CN109021728A - Heat insulating coat and preparation method thereof - Google Patents
Heat insulating coat and preparation method thereof Download PDFInfo
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- CN109021728A CN109021728A CN201810611957.8A CN201810611957A CN109021728A CN 109021728 A CN109021728 A CN 109021728A CN 201810611957 A CN201810611957 A CN 201810611957A CN 109021728 A CN109021728 A CN 109021728A
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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
- C09D129/00—Coating 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 an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Coating compositions based on hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Coating compositions based on derivatives of such polymers
- C09D129/02—Homopolymers or copolymers of unsaturated alcohols
- C09D129/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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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
- 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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- 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
- 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
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
Abstract
The invention discloses a kind of heat insulating coats and preparation method thereof；The functional stuffing based on graphene oxide is prepared first, then is reacted by organic inorganic hybridization, is prepared function modified system, is finally obtained the product of best performance in the case where limiting material rate using rational formula binding function modified system between organic matter.Due to introducing a certain amount of siloxy group in product structure, epoxy group, obtained product heat resistance and adhesive property is excellent, and have preparation process simple, it is low for equipment requirements, it is suitble to industrial amplification production, the preparation of especially creative proposition functional stuffing, in conjunction with the use of different organic components, it is more dispersible in coating, the phenomenon that reducing reunion, improve the adhesive force of coating, obtained coating performance is excellent, outer surface temperature and interior environment temperature can be effectively reduced, play heat-insulated effect, and abrasion resistance, waterproofness, flexibility, rheological characteristic, acid resistance is all more excellent than the prior art.
Description
Technical field
The present invention relates to a kind of organic composite materials and preparation method thereof, and in particular to heat insulating coat and preparation method thereof.
Background technique
Currently, heat insulating coat is widely used in the fields such as space flight and aviation, building, chemical industry, such as building field
In, heat insulating coat is coated on the large-area glass such as luxurious hotel, office building, exhibition room window and the glass curtain wall of luxurious style, is dropped
Low indoor temperature.Heat insulating coat refers to coated on body surface, covers so that Coated Surface Temperature be inhibited to rise and reduce simultaneously
Cover material internal temperature, to play the coating of heat-blocking action.
Currently, research emphasis is mainly the selection of functional material, such as tin indium oxide, antimony oxidation tin, titanium dioxide.Substantially
Principle be the spectral selection of such nano material is utilized, but such thermal isolation film need to be improved there is also heat insulation and
Thermal isolation film stability, ultraviolet aging resistance, in terms of performance be also lacking the problem of.
Summary of the invention
The status that the present invention is insufficient for heat resistance existing for existing heat insulating coat agent, heat insulation is poor, provides one kind
Heat insulating coat and preparation method thereof.
To reach goal of the invention of the present invention, the technical solution adopted is as follows:
A kind of preparation method of heat insulating coat, which comprises the steps of:
(1) under nitrogen protection, six ammonium chloroiridates, nitric hydrate nickel, cobalt nitrate, ethyl alcohol and propionic acid are mixed；It is then refluxed for stirring
110 minutes, ammonium hydroxide, sodium chloride is then added；Back flow reaction 10 minutes；Then it removes solvent and obtains solids；By solids heat
It is ground after processing, water impregnates, is dried to obtain filler；The heat treatment is sintered 15 minutes for 200 DEG C, then calcines 15 in 400 DEG C
Minute, then calcined 5 minutes in 650 DEG C；By filler, graphene oxide, hexamethylene diisocyanate, N- crassitude
After ketone, 2- mercaptopyridine, triphenyl silanol mixing, mechanical stirring 2 hours, then it is ultrasonically treated 3 hours, obtains functional stuffing；
(2) mix polyethylene alcohol solution, tetraphenylporphyrin iron, peroxidized t-butyl perbenzoate, 80 DEG C stir 1 hour, then
Water is removed, dimethyldimethoxysil,ne solution, 1 is then added, 3,5- three-glycidyl-S- triazinetriones, functional stuffing stir
It mixes 50 minutes, adds glycerine, ethyl orthosilicate, stirring obtains modified system in 30 minutes；
(3) modified system and hexamethyl trien, one chlorosilane of trialkyl, isopropanol, phthalic acid two are shunk
After glyceride mixing, 80 DEG C are stirred 1 hour；Calgon, maleic anhydride, anacardol are added, is stirred 1 hour in 110 DEG C,
Obtain thermal-insulating system；
(4) thermal-insulating system is dried 10 minutes in 85 DEG C；Then solidify 2.5~3 minutes in 125 DEG C, obtain heat insulating coat.
