CN110564253A - heat-absorbing photoelectric conversion fluorescent exterior wall coating and manufacturing method thereof - Google Patents

heat-absorbing photoelectric conversion fluorescent exterior wall coating and manufacturing method thereof Download PDF

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CN110564253A
CN110564253A CN201910917698.6A CN201910917698A CN110564253A CN 110564253 A CN110564253 A CN 110564253A CN 201910917698 A CN201910917698 A CN 201910917698A CN 110564253 A CN110564253 A CN 110564253A
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parts
liquid
prepared
fluorescent
mixed
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刘英武
刘丰毓
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Qingdao Tiandi Color Paint Engineering Application Co Ltd
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Qingdao Tiandi Color Paint Engineering Application 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
    • C09D133/00Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
    • C09D133/04Homopolymers or copolymers of esters
    • C09D133/06Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C09D133/062Copolymers with monomers not covered by C09D133/06
    • C09D133/064Copolymers with monomers not covered by C09D133/06 containing anhydride, COOH or COOM groups, with M being metal or onium-cation
    • 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
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/22Luminous paints
    • 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
    • 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
    • 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
    • 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
    • C09D7/63Additives non-macromolecular organic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
    • C08K2003/0818Alkali metal
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/30Sulfur-, selenium- or tellurium-containing compounds
    • C08K2003/3045Sulfates
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • C08K2003/321Phosphates
    • C08K2003/324Alkali metal phosphate

Abstract

The invention discloses an endothermic photoelectric conversion fluorescent exterior wall coating and a manufacturing method thereof, wherein the endothermic photoelectric conversion fluorescent exterior wall coating consists of three parts, namely a real stone matrix, a photoelectric independent component and a fluorescent adhesive component; wherein the fluorescent adhesive component is colloid obtained by reacting barite, epsom salt, lithium phosphate, copper nitrate, methyl methacrylate, azobisisobutyronitrile, dibutyl phthalate, stearic acid and methacrylic acid monomers; the photoelectric independent component is a photo-thermal conversion dispersoid which is constructed by the reaction of metallic sodium, diethyl dimethylmalonate, 2-bromobenzyl, sodium hydroxide, thionyl chloride, lead powder and tin powder; the stone substrate is a stone substrate constructed by quartz sand and Istmann C-12 film-forming assistant. The invention is environment-friendly and weather-resistant, has the functions of heat absorption and heat resistance, has the fluorescent decoration effect and has the photoelectric conversion basic capability.

Description

heat-absorbing photoelectric conversion fluorescent exterior wall coating and manufacturing method thereof
Technical Field
The invention relates to the technical field of exterior wall coatings, in particular to an endothermic photoelectric conversion fluorescent exterior wall coating and a manufacturing method thereof.
background
the exterior wall coating in the prior art generally only has a surface protection function and a decoration function, so that the great exterior surface area of a building is wasted, and more light and heat energy is wasted.
therefore, an exterior wall coating which is environment-friendly, weather-resistant, has the functions of heat absorption and heat resistance, has the fluorescent decorative effect and has the photoelectric conversion basic capability is urgently needed in the market.
disclosure of Invention
the invention aims to provide an exterior wall coating which is environment-friendly, weather-resistant, has the functions of heat absorption and heat resistance, has the fluorescent decorative effect and has the photoelectric conversion basic capability.
