CN112521855A - Preparation method of high-weather-resistance heat-insulation composite coating - Google Patents

Preparation method of high-weather-resistance heat-insulation composite coating Download PDF

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CN112521855A
CN112521855A CN202110012064.3A CN202110012064A CN112521855A CN 112521855 A CN112521855 A CN 112521855A CN 202110012064 A CN202110012064 A CN 202110012064A CN 112521855 A CN112521855 A CN 112521855A
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boric acid
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谭祖干
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Chengdu Zhanyiyu Coating Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D183/00Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
    • C09D183/14Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers in which at least two but not all the silicon atoms are connected by linkages other than oxygen atoms
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/48Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule in which at least two but not all the silicon atoms are connected by linkages other than oxygen atoms
    • C08G77/56Boron-containing linkages
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
    • C09D7/62Additives non-macromolecular inorganic modified by treatment with other compounds
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/70Additives characterised by shape, e.g. fibres, flakes or microspheres
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

Abstract

The invention relates to a preparation method of a high weather-resistant heat-insulating composite coating, belonging to the technical field of heat insulation. According to the invention, boric acid modified organic silicon resin emulsion is used as a base material to prepare the high weather-resistant heat-insulating composite coating, the organic silicon resin contains Si-O bonds, and the difference of the relative electronegativities of silicon atoms and oxygen atoms is large, so that the Si-O bonds have large polarity, a shielding effect on the oxidation energy of the connected hydrocarbyl groups is achieved, the thermal decomposition speed of the organic silicon resin is slowed down, and the heat resistance is improved; the boric acid modified organic silicon resin is adopted, because boron atoms enter the main chain of the molecule, the bond energy of the formed B-O bond is much higher than that of the Si-O bond, the main chain of the modified silicon resin is firmer and is not easy to break, so that the temperature resistance of the modified silicon resin is improved, and the introduction of multifunctional groups such as boric acid enables the interior of the modified silicon resin molecule to present a compact body type network structure, so that the weather resistance and the mechanical property of the coating are improved.

Description

Preparation method of high-weather-resistance heat-insulation composite coating
Technical Field
The invention relates to a preparation method of a high weather-resistant heat-insulating composite coating, belonging to the technical field of heat insulation.
Background
The high-performance environment-friendly building energy-saving material becomes a breakthrough for solving the heat preservation and energy conservation of buildings, the building energy-saving heat-preservation coating in the building energy-saving material is more and more favored by people due to the advantages of economy, convenient use, good environment protection and energy conservation effects and the like, has bright development prospect, and is expected to promote the expansion of the coating market and the application field of the energy-saving heat-preservation material. The development of the building energy-saving heat-insulating coating technology is developed from the previous single, local and heat-insulating technology which emphasizes a certain aspect to the integrated direction. Based on the development trend, the research on the energy-saving heat-insulating coating is carried out on the wall, the roof and the glass of the door and the window, and the best energy-saving heat-insulating effect of the building is strived to be achieved. In the future, architectural coatings should be developed toward excellent weatherability, stain resistance, VOC reduction and functional composition.
The production technology of the high-performance exterior wall coating is developed, and the requirements of exterior decoration of high-rise buildings are met. High performance means high weatherability, high stain resistance, high color retention, and low toxicity. The high-performance exterior wall building coating mainly comprises: the water-emulsion high-performance exterior wall coating has excellent weather resistance and stain resistance, and is particularly suitable for the exterior wall decoration of high-rise, super high-rise and public buildings; the aliphatic solvent type acrylic coating has the characteristics of low pollution and high solid content, and has excellent aging resistance and stain resistance.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the problem of low weather resistance of common heat-insulating coatings, a preparation method of a high weather-resistant heat-insulating composite coating is provided.