In above-mentioned technical proposal, solvent is removed using ventilation method；The mass concentration of ammonium hydroxide is 22%；The partial size of the filler
It is 0.23~0.28 micron.The skin effect of nanoparticle enables nanoparticle to have very high surface, it is easy to and coating
In organic component combine, so that the compactness of coating is greatly improved, greatly reduce the hole of coating and defect, and with changing
Functional stuffing after property, the phenomenon that being more dispersible in coating, reduce reunion, the adhesive force of coating, thermal insulation, waterproofness,
Rheological characteristic, glossiness are all more excellent than the prior art.
In above-mentioned technical proposal, six ammonium chloroiridate, nitric hydrate nickel, cobalt nitrate, ethyl alcohol, propionic acid, ammonium hydroxide, sodium chloride
Mass ratio be 100: 73: 42: 220: 32: 29: 15.Propionic acid, ammonium hydroxide can provide good mixing condition, so that playing a role
Metallic element no-float, sodium chloride then makes solids heat be uniformly dispersed when sintering, more crucially can be with
Obtain nanoscale product, and cavity is presented in nano grain surface, improve the attachment interface interaction area of organic matter and filler with
And interface interaction power, it can find out from coating thermal stability, the water absorption rate of embodiment comparative example.Functional stuffing of the present invention can be
High reflectance is obtained under low cost, the cost of reflective heat-insulation paint can be greatly reduced.
In above-mentioned technical proposal, in the dimethyldimethoxysil,ne solution, solvent is toluene.Add in coating of the present invention
Graphene is entered, graphene is since small-size effect is filled into graphene among the cavity and defect of coating, two-dimensional layer
Structure is layering in coating, forms physical isolation, and the skin effect of graphene can make heat rest on coating surface,
Not to matrix permeability, especially graphene auxiliary packing is functioned, and effectively improves the dispersibility and thermal insulation of filler, because
The present invention uses graphene oxide, and surface group can be chemically reacted with the organic matter of function ingredients, divides to improve
It dissipates property, interfacial effect and avoids particle aggregation.
In above-mentioned technical proposal, the filler, graphene oxide, hexamethylene diisocyanate, N-Methyl pyrrolidone,
2- mercaptopyridine, triphenyl silanol mass ratio be 100: 13: 82: 33: 32: 59.Using hexamethylene diisocyanate, N- first
The modified nanoparticle of base pyrrolidones, 2- mercaptopyridine, triphenyl silanol is functional stuffing, and organic matter unit is in nanoparticle
Surface reacts to form one layer of organic matter film, can not only react to each other, can also prevent with other organic components of thermal-insulating system
It contacts with each other between nanoparticle, so as to improve the interface binding power of nanoparticle, reduces material internal defect.
In above-mentioned technical proposal, the polyvinyl alcohol, tetraphenylporphyrin iron, peroxidized t-butyl perbenzoate, dimethyl two
Methyldimethoxysilane solution, 1,3,5- three-glycidyl-S- triazinetrione, functional stuffing, glycerine, ethyl orthosilicate mass ratio
It is 100: 8: 35: 70: 55: 22.
Solidify coating of the present invention contains stable phenyl ring, silicon, phosphorus etc., and paint film is good to substrate adhesive force, and structure stomata is small, knot
Structure is fine and close, has excellent heat-proof quality, shields to matrix.
In above-mentioned technical proposal, the modified system, hexamethyl trien, one chlorosilane of trialkyl, isopropanol, adjacent benzene
Dicarboxylic acid diglycidyl ester, calgon, maleic anhydride, anacardol mass ratio be 100: 55: 28: 80: 12: 9: 38:
16。
The invention avoids usual resins, such as the use of epoxy resin, amino resins, phenolic resin, acrylic resin,
It is limited using multiple groups organic compound by proportion and is selected with preparation process, obtained coating has lower voc content, stingless
The advantages that swashing property smell, after film-forming, moreover it is possible to show the advantage that general resin does not have, for example there is good light
The features such as pool, waterproofness and adhesion.
