CN107474722A - A kind of heat radiation coating and preparation method thereof - Google Patents

A kind of heat radiation coating and preparation method thereof Download PDF

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Publication number
CN107474722A
CN107474722A CN201710775781.5A CN201710775781A CN107474722A CN 107474722 A CN107474722 A CN 107474722A CN 201710775781 A CN201710775781 A CN 201710775781A CN 107474722 A CN107474722 A CN 107474722A
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heat radiation
radiation coating
water
catalyst
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薛加联
王磊
潘宏梅
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Changzhou Hai Textile Co Ltd
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Changzhou Hai Textile 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
    • C09D175/00Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
    • C09D175/04Polyurethanes
    • C09D175/08Polyurethanes from polyethers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40High-molecular-weight compounds
    • C08G18/4009Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40High-molecular-weight compounds
    • C08G18/48Polyethers
    • C08G18/4833Polyethers containing oxyethylene units
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40High-molecular-weight compounds
    • C08G18/61Polysiloxanes
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/18Fireproof paints including high temperature resistant paints
    • 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
    • C08K3/38Boron-containing compounds
    • C08K2003/382Boron-containing compounds and nitrogen
    • C08K2003/385Binary compounds of nitrogen with boron
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
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    • 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
    • C08K3/34Silicon-containing compounds
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    • 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
    • C08K3/34Silicon-containing compounds
    • C08K3/36Silica
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    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances
    • C08K9/06Ingredients treated with organic substances with silicon-containing compounds

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Abstract

The invention belongs to technical field of paint preparation, and in particular to a kind of heat radiation coating and preparation method thereof.The present invention is by N,N dimethylformamides,The stirrings such as IPDI preheating after with amino-terminated dimethyl silicone polymer,Ethylenediamine and catalyst reaction,Reactant mixture is collected to be distilled,Regather residue and water,Azodiisobutyronitrile polymerisation,Obtain base fluid,Kyanite is calcined again,Crush,After sieving with water,Sodium metasilicate etc. is stood overnight after mixing,Filtrate is collected after filtering to dry,And mixed with boron nitride,Add after surfactant ball milling with base fluid,Dispersant,Heat radiation coating can be obtained,Heat radiation coating produced by the present invention has excellent heat dispersion,Coated in substrate surface,The higher thermal dispersant coatings of hardness can be formed,Coating adhesion is higher simultaneously,Mechanical performance is excellent,Resistance to elevated temperatures is good,Energy long-term temperature plays thermolysis,Effectively extend the service life of matrix material.

Description

A kind of heat radiation coating and preparation method thereof
Technical field
The invention belongs to technical field of paint preparation, and in particular to a kind of heat radiation coating and preparation method thereof.
Background technology
With the rapid development of economy, various LEDs, electrical equipment and electronic equipment obtain high speed development, but it is LED, various Electrical equipment and electronic equipment can produce substantial amounts of heat during working long hours, and area of dissipation of various electronic equipments itself compared with Small, heat dispersion is poor, the service life and performance of substantial amounts of heat affecting equipment, therefore is frequently necessary to coat one on the surface of equipment The coating of layer auxiliary heat dissipation, the heat radiation coating of prior art developed comparatively fast, such as number of patent application in recent years CN200810146607.5 is disclosed " a kind of heat radiation coating and preparation method thereof ", and the coating includes following raw material:Silicones, it is molten Agent, anti-settling agent, zinc oxide, carborundum, aluminium powder, dispersant and smooth agent, its preparation method comprise the following steps:(a)Silicon is provided Resin and more than one solvents, and it is sufficiently mixed it to form the first mixed solution;(b)Add again Zinc oxide powder in this In one mixed solution and it is sufficiently mixed, forms the second mixed solution;(c)Silicon carbide powder and aluminium powder are added in the second mixed solution In and be sufficiently mixed, formed the 3rd mixed solution;(d)Addition anti-settling agent and dispersant in the 3rd mixed solution and are sufficiently mixed To form heat radiation coating, the heat radiation coating, which can be directly coated on heat abstractor, can increase its area of dissipation, be imitated with heat radiation Fruit.And for example number of patent application CN200910199955.3 discloses a kind of " environmental protection type self-radiation nano ecological paint and its preparation Method ", the preparation method for coating are:Alumina gel, nano heat-conductive filler, pigment and anti-settling agent etc. are mixed, be scattered at a high speed, As a components, and using Ludox as b components, then a components and b components mixed, low speed disperses, stand curing, produce nanometer Ecologic coating, described nano heat-conductive filler are the mixture of CNT and nanometer cobalt oxide or nano zircite, the coating With preferably from thermolysis.
