CN110746847A - Preparation method of efficient heat reflection coating - Google Patents
Preparation method of efficient heat reflection coating Download PDFInfo
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- CN110746847A CN110746847A CN201910958008.1A CN201910958008A CN110746847A CN 110746847 A CN110746847 A CN 110746847A CN 201910958008 A CN201910958008 A CN 201910958008A CN 110746847 A CN110746847 A CN 110746847A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/004—Reflecting paints; Signal paints
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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- Y02P20/10—Process efficiency
Abstract
The invention relates to a preparation method of an efficient heat reflection coating, and belongs to the technical field of coatings. According to the invention, epoxy resin is used as a raw material, and the epoxy resin molecules are rich in hydroxyl, ether bond and epoxy group with extremely high activity, so that the epoxy resin molecules and adjacent interfaces generate electromagnetic adsorption or chemical bonds; the epoxy group can generate cross-linking polymerization reaction with a curing agent to generate three-dimensional reticular macromolecules, and the cured epoxy resin has extremely strong cohesiveness and has good cohesiveness to most metal and non-metal materials; the epoxy resin has no low molecular substances in the curing process, and the molecules are tightly arranged due to the association of hydrogen bonds, so the curing shrinkage rate is low; the epoxy resin film forming material has the advantages of good stability, high mechanical strength, low water absorption, and excellent electrical insulation performance, corrosion resistance and heat resistance.
Description
Technical Field
The invention relates to a preparation method of an efficient heat reflection coating, and belongs to the technical field of coatings.
Background
Solar energy is a necessary condition for human survival and life, but strong radiation brings inconvenience to human life. For example, the surface temperature of the metal plate can reach 70-80 ℃ when the sunshine is irradiated on the metal plate in summer, which inevitably brings inconvenience and causes material loss. In urban areas, black asphalt roads, asphalt roofs, and the like absorb heat from the sun, forming a so-called "heat island" effect, which causes urban temperatures to be about 1-3 ℃ higher than in rural areas.
Generally, to improve the heat insulation performance of exterior walls and roofs, the main measures are as follows:
(1) the thermal performance of the building is improved;
(2) the reflectivity of the outer surface is improved, and the heat transmitted into the room is reduced;
(3) the emissivity of the outer surface is improved;
(4) improving the heat capacity of the roof, reducing the heat transferred into the room, and the like.
At present, the building energy consumption of China accounts for about 1/3 of the total energy consumption, and the energy consumption of a building unit area is 2-3 times of that of a developed country with similar international climate conditions. Therefore, the development of novel materials with low energy consumption and good heat insulation performance becomes the mainstream trend, and the construction department has comprehensively promoted an energy-saving building certification system since 2007. The huge building energy-saving market will drive the new development of the building coating industry, so China is the big market with the most development potential of the energy-saving coating.
According to the used heat insulation functional material, domestic heat insulation reflective coatings can be divided into two main categories:
(1) heat-insulating reflective coatings using hollow microspheres as a main reflective functional material, such as ceramic hollow microspheres and glass hollow microspheres;
(2) various high-reflectivity and high-emission powders are used as basic functional materials to prepare the functional coating with infrared reflection and heat emission.
At present, the reflective coating for buildings in the market mostly takes hollow microspheres as main functional fillers so as to achieve the effect of heat insulation. However, the heat-insulating coating industry has the following unavoidable problems:
(1) the addition of the hollow microspheres can reduce the reflectivity of the coating to visible light;
(2) the particle size of the hollow microspheres is generally larger, and in the occasion with strict requirement on the coating fineness, the use of the hollow microspheres is limited, and the hollow microspheres are thin-walled porous structures, are easy to break under the action of high shear, and reduce the heat insulation effect;
(3) the heat insulation effect of the coating taking the hollow microspheres as the main solar heat reflection functional material is not only related to heat reflection and infrared reflectivity, but also directly related to heat conductivity coefficient, generally needs thick coating, is difficult to obtain a flat paint film, has poor anti-pollution capability, causes the reduction of emissivity and reflectivity in the using process, and further influences the heat insulation performance;
(4) the hollow microspheres are light in weight, so that the problems of upward condensation and poor leveling property of a construction part easily occur in the storage process of the coating.