In above-mentioned technical proposal, the heat insulating coat with a thickness of 0.1~0.15 millimeter.The use of filler is of the invention
One innovative point, in terms of the application effect that the present invention is implemented, iridium nickel cobalt cooperates the thermal insulation that coating material can be enhanced, with graphite
Alkene cooperates the intensity that can promote coating, can extend the service life of coating.
Organic compound of the invention such as hexamethylene diisocyanate, peroxidized t-butyl perbenzoate, 2- sulfydryl pyrrole
Pyridine, maleic anhydride, anacardol etc. not only possess the effect of conventional coupling agents dispersion aggregate, more mainly have reaction efficiency
It is high, dispersion effect is good, and can be stable be present between particle, ensure that filler dispersion and with other components such as pregnancy
Sound response occurs for base trien, o-phthalic acid diglycidyl ester, triphenyl silanol, one chlorosilane of trialkyl etc.
The advantages of, coating material Shrinkage Problem due to caused by surface tension can also be improved, system viscosity can significantly reduced
Simultaneous reactions finally participate in film-forming, smaller to system material properties affect.
The heat insulating coat prepared according to the preparation method of above-mentioned heat insulating coat.The present invention has high thermal insulation and excellent flexible
Property, oil resistant ageing properties, it is a kind of good environmental protection coating material that volatile solvent is seldom, greatly reduces the discharge of VOC, film forming
Substance combines o-phthalic acid diglycidyl ester, 1,3,5- three-glycidyl-S- triazinetrione, hexa-methylene diisocyanate
The excellent flexibility of high adhesion force, high intensity, low-shrinkage and the polyvinyl alcohol of ester, N-Methyl pyrrolidone, 2- mercaptopyridine
And triphenyl silanol, hexamethyl trien, one chlorosilane oil resistant ageing properties of trialkyl and calgon, cashew nut
The advantages of phenol filming performance, can also play the role of cured due to containing reactive group in maleic anhydride, ethyl orthosilicate；
In short, making resin film high for the reflectivity of sunlight, there is excellent heat-proof quality.
Existing heat-proof coating material general thickness is at 300~500 μm, and heat-proof coating material of the present invention is a kind of thin material
Material, thickness range are 0.1~0.15 millimeter；Heat insulating coat of the invention can form one layer fine and close thin in substrate surface
Film can reflect heat, to play heat-insulated efficiency, while also at low cost, formula is simple, easy for construction, oil resistant is resistance to
The advantages that aging and waterproof performance, overcomes the single problem of the generally existing performance of existing heat-proof coating material.
Specific embodiment
Below with reference to embodiment, technical solution of the present invention is further elaborated.
Each compound combination of the present invention uses, and product surface drying time does solid work that the time is very short, and adhesive force is high, and water absorption rate is low,
Good luster, flexibility is good, film long service life, can produce extensively and constantly replace current material.Coating is with functional stuffing
Based on organic component, weatherability is preferable, and filler thermal insulation, refraction index are high, has the reflectivity high to solar radiant heat
Can and to the very low thermal conductivity of heat transfer, be a kind of coating for having reflection, the dual heat-proof quality of barrier, can be effectively reduced
The hull-skin temperature and interior environment temperature of matrix, embodiment the result shows that, when band coating hull-skin temperature ratio is not coated with brush applied coating
There is a sharp decline；Coating of the invention in atmosphere oxygen, hydrogen sulfide, sulfur sesquioxide and ammonia it is all more stable, simultaneously
Also there is good heat resistance, functional stuffing reduces the thermal coefficient of coating, improves the abrasion resistance and film table of coating
Face self-cleaning, moreover it is possible to the stability for increasing coating system can improve filler wetability using function component, prevent coating loose colour and
Floating has preferable antifoaming ability, levelability when dispersing to coating, can prevent coating from flocculating, and is suitable for various matrix surfaces.
