and taking the stirring mixture a according to the mass ratio of 3-7: 10-20, adding ethyl acetate, standing, and drying the precipitate to obtain the anti-cracking additive; the activating agent is: taking 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride according to a mass ratio of 3-7: 2-5: 1-4, adding N-hydroxysuccinimide and 1-hydroxybenzotriazole and mixing to obtain the composition; the preparation method of the reaction raw materials comprises the following steps: taking sodium tetraborate according to a mass ratio of 1-3: 0.2-0.5: 20-30, adding sodium bicarbonate and N-methyl pyrrolidone, stirring and mixing to obtain a mixture, and mixing the mixture according to a mass ratio of 20-40: 1-5, adding dopamine hydrochloride, and stirring and mixing at 20-30 ℃ to obtain a reaction raw material;
the preparation method of the auxiliary heat conducting agent comprises the following steps: taking graphene oxide according to a mass ratio of 3-7: 10-30, adding deionized water, performing ultrasound to obtain an ultrasound solution, and taking carbon fibers according to a mass ratio of 2-7: 3-5: 10-20, adding corn straws and absolute ethyl alcohol, and performing ultrasonic treatment to obtain ultrasonic liquid a, wherein the ultrasonic liquid is prepared from the following components in a mass ratio of 5-10: 2-7, adding the ultrasonic liquid a, mixing, adding a phase change active agent accounting for 20-40% of the mass of the ultrasonic liquid, oscillating, performing suction filtration, taking suction filtration residues, and performing vacuum drying to obtain an auxiliary heat conducting agent;
the phase change active agent is: mixing 10-20 parts by weight of capric acid, 5-10 parts by weight of lauric acid, 3-7 parts by weight of myristic acid, 2-5 parts by weight of palmitic acid and 10-15 parts by weight of disodium hydrogen phosphate dodecahydrate to obtain the composition;
the putty powder base material is as follows: mixing 200-300 parts of ordinary portland cement, 20-50 parts of fly ash, 20-40 parts of heavy calcium carbonate, 15-20 parts of quartz powder, 20-40 parts of talcum powder and 30-50 parts of coal gangue according to parts by mass to obtain the cement;
the preparation method of the component crosslinking activator comprises the following steps:
(1) taking 100-130 parts of p-toluic acid, 100-110 parts of hydroquinone, 100-150 parts of methylbenzene and 20-60 parts of carbon tetrachloride, stirring and mixing at 30-50 ℃ to obtain a mixture a, and taking the mixture a according to a mass ratio of 90-120: 1-5, adding a catalyst, introducing nitrogen for protection, stirring and mixing at 50-80 ℃, filtering, washing filter residues, and drying to obtain a dried substance;
(2) taking a dried substance according to a mass ratio of 2-7: 10-15, adding a solvent, adding triethylamine with the mass of 5-10% of that of the dry substance, stirring and mixing at 0-4 ℃ to obtain a mixed solution, and taking acryloyl chloride according to the mass ratio of 2-7: 20-30, stirring and mixing at 0-5 ℃, carrying out suction filtration, washing the filtrate with a sodium bicarbonate solution, carrying out suction filtration, washing the filter residue a with absolute ethyl alcohol, and drying to obtain the component crosslinking activator.
2. The putty powder for exterior walls insulation according to claim 1, wherein the catalyst in the step (1) is: taking boric acid according to the mass ratio of 3-9: and 2-5, adding sulfuric acid and mixing to obtain the catalyst.
3. The putty powder for exterior walls insulation according to claim 1, wherein the solvent in the step (2) is: taking tetrahydrofuran according to a mass ratio of 5-10: and 3-5, adding N, N-dimethylformamide and mixing to obtain the finished product.
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