The main principle of the heat reflection coating is that the coating reflects sunlight heat, so that the solar heat absorbed by the surface of an object is reduced, the heat conducted to the inside of the object is reduced, and the function of keeping the temperature inside the object relatively stable is achieved. The solar radiation energy is mainly concentrated in the visible (wavelength 0.4-0.76 μm) and infrared (wavelength >0.76 μm) parts, and the energy of ultraviolet (wavelength <0.4 μm) is less. Of the total radiant energy, the visible region accounts for about 50% of the total energy of solar radiation, the infrared region accounts for about 43%, and the ultraviolet region is very little solar radiation, accounting for only about 7% of the total.
The heat reflection coating on the market at present can only be used in the fields of buildings and the like with low requirements on appearance effects, and has low physical and chemical properties. Similar coatings are different due to different carriers and functional fillers, and different material proportioning modes lead to related characteristic differences, such as solar light reflectance, backboard temperature difference, paint surface anti-fouling capacity, temperature range, whether waterproof, whether anticorrosion, whether fireproof and the like. The existing heat reflection coating has rough and uneven surface, is not beautiful, is easy to store dirt and dirty, and greatly reduces the heat reflection performance once the dirt is dirty. The existing heat-reflecting coating has poor physical and chemical properties such as impact resistance, flexibility, weather resistance and the like, and can not meet some special use requirements.
CN107739562A discloses a heat-reflecting paint, which comprises 50-60 parts of elastic polyacrylic emulsion, 10-15 parts of titanium dioxide, 5-10 parts of lead white, 15-20 parts of talcum powder, 10-20 parts of hollow borosilicate glass beads, 1-3 parts of butyl cellosolve acetate, 3-5 parts of carboxymethyl cellulose, 1-3 parts of sodium pentachlorophenate, 1-3 parts of tributyl phosphate and 3-5 parts of diisobutylene-maleic copolymer. Although the method can prepare the solar heat reflection elastic coating with good heat insulation performance and heat reflection performance, other physical and chemical properties of the coating are poor.
CN106010005A discloses a heat-reflecting heat-insulating coating, which is prepared from the following raw materials in parts by weight: 1-20 parts of water, 10-20 parts of acrylic emulsion, 15-25 parts of hollow glass beads, 5-15 parts of pigment, 15-25 parts of titanium dioxide, 15-25 parts of aluminum silicate, 20-30 parts of calcium carbonate, 3-9 parts of sodium polyacrylate, 10-20 parts of heat insulation synergist and 0.5-5 parts of antifreeze. The heat-reflecting heat-insulating coating can effectively prevent the heat of the sun from being accumulated on the surface of an object to be heated, can automatically radiate heat to cool, and has excellent antibacterial property and wear resistance, convenient construction and high efficiency. But the appearance effect is poor and the heat reflection performance is general.
CN106082809A discloses a heat-reflecting heat-insulating coating and a preparation method thereof, wherein the heat-reflecting heat-insulating coating is prepared from the following raw materials in parts by weight: 45-55 parts of cement, 35-55 parts of redispersible rubber powder, 20-35 parts of hollow glass beads, 5-15 parts of pigment, 15-25 parts of titanium dioxide, 15-25 parts of zinc oxide, 20-30 parts of kaolin, 3-9 parts of dispersant and 1-5 parts of thickening agent. According to the heat reflection heat insulation coating and the preparation method thereof, the type and the using amount of the dispersing agent and the thickening agent suitable for the heat reflection heat insulation coating are preferably selected through reasonable proportioning, so that the heat reflection property, the antibacterial property, the waterproofness, the corrosion resistance and the stability are improved, the bonding strength is high, the heat reflection heat insulation coating is safe and non-toxic, the curing time is short, the construction is convenient, the efficiency is high, and the heat reflection efficiency is still to be enhanced.