Embodiment one
A kind of preparation method of heat insulating coat, includes the following steps:
(1) under nitrogen protection, six ammonium chloroiridate of 100g, 73g nitric hydrate nickel, 42g cobalt nitrate, 220g ethyl alcohol and 32g are mixed
Propionic acid；It is then refluxed for stirring 110 minutes, 29g ammonium hydroxide (22wt%), 15g sodium chloride is then added；Back flow reaction 10 minutes；Then
Ventilation removes solvent and obtains solids；It is ground after solids is heat-treated, water impregnates, is dried to obtain filler；The heat treatment is
200 DEG C are sintered 15 minutes, then calcine in 400 DEG C 15 minutes, then calcine 5 minutes in 650 DEG C；By 100g partial size be 0.23~
0.28 micron of filler, 13g graphene oxide, 82g hexamethylene diisocyanate, 33gN- methyl pyrrolidone, 32g2- mercapto
After yl pyridines, the mixing of 59g triphenyl silanol, mechanical stirring 2 hours, then it is ultrasonically treated 3 hours, obtains functional stuffing；
(2) mixing 1Kg polyvinyl alcohol water solution (10wt%), 8g tetraphenylporphyrin iron, 35g peroxidized t-butyl perbenzoate, 80 DEG C
Stirring 1 hour, then removes water, then addition 200g dimethyldimethoxysil,ne toluene solution (35wt%), 55g1, and 3,5-
Three-glycidyl-S- triazinetrione, 22g functional stuffing stir 50 minutes, add glycerine, ethyl orthosilicate, stir 30 points
Clock obtains modified system；
(3) by 100g modified system and 55g hexamethyl trien, one chlorosilane of 28g trialkyl, 80g isopropanol, 12g
After o-phthalic acid diglycidyl ester mixing, 80 DEG C are stirred 1 hour；Add 9g calgon, 38g maleic anhydride, 16g
Anacardol stirs 1 hour in 110 DEG C, obtains thermal-insulating system；
(4) thermal-insulating system is dried 10 minutes in 85 DEG C；Then solidify 2.5~3 minutes in 125 DEG C, obtain heat insulating coat.
Comparative example one
A kind of preparation method of heat insulating coat, includes the following steps:
(1) by 100g nano-titanium dioxide, 13g graphene oxide, 82g hexamethylene diisocyanate, 33gN- crassitude
After ketone, 32g2- mercaptopyridine, the mixing of 59g triphenyl silanol, mechanical stirring 2 hours, then it is ultrasonically treated 3 hours, obtains function
Filler；
(2) mixing 1Kg polyvinyl alcohol water solution (10wt%), 8g tetraphenylporphyrin iron, 35g peroxidized t-butyl perbenzoate, 80 DEG C
Stirring 1 hour, then removes water, then addition 200g dimethyldimethoxysil,ne toluene solution (35wt%), 55g1, and 3,5-
Three-glycidyl-S- triazinetrione, 22g functional stuffing stir 50 minutes, add glycerine, ethyl orthosilicate, stir 30 points
Clock obtains modified system；
(3) by 100g modified system and 55g hexamethyl trien, one chlorosilane of 28g trialkyl, 80g isopropanol, 12g
After o-phthalic acid diglycidyl ester mixing, 80 DEG C are stirred 1 hour；Add 9g calgon, 38g maleic anhydride, 16g
Anacardol stirs 1 hour in 110 DEG C, obtains thermal-insulating system；
(4) thermal-insulating system is dried 10 minutes in 85 DEG C；Then solidify 2.5~3 minutes in 125 DEG C, obtain heat insulating coat.