Can be seen that existing heat radiation coating from above-mentioned technology is typically using high polymer material as matrix, is led by adding height The filler of heat comes heat conduction and the radianting capacity of strengthened coat, and then the purpose of cooling, and heat filling therein with The heat dispersion of coating is closely related.At present, the conventional heat filling of heat radiation coating is inorganic heat filling, mainly there is oxidation Zinc, carborundum, aluminium nitride, aluminum oxide, magnesia etc., the addition of these fillers, the thermal conductivity factor of coating is effectively increased, so as to Improve the heat dispersion of coating.However, although existing heat radiation coating achieves good achievement, but some are still faced with urgently Inorganic filler particle used in technical problem to be solved, mainly heat radiation coating and Matrix Match are bad, so as to result in Coating adhesion it is poor, mechanical performance is bad, and coating can not be long-term use of at relatively high temperatures.
In view of this, it would be highly desirable to develop that a kind of good heat dissipation effect, coating adhesion be strong, good mechanical property, and with good resistance to The heat radiation coating of high-temperature behavior.
The content of the invention
The technical problems to be solved by the invention:For inorganic filler particle used in current heat radiation coating and Matrix Match Bad, so as to which the coating adhesion resulted in is poor, mechanical performance is bad, and can not be long-term use of at high temperature the problem of, carry A kind of heat radiation coating and preparation method thereof is supplied.
In order to solve the above technical problems, the present invention is using technical scheme as described below:
A kind of heat radiation coating, include the raw material of following parts by weight:60~80 parts of N,N-dimethylformamides, 50~53 parts of water, 35~40 parts of IPDIs, 20~24 parts of polyethylene glycol, 15~18 parts of amino-terminated dimethyl silicone polymers, 7 ~9 parts of sodium metasilicate, 6~10 parts of kyanites, 3~5 parts of dispersants, 3.2~4.5 parts of azodiisobutyronitriles, 2~4 parts of boron nitride, 1 ~3 parts of 1,4- butanediols, 1.0~1.3 parts of ethylenediamines, 0.6~0.9 part of surfactant, 0.5~1.3 part of silane coupler, 0.4~1.2 part of catalyst.
The dispersant is any one in propylene glycol methyl ether acetate, ethylene bis stearamide.
The surfactant is any one in lauryl amine propionate, sulfobetaines.
The silane coupler is any one in isobutyl triethoxy silane, gamma-aminopropyl-triethoxy-silane.
The catalyst is Ziegler-Natta catalyst.