In order to solve the technical problems, the invention adopts the technical scheme that:
(1) respectively weighing 80-100 parts by weight of boric acid modified organic silicon resin emulsion, 40-50 parts by weight of modified vitrified micro bubbles, 4-5 parts by weight of hydroxy silicone oil, 1.6-2.0 parts by weight of sodium dodecyl benzene sulfonate, 8-10 parts by weight of sodium carboxymethyl cellulose, 4-5 parts by weight of dimethyl polysiloxane, 4-5 parts by weight of polyvinyl alcohol, 2.0-2.5 parts by weight of sodium stearate and 40-50 parts by weight of deionized water;
(2) adding hydroxyl silicone oil and sodium dodecyl benzene sulfonate into deionized water, and stirring at the normal temperature at the rotating speed of 200-300 r/min for 10-20 min to obtain an emulsifier solution;
(3) adding dimethyl polysiloxane, polyvinyl alcohol and sodium stearate into an emulsifier solution, placing the mixture into a high-shear emulsifying machine, and stirring the mixture for 1-2 hours at the rotating speed of 10000-140000 r/min under the water bath condition of 60-70 ℃ to obtain polymer emulsion;
(4) and adding the polymer emulsion and the modified mixed nano ceramic powder into the water-based epoxy emulsion, stirring at 12000-16000 r/min for 2-4 h at normal temperature, then placing the mixture into an ultrasonic dispersion machine, and performing ultrasonic dispersion for 30-40 min at normal temperature to obtain the high-weather-resistance heat-preservation composite coating.
And (4) the power of ultrasonic dispersion in the step (4) is 500-600W.
The specific preparation steps of the modified vitrified micro bubbles are as follows:
(1) respectively weighing 20-30 parts of vitrified micro bubbles, 2-3 parts of methyltriethoxysilane, 20-30 parts of absolute ethyl alcohol and 200-300 parts of deionized water in parts by weight;
(2) adding methyltriethoxysilane and absolute ethyl alcohol into deionized water, stirring at the rotating speed of 200-300 r/min for 20-30 min under the water bath condition of 60-70 ℃, and preserving heat to obtain a modified solution;
(3) adding the vitrified micro bubbles into the modification liquid, and stirring for 30-40 min at the rotating speed of 300-400 r/min under the water bath condition of 60-70 ℃ to obtain suspension;
(4) placing the suspension in an ultrasonic dispersion machine, and performing ultrasonic treatment for 10-20 min at normal temperature to obtain dispersion liquid;
(5) and placing the dispersion liquid in a centrifuge, carrying out centrifugal separation at the rotation speed of 5000-6000 r/min for 20-30 min at normal temperature, removing lower-layer solids, washing with deionized water for 3-5 times, and placing in an oven at the temperature of 60-80 ℃ for drying for 1-2 h to obtain the modified vitrified micro bubbles.
The average particle size of the vitrified micro bubbles in the step (1) is 80-100 mu m.
And (4) the power of ultrasonic treatment in the step (4) is 300-400W.
The specific preparation steps of the boric acid modified organic silicon resin emulsion are as follows:
(1) respectively weighing 10-20 parts by weight of methyltrimethoxysilane, 10-20 parts by weight of vinyltrimethoxysilane, 5-10 parts by weight of vinyltriethoxysilane, 20-25 parts by weight of xylene, 10-20 parts by weight of boric acid and 50-100 parts by weight of deionized water;
(2) adding methyltrimethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane and 1/2 parts by weight of boric acid into deionized water, stirring for 10-20 min at a rotating speed of 200-300 r/min under the condition of a water bath at the temperature of 80-90 ℃, and preserving heat to obtain a mixed solution;
(3) adding the residual 1/2 parts by weight of boric acid into the mixed solution, and stirring and reacting for 1-2 hours at a rotating speed of 200-300 r/min under a water bath condition of 80-90 ℃ to obtain a reaction solution;
(4) putting the reaction solution into a reduced pressure distillation device for reduced pressure distillation for 30-40 min to obtain a mixture;
(5) adding dimethylbenzene into the mixture, stirring at the normal temperature at the rotating speed of 180-200 r/min for 10-20 min, and sealing and storing to obtain boric acid modified organic silicon resin emulsion;
the boric acid in the step (1) has an average particle size of 100-200 μm.
The reduced pressure distillation in the step (4) is carried out under the conditions of temperature of 80-90 ℃ and pressure of 20-60 KPa.