in order to achieve the purpose, the invention adopts the following technical scheme: a method for manufacturing an endothermic photoelectric conversion fluorescent exterior wall coating comprises the following steps;
1) Raw material preparation
Preparing raw materials: preparing 5.5-6.5 parts of barite, 5-6 parts of epsom salt, 0.3-0.5 part of lithium phosphate, 0.5-0.7 part of copper nitrate, 50-60 parts of methyl methacrylate, 0.1-0.2 part of azodiisobutyronitrile, 10-12 parts of tin powder, 5-6 parts of dibutyl phthalate, 1-1.2 parts of stearic acid, 0.5-0.8 part of methacrylic acid monomer, 0.8-0.9 part of metallic sodium, 7-8 parts of diethyl dimethylmalonate, 7-8 parts of 2-bromobenzyl bromide, 5-6 parts of sodium hydroxide, 2.5-2.8 parts of thionyl chloride, 3-4 parts of lead powder, 75-80 parts of quartz sand and 0.4-0.6 part of Istmann C-12 film-forming aid by weight;
preparing auxiliary materials: preparing enough ethanol, enough ethyl acetate, enough deionized water, enough hydrochloric acid aqueous solution with solute mass fraction of 20%, enough saturated sodium chloride aqueous solution and enough N, N-dimethylformamide;
2) Fluorescent mixed colloid manufacturing
Grinding the barite, epsom salt, lithium phosphate and copper nitrate prepared in the step 1) into 1200-1600 meshes of powder, and then uniformly mixing to obtain a fluorescent material;
secondly, mixing the fluorescent material obtained in the step I with the methyl methacrylate, azodiisobutyronitrile, dibutyl phthalate, stearic acid and methacrylic acid monomers prepared in the step 1) and uniformly stirring, then heating to 93-98 ℃, and carrying out prepolymerization for 10-12 min to obtain a mixed prepolymer;
Thirdly, placing the mixed prepolymer prepared in the second step in a water bath, preserving heat to 50-53 ℃, preserving heat for 11-12 h, then heating to 100 ℃, preserving heat for 60-80 min, cooling to room temperature at a cooling rate of 0.3-0.5 ℃/min, and spray-drying the reaction liquid cooled to room temperature to obtain colloidal particles, namely the required fluorescent mixed colloid;
3) photo-thermal induction liquid manufacturing
putting the sodium metal prepared in the step 1) into ethanol with the mass 30-40 times of that of the sodium metal, and stirring the sodium metal until the sodium metal is completely dissolved to obtain a mixed solution A;
Secondly, uniformly mixing diethyl dimethylmalonate prepared in the step 1) with ethanol with the volume of 1.2-1.3 times that of the diethyl dimethylmalonate to obtain a mixed solution B;
Slowly dripping the mixed liquid B obtained in the step II into the mixed liquid A obtained in the step I through a constant-pressure funnel, and stirring for 12-15 min to obtain mixed liquid C;
Slowly adding the 2-bromobenzyl prepared in the step 1) into the mixed liquid C obtained in the step three, heating to 92-95 ℃, stably refluxing until the reaction is complete, and cooling to room temperature to obtain a mixed liquid D containing solid substances;
fifthly, filtering solid content in the mixed solution D obtained in the step (iv), washing the obtained solution with sufficient ethyl acetate, and performing rotary evaporation extraction for 3-5 times to obtain colorless liquid;
dissolving the colorless liquid obtained in the fifth step into ethanol with the volume 5-8 times of that of the colorless liquid, uniformly adding deionized water with the volume equal to that of the colorless liquid and the sodium hydroxide prepared in the step 1) into the mixed liquid of the colorless liquid and the ethanol, heating to boil, refluxing to react completely, cooling to room temperature, removing the solvent by rotary evaporation, adding deionized water with the volume of 10% of that of the original colorless liquid, adjusting the pH to 1-1.5 by adopting the hydrochloric acid aqueous solution prepared in the step 1), keeping the pH at the temperature of 0-5 ℃ for 18-20 hours, and then completely drying by rotary evaporation to obtain white solid;
Seventhly, dissolving the white solid obtained in the step (c) in N, N-dimethylformamide with the mass 2 times of that of the white solid, heating to 135-140 ℃, keeping the temperature for 2.5-3 hours, removing the N, N-dimethylformamide by rotary evaporation, extracting residues by using ethyl acetate, washing by using the saturated sodium chloride aqueous solution prepared in the step (1) until the pH value is stable, and filtering to remove solid content after completely drying by rotary evaporation to obtain light yellow oily liquid;
mixing thionyl chloride prepared in the step 1) into light yellow oily liquid, heating to 42-45 ℃, reacting for 13-14 h, carrying out reduced pressure distillation treatment on reaction liquid, intercepting a component with the distillation temperature of 120-124 ℃, wherein the component is yellow liquid, mixing the lead powder prepared in the step 1) into the obtained yellow liquid, and then uniformly stirring, wherein the yellow liquid mixed with the lead powder is the required photo-thermal induction liquid;
4) paint manufacture
mixing and uniformly stirring tin powder and quartz sand prepared in the step 1) in the stage 1), fluorescent mixed colloid obtained in the step 2) and photo-thermal induction liquid obtained in the step 3), heating the obtained mixture to 55-60 ℃, keeping the temperature for 30-40 min, obtaining a primary reactant, and maintaining the temperature;
secondly, mixing the Istman C-12 film-forming additive prepared in the step 1) into the primary reactant obtained in the step I, uniformly stirring, and continuously preserving the heat for 20-25 min to obtain a gelatinized reactant;
Thirdly, after the gelatinization reactant obtained in the second step is cooled to room temperature, the deionized water prepared in the first step 1) is injected into the gelatinization reactant until the kinematic viscosity of the gelatinization reactant is reduced to 35mm2/s-38mm2And/s, obtaining the product, namely the required wear-resistant environment-friendly composite light real stone paint coating.