Therefore, how to develop a heat reflection film with high efficiency has important significance in the application thereof.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the problem that the existing heat-reflecting coating has poor physical and chemical properties such as impact resistance, weather resistance and the like, the preparation method of the high-efficiency heat-reflecting coating is provided.
In order to solve the technical problems, the invention adopts the technical scheme that:
(1) mixing epoxy resin, carbon fiber, OP-10, triethylene tetramine, ethylene glycol and deionized water, stirring to obtain reaction emulsion A, adding deionized water into the reaction liquid A, continuously stirring for 10-15 min to obtain reaction emulsion B, adding ethylene glycol and carbon fiber into the reaction emulsion B, stirring at constant temperature to obtain composite emulsion, curing the composite emulsion, filtering to obtain filter residue, washing the filter residue with deionized water for 2-3 times to obtain a blank, drying the blank in an oven at the temperature of 90-100 ℃ to constant weight, and cooling to room temperature to obtain a semi-finished product;
(2) mixing the semi-finished product and deionized water according to the mass ratio of 1: 15, stirring for 3-5 min at the temperature of 60-70 ℃ and the stirring speed of 300-500 r/min to obtain a suspension, adjusting the pH value of the suspension to obtain a dispersion, adding a titanium tetrachloride solution with the mass fraction of 10% into the dispersion according to the mass ratio of 1: 5, continuously stirring for 3-5 h, filtering to obtain a precipitate, washing the precipitate with deionized water for 3-5 times to obtain a matrix, placing the matrix in a muffle furnace, calcining, and cooling to room temperature to obtain a filler;
(3) taking epoxy resin, a filler, lauryl alcohol, span 20, dibutyltin dilaurate, polydimethylsiloxane, titanium dioxide and deionized water, mixing the epoxy resin, the span 20 and the deionized water, stirring to obtain mixed slurry A, sequentially adding the filler and the titanium dioxide into the mixed slurry A, continuously stirring and dispersing for 1-2 hours to obtain mixed slurry B, adding the lauryl alcohol, the dibutyltin dilaurate and the polydimethylsiloxane into the mixed slurry B, and quickly stirring to obtain the high-efficiency heat reflecting coating.
The epoxy resin, the carbon fiber, the OP-10, the triethylene tetramine, the ethylene glycol and the deionized water in the step (1) are in the following proportion: respectively weighing 10-15 parts of epoxy resin, 1-5 parts of carbon fiber, 0.5-0.7 part of OP-10, 1-3 parts of triethylene tetramine, 60-80 parts of ethylene glycol and 4-6 parts of deionized water according to parts by weight.
The stirring treatment step in the step (1) is as follows: mixing epoxy resin, OP-10 and triethylene tetramine, and stirring for 5-10 min at the temperature of 30-35 ℃ and the stirring speed of 1500-2000 r/min.
The constant-temperature stirring treatment step in the step (1) is as follows: and adding ethylene glycol and carbon fiber into the reaction emulsion B, and stirring for 15-20 min at the temperature of 50-70 ℃ and the stirring speed of 1500-2000 r/min.
The curing treatment step in the step (1) is as follows: and curing the composite emulsion at the temperature of 90-100 ℃.
The step (2) of adjusting the pH value of the suspension comprises the following steps: and adjusting the pH value of the suspension to 2.0-2.5 by using hydrochloric acid with the mass fraction of 5%.
The calcining treatment step in the step (2) is as follows: and placing the substrate in a muffle furnace, and calcining for 2-3 h at the temperature of 700-800 ℃.
The epoxy resin, the filler, the lauryl alcohol, the span 20, the dibutyltin dilaurate, the polydimethylsiloxane, the titanium dioxide and the deionized water in the step (3) are in the following proportion: weighing 40-50 parts of epoxy resin, 20-25 parts of filler, 1-10 parts of alcohol ester dodeca, 1-5 parts of span 20, 0.5-0.7 part of dibutyltin dilaurate, 0.3-0.5 part of polydimethylsiloxane, 5-10 parts of titanium dioxide and 100-120 parts of deionized water according to parts by weight.