Compared with other methods, the method has the beneficial technical effects that:
the invention takes boric acid modified organic silicon resin emulsion as a base material to prepare a high weather-resistant heat-insulating composite coating, the organic silicon resin is a polymer which is formed by alternately connecting silicon atoms and oxygen atoms and then connecting different organic groups with the silicon atoms, and has the characteristics of organic polymers and inorganic polymers, the organic silicon resin takes Si-O-Si bonds as main chains and has excellent heat resistance, mainly because the Si-0 bonds have high bond energy, the stable Si-O-Si bonds are generated after the organic groups connected on the Si atoms are heated, oxidized and decomposed, a stable protective layer rich in the Si-O-Si bonds is generated on the surface of the organic silicon polymer, and the influence on partial molecular chain segments in the high polymer is reduced. In the Si-O bond, the difference of the relative electronegativity of the silicon atom and the oxygen atom is large, so that the polarity of the Si-O bond is large, the oxidation energy of the connected hydrocarbyl group is shielded, the thermal decomposition speed of the organic silicon resin is slowed, and the heat resistance is improved; the boric acid modified organic silicon resin is adopted, because boron atoms enter the main chain of the molecule, the bond energy of the formed B-O bond is much higher than that of the Si-O bond, the main chain of the modified silicon resin is firmer and is not easy to break, so that the temperature resistance of the modified silicon resin is improved, and the introduction of multifunctional groups such as boric acid enables the interior of the modified silicon resin molecule to present a compact body type network structure, so that the weather resistance and the mechanical property of the coating are improved.
According to the invention, the modified vitrified micro bubbles are added to prepare the high-weather-resistance heat-insulation composite coating, the outer walls of the hollow vitrified micro bubbles are made of glass materials, so that the high-weather-resistance heat-insulation composite coating has high compression resistance, the compressive strength of concrete can be obviously improved by adding the vitrified micro bubbles, the thermal expansion coefficient of the hollow vitrified micro bubbles is small, the stability of the performance of a coating film can be ensured, the vitrified micro bubbles can be uniformly dispersed into the coating after being modified by the silane coupling agent, so that gaps in the coating can be filled, inert gas is filled in the vitrified micro bubbles, the heat-insulation performance is good, and the heat-insulation performance of the coating film can be effectively improved by adding the modified vitrified micro bubbles.
Detailed Description
Respectively weighing 10-20 parts by weight of methyltrimethoxysilane, 10-20 parts by weight of vinyltrimethoxysilane, 5-10 parts by weight of vinyltriethoxysilane, 20-25 parts by weight of xylene, 10-20 parts by weight of boric acid with the average particle size of 100-200 mu m and 50-100 parts by weight of deionized water, adding the methyltrimethoxysilane, the vinyltrimethoxysilane, the vinyltriethoxysilane and 1/2 parts by weight of the boric acid into the deionized water, stirring for 10-20 min at a rotating speed of 200-300 r/min under a water bath condition of 80-90 ℃, preserving heat to obtain a mixed solution, adding the rest 1/2 parts by weight of the boric acid into the mixed solution, stirring for reaction for 1-2 h at a rotating speed of 200-300 r/min under a water bath condition of 80-90 ℃ to obtain a reaction solution, placing the reaction solution into a reduced pressure distillation device, and distilling for 30-40 min under a temperature of 80-90 ℃ and a pressure of 20-60 KPa, adding dimethylbenzene into the mixture, stirring at the normal temperature at the rotating speed of 180-200 r/min for 10-20 min, and sealing and storing to obtain boric acid modified organic silicon resin emulsion;