A heat-absorbing photoelectric conversion fluorescent exterior wall coating comprises three parts, namely a real stone matrix, a photoelectric independent component and a fluorescent adhesive component; wherein the fluorescent adhesive component is colloid obtained by reaction of 5.5-6.5 parts of barite, 5-6 parts of epsom salt, 0.3-0.5 part of lithium phosphate, 0.5-0.7 part of copper nitrate, 50-60 parts of methyl methacrylate, 0.1-0.2 part of azodiisobutyronitrile, 5-6 parts of dibutyl phthalate, 1-1.2 parts of stearic acid and 0.5-0.8 part of methacrylic acid monomer; the photoelectric independent component is a photo-thermal conversion dispersoid which is constructed by reacting 0.8 to 0.9 part of metallic sodium, 7 to 8 parts of diethyl dimethylmalonate, 7 to 8 parts of 2-bromobenzyl bromide, 5 to 6 parts of sodium hydroxide, 2.5 to 2.8 parts of thionyl chloride, 3 to 4 parts of lead powder and 10 to 12 parts of tin powder; the real stone substrate is a real stone substrate constructed by 75-80 parts of quartz sand and 0.4-0.6 part of Istmann C-12 film-forming assistant.
the complete use method of the invention is to brush and coat the conductive primer on the wall surface, then brush and coat the coating, then arrange the conductive structure on the surface of the coating, the conductive structure and the conductive primer are divided into a positive electrode and a negative electrode, and the electric energy storage device is assisted, so that the emergency lighting device in the building can be loaded, and certainly, the emergency lighting device can not be loaded with a large load.
compared with the prior art, the invention has the following advantages: (1) by doping part of electrothermal induction liquid into the excessively hard polymeric colloid and the real stone substrate, the essence of the coating is softened, the coating performance is improved, weak photothermal-electric conversion capability is obtained, the energy of sunlight (absorbing heat to generate electric energy) is consumed to achieve the purposes of heat resistance and temperature reduction, certain available energy is obtained, and part of residual energy is provided for the brightness excitation of the fluorescent material. (2) Compared with the prior art, the real stone coating serving as the matrix is not added with an adhesive or any other additive except a film-forming additive, so that the real stone coating is more environment-friendly, and the real stone components without the functional additive cannot be cured on the surface of a building, so that a semi-finished product PMMA which is not completely polymerized and has a fluorescent component cured inside, still retains part of activity and does not terminate polymerization reaction is added, the material can be cured at an accelerated speed under the action of a purple line, a short plate which is lower in binding force and strength due to the fact that no additive is used is exactly compensated, the wall surface binding force equivalent to that of the conventional real stone coating is obtained, the surface hardness is far higher than that of the conventional real stone coating, and the real stone coating is more wear-resistant. (3) PMMA has good weather resistance but poor oxygen resistance, a fluorescent material has good oxygen resistance but poor water resistance, a photoelectric conversion material has good water resistance, oxygen resistance and poor weather resistance (mainly poor acid resistance), and a real stone base material is used as an auxiliary material, so that the invention has complementary short phases, and obtains a coating with good overall performance, but the invention has the defects of poor high temperature resistance (the coating can only be maintained for 24 hours at 65 ℃ by actual measurement, namely the coating can be slowly deteriorated, and the coating has no obvious change after being tested for 1000 hours at 50 ℃) and poor acid resistance (so the coating can not be applied to areas with heavy air pollution and more acid rain) except that the weather resistance is superior to the prior art. (4) The fluorescent powder is low-cost mineral powder, can absorb light waves with longer wavelength (light waves with the wavelength of 900nm-1500 nm) when sunlight is sufficient in the daytime, consumes partial light energy, achieves the technical purpose of slight cooling, emits slightly red light at night, and has obvious decorative effect by twinkling stars. Therefore, the invention has the characteristics of environmental protection, weather resistance, heat absorption and heat resistance, fluorescent decoration effect and photoelectric conversion basic capability.