The stirring treatment step in the step (3) is as follows: mixing the epoxy resin, span 20 and deionized water, and stirring for 20-30 min at the temperature of 60-80 ℃ and the stirring speed of 800-1000 r/min.
The rapid stirring treatment step in the step (3) is as follows: and adding the alcohol ester dodeca, dibutyltin dilaurate and polydimethylsiloxane into the mixed slurry B, and quickly stirring for 5-10 min at the stirring speed of 1500-2000 r/min.
Compared with other methods, the method has the beneficial technical effects that:
(1) the invention takes water as a core, epoxy resin as a shell and carbon fiber as a core, and adopts an in-situ polymerization method to prepare a 'core-shell-core' epoxy resin microsphere, a layer of titanium dioxide is coated on the surface of the epoxy resin microsphere as a filler, the epoxy resin is taken as a raw material, and the filler, an auxiliary agent and a pigment filler are combined to prepare the high-efficiency heat reflection coating; the epoxy resin microspheres have the advantages of heat resistance, chemical reagent resistance, high strength and the like, and the prepared epoxy resin microspheres have thin shell layers and high curing degree, which indicates that the prepared epoxy resin microspheres have good heat resistance; the carbon fiber is used as a core material, and the carbon fiber is protruded on the surface of the prepared epoxy resin microsphere, so that the prepared efficient heat-reflecting coating has good mechanical property and impact resistance; the surface of the epoxy resin microsphere is coated with a layer of titanium dioxide to form a heat dissipation-insulation structure, so that the heat dissipation-insulation structure has a good reflection and heat insulation effect, sunlight reaches the ground in the form of electromagnetic wave radiation, the coating absorbs the heat radiation temperature rise of the sun, heat is transmitted from the outside to the inside through heat conduction, and the titanium dioxide reflects the sunlight irradiating the surface of the fabric into the atmosphere at the original incident wavelength;
(2) according to an in-situ polymerization method, microspheres with water as a core, epoxy resin as a shell and carbon fibers as a core are prepared by utilizing the physical adsorption effect of OP-10; then, slowly removing water in the microspheres through vacuum drying to obtain the epoxy resin microspheres with hollow closed pore structures and good thermal stability; forming a layer of film-shaped structure on a water-oil interface by OP-10 through physical adsorption to obtain a stable emulsifying system; OP-10 molecules are tightly arranged on the surface of the epoxy prepolymer emulsion droplets to form a film-shaped structure with the functions of isolation and protection, so that the adhesion condition of the droplets due to collision is gradually reduced, and the prepared microspheres can keep independent spheres and have the advantages of good thermal stability, high mechanical strength and the like;
(3) according to the invention, epoxy resin is used as a raw material, and the epoxy resin molecules are rich in hydroxyl, ether bond and epoxy group with extremely high activity, so that the epoxy resin molecules and adjacent interfaces generate electromagnetic adsorption or chemical bonds; the epoxy group can generate cross-linking polymerization reaction with a curing agent to generate three-dimensional reticular macromolecules, and the cured epoxy resin has extremely strong cohesiveness and has good cohesiveness to most metal and non-metal materials; the epoxy resin has no low molecular substances in the curing process, and the molecules are tightly arranged due to the association of hydrogen bonds, so the curing shrinkage rate is low; the epoxy resin film forming material has the advantages of good stability, high mechanical strength, low water absorption, and excellent electrical insulation performance, corrosion resistance and heat resistance.