A kind of preparation method of heat radiation coating, the preparation method comprise the following steps:
(1)Count in parts by weight, carry out taking raw material;
(2)DMF, IPDI, polyethylene glycol, BDO are put into reactor, Protected using nitrogen, preheated at 65~72 DEG C, add amino-terminated dimethyl silicone polymer, ethylenediamine and catalyst, risen Temperature is to 85~90 DEG C, after being reacted, is cooled to 50~55 DEG C, collects reactant mixture;
(3)Reactant mixture is distilled, reclaims DMF, collects residue, by residue and raw material The water of water gross mass 60~70% is well mixed, and is put into reactor, adds azodiisobutyronitrile, is warming up to 90~95 DEG C, is gathered Reaction is closed, discharging, material is collected out, obtains base fluid, it is standby;
(4)Kyanite is calcined, crushed, sieving, collects sieving particle, by sieving particle, remaining water, sodium metasilicate and silicon Alkane coupling agent, which is put into container, to stir, and adds the 1.5mol/L sodium chloride solutions of sodium metasilicate quality 50~60%, and stirring is equal It is even, stand, filtering, collect filtrate, and dried at 90 DEG C, dried object is collected, dried object is put into container, and using high Flush coater is pressed, boron nitride is sprayed into container, remixed, mixture is collected, mixture, surfactant is put into ball mill Ball milling, collect ball milling thing;
(5)By step(3)Standby base fluid, ball milling thing and dispersant are put into high-pressure reactor, in 1.2~1.5MPa, 70~75 DEG C Under, it is stirred, collects stirring mixture, you can obtain heat radiation coating.
Compared with other method, advantageous effects are the present invention:
The present invention is using IPDI, polyethylene glycol as raw material, during synthesis of polyurethane, by adding ammonia Base blocks dimethyl silicone polymer, in the presence of catalyst, obtains organic silicon modified polyurethane, adds the temperature tolerance of base fluid Energy and adhesive force, the present invention are attached to the white carbon of preparation by the use of irreversible kyanite is once expanded as pore channel In hole, and it is connected with each other the white carbon to be formed using silane coupler and forms two dimension or three-dimensional structure in the channel, and Surface is carried hydroxyl, can and base-material carry out the combination of chemical bond, improve the matching of inorganic filler particle and matrix, enhancing The mechanical performance and heat-resisting quantity of coating, service life is extended, while sprays into boron nitride in hole under high pressure effect, Boron nitride is set to improve radiating effect in two dimension or three-dimensional structure.
Embodiment
The selection of dispersant:Any one in propylene glycol methyl ether acetate, ethylene bis stearamide.
The selection of surfactant:Any one in lauryl amine propionate, sulfobetaines.
The selection of silane coupler:It is any one in isobutyl triethoxy silane, gamma-aminopropyl-triethoxy-silane Kind.
The selection of catalyst:Ziegler-Natta catalyst.
The heat radiation coating of the present invention, includes the raw materials of following parts by weight, and 60~80 parts of DMFs, 50~ 53 parts of water, 35~40 parts of IPDIs, 20~24 parts of polyethylene glycol, 15~18 parts of amino-terminated poly dimethyl silicon Oxygen alkane, 7~9 parts of sodium metasilicate, 6~10 parts of kyanites, 3~5 parts of dispersants, 3.2~4.5 parts of azodiisobutyronitriles, 2~4 parts of nitrogen Change boron, 1~3 part of 1,4- butanediol, 1.0~1.3 parts of ethylenediamines, 0.6~0.9 part of surfactant, 0.5~1.3 part of silane idol Join agent, 0.4~1.2 part of catalyst.