respectively weighing 20-30 parts by weight of vitrified micro bubbles with the average particle size of 80-100 mu m, 2-3 parts by weight of methyltriethoxysilane, 20-30 parts by weight of absolute ethyl alcohol and 200-300 parts by weight of deionized water, adding the methyltriethoxysilane and the absolute ethyl alcohol into the deionized water, stirring for 20-30 min at the rotating speed of 200-300 r/min under the water bath condition of 60-70 ℃, preserving heat to obtain a modified solution, adding the vitrified micro bubbles into the modified solution, stirring for 30-40 min at the rotating speed of 300-400 r/min under the water bath condition of 60-70 ℃ to obtain a suspension, placing the suspension into an ultrasonic dispersion machine, carrying out ultrasonic treatment for 10-20 min at the power of 300-400W at normal temperature to obtain a dispersion solution, placing the dispersion solution into a centrifuge, centrifuging for 20-30 min at the rotating speed of 5000-6000 r/min at normal temperature, removing lower-layer solids, washing for 3-5 times by using deionized water, drying in an oven at 60-80 ℃ for 1-2 h to obtain modified vitrified micro bubbles;
respectively weighing 80-100 parts by weight of boric acid modified organic silicon resin emulsion, 40-50 parts by weight of modified vitrified micro bubbles, 4-5 parts by weight of hydroxy silicone oil, 1.6-2.0 parts by weight of sodium dodecyl benzene sulfonate, 8-10 parts by weight of sodium carboxymethyl cellulose, 4-5 parts by weight of dimethyl polysiloxane, 4-5 parts by weight of polyvinyl alcohol, 2.0-2.5 parts by weight of sodium stearate and 40-50 parts by weight of deionized water, adding the hydroxy silicone oil and the sodium dodecyl benzene sulfonate into the deionized water, stirring at the normal temperature at the rotating speed of 200-300 r/min for 10-20 min to obtain an emulsifier solution, adding the dimethyl polysiloxane, the polyvinyl alcohol and the sodium stearate into the emulsifier solution, placing the emulsifier solution into a high-shear emulsifying machine, stirring at the rotating speed of 10000-140000 r/min for 1-2 h under the water bath condition of 60-70 ℃ to obtain polymer emulsion, adding the polymer emulsion and modified mixed nano ceramic powder into the aqueous epoxy, stirring for 2-4 h at 12000-16000 r/min at normal temperature, then placing in an ultrasonic dispersion machine, and ultrasonically dispersing for 30-40 min at 500-600W at normal temperature to obtain the high weather-resistant heat-preservation composite coating.
Example 1
Respectively weighing 10-20 parts by weight of methyltrimethoxysilane, 10-20 parts by weight of vinyltrimethoxysilane, 5-10 parts by weight of vinyltriethoxysilane, 20-25 parts by weight of xylene, 10-20 parts by weight of boric acid with the average particle size of 100-200 mu m and 50-100 parts by weight of deionized water, adding the methyltrimethoxysilane, the vinyltrimethoxysilane, the vinyltriethoxysilane and 1/2 parts by weight of the boric acid into the deionized water, stirring for 10-20 min at a rotating speed of 200-300 r/min under a water bath condition of 80-90 ℃, preserving heat to obtain a mixed solution, adding the rest 1/2 parts by weight of the boric acid into the mixed solution, stirring for reaction for 1-2 h at a rotating speed of 200-300 r/min under a water bath condition of 80-90 ℃ to obtain a reaction solution, placing the reaction solution into a reduced pressure distillation device, and distilling for 30-40 min under a temperature of 80-90 ℃ and a pressure of 20-60 KPa, adding dimethylbenzene into the mixture, stirring at the normal temperature at the rotating speed of 180-200 r/min for 10-20 min, and sealing and storing to obtain boric acid modified organic silicon resin emulsion;
respectively weighing 20-30 parts by weight of vitrified micro bubbles with the average particle size of 80-100 mu m, 2-3 parts by weight of methyltriethoxysilane, 20-30 parts by weight of absolute ethyl alcohol and 200-300 parts by weight of deionized water, adding the methyltriethoxysilane and the absolute ethyl alcohol into the deionized water, stirring for 20-30 min at the rotating speed of 200-300 r/min under the water bath condition of 60-70 ℃, preserving heat to obtain a modified solution, adding the vitrified micro bubbles into the modified solution, stirring for 30-40 min at the rotating speed of 300-400 r/min under the water bath condition of 60-70 ℃ to obtain a suspension, placing the suspension into an ultrasonic dispersion machine, carrying out ultrasonic treatment for 10-20 min at the power of 300-400W at normal temperature to obtain a dispersion solution, placing the dispersion solution into a centrifuge, centrifuging for 20-30 min at the rotating speed of 5000-6000 r/min at normal temperature, removing lower-layer solids, washing for 3-5 times by using deionized water, drying in an oven at 60-80 ℃ for 1-2 h to obtain modified vitrified micro bubbles;