Detailed Description
Respectively weighing 10-15 parts of epoxy resin, 1-5 parts of carbon fiber, 0.5-0.7 part of OP-10, 1-3 parts of triethylene tetramine, 60-80 parts of ethylene glycol and 4-6 parts of deionized water according to parts by weight, mixing the epoxy resin, OP-10 and triethylene tetramine, stirring for 5-10 min at the temperature of 30-35 ℃ and the stirring speed of 1500-2000 r/min to obtain a reaction emulsion A, adding the deionized water into the reaction solution A, continuously stirring for 10-15 min to obtain a reaction emulsion B, adding the ethylene glycol and the carbon fiber into the reaction emulsion B, stirring for 15-20 min at the temperature of 50-70 ℃ and the stirring speed of 1500-2000 r/min to obtain a composite emulsion, curing the composite emulsion at the temperature of 90-100 ℃, filtering to obtain filter residue, washing the filter residue for 2-3 times with the deionized water to obtain a blank body, placing the blank body into an oven at the temperature of 90-100 ℃ and drying to constant weight, cooling to room temperature to obtain a semi-finished product; mixing the semi-finished product and deionized water according to the mass ratio of 1: 15, stirring for 3-5 min at the temperature of 60-70 ℃ and the stirring speed of 300-500 r/min to obtain a suspension, adjusting the pH value of the suspension to 2.0-2.5 by using 5% hydrochloric acid to obtain a dispersion, adding 10% titanium tetrachloride solution into the dispersion according to the mass ratio of 1: 5, continuously stirring for 3-5 h, filtering to obtain a precipitate, washing the precipitate for 3-5 times by using deionized water to obtain a matrix, placing the matrix in a muffle furnace, calcining for 2-3 h at the temperature of 700-800 ℃, and cooling to room temperature to obtain a filler; respectively weighing 40-50 parts of epoxy resin, 20-25 parts of filler, 1-10 parts of alcohol ester dodecamethylene, 1-5 parts of span 20, 0.5-0.7 part of dibutyltin dilaurate, 0.3-0.5 part of polydimethylsiloxane, 5-10 parts of titanium dioxide and 100-120 parts of deionized water according to parts by weight, mixing the epoxy resin, the span 20 and the deionized water, stirring at the temperature of 60-80 ℃ and the stirring speed of 800-1000 r/min for 20-30 min to obtain mixed slurry A, sequentially adding the filler and the titanium dioxide into the mixed slurry A, continuously stirring and dispersing for 1-2 h to obtain mixed slurry B, adding the alcohol ester dodecamethylene, the dibutyltin dilaurate and the polydimethylsiloxane into the mixed slurry B, and rapidly stirring at the stirring speed of 1500-2000 r/min for 5-10 min to obtain the high-efficiency heat reflection coating.
Example 1
Respectively weighing 10 parts of epoxy resin, 1 part of carbon fiber, 0.5 part of OP-10, 1 part of triethylene tetramine, 60 parts of ethylene glycol and 4 parts of deionized water, mixing the epoxy resin, the OP-10 and the triethylene tetramine, stirring for 5min at the temperature of 30 ℃ and the stirring speed of 1500r/min to obtain reaction emulsion A, adding the deionized water into the reaction liquid A, continuously stirring for 10min to obtain reaction emulsion B, adding the ethylene glycol and the carbon fiber into the reaction emulsion B, stirring for 15min at the temperature of 50 ℃ and the stirring speed of 1500r/min to obtain composite emulsion, curing the composite emulsion at the temperature of 90 ℃, filtering to obtain filter residue, washing the filter residue for 2 times by using the deionized water to obtain a blank body, drying the blank body in an oven at the temperature of 90 ℃ to constant weight, and cooling to room temperature to obtain a semi-finished product; mixing the semi-finished product and deionized water according to the mass ratio of 1: 15, stirring for 3min at the temperature of 60 ℃ and the stirring speed of 300r/min to obtain a suspension, adjusting the pH value of the suspension to 2.0 by using hydrochloric acid with the mass fraction of 5% to obtain a dispersion, adding titanium tetrachloride solution with the mass fraction of 10% into the dispersion according to the mass ratio of 1: 5, continuously stirring for 3h, filtering to obtain a precipitate, washing the precipitate with deionized water for 3 times to obtain a matrix, placing the matrix in a muffle furnace, calcining for 2h at the temperature of 700 ℃, and cooling to room temperature to obtain a filler; respectively weighing 40 parts of epoxy resin, 20 parts of filler, 1 part of alcohol ester dodeca, 1 part of span 20, 0.5 part of dibutyltin dilaurate, 0.3 part of polydimethylsiloxane, 5 parts of titanium dioxide and 100 parts of deionized water according to parts by weight, mixing the epoxy resin, the span 20 and the deionized water, stirring for 20min at the temperature of 60 ℃ and the stirring speed of 800r/min to obtain mixed slurry A, sequentially adding the filler and the titanium dioxide into the mixed slurry A, continuously stirring and dispersing for 1h to obtain mixed slurry B, adding the alcohol ester dodeca, the dibutyltin dilaurate and the polydimethylsiloxane into the mixed slurry B, and quickly stirring for 5min at the stirring speed of 1500r/min to obtain the high-efficiency heat reflecting coating.