Detailed Description
Example 1:
a heat-absorbing photoelectric conversion fluorescent exterior wall coating comprises three parts, namely a real stone matrix, a photoelectric independent component and a fluorescent adhesive component; wherein the fluorescent adhesive component is colloid obtained by reacting barite, epsom salt, lithium phosphate, copper nitrate, methyl methacrylate, azobisisobutyronitrile, dibutyl phthalate, stearic acid and methacrylic acid monomers; the photoelectric independent component is a photo-thermal conversion dispersoid which is constructed by the reaction of metallic sodium, diethyl dimethylmalonate, 2-bromobenzyl, sodium hydroxide, thionyl chloride, lead powder and tin powder; the real stone substrate is a real stone substrate constructed by quartz sand and Istmann C-12 film-forming auxiliary agent;
The manufacturing method of the exterior wall coating comprises the following steps;
1) raw material preparation
Preparing raw materials: preparing 6.2kg of barite, 5.6kg of epsom salt, 0.35kg of lithium phosphate, 0.57kg of copper nitrate, 54kg of methyl methacrylate, 0.18kg of azodiisobutyronitrile, 11kg of tin powder, 5.4kg of dibutyl phthalate, 1.2kg of stearic acid, 0.7kg of methacrylic acid monomer, 0.8kg of metal sodium, 7.8kg of diethyl dimethylmalonate, 7.4kg of 2-bromobenzyl, 5.6kg of sodium hydroxide, 2.7kg of thionyl chloride, 3.8kg of lead powder, 78kg of quartz sand and 0.5kg of Istmann C-12 film-forming aid in parts by weight;
preparing auxiliary materials: preparing enough ethanol, enough ethyl acetate, enough deionized water, enough hydrochloric acid aqueous solution with solute mass fraction of 20%, enough saturated sodium chloride aqueous solution and enough N, N-dimethylformamide;
2) Fluorescent mixed colloid manufacturing
grinding the barite, epsom salt, lithium phosphate and copper nitrate prepared in the step 1) into 1200-1600 meshes of powder, and then uniformly mixing to obtain a fluorescent material;
secondly, mixing the fluorescent material obtained in the step I with the methyl methacrylate, azodiisobutyronitrile, dibutyl phthalate, stearic acid and methacrylic acid monomers prepared in the step 1) and uniformly stirring, then heating to 93-98 ℃, and carrying out prepolymerization for 10-12 min to obtain a mixed prepolymer;
thirdly, placing the mixed prepolymer prepared in the second step in a water bath, preserving heat to 50-53 ℃, preserving heat for 11-12 h, then heating to 100 ℃, preserving heat for 60-80 min, cooling to room temperature at a cooling rate of 0.3-0.5 ℃/min, and spray-drying the reaction liquid cooled to room temperature to obtain colloidal particles, namely the required fluorescent mixed colloid;
3) photo-thermal induction liquid manufacturing
Putting the sodium metal prepared in the step 1) into ethanol with the mass 30-40 times of that of the sodium metal, and stirring the sodium metal until the sodium metal is completely dissolved to obtain a mixed solution A;
secondly, uniformly mixing diethyl dimethylmalonate prepared in the step 1) with ethanol with the volume of 1.2-1.3 times that of the diethyl dimethylmalonate to obtain a mixed solution B;
slowly dripping the mixed liquid B obtained in the step II into the mixed liquid A obtained in the step I through a constant-pressure funnel, and stirring for 12-15 min to obtain mixed liquid C;
slowly adding the 2-bromobenzyl prepared in the step 1) into the mixed liquid C obtained in the step three, heating to 92-95 ℃, stably refluxing until the reaction is complete, and cooling to room temperature to obtain a mixed liquid D containing solid substances;