respectively weighing 80-100 parts by weight of boric acid modified organic silicon resin emulsion, 40-50 parts by weight of modified vitrified micro bubbles, 4-5 parts by weight of hydroxy silicone oil, 1.6-2.0 parts by weight of sodium dodecyl benzene sulfonate, 8-10 parts by weight of sodium carboxymethyl cellulose, 4-5 parts by weight of dimethyl polysiloxane, 4-5 parts by weight of polyvinyl alcohol, 2.0-2.5 parts by weight of sodium stearate and 40-50 parts by weight of deionized water, adding the hydroxy silicone oil and the sodium dodecyl benzene sulfonate into the deionized water, stirring at the normal temperature at the rotating speed of 200-300 r/min for 10-20 min to obtain an emulsifier solution, adding the dimethyl polysiloxane, the polyvinyl alcohol and the sodium stearate into the emulsifier solution, placing the emulsifier solution into a high-shear emulsifying machine, stirring at the rotating speed of 10000-140000 r/min for 1-2 h under the water bath condition of 60-70 ℃ to obtain polymer emulsion, adding the polymer emulsion and modified mixed nano ceramic powder into the aqueous epoxy, stirring for 2-4 h at 12000-16000 r/min at normal temperature, then placing in an ultrasonic dispersion machine, and ultrasonically dispersing for 30-40 min at 500-600W at normal temperature to obtain the high weather-resistant heat-preservation composite coating.
Example 2
Respectively weighing 10-20 parts by weight of methyltrimethoxysilane, 10-20 parts by weight of vinyltrimethoxysilane, 5-10 parts by weight of vinyltriethoxysilane, 20-25 parts by weight of xylene, 10-20 parts by weight of boric acid with the average particle size of 100-200 mu m and 50-100 parts by weight of deionized water, adding the methyltrimethoxysilane, the vinyltrimethoxysilane, the vinyltriethoxysilane and 1/2 parts by weight of the boric acid into the deionized water, stirring for 10-20 min at a rotating speed of 200-300 r/min under a water bath condition of 80-90 ℃, preserving heat to obtain a mixed solution, adding the rest 1/2 parts by weight of the boric acid into the mixed solution, stirring for reaction for 1-2 h at a rotating speed of 200-300 r/min under a water bath condition of 80-90 ℃ to obtain a reaction solution, placing the reaction solution into a reduced pressure distillation device, and distilling for 30-40 min under a temperature of 80-90 ℃ and a pressure of 20-60 KPa, adding dimethylbenzene into the mixture, stirring at the normal temperature at the rotating speed of 180-200 r/min for 10-20 min, and sealing and storing to obtain boric acid modified organic silicon resin emulsion;
respectively weighing 20-30 parts by weight of vitrified micro bubbles with the average particle size of 80-100 mu m, 2-3 parts by weight of methyltriethoxysilane, 20-30 parts by weight of absolute ethyl alcohol and 200-300 parts by weight of deionized water, adding the methyltriethoxysilane and the absolute ethyl alcohol into the deionized water, stirring for 20-30 min at the rotating speed of 200-300 r/min under the water bath condition of 60-70 ℃, preserving heat to obtain a modified solution, adding the vitrified micro bubbles into the modified solution, stirring for 30-40 min at the rotating speed of 300-400 r/min under the water bath condition of 60-70 ℃ to obtain a suspension, placing the suspension into an ultrasonic dispersion machine, carrying out ultrasonic treatment for 10-20 min at the power of 300-400W at normal temperature to obtain a dispersion solution, placing the dispersion solution into a centrifuge, centrifuging for 20-30 min at the rotating speed of 5000-6000 r/min at normal temperature, removing lower-layer solids, washing for 3-5 times by using deionized water, drying in an oven at 60-80 ℃ for 1-2 h to obtain modified vitrified micro bubbles;