Example 2
Respectively weighing 13 parts of epoxy resin, 3 parts of carbon fiber, 0.6 part of OP-10, 2 parts of triethylene tetramine, 70 parts of ethylene glycol and 5 parts of deionized water, mixing the epoxy resin, the OP-10 and the triethylene tetramine, stirring for 7min at the temperature of 33 ℃ and the stirring speed of 1750r/min to obtain reaction emulsion A, adding the deionized water into the reaction liquid A, continuously stirring for 13min to obtain reaction emulsion B, adding the ethylene glycol and the carbon fiber into the reaction emulsion B, stirring for 13min at the temperature of 60 ℃ and the stirring speed of 1750r/min to obtain composite emulsion, curing the composite emulsion at the temperature of 95 ℃, filtering to obtain filter residue, washing the filter residue for 2 times with the deionized water to obtain a blank body, drying the blank body in an oven at the temperature of 95 ℃ to constant weight, and cooling to room temperature to obtain a semi-finished product; mixing the semi-finished product and deionized water according to the mass ratio of 1: 15, stirring for 4min at the temperature of 65 ℃ and the stirring speed of 400r/min to obtain suspension, adjusting the pH value of the suspension to 2.3 by using hydrochloric acid with the mass fraction of 5% to obtain dispersion, adding titanium tetrachloride solution with the mass fraction of 10% into the dispersion according to the mass ratio of 1: 5, continuously stirring for 4h, filtering to obtain precipitate, washing the precipitate with deionized water for 4 times to obtain a matrix, placing the matrix in a muffle furnace, calcining for 2.5h at the temperature of 750 ℃, and cooling to room temperature to obtain a filler; respectively weighing 45 parts of epoxy resin, 23 parts of filler, 5 parts of alkyd resin dodeca, 3 parts of span 20, 0.6 part of dibutyltin dilaurate, 0.4 part of polydimethylsiloxane, 7 parts of titanium dioxide and 110 parts of deionized water according to parts by weight, mixing the epoxy resin, span 20 and deionized water, stirring at the temperature of 70 ℃ and the stirring speed of 900r/min for 25min to obtain mixed slurry A, sequentially adding the filler and the titanium dioxide into the mixed slurry A, continuously stirring and dispersing for 1.5h to obtain mixed slurry B, adding the alkyd resin dodeca, the dibutyltin dilaurate and the polydimethylsiloxane into the mixed slurry B, and quickly stirring for 7min at the stirring speed of 1750r/min to obtain the high-efficiency heat reflecting coating.