Comparative example two
A kind of preparation method of heat insulating coat, includes the following steps:
(1) under nitrogen protection, six ammonium chloroiridate of 100g, 73g nitric hydrate nickel, 42g cobalt nitrate, 220g ethyl alcohol and 32g are mixed
Propionic acid；It is then refluxed for stirring 110 minutes, 29g ammonium hydroxide (22wt%), 15g sodium chloride is then added；Back flow reaction 10 minutes；Then
Ventilation removes solvent and obtains solids；It is ground after solids is heat-treated, water impregnates, is dried to obtain filler；The heat treatment is
200 DEG C are sintered 15 minutes, then calcine in 400 DEG C 15 minutes, then calcine 5 minutes in 650 DEG C；By 100g partial size be 0.23~
0.28 micron of filler, 82g hexamethylene diisocyanate, 33gN- methyl pyrrolidone, 32g2- mercaptopyridine, 59g triphen
After the mixing of base silanol, mechanical stirring 2 hours, then it is ultrasonically treated 3 hours, obtains functional stuffing；
(2) mixing 1Kg polyvinyl alcohol water solution (10wt%), 8g tetraphenylporphyrin iron, 35g peroxidized t-butyl perbenzoate, 80 DEG C
Stirring 1 hour, then removes water, then addition 200g dimethyldimethoxysil,ne toluene solution (35wt%), 55g1, and 3,5-
Three-glycidyl-S- triazinetrione, 22g functional stuffing stir 50 minutes, add glycerine, ethyl orthosilicate, stir 30 points
Clock obtains modified system；
(3) by 100g modified system and 55g hexamethyl trien, one chlorosilane of 28g trialkyl, 80g isopropanol, 12g
After o-phthalic acid diglycidyl ester mixing, 80 DEG C are stirred 1 hour；Add 9g calgon, 38g maleic anhydride, 16g
Anacardol stirs 1 hour in 110 DEG C, obtains thermal-insulating system；
(4) thermal-insulating system is dried 10 minutes in 85 DEG C；Then solidify 2.5~3 minutes in 125 DEG C, obtain heat insulating coat.
Comparative example three
A kind of preparation method of heat insulating coat, includes the following steps:
(1) under nitrogen protection, six ammonium chloroiridate of 100g, 73g nitric hydrate nickel, 42g cobalt nitrate, 220g ethyl alcohol and 32g are mixed
Propionic acid；It is then refluxed for stirring 110 minutes, 29g ammonium hydroxide (22wt%), 15g sodium chloride is then added；Back flow reaction 10 minutes；Then
Ventilation removes solvent and obtains solids；It is ground after solids is heat-treated, water impregnates, is dried to obtain filler；The heat treatment is
200 DEG C are sintered 15 minutes, then calcine in 400 DEG C 15 minutes, then calcine 5 minutes in 650 DEG C；By 100g partial size be 0.23~
After 0.28 micron of filler, 13g graphene oxide, 1.8gKH550 mixing, mechanical stirring 2 hours, then it is ultrasonically treated 3 hours,
Obtain functional stuffing；
(2) mixing 1Kg polyvinyl alcohol water solution (10wt%), 8g tetraphenylporphyrin iron, 35g peroxidized t-butyl perbenzoate, 80 DEG C
Stirring 1 hour, then removes water, then addition 200g dimethyldimethoxysil,ne toluene solution (35wt%), 55g1, and 3,5-
Three-glycidyl-S- triazinetrione, 22g functional stuffing stir 50 minutes, add glycerine, ethyl orthosilicate, stir 30 points
Clock obtains modified system；
(3) by 100g modified system and 55g hexamethyl trien, one chlorosilane of 28g trialkyl, 80g isopropanol, 12g
After o-phthalic acid diglycidyl ester mixing, 80 DEG C are stirred 1 hour；Add 9g calgon, 38g maleic anhydride, 16g
Anacardol stirs 1 hour in 110 DEG C, obtains thermal-insulating system；
(4) thermal-insulating system is dried 10 minutes in 85 DEG C；Then solidify 2.5~3 minutes in 125 DEG C, obtain heat insulating coat.