respectively weighing 80-100 parts by weight of boric acid modified organic silicon resin emulsion, 40-50 parts by weight of modified vitrified micro bubbles, 4-5 parts by weight of hydroxy silicone oil, 1.6-2.0 parts by weight of sodium dodecyl benzene sulfonate, 8-10 parts by weight of sodium carboxymethyl cellulose, 4-5 parts by weight of dimethyl polysiloxane, 4-5 parts by weight of polyvinyl alcohol, 2.0-2.5 parts by weight of sodium stearate and 40-50 parts by weight of deionized water, adding the hydroxy silicone oil and the sodium dodecyl benzene sulfonate into the deionized water, stirring at the normal temperature at the rotating speed of 200-300 r/min for 10-20 min to obtain an emulsifier solution, adding the dimethyl polysiloxane, the polyvinyl alcohol and the sodium stearate into the emulsifier solution, placing the emulsifier solution into a high-shear emulsifying machine, stirring at the rotating speed of 10000-140000 r/min for 1-2 h under the water bath condition of 60-70 ℃ to obtain polymer emulsion, adding the polymer emulsion and modified mixed nano ceramic powder into the aqueous epoxy, stirring for 2-4 h at 12000-16000 r/min at normal temperature, then placing in an ultrasonic dispersion machine, and ultrasonically dispersing for 30-40 min at 500-600W at normal temperature to obtain the high weather-resistant heat-preservation composite coating.
Example 3
Respectively weighing 10-20 parts by weight of methyltrimethoxysilane, 10-20 parts by weight of vinyltrimethoxysilane, 5-10 parts by weight of vinyltriethoxysilane, 20-25 parts by weight of xylene, 10-20 parts by weight of boric acid with the average particle size of 100-200 mu m and 50-100 parts by weight of deionized water, adding the methyltrimethoxysilane, the vinyltrimethoxysilane, the vinyltriethoxysilane and 1/2 parts by weight of the boric acid into the deionized water, stirring for 10-20 min at a rotating speed of 200-300 r/min under a water bath condition of 80-90 ℃, preserving heat to obtain a mixed solution, adding the rest 1/2 parts by weight of the boric acid into the mixed solution, stirring for reaction for 1-2 h at a rotating speed of 200-300 r/min under a water bath condition of 80-90 ℃ to obtain a reaction solution, placing the reaction solution into a reduced pressure distillation device, and distilling for 30-40 min under a temperature of 80-90 ℃ and a pressure of 20-60 KPa, adding dimethylbenzene into the mixture, stirring at the normal temperature at the rotating speed of 180-200 r/min for 10-20 min, and sealing and storing to obtain boric acid modified organic silicon resin emulsion;
respectively weighing 20-30 parts by weight of vitrified micro bubbles with the average particle size of 80-100 mu m, 2-3 parts by weight of methyltriethoxysilane, 20-30 parts by weight of absolute ethyl alcohol and 200-300 parts by weight of deionized water, adding the methyltriethoxysilane and the absolute ethyl alcohol into the deionized water, stirring for 20-30 min at the rotating speed of 200-300 r/min under the water bath condition of 60-70 ℃, preserving heat to obtain a modified solution, adding the vitrified micro bubbles into the modified solution, stirring for 30-40 min at the rotating speed of 300-400 r/min under the water bath condition of 60-70 ℃ to obtain a suspension, placing the suspension into an ultrasonic dispersion machine, carrying out ultrasonic treatment for 10-20 min at the power of 300-400W at normal temperature to obtain a dispersion solution, placing the dispersion solution into a centrifuge, centrifuging for 20-30 min at the rotating speed of 5000-6000 r/min at normal temperature, removing lower-layer solids, washing for 3-5 times by using deionized water, drying in an oven at 60-80 ℃ for 1-2 h to obtain modified vitrified micro bubbles;
respectively weighing 80-100 parts by weight of boric acid modified organic silicon resin emulsion, 40-50 parts by weight of modified vitrified micro bubbles, 4-5 parts by weight of hydroxy silicone oil, 1.6-2.0 parts by weight of sodium dodecyl benzene sulfonate, 8-10 parts by weight of sodium carboxymethyl cellulose, 4-5 parts by weight of dimethyl polysiloxane, 4-5 parts by weight of polyvinyl alcohol, 2.0-2.5 parts by weight of sodium stearate and 40-50 parts by weight of deionized water, adding the hydroxy silicone oil and the sodium dodecyl benzene sulfonate into the deionized water, stirring at the normal temperature at the rotating speed of 200-300 r/min for 10-20 min to obtain an emulsifier solution, adding the dimethyl polysiloxane, the polyvinyl alcohol and the sodium stearate into the emulsifier solution, placing the emulsifier solution into a high-shear emulsifying machine, stirring at the rotating speed of 10000-140000 r/min for 1-2 h under the water bath condition of 60-70 ℃ to obtain polymer emulsion, adding the polymer emulsion and modified mixed nano ceramic powder into the aqueous epoxy, stirring for 2-4 h at 12000-16000 r/min at normal temperature, then placing in an ultrasonic dispersion machine, and ultrasonically dispersing for 30-40 min at 500-600W at normal temperature to obtain the high weather-resistant heat-preservation composite coating.