Fifthly, filtering solid content in the mixed solution D obtained in the step (iv), washing the obtained solution with sufficient ethyl acetate, and performing rotary evaporation extraction for 3-5 times to obtain colorless liquid;
dissolving the colorless liquid obtained in the fifth step into ethanol with the volume 5-8 times of that of the colorless liquid, uniformly adding deionized water with the volume equal to that of the colorless liquid and the sodium hydroxide prepared in the step 1) into the mixed liquid of the colorless liquid and the ethanol, heating to boil, refluxing to react completely, cooling to room temperature, removing the solvent by rotary evaporation, adding deionized water with the volume of 10% of that of the original colorless liquid, adjusting the pH to 1-1.5 by adopting the hydrochloric acid aqueous solution prepared in the step 1), keeping the pH at the temperature of 0-5 ℃ for 18-20 hours, and then completely drying by rotary evaporation to obtain white solid;
seventhly, dissolving the white solid obtained in the step (c) in N, N-dimethylformamide with the mass 2 times of that of the white solid, heating to 135-140 ℃, keeping the temperature for 2.5-3 hours, removing the N, N-dimethylformamide by rotary evaporation, extracting residues by using ethyl acetate, washing by using the saturated sodium chloride aqueous solution prepared in the step (1) until the pH value is stable, and filtering to remove solid content after completely drying by rotary evaporation to obtain light yellow oily liquid;
Mixing thionyl chloride prepared in the step 1) into light yellow oily liquid, heating to 42-45 ℃, reacting for 13-14 h, carrying out reduced pressure distillation treatment on reaction liquid, intercepting a component with the distillation temperature of 120-124 ℃, wherein the component is yellow liquid, mixing the lead powder prepared in the step 1) into the obtained yellow liquid, and then uniformly stirring, wherein the yellow liquid mixed with the lead powder is the required photo-thermal induction liquid;
4) paint manufacture
Mixing and uniformly stirring tin powder and quartz sand prepared in the step 1) in the stage 1), fluorescent mixed colloid obtained in the step 2) and photo-thermal induction liquid obtained in the step 3), heating the obtained mixture to 55-60 ℃, keeping the temperature for 30-40 min, obtaining a primary reactant, and maintaining the temperature;
Secondly, mixing the Istman C-12 film-forming additive prepared in the step 1) into the primary reactant obtained in the step I, uniformly stirring, and continuously preserving the heat for 20-25 min to obtain a gelatinized reactant;
thirdly, after the gelatinization reactant obtained in the second step is cooled to room temperature, the deionized water prepared in the first step 1) is injected into the gelatinization reactant until the kinematic viscosity of the gelatinization reactant is reduced to 35mm2/s-38mm2And/s, obtaining the product, namely the required wear-resistant environment-friendly composite light real stone paint coating.
the bonding force grade of the invention is 1-2 grade according to GB/T9286-1998 detection, the surface hardness after curing is 2.5H-4H, the photoelectric conversion efficiency is 2.3-3.1%, under the outdoor environment of 30 ℃, the indoor temperature of 4-5 ℃ can be reduced, weak red light can be emitted at night, the mechanical property can be ensured to be reduced by not more than 5% in 20 years and the wall surface bonding force can be ensured to be reduced by not more than 8% under the conditions of no acid and 25 ℃, and the structure is compact, the neutral rainwater is not feared, and the method is different.