The preparation method of heat radiation coating of the present invention, comprises the following steps:
(1)Count in parts by weight, carry out taking raw material;
(2)DMF, IPDI, polyethylene glycol, BDO are put into reactor, Protected using nitrogen, 20~25min of preheating is stirred with 200r/min at 65~72 DEG C, adds amino-terminated poly dimethyl silicon Oxygen alkane, ethylenediamine and catalyst, 85~90 DEG C are warming up to, after carrying out 4~6h of reaction, are cooled to 50~55 DEG C, it is mixed to collect reaction Compound;
(3)Reactant mixture is distilled, reclaims DMF, collects residue, by residue and raw material The water of water gross mass 60~70% is well mixed, and is put into reactor, adds azodiisobutyronitrile, is warming up to 90~95 DEG C, is gathered 10~15h of reaction is closed, discharging, material is collected out, obtains base fluid, it is standby;
(4)Kyanite is put into 1200~1500 DEG C of calcining furnaces and calcined, is crushed, crosses 100 mesh sieves, collects sieving particle, Sieving particle, remaining water, sodium metasilicate, silane coupler are put into container and stirred, add sodium metasilicate quality 50~ 60% 1.5mol/L sodium chloride solutions, are stirred with 500r/min, stood overnight, and filtering, collect filtrate, and at 90 DEG C Lower drying, dried object is collected, dried object is put into container, using high-pressure spraying machine under 24~26MPa, boron nitride sprayed into In container, then mixed with 300r/min, collect mixture, mixture, surfactant are put into ball mill, and add drying The a diameter of 30mm steel balls of 7~9 times of amount of substance, 4~6h of ball milling is carried out with 600r/min, collects ball milling thing;
(5)By step(3)Standby base fluid, mixture, dispersant are put into high-pressure reactor, in 1.2~1.5MPa, 70~75 DEG C Under, 3~6h is stirred, collects stirring ball-milling thing, you can obtains heat radiation coating.
Example 1
The selection of dispersant:Propylene glycol methyl ether acetate.
The selection of surfactant:Lauryl amine propionate.
The selection of silane coupler:Isobutyl triethoxy silane.
The selection of catalyst:Ziegler-Natta catalyst(Manufacturer:Dalian Hai Chen chemical minerals Co., Ltd).
The heat radiation coating of the present invention, includes the raw materials of following parts by weight, 60 parts of DMFs, 50 parts of water, 35 parts of IPDIs, 20 parts of polyethylene glycol, 15 parts of amino-terminated dimethyl silicone polymers, 7 parts of sodium metasilicate, 6 parts Kyanite, 3 parts of dispersants, 3.2 parts of azodiisobutyronitriles, 2 parts of boron nitride, 1 part of 1,4- butanediol, 1.0 parts of ethylenediamines, 0.6 part Surfactant, 0.5 part of silane coupler, 0.4 part of catalyst.
The preparation method of heat radiation coating of the present invention, comprises the following steps:
(1)Count in parts by weight, carry out taking raw material;
(2)DMF, IPDI, polyethylene glycol, BDO are put into reactor, Protected using nitrogen, preheating 20min is stirred with 200r/min at 65 DEG C, adds amino-terminated dimethyl silicone polymer, second Diamines and catalyst, 85 DEG C are warming up to, after carrying out reaction 4h, are cooled to 50 DEG C, collect reactant mixture;
(3)Reactant mixture is distilled, reclaims DMF, collects residue, by residue and raw material The water of water gross mass 60% is well mixed, and is put into reactor, adds azodiisobutyronitrile, is warming up to 90 DEG C, polymerisation 10h, discharging, collects out material, obtains base fluid, standby;
(4)Kyanite is put into 1200 DEG C of calcining furnaces and calcined, is crushed, crosses 100 mesh sieves, sieving particle is collected, will sieve Particle, remaining water, sodium metasilicate, silane coupler are put into container and stirred, and add sodium metasilicate quality 50% 1.5mol/L sodium chloride solutions, are stirred with 500r/min, are stood overnight, filtering, collect filtrate, and done at 90 DEG C It is dry, dried object is collected, dried object is put into container, using high-pressure spraying machine under 24MPa, boron nitride is sprayed into container, Mixed again with 300r/min, collect mixture, mixture, surfactant are put into ball mill, and add dried object quality 7 A diameter of 30mm steel balls again, ball milling 4h is carried out with 600r/min, collects ball milling thing;
(5)By step(3)Standby base fluid, ball milling thing, dispersant are put into high-pressure reactor, at 1.2MPa, 70 DEG C, are stirred 3h, collect stirring mixture, you can obtain heat radiation coating.
Example 2
The selection of dispersant:Propylene glycol methyl ether acetate.
The selection of surfactant:Lauryl amine propionate.
The selection of silane coupler:Isobutyl triethoxy silane.