Claims (8)

1. A preparation method of a high weather-resistant heat-insulating composite coating is characterized by comprising the following specific preparation steps:
(1) respectively weighing 80-100 parts by weight of boric acid modified organic silicon resin emulsion, 40-50 parts by weight of modified vitrified micro bubbles, 4-5 parts by weight of hydroxy silicone oil, 1.6-2.0 parts by weight of sodium dodecyl benzene sulfonate, 8-10 parts by weight of sodium carboxymethyl cellulose, 4-5 parts by weight of dimethyl polysiloxane, 4-5 parts by weight of polyvinyl alcohol, 2.0-2.5 parts by weight of sodium stearate and 40-50 parts by weight of deionized water;
(2) adding hydroxyl silicone oil and sodium dodecyl benzene sulfonate into deionized water, and stirring at the normal temperature at the rotating speed of 200-300 r/min for 10-20 min to obtain an emulsifier solution;
(3) adding dimethyl polysiloxane, polyvinyl alcohol and sodium stearate into an emulsifier solution, placing the mixture into a high-shear emulsifying machine, and stirring the mixture for 1-2 hours at the rotating speed of 10000-140000 r/min under the water bath condition of 60-70 ℃ to obtain polymer emulsion;
(4) and adding the polymer emulsion and the modified mixed nano ceramic powder into the water-based epoxy emulsion, stirring at 12000-16000 r/min for 2-4 h at normal temperature, then placing the mixture into an ultrasonic dispersion machine, and performing ultrasonic dispersion for 30-40 min at normal temperature to obtain the high-weather-resistance heat-preservation composite coating.
2. The preparation method of the high weather-resistant heat-insulating composite coating according to claim 1, wherein the power of the ultrasonic dispersion in the step (4) is 500-600W.
3. The preparation method of the high weather-resistant heat-insulating composite coating according to claim 1, wherein the modified vitrified micro bubbles in the step (1) are prepared by the following specific steps:
(1) respectively weighing 20-30 parts of vitrified micro bubbles, 2-3 parts of methyltriethoxysilane, 20-30 parts of absolute ethyl alcohol and 200-300 parts of deionized water in parts by weight;
(2) adding methyltriethoxysilane and absolute ethyl alcohol into deionized water, stirring at the rotating speed of 200-300 r/min for 20-30 min under the water bath condition of 60-70 ℃, and preserving heat to obtain a modified solution;
(3) adding the vitrified micro bubbles into the modification liquid, and stirring for 30-40 min at the rotating speed of 300-400 r/min under the water bath condition of 60-70 ℃ to obtain suspension;
(4) placing the suspension in an ultrasonic dispersion machine, and performing ultrasonic treatment for 10-20 min at normal temperature to obtain dispersion liquid;
(5) and placing the dispersion liquid in a centrifuge, carrying out centrifugal separation at the rotation speed of 5000-6000 r/min for 20-30 min at normal temperature, removing lower-layer solids, washing with deionized water for 3-5 times, and placing in an oven at the temperature of 60-80 ℃ for drying for 1-2 h to obtain the modified vitrified micro bubbles.