Example 3
Respectively weighing 15 parts of epoxy resin, 5 parts of carbon fiber, 0.7 part of OP-10, 3 parts of triethylene tetramine, 80 parts of ethylene glycol and 6 parts of deionized water, mixing the epoxy resin, the OP-10 and the triethylene tetramine, stirring for 10min at the temperature of 35 ℃ and the stirring speed of 2000r/min to obtain a reaction emulsion A, adding the deionized water into the reaction liquid A, continuously stirring for 15min to obtain a reaction emulsion B, adding the ethylene glycol and the carbon fiber into the reaction emulsion B, stirring for 20min at the temperature of 70 ℃ and the stirring speed of 2000r/min to obtain a composite emulsion, curing the composite emulsion at the temperature of 100 ℃, filtering to obtain filter residue, washing the filter residue for 3 times by using the deionized water to obtain a blank body, drying the blank body in an oven at the temperature of 100 ℃ to constant weight, and cooling to room temperature to obtain a semi-finished product; mixing the semi-finished product and deionized water according to the mass ratio of 1: 15, stirring for 5min at the temperature of 70 ℃ and the stirring speed of 500r/min to obtain a suspension, adjusting the pH value of the suspension to 2.5 by using hydrochloric acid with the mass fraction of 5% to obtain a dispersion, adding a titanium tetrachloride solution with the mass fraction of 10% into the dispersion according to the mass ratio of 1: 5, continuously stirring for 5h, filtering to obtain a precipitate, washing the precipitate with deionized water for 5 times to obtain a matrix, placing the matrix in a muffle furnace, calcining for 3h at the temperature of 800 ℃, and cooling to room temperature to obtain a filler; respectively weighing 50 parts of epoxy resin, 25 parts of filler, 10 parts of alkyd resin dodeca, 5 parts of span 20, 0.7 part of dibutyltin dilaurate, 0.5 part of polydimethylsiloxane, 10 parts of titanium dioxide and 120 parts of deionized water according to parts by weight, mixing the epoxy resin, span 20 and deionized water, stirring at the temperature of 80 ℃ and the stirring speed of 1000r/min for 30min to obtain mixed slurry A, sequentially adding the filler and the titanium dioxide into the mixed slurry A, continuously stirring and dispersing for 2h to obtain mixed slurry B, adding the alkyd resin dodeca, the dibutyltin dilaurate and the polydimethylsiloxane into the mixed slurry B, and quickly stirring at the stirring speed of 2000r/min for 5-10 min to obtain the high-efficiency heat-reflecting coating.
The high-efficiency heat-reflecting coating prepared by the invention is detected, and the specific detection results are shown in the following table 1:
and (3) carrying out a heat reflection test on the heat reflection heat insulation coating prepared in the embodiment 1-3, respectively taking 15kg of the heat reflection heat insulation coating prepared in the embodiment 1-3 and 7.5kg of water, stirring and mixing uniformly to obtain the heat reflection heat insulation coating which can be used for construction, and carrying out a test according to JC/T1040-2007 Heat reflection heat insulation coating for building external surfaces.
And (5) observing the appearance of the coating after the artificial climate aging performance test for 500 h.
TABLE 1 characterization of high-efficiency heat-reflective coating properties
From table 1, it can be seen that the high-efficiency heat-reflecting coating prepared by the invention has high reflectivity and good aging resistance.
Claims (10)
1. A preparation method of a high-efficiency heat reflection coating is characterized by comprising the following specific preparation steps:
(1) mixing epoxy resin, carbon fiber, OP-10, triethylene tetramine, ethylene glycol and deionized water, stirring to obtain reaction emulsion A, adding deionized water into the reaction liquid A, continuously stirring for 10-15 min to obtain reaction emulsion B, adding ethylene glycol and carbon fiber into the reaction emulsion B, stirring at constant temperature to obtain composite emulsion, curing the composite emulsion, filtering to obtain filter residue, washing the filter residue with deionized water for 2-3 times to obtain a blank, drying the blank in an oven at the temperature of 90-100 ℃ to constant weight, and cooling to room temperature to obtain a semi-finished product;
(2) mixing the semi-finished product and deionized water according to the mass ratio of 1: 15, stirring for 3-5 min at the temperature of 60-70 ℃ and the stirring speed of 300-500 r/min to obtain a suspension, adjusting the pH value of the suspension to obtain a dispersion, adding a titanium tetrachloride solution with the mass fraction of 10% into the dispersion according to the mass ratio of 1: 5, continuously stirring for 3-5 h, filtering to obtain a precipitate, washing the precipitate with deionized water for 3-5 times to obtain a matrix, placing the matrix in a muffle furnace, calcining, and cooling to room temperature to obtain a filler;
(3) taking epoxy resin, a filler, lauryl alcohol, span 20, dibutyltin dilaurate, polydimethylsiloxane, titanium dioxide and deionized water, mixing the epoxy resin, the span 20 and the deionized water, stirring to obtain mixed slurry A, sequentially adding the filler and the titanium dioxide into the mixed slurry A, continuously stirring and dispersing for 1-2 hours to obtain mixed slurry B, adding the lauryl alcohol, the dibutyltin dilaurate and the polydimethylsiloxane into the mixed slurry B, and quickly stirring to obtain the high-efficiency heat reflecting coating.