The selection of catalyst:Ziegler-Natta catalyst(Manufacturer:Dalian Hai Chen chemical minerals Co., Ltd).
The heat radiation coating of the present invention, includes the raw materials of following parts by weight, 70 parts of DMFs, 52 parts of water, 38 parts of IPDIs, 22 parts of polyethylene glycol, 17 parts of amino-terminated dimethyl silicone polymers, 7 parts of sodium metasilicate, 7 parts Kyanite, 2 parts of dispersants, 3.9 parts of azodiisobutyronitriles, 3 parts of boron nitride, 2 parts of 1,4- butanediols, 1.2 parts of ethylenediamines, 0.7 part Surfactant, 0.8 part of silane coupler, 0.8 part of catalyst.
The preparation method of heat radiation coating of the present invention, comprises the following steps:
(1)Count in parts by weight, carry out taking raw material;
(2)DMF, IPDI, polyethylene glycol, BDO are put into reactor, Protected using nitrogen, preheating 23min is stirred with 200r/min at 69 DEG C, adds amino-terminated dimethyl silicone polymer, second Diamines and catalyst, 88 DEG C are warming up to, after carrying out reaction 5h, are cooled to 53 DEG C, collect reactant mixture;
(3)Reactant mixture is distilled, reclaims DMF, collects residue, by residue and raw material The water of water gross mass 65% is well mixed, and is put into reactor, adds azodiisobutyronitrile, is warming up to 93 DEG C, polymerisation 13h, discharging, collects out material, obtains base fluid, standby;
(4)Kyanite is put into 1350 DEG C of calcining furnaces and calcined, is crushed, crosses 100 mesh sieves, sieving particle is collected, will sieve Particle, remaining water, sodium metasilicate, silane coupler are put into container and stirred, and add sodium metasilicate quality 55% 1.5mol/L sodium chloride solutions, are stirred with 500r/min, are stood overnight, filtering, collect filtrate, and done at 90 DEG C It is dry, dried object is collected, dried object is put into container, using high-pressure spraying machine under 25MPa, boron nitride is sprayed into container, Mixed again with 300r/min, collect mixture, mixture, surfactant are put into ball mill, and add dried object quality 8 A diameter of 30mm steel balls again, ball milling 5h is carried out with 600r/min, collects ball milling thing;
(5)By step(3)Standby base fluid, ball milling thing, dispersant are put into high-pressure reactor, at 1.4MPa, 73 DEG C, are stirred 5h, collect stirring mixture, you can obtain heat radiation coating.
Example 3
The selection of dispersant:Ethylene bis stearamide.
The selection of surfactant:Sulfobetaines.
The selection of silane coupler:Gamma-aminopropyl-triethoxy-silane.
The selection of catalyst:Ziegler-Natta catalyst(Manufacturer:Dalian Hai Chen chemical minerals Co., Ltd).
The heat radiation coating of the present invention, includes the raw materials of following parts by weight, 80 parts of DMFs, 53 parts of water, 40 parts of IPDIs, 24 parts of polyethylene glycol, 18 parts of amino-terminated dimethyl silicone polymers, 9 parts of sodium metasilicate, 10 parts Kyanite, 5 parts of dispersants, 4.5 parts of azodiisobutyronitriles, 4 parts of boron nitride, 3 parts of 1,4- butanediols, 1.3 parts of ethylenediamines, 0.9 part Surfactant, 1.3 parts of silane couplers, 1.2 parts of catalyst.