Comparative example four
A kind of preparation method of heat insulating coat, includes the following steps:
(1) under nitrogen protection, six ammonium chloroiridate of 100g, 73g nitric hydrate nickel, 42g cobalt nitrate, 220g ethyl alcohol and 32g are mixed
Propionic acid；It is then refluxed for stirring 110 minutes, 29g ammonium hydroxide (22wt%) then is added；Back flow reaction 10 minutes；Then ventilation removes molten
Agent obtains solids；It is ground after solids is heat-treated, water impregnates, is dried to obtain filler；The heat treatment is 200 DEG C of sintering 15
Minute, it then calcines in 400 DEG C 15 minutes, is then calcined 5 minutes in 650 DEG C；It is 0.23~0.28 micron by 100g partial size
Filler, 13g graphene oxide, 82g hexamethylene diisocyanate, 33gN- methyl pyrrolidone, 32g2- mercaptopyridine, 59g
After triphenyl silanol mixing, mechanical stirring 2 hours, then it is ultrasonically treated 3 hours, obtains functional stuffing；
(2) mixing 1Kg polyvinyl alcohol water solution (10wt%), 8g tetraphenylporphyrin iron, 35g peroxidized t-butyl perbenzoate, 80 DEG C
Stirring 1 hour, then removes water, then addition 200g dimethyldimethoxysil,ne toluene solution (35wt%), 55g1, and 3,5-
Three-glycidyl-S- triazinetrione, 22g functional stuffing stir 50 minutes, add glycerine, ethyl orthosilicate, stir 30 points
Clock obtains modified system；
(3) by 100g modified system and 55g hexamethyl trien, one chlorosilane of 28g trialkyl, 80g isopropanol, 12g
After o-phthalic acid diglycidyl ester mixing, 80 DEG C are stirred 1 hour；Add 9g calgon, 38g maleic anhydride, 16g
Anacardol stirs 1 hour in 110 DEG C, obtains thermal-insulating system；
(4) thermal-insulating system is dried 10 minutes in 85 DEG C；Then solidify 2.5~3 minutes in 125 DEG C, obtain heat insulating coat.
Comparative example five
A kind of preparation method of heat insulating coat, includes the following steps:
(1) under nitrogen protection, six ammonium chloroiridate of 100g, 73g nitric hydrate nickel, 42g cobalt nitrate, 220g ethyl alcohol and 32g are mixed
Propionic acid；It is then refluxed for stirring 110 minutes, 29g ammonium hydroxide (22wt%), 15g sodium chloride is then added；Back flow reaction 10 minutes；Then
Ventilation removes solvent and obtains solids；It is ground after solids is heat-treated, water impregnates, is dried to obtain filler；The heat treatment is
200 DEG C are sintered 15 minutes, then calcine in 400 DEG C 15 minutes, then calcine 5 minutes in 650 DEG C；By 100g partial size be 0.23~
0.28 micron of filler, 13g graphene oxide, 82g hexamethylene diisocyanate, 33gN- methyl pyrrolidone, 32g2- mercapto
After yl pyridines, the mixing of 59g triphenyl silanol, mechanical stirring 2 hours, then it is ultrasonically treated 3 hours, obtains functional stuffing；
(2) mixing 1Kg polyvinyl alcohol water solution (10wt%), 8g tetraphenylporphyrin iron, 35g peroxidized t-butyl perbenzoate, 80 DEG C
Stirring 1 hour, then removes water, then addition 200g dimethyldimethoxysil,ne toluene solution (35wt%), 55g1, and 3,5-
Three-glycidyl-S- triazinetrione, 22g functional stuffing stir 50 minutes, add glycerine, and stirring is modified for 30 minutes
System；
(3) 100g modified system is shunk with 55g hexamethyl trien, 80g isopropanol, 12g phthalic acid two sweet
After grease mixing, 80 DEG C are stirred 1 hour；9g calgon, 38g maleic anhydride, 16g anacardol are added, is stirred in 110 DEG C
1 hour, obtain thermal-insulating system；
(4) thermal-insulating system is dried 10 minutes in 85 DEG C；Then solidify 2.5~3 minutes in 125 DEG C, obtain heat insulating coat.