Example 2:
the whole is in accordance with example 1, with the difference that:
the manufacturing method of the exterior wall coating comprises the following steps;
1) raw material preparation
preparing raw materials: according to parts by weight, 5.5kg of barite, 5kg of epsom salt, 0.3kg of lithium phosphate, 0.5kg of copper nitrate, 50kg of methyl methacrylate, 0.1kg of azodiisobutyronitrile, 12kg of tin powder, 5kg of dibutyl phthalate, 1kg of stearic acid, 0.5kg of methacrylic acid monomer, 0.9kg of metal sodium, 8kg of diethyl dimethylmalonate, 8kg of 2-bromobenzyl, 6kg of sodium hydroxide, 2.8kg of thionyl chloride, 4kg of lead powder, 80kg of quartz sand and 0.6kg of Istmann C-12 film-forming aid are prepared;
example 3:
The whole is in accordance with example 1, with the difference that:
the manufacturing method of the exterior wall coating comprises the following steps;
1) raw material preparation
preparing raw materials: preparing 6.5kg of barite, 6kg of epsom salt, 0.5kg of lithium phosphate, 0.7kg of copper nitrate, 60kg of methyl methacrylate, 0.2kg of azodiisobutyronitrile, 10kg of tin powder, 6kg of dibutyl phthalate, 1.2kg of stearic acid, 0.8kg of methacrylic acid monomer, 0.8kg of metal sodium, 7kg of diethyl dimethylmalonate, 7kg of 2-bromobenzyl, 5kg of sodium hydroxide, 2.5kg of thionyl chloride, 3kg of lead powder, 75kg of quartz sand and 0.4kg of Istmann C-12 film-forming aid in parts by weight;
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (2)

1. a manufacturing method of heat absorption photoelectric conversion fluorescent exterior wall paint is characterized by comprising the following steps;
1) raw material preparation
preparing raw materials: preparing 5.5-6.5 parts of barite, 5-6 parts of epsom salt, 0.3-0.5 part of lithium phosphate, 0.5-0.7 part of copper nitrate, 50-60 parts of methyl methacrylate, 0.1-0.2 part of azodiisobutyronitrile, 10-12 parts of tin powder, 5-6 parts of dibutyl phthalate, 1-1.2 parts of stearic acid, 0.5-0.8 part of methacrylic acid monomer, 0.8-0.9 part of metallic sodium, 7-8 parts of diethyl dimethylmalonate, 7-8 parts of 2-bromobenzyl bromide, 5-6 parts of sodium hydroxide, 2.5-2.8 parts of thionyl chloride, 3-4 parts of lead powder, 75-80 parts of quartz sand and 0.4-0.6 part of Istmann C-12 film-forming aid by weight;
preparing auxiliary materials: preparing enough ethanol, enough ethyl acetate, enough deionized water, enough hydrochloric acid aqueous solution with solute mass fraction of 20%, enough saturated sodium chloride aqueous solution and enough N, N-dimethylformamide;
2) fluorescent mixed colloid manufacturing
grinding the barite, epsom salt, lithium phosphate and copper nitrate prepared in the step 1) into 1200-1600 meshes of powder, and then uniformly mixing to obtain a fluorescent material;
secondly, mixing the fluorescent material obtained in the step I with the methyl methacrylate, azodiisobutyronitrile, dibutyl phthalate, stearic acid and methacrylic acid monomers prepared in the step 1) and uniformly stirring, then heating to 93-98 ℃, and carrying out prepolymerization for 10-12 min to obtain a mixed prepolymer;
thirdly, placing the mixed prepolymer prepared in the second step in a water bath, preserving heat to 50-53 ℃, preserving heat for 11-12 h, then heating to 100 ℃, preserving heat for 60-80 min, cooling to room temperature at a cooling rate of 0.3-0.5 ℃/min, and spray-drying the reaction liquid cooled to room temperature to obtain colloidal particles, namely the required fluorescent mixed colloid;
3) Photo-thermal induction liquid manufacturing
Putting the sodium metal prepared in the step 1) into ethanol with the mass 30-40 times of that of the sodium metal, and stirring the sodium metal until the sodium metal is completely dissolved to obtain a mixed solution A;
Secondly, uniformly mixing diethyl dimethylmalonate prepared in the step 1) with ethanol with the volume of 1.2-1.3 times that of the diethyl dimethylmalonate to obtain a mixed solution B;
Slowly dripping the mixed liquid B obtained in the step II into the mixed liquid A obtained in the step I through a constant-pressure funnel, and stirring for 12-15 min to obtain mixed liquid C;
slowly adding the 2-bromobenzyl prepared in the step 1) into the mixed liquid C obtained in the step three, heating to 92-95 ℃, stably refluxing until the reaction is complete, and cooling to room temperature to obtain a mixed liquid D containing solid substances;
fifthly, filtering solid content in the mixed solution D obtained in the step (iv), washing the obtained solution with sufficient ethyl acetate, and performing rotary evaporation extraction for 3-5 times to obtain colorless liquid;