The preparation method of heat radiation coating of the present invention, comprises the following steps:
(1)Count in parts by weight, carry out taking raw material;
(2)DMF, IPDI, polyethylene glycol, BDO are put into reactor, Protected using nitrogen, preheating 25min is stirred with 200r/min at 72 DEG C, adds amino-terminated dimethyl silicone polymer, second Diamines and catalyst, 90 DEG C are warming up to, after carrying out reaction 6h, are cooled to 55 DEG C, collect reactant mixture;
(3)Reactant mixture is distilled, reclaims DMF, collects residue, by residue and raw material The water of water gross mass 70% is well mixed, and is put into reactor, adds azodiisobutyronitrile, is warming up to 95 DEG C, polymerisation 15h, discharging, collects out material, obtains base fluid, standby;
(4)Kyanite is put into 1500 DEG C of calcining furnaces and calcined, is crushed, crosses 100 mesh sieves, sieving particle is collected, will sieve Particle, remaining water, sodium metasilicate, silane coupler are put into container and stirred, and add sodium metasilicate quality 60% 1.5mol/L sodium chloride solutions, are stirred with 500r/min, are stood overnight, filtering, collect filtrate, and done at 90 DEG C It is dry, dried object is collected, dried object is put into container, using high-pressure spraying machine under 26MPa, boron nitride is sprayed into container, Mixed again with 300r/min, collect mixture, mixture, surfactant are put into ball mill, and add dried object quality 9 A diameter of 30mm steel balls again, ball milling 6h is carried out with 600r/min, collects ball milling thing;
(5)By step(3)Standby base fluid, ball milling thing, dispersant are put into high-pressure reactor, at 1.5MPa, 75 DEG C, are stirred 6h, collect stirring mixture, you can obtain heat radiation coating.
Comparative example:The heat radiation coating of Energy Saving Technology Co of Shenzhen production.
It is in power by the heat radiation coating even application of heat radiation coating made from present example 1~3 and comparative example respectively 20W LED substrate material surfaces, it is 150 μm to control coating thickness, and after the completion of to be sprayed, standing is dried, you can forms heat-radiation coating Then thermal dispersant coatings are carried out performance detection by layer, its testing result is as shown in table 1:
Table 1
Temperature tolerance is tested:Using thermogravimetric analyzer(TGA)The temperature tolerance of coating is tested, the LED of thermal dispersant coatings will be scribbled Material is placed in thermogravimetric analyzer, under nitrogen atmosphere, sets 10 DEG C/min programming rate, 20mL/min air velocity, Scanning temperature progressively heats up since 100 DEG C, and observation LED material surface thermal dispersant coatings weight reduces situation, treats thermal dispersant coatings weight When amount reduction reaches extreme value, the moment temperature is the resistance to highest temperature temperature of thermal dispersant coatings.
Adhesive force:According to ISO2409 cross-hatchings, measure of the lattice device to thermal dispersant coatings progress adhesive force is drawn using F107, first The shape of cross grid is marked on the thermal dispersant coatings surface of LED materials with a lattice device is drawn, and otch will be up to LED matrix materials, then With hairbrush along respectively brush 5 times, then be close to adhesive tape on otch and pulled open rapidly of the cornerwise direction of cross grid, seen with magnifying glass Examine, and the grade of coating adhesion is determined according to ISO2409 standards.
Impact resistance:Impact resistance measure is carried out to thermal dispersant coatings with paint film impactor according to GB/T1732, will be scribbled The LED materials of thermal dispersant coatings are placed on impactor, are made to bore again as far as possible and are fallen within material center, and thermal dispersant coatings are face-up, bore again(Standard Weight is 1kg)Freely fallen by some height, each Height Impact 3~5 times, while amplify sem observation thermal dispersant coatings with 4 times to be It is no it is cracked, peel off phenomena such as, such as without obvious crackle and peeling phenomenon, increase the height fallen, test again, until appearance Crackle or the phenomenon of peeling, the height that weight is fallen at that time is recorded, determine the impact strength of coating.
Pencil hardness:According to GB/T6739 standards, LED material surfaces are determined using QHQ type film pencil scratch hardness instrument Pencil hardness of the thermal dispersant coatings at 25 DEG C.
Thermal conductivity factor:Using the thermal conductivity factor of measuring thermal conductivity instrument measure LED material surface thermal dispersant coatings.