Comparative example six
A kind of preparation method of heat insulating coat, includes the following steps:
(1) under nitrogen protection, six ammonium chloroiridate of 100g, 73g nitric hydrate nickel, 42g cobalt nitrate, 220g ethyl alcohol and 32g are mixed
Propionic acid；It is then refluxed for stirring 110 minutes, 29g ammonium hydroxide (22wt%), 15g sodium chloride is then added；Back flow reaction 10 minutes；Then
Ventilation removes solvent and obtains solids；It is ground after solids is heat-treated, water impregnates, is dried to obtain filler；The heat treatment is
200 DEG C are sintered 15 minutes, then calcine in 400 DEG C 15 minutes, then calcine 5 minutes in 650 DEG C；By 100g partial size be 0.23~
0.28 micron of filler, 13g graphene oxide, 82g hexamethylene diisocyanate, 33gN- methyl pyrrolidone, 32g2- mercapto
After yl pyridines, the mixing of 59g triphenyl silanol, mechanical stirring 2 hours, then it is ultrasonically treated 3 hours, obtains functional stuffing；
(2) mixing 1Kg polyvinyl alcohol water solution (10wt%), 8g tetraphenylporphyrin iron, 35g peroxidized t-butyl perbenzoate, 80 DEG C
Stirring 1 hour, then removes water, then addition 200g dimethyldimethoxysil,ne toluene solution (35wt%), 55g1, and 3,5-
Three-glycidyl-S- triazinetrione, 22g functional stuffing stir 50 minutes, add glycerine, ethyl orthosilicate, stir 30 points
Clock obtains modified system；
(3) by 100g modified system and 55g hexamethyl trien, one chlorosilane of 28g trialkyl, 80g isopropanol, 12g
After o-phthalic acid diglycidyl ester mixing, 80 DEG C are stirred 1 hour；38g maleic anhydride is added, it is small in 110 DEG C of stirrings 1
When, obtain thermal-insulating system；
(4) thermal-insulating system is dried 10 minutes in 85 DEG C；Then solidify 2.5~3 minutes in 125 DEG C, obtain heat insulating coat.
Coating material performance detection, obtained heat insulating coat with a thickness of 0.12~0.13 millimeter.
Above-mentioned thermal-insulating system spreader is coated in aluminium alloy plate surface, is solidified according to aforesaid way, it is desirable that coating is flat
Whole, the defects of bubble-free, crackle, aluminium sheet sample length and width dimensions are 40mm × 40mm.Then using ultraviolet specrophotometer to painting
The sun reflectivity of layer measures.The visible light and near-infrared that the heat insulating coat of embodiment is concentrated in the main energetic of sunlight
The sun reflectivity of wave band has reached 94%, and comparative example one to six is respectively 76%, 85%, 83%, 88%, 92%, 90%, this illustrates this
The coating of invention has high reflectivity to sunlight.
The body of thermal insulating box that eight sides 50cm are built with polystyrene board uniformly brushes above-mentioned thermal-insulating system a side
On, solidified according to aforesaid way, outside tinfoil environmental sealing, testing light source is the iodine-tungsten lamp of 500w, distance test side
50cm, sets up a temperature measuring point at test side surface center and box house center respectively, then compares internal temperature measuring point
Ramp case, testing time 1h.By test, brush applied coating internal temperature does not increase 15.3 DEG C, the heat insulating coat of embodiment
Internal temperature increases 6.3 DEG C, comparative example one to six increase respectively for 13.8 DEG C, 11.3 DEG C, 11.1 DEG C, 9.5 DEG C, 8.1 DEG C,
8.0 DEG C, this illustrates that heat insulating coat of the invention has excellent heat-insulating cooling effect.
Paint film adhesion test, on the steel plate by coating uniform brushing, plate size are 50mm × 100mm × 0.2mm, so
It is detected afterwards with adherometer, paint film of the heat insulating coat of the present embodiment within the scope of cycloid scratch is complete, does not have
Fall off, adhesive force is 1 grade, comparative example one to six distinguish 1 grade, 1 grade, 2 grades with slightly damaged, 1 grade, 2 grades, 2 grades.
One to 6 120 hour boiling water absorption rate of embodiment one and comparative example is respectively 1.16%, 1.36%, 1.26%,
2.58%、2.01%、2.32%、1.86%。
It is embodiment one and comparative example two, six non-scales, not blistering under test in wet-heat resisting 2000 hours, comparative example one,
Four, five slight blistering, three severe blister of comparative example.
Abrasion resistance test is carried out according to GB/T 9266-2009, the heat insulating coat washability number of embodiment one is more than
4000 times, comparative example one to six is respectively 3000 times, 3500 times, 2000 times, 3800 times, 4000 times, 3500 times, this illustrates this hair
Bright heat insulating coat has excellent wash-resistant property.
250 DEG C of calcinings, embodiment one and comparative example one, two, six do not occur carbonization phenomenon, and obvious carbon occurs in comparative example three
Change phenomenon, slight carbonization phenomenon occurs in comparative example four, five.