4. The preparation method of the high weather-resistant heat-insulating composite coating as claimed in claim 3, wherein the average particle size of the vitrified micro bubbles in the step (1) is 80-100 μm.
5. The preparation method of the high weather-resistant heat-insulating composite coating according to claim 3, wherein the power of the ultrasonic treatment in the step (4) is 300-400W.
6. The preparation method of the high weather-resistant heat-insulating composite coating as claimed in claim 1, wherein the boric acid modified silicone resin emulsion in step (1) is prepared by the following specific steps:
(1) respectively weighing 10-20 parts by weight of methyltrimethoxysilane, 10-20 parts by weight of vinyltrimethoxysilane, 5-10 parts by weight of vinyltriethoxysilane, 20-25 parts by weight of xylene, 10-20 parts by weight of boric acid and 50-100 parts by weight of deionized water;
(2) adding methyltrimethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane and 1/2 parts by weight of boric acid into deionized water, stirring for 10-20 min at a rotating speed of 200-300 r/min under the condition of a water bath at the temperature of 80-90 ℃, and preserving heat to obtain a mixed solution;
(3) adding the residual 1/2 parts by weight of boric acid into the mixed solution, and stirring and reacting for 1-2 hours at a rotating speed of 200-300 r/min under a water bath condition of 80-90 ℃ to obtain a reaction solution;
(4) putting the reaction solution into a reduced pressure distillation device for reduced pressure distillation for 30-40 min to obtain a mixture;
(5) and adding dimethylbenzene into the mixture, stirring at the normal temperature at the rotating speed of 180-200 r/min for 10-20 min, and sealing and storing to obtain the boric acid modified organic silicon resin emulsion.
7. The preparation method of the high weather-resistant heat-insulating composite coating as claimed in claim 6, wherein the boric acid in the step (1) has an average particle size of 100-200 μm.
8. The preparation method of the high weather-resistant heat-insulating composite coating as claimed in claim 6, wherein the reduced pressure distillation in the step (4) is carried out at a temperature of 80-90 ℃ and a pressure of 20-60 KPa.
CN202110012064.3A 2021-01-06 2021-01-06 Preparation method of high-weather-resistance heat-insulation composite coating Pending CN112521855A (en)

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CN113337128A (en) * 2021-05-31 2021-09-03 福建臻璟新材料科技有限公司 High-weather-resistance heat-conducting gel composition and preparation method thereof
CN115074027A (en) * 2022-05-31 2022-09-20 辽宁大学 Organic-inorganic composite high-temperature heat-insulating coating and preparation method thereof

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CN105273603A (en) * 2015-08-27 2016-01-27 浙江工商大学 Building facade coating and preparation method thereof
CN108727978A (en) * 2018-06-28 2018-11-02 安徽稀饭智能家居有限公司 A kind of composite, insulating environmental protection coating material
CN109554111A (en) * 2018-11-24 2019-04-02 浙江时进节能环保涂料有限公司 Nano-thermal-insulating coating for building and preparation method thereof
CN110452614A (en) * 2019-09-03 2019-11-15 陈长仙 A kind of silicone industry coating and preparation method

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CN105273603A (en) * 2015-08-27 2016-01-27 浙江工商大学 Building facade coating and preparation method thereof
CN108727978A (en) * 2018-06-28 2018-11-02 安徽稀饭智能家居有限公司 A kind of composite, insulating environmental protection coating material
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CN113337128A (en) * 2021-05-31 2021-09-03 福建臻璟新材料科技有限公司 High-weather-resistance heat-conducting gel composition and preparation method thereof
CN115074027A (en) * 2022-05-31 2022-09-20 辽宁大学 Organic-inorganic composite high-temperature heat-insulating coating and preparation method thereof
CN115074027B (en) * 2022-05-31 2023-09-15 辽宁大学 Organic-inorganic composite high-temperature heat-insulating coating and preparation method thereof

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Application publication date: 20210319