In summary, heat radiation coating produced by the present invention has excellent heat dispersion, coated in substrate surface, can be formed The higher thermal dispersant coatings of hardness, while coating adhesion is higher, mechanical performance is excellent, and resistance to elevated temperatures is good, can long-term temperature The service life for playing thermolysis, effectively extending matrix material.

Claims (6)

1. a kind of heat radiation coating, it is characterised in that include the raw material of following parts by weight, 60~80 parts of N, N- dimethyl formyls Amine, 50~53 parts of water, 35~40 parts of IPDIs, 20~24 parts of polyethylene glycol, 15~18 parts it is amino-terminated poly- Dimethyl siloxane, 7~9 parts of sodium metasilicate, 6~10 parts of kyanites, 3~5 parts of dispersants, 3.2~4.5 parts of azodiisobutyronitriles, 2 ~4 parts of boron nitride, 1~3 part of 1,4- butanediol, 1.0~1.3 parts of ethylenediamines, 0.6~0.9 part of surfactant, 0.5~1.3 part Silane coupler, 0.4~1.2 part of catalyst.
2. heat radiation coating according to claim 1, it is characterised in that the dispersant be propylene glycol methyl ether acetate,
Any one in ethylene bis stearamide.
3. heat radiation coating according to claim 1, it is characterised in that the surfactant be lauryl amine propionate, Any one in sulfobetaines.
4. heat radiation coating according to claim 1, it is characterised in that the silane coupler is isobutyl ethyl triethoxy silicane Any one in alkane, gamma-aminopropyl-triethoxy-silane.
5. heat radiation coating according to claim 1, it is characterised in that the catalyst is Ziegler-Natta catalyst.
6. according to the preparation method of heat radiation coating described in claim 1 to 5 any one, it is characterised in that the preparation method bag Include following steps:
(1)Count in parts by weight, carry out taking raw material;
(2)DMF, IPDI, polyethylene glycol, BDO are put into reactor, Protected using nitrogen, preheated at 65~72 DEG C, add amino-terminated dimethyl silicone polymer, ethylenediamine and catalyst, risen Temperature is to 85~90 DEG C, after being reacted, is cooled to 50~55 DEG C, collects reactant mixture;
(3)Reactant mixture is distilled, reclaims DMF, collects residue, by residue and raw material The water of water gross mass 60~70% is well mixed, and is put into reactor, adds azodiisobutyronitrile, is warming up to 90~95 DEG C, is gathered Reaction is closed, discharging, material is collected out, obtains base fluid, it is standby;
(4)Kyanite is calcined, crushed, sieving, collects sieving particle, by sieving particle, remaining water, sodium metasilicate and silicon Alkane coupling agent, which is put into container, to stir, and adds the 1.5mol/L sodium chloride solutions of sodium metasilicate quality 50~60%, and stirring is equal It is even, stand, filtering, collect filtrate, and dried at 90 DEG C, dried object is collected, dried object is put into container, and using high Flush coater is pressed, boron nitride is sprayed into container, remixed, mixture is collected, mixture, surfactant is put into ball mill Ball milling, collect ball milling thing;
(5)By step(3)Standby base fluid, ball milling thing and dispersant are put into high-pressure reactor, in 1.2~1.5MPa, 70~75 DEG C Under, it is stirred, collects stirring mixture, you can obtain heat radiation coating.
CN201710775781.5A 2017-08-31 2017-08-31 A kind of heat radiation coating and preparation method thereof Pending CN107474722A (en)

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Publication number Priority date Publication date Assignee Title
CN108395801A (en) * 2018-02-06 2018-08-14 合肥东恒锐电子科技有限公司 A kind of high-performance coating and preparation method thereof for main frame heat dissipation
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CN117601456B (en) * 2024-01-22 2024-03-26 四川省宜宾普什建材有限责任公司 Processing technology of large-caliber electric melting type plastic pipe fitting

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