Claims (10)
1. a kind of preparation method of heat insulating coat, which comprises the steps of:
(1) under nitrogen protection, six ammonium chloroiridates, nitric hydrate nickel, cobalt nitrate, ethyl alcohol and propionic acid are mixed；It is then refluxed for stirring
110 minutes, ammonium hydroxide, sodium chloride is then added；Back flow reaction 10 minutes；Then it removes solvent and obtains solids；By solids heat
It is ground after processing, water impregnates, is dried to obtain filler；The heat treatment is sintered 15 minutes for 200 DEG C, then calcines 15 in 400 DEG C
Minute, then calcined 5 minutes in 650 DEG C；By filler, graphene oxide, hexamethylene diisocyanate, N- crassitude
After ketone, 2- mercaptopyridine, triphenyl silanol mixing, mechanical stirring 2 hours, then it is ultrasonically treated 3 hours, obtains functional stuffing；
(2) mix polyethylene alcohol solution, tetraphenylporphyrin iron, peroxidized t-butyl perbenzoate, 80 DEG C stir 1 hour, then
Water is removed, dimethyldimethoxysil,ne solution, 1 is then added, 3,5- three-glycidyl-S- triazinetriones, functional stuffing stir
It mixes 50 minutes, adds glycerine, ethyl orthosilicate, stirring obtains modified system in 30 minutes；
(3) modified system and hexamethyl trien, one chlorosilane of trialkyl, isopropanol, phthalic acid two are shunk
After glyceride mixing, 80 DEG C are stirred 1 hour；Calgon, maleic anhydride, anacardol are added, is stirred 1 hour in 110 DEG C,
Obtain thermal-insulating system；
(4) thermal-insulating system is dried 10 minutes in 85 DEG C；Then solidify 2.5~3 minutes in 125 DEG C, obtain heat insulating coat.
2. the preparation method of heat insulating coat according to claim 1, which is characterized in that remove solvent using ventilation method；Ammonium hydroxide
Mass concentration be 22%.
3. the preparation method of heat insulating coat according to claim 1, which is characterized in that six ammonium chloroiridate, nitric hydrate
Nickel, cobalt nitrate, ethyl alcohol, propionic acid, ammonium hydroxide, sodium chloride mass ratio be 100: 73: 42: 220: 32: 29: 15.
4. the preparation method of heat insulating coat according to claim 1, which is characterized in that the dimethyldimethoxysil,ne is molten
In liquid, solvent is toluene.
5. the preparation method of heat insulating coat according to claim 1, which is characterized in that the filler, graphene oxide, six Asias
Methyl diisocyanate, N-Methyl pyrrolidone, 2- mercaptopyridine, triphenyl silanol mass ratio be 100: 13: 82: 33: 32:
59。
6. the preparation method of heat insulating coat according to claim 1, which is characterized in that the polyvinyl alcohol, tetraphenylporphyrin
Iron, peroxidized t-butyl perbenzoate, dimethyldimethoxysil,ne solution, 1,3,5- three-glycidyl-S- triazinetrione, function
Filler, glycerine, ethyl orthosilicate mass ratio be 100: 8: 35: 70: 55: 22.
7. the preparation method of heat insulating coat according to claim 1, which is characterized in that the modified system, hexamethyl Sanya
Tetramine, one chlorosilane of trialkyl, isopropanol, o-phthalic acid diglycidyl ester, calgon, maleic anhydride, waist
The mass ratio of fruit phenol is 100: 55: 28: 80: 12: 9: 38: 16.
8. the preparation method of heat insulating coat according to claim 1, which is characterized in that the partial size of the filler be 0.23~
0.28 micron.
9. the preparation method of heat insulating coat according to claim 1, which is characterized in that the heat insulating coat with a thickness of 0.1
~0.15 millimeter.
10. the heat insulating coat of the preparation method preparation of heat insulating coat according to claim 1.
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| CN201810611957.8A CN109021728A (en) | 2018-06-14 | 2018-06-14 | Heat insulating coat and preparation method thereof |
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| CN201810611957.8A CN109021728A (en) | 2018-06-14 | 2018-06-14 | Heat insulating coat and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109943223A (en) * | 2019-03-27 | 2019-06-28 | 浙江中科应化科技有限公司 | A kind of modified cyanate ester paint |
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Application publication date: 20181218 |