dissolving the colorless liquid obtained in the fifth step into ethanol with the volume 5-8 times of that of the colorless liquid, uniformly adding deionized water with the volume equal to that of the colorless liquid and the sodium hydroxide prepared in the step 1) into the mixed liquid of the colorless liquid and the ethanol, heating to boil, refluxing to react completely, cooling to room temperature, removing the solvent by rotary evaporation, adding deionized water with the volume of 10% of that of the original colorless liquid, adjusting the pH to 1-1.5 by adopting the hydrochloric acid aqueous solution prepared in the step 1), keeping the pH at the temperature of 0-5 ℃ for 18-20 hours, and then completely drying by rotary evaporation to obtain white solid;
seventhly, dissolving the white solid obtained in the step (c) in N, N-dimethylformamide with the mass 2 times of that of the white solid, heating to 135-140 ℃, keeping the temperature for 2.5-3 hours, removing the N, N-dimethylformamide by rotary evaporation, extracting residues by using ethyl acetate, washing by using the saturated sodium chloride aqueous solution prepared in the step (1) until the pH value is stable, and filtering to remove solid content after completely drying by rotary evaporation to obtain light yellow oily liquid;
mixing thionyl chloride prepared in the step 1) into light yellow oily liquid, heating to 42-45 ℃, reacting for 13-14 h, carrying out reduced pressure distillation treatment on reaction liquid, intercepting a component with the distillation temperature of 120-124 ℃, wherein the component is yellow liquid, mixing the lead powder prepared in the step 1) into the obtained yellow liquid, and then uniformly stirring, wherein the yellow liquid mixed with the lead powder is the required photo-thermal induction liquid;
4) Paint manufacture
Mixing and uniformly stirring tin powder and quartz sand prepared in the step 1) in the stage 1), fluorescent mixed colloid obtained in the step 2) and photo-thermal induction liquid obtained in the step 3), heating the obtained mixture to 55-60 ℃, keeping the temperature for 30-40 min, obtaining a primary reactant, and maintaining the temperature;
secondly, mixing the Istman C-12 film-forming additive prepared in the step 1) into the primary reactant obtained in the step I, uniformly stirring, and continuously preserving the heat for 20-25 min to obtain a gelatinized reactant;
Thirdly, after the gelatinization reactant obtained in the second step is cooled to room temperature, the deionized water prepared in the first step 1) is injected into the gelatinization reactant until the kinematic viscosity of the gelatinization reactant is reduced to 35mm2/s-38mm2And/s, obtaining the product, namely the required wear-resistant environment-friendly composite light real stone paint coating.
2. The heat-absorbing photoelectric conversion fluorescent exterior wall coating is characterized in that: the heat-absorbing photoelectric conversion fluorescent exterior wall coating consists of three parts, namely a real stone substrate, a photoelectric independent component and a fluorescent adhesive component; wherein the fluorescent adhesive component is colloid obtained by reaction of 5.5-6.5 parts of barite, 5-6 parts of epsom salt, 0.3-0.5 part of lithium phosphate, 0.5-0.7 part of copper nitrate, 50-60 parts of methyl methacrylate, 0.1-0.2 part of azodiisobutyronitrile, 5-6 parts of dibutyl phthalate, 1-1.2 parts of stearic acid and 0.5-0.8 part of methacrylic acid monomer; the photoelectric independent component is a photo-thermal conversion dispersoid which is constructed by reacting 0.8 to 0.9 part of metallic sodium, 7 to 8 parts of diethyl dimethylmalonate, 7 to 8 parts of 2-bromobenzyl bromide, 5 to 6 parts of sodium hydroxide, 2.5 to 2.8 parts of thionyl chloride, 3 to 4 parts of lead powder and 10 to 12 parts of tin powder; the real stone substrate is a real stone substrate constructed by 75-80 parts of quartz sand and 0.4-0.6 part of Istmann C-12 film-forming assistant.
CN201910917698.6A 2019-09-26 2019-09-26 heat-absorbing photoelectric conversion fluorescent exterior wall coating and manufacturing method thereof Pending CN110564253A (en)

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CN1241603A (en) * 1998-07-10 2000-01-19 张宝山 Production process and product of decorative color luminous paint without quenching
CN203113688U (en) * 2013-02-02 2013-08-07 张志坚 Luminous stone material
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CN104004126A (en) * 2014-05-30 2014-08-27 盐城工学院 Preparation method of organic fluorescent luminous film
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