2. The preparation method of the high-efficiency heat-reflecting coating according to claim 1, characterized in that: the epoxy resin, the carbon fiber, the OP-10, the triethylene tetramine, the ethylene glycol and the deionized water in the step (1) are in the following proportion: respectively weighing 10-15 parts of epoxy resin, 1-5 parts of carbon fiber, 0.5-0.7 part of OP-10, 1-3 parts of triethylene tetramine, 60-80 parts of ethylene glycol and 4-6 parts of deionized water according to parts by weight.
3. The preparation method of the high-efficiency heat-reflecting coating according to claim 1, characterized in that: the stirring treatment step in the step (1) is as follows: mixing epoxy resin, OP-10 and triethylene tetramine, and stirring for 5-10 min at the temperature of 30-35 ℃ and the stirring speed of 1500-2000 r/min.
4. The preparation method of the high-efficiency heat-reflecting coating according to claim 1, characterized in that: the constant-temperature stirring treatment step in the step (1) is as follows: and adding ethylene glycol and carbon fiber into the reaction emulsion B, and stirring for 15-20 min at the temperature of 50-70 ℃ and the stirring speed of 1500-2000 r/min.
5. The preparation method of the high-efficiency heat-reflecting coating according to claim 1, characterized in that: the curing treatment step in the step (1) is as follows: and curing the composite emulsion at the temperature of 90-100 ℃.
6. The preparation method of the high-efficiency heat-reflecting coating according to claim 1, characterized in that: the step (2) of adjusting the pH value of the suspension comprises the following steps: and adjusting the pH value of the suspension to 2.0-2.5 by using hydrochloric acid with the mass fraction of 5%.
7. The preparation method of the high-efficiency heat-reflecting coating according to claim 1, characterized in that: the calcining treatment step in the step (2) is as follows: and placing the substrate in a muffle furnace, and calcining for 2-3 h at the temperature of 700-800 ℃.
8. The preparation method of the high-efficiency heat-reflecting coating according to claim 1, characterized in that: the epoxy resin, the filler, the lauryl alcohol, the span 20, the dibutyltin dilaurate, the polydimethylsiloxane, the titanium dioxide and the deionized water in the step (3) are in the following proportion: weighing 40-50 parts of epoxy resin, 20-25 parts of filler, 1-10 parts of alcohol ester dodeca, 1-5 parts of span 20, 0.5-0.7 part of dibutyltin dilaurate, 0.3-0.5 part of polydimethylsiloxane, 5-10 parts of titanium dioxide and 100-120 parts of deionized water according to parts by weight.
9. The preparation method of the high-efficiency heat-reflecting coating according to claim 1, characterized in that: the stirring treatment step in the step (3) is as follows: mixing the epoxy resin, span 20 and deionized water, and stirring for 20-30 min at the temperature of 60-80 ℃ and the stirring speed of 800-1000 r/min.
10. The preparation method of the high-efficiency heat-reflecting coating according to claim 1, characterized in that: the rapid stirring treatment step in the step (3) is as follows: and adding the alcohol ester dodeca, dibutyltin dilaurate and polydimethylsiloxane into the mixed slurry B, and quickly stirring for 5-10 min at the stirring speed of 1500-2000 r/min.
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