CN105860395A - Silicon-free heat-conducting gasket and preparation method thereof - Google Patents

Silicon-free heat-conducting gasket and preparation method thereof Download PDF

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CN105860395A
CN105860395A CN201610440610.2A CN201610440610A CN105860395A CN 105860395 A CN105860395 A CN 105860395A CN 201610440610 A CN201610440610 A CN 201610440610A CN 105860395 A CN105860395 A CN 105860395A
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preparation
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parts
silicon
conducting pad
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CN105860395B (en
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陈淑兰
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Kunshan Zhaoke Electronic Material Co ltd
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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
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/02Organic and inorganic ingredients
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C35/00Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
    • B29C35/02Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/24Crosslinking, e.g. vulcanising, of macromolecules
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    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
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    • C08K5/17Amines; Quaternary ammonium compounds
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    • C09K5/00Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/08Materials not undergoing a change of physical state when used
    • C09K5/14Solid materials, e.g. powdery or granular
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    • C08J2333/00Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
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Abstract

The invention provides a preparation method of a silicon-free heat-conducting gasket. The preparation method comprises the following main steps: weighing a first raw material and a second raw material for preparing the silicon-free heat-conducting gasket for later use; carrying out vacuum kneading and stirring on the first raw material at 150-180 DEG C for 2-6 hours; mixing the first raw material subjected to vacuum kneading and stirring with the second raw material and stirring the mixture for 4-40 minutes, thus obtaining a rubber compound; putting the rubber compound in a mold; carrying out hot pressed vulcanization on the mold to which the rubber compound is added under the vacuum condition of 130-160 DEG C for 4-15 minutes; cooling the product, thus obtaining the finished product. The preparation method of the silicon-free heat-conducting gasket has the advantages of simplicity in operation, high production efficiency, high quality of the produced finished product, low defective rate and low manpower cost. The silicon-free heat-conducting gasket prepared by the method has the characteristics that the silicon-free heat-conducting gasket has good heat-conducting property and does not yield oil in the extreme environment.

Description

A kind of no-silicon type heat-conducting pad and preparation method thereof
Technical field
The present invention relates to a kind of heat-conducting pad field, and particularly to a kind of no-silicon type heat-conducting pad And preparation method thereof.
Background technology
Along with the progress of science and technology, the usage amount of electronic equipments is increasing, needs under the high temperature conditions The part with sealing function wanted increases the most accordingly, and heat-conducting pad of the prior art contains mostly There is silicon, and be heated containing the silicone oil in silicon spacer and can ooze out under pressure between parts, make Obtain the lost of life of heat-conducting pad.
And no-silicon type heat-conducting pad on the market prepares material because of it and preparation technology is the most perfect, Production cost is higher, therefore, and a kind of advantage inheriting silica gel heat-conducting pad completely, the most not Permeability, and the no-silicon type that its preparation cost is lower than the preparation cost of commercially available no-silicon type heat-conducting pad Heat-conducting pad can fill up the blank of this respect very well.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of no-silicon type heat-conducting pad, this is without silicon The preparation method of type heat-conducting pad has simple to operate, and production efficiency is high, goes out finished product high-quality, Defect rate is low, the advantage that human cost is low.
Another object of the present invention is to provide a kind of no-silicon type heat-conducting pad, this no-silicon type heat conduction It is good that pad has heat conductivility, and does not go out the feature of silicone oil under multiple extreme environmental conditions.
The present invention solves it and technical problem is that and realize by the following technical solutions:
The present invention proposes the preparation method of a kind of no-silicon type heat-conducting pad, this preparation method main Step includes:
The first raw material and the second raw material of preparing no-silicon type heat-conducting pad are weighed standby, presses Weight portion meter, the first raw material includes: liquid methacrylate class rubber 100 parts, conductive powder 100~1000 parts, (2-(2-Butoxyethoxy) ethyl) ester 10~40 parts;Second former material Material meter by weight includes vulcanizing agent 0.1~1 part;By the first raw material at 150~180 DEG C Vacuum kneading stir 2~6 hours, then by through vacuum kneading stir after the first raw material with Second raw material mixing, is stirred for 4~40 minutes obtaining sizing material, sizing material is put in mould and Hot-press vulcanization 4~15 minutes under 130~160 DEG C of vacuum conditions, then cool down to obtain finished product.
Liquid methacrylate resin has good mobility, can preferably coated powder, increasing Add the fusion between conduction powder and colloid, thus improve the heat conductivity of product.Add (2- (2-Butoxyethoxy) ethyl) ester improves pliability.Conductive powder improves heat conductive pad The heat conductivility of sheet.The addition of antioxidant adds the service life of pad.Vulcanizing agent is heat The important source material of pressure sulfidation.
The present invention proposes a kind of no-silicon type heat-conducting pad, and this no-silicon type heat-conducting pad is by above-mentioned system Preparation Method prepares.
The no-silicon type heat-conducting pad of the embodiment of the present invention and preparation technology provide the benefit that: this no-silicon type The preparation method of heat-conducting pad is simple to operate, it is possible to achieve whole process is intelligent and once feeds intake the highest Can reach 600kg, greatly improve work efficiency, and saved human cost, produce effect Rate is high, goes out finished product high-quality.The service life of this no-silicon type heat-conducting pad is long, and does not leak silicone oil.
Detailed description of the invention
For making the purpose of the embodiment of the present invention, technical scheme and advantage clearer, below by right Technical scheme in the embodiment of the present invention is clearly and completely described.In embodiment unreceipted Actual conditions person, the condition advised according to normal condition or manufacturer is carried out.Agents useful for same or instrument Device unreceipted production firm person, being can be by the commercially available conventional products bought and obtain.
Below the embodiment of the present invention is specifically described.
The present invention provides the preparation method of a kind of no-silicon type heat-conducting pad, this preparation method main Step includes:
The first raw material and the second raw material of preparing no-silicon type heat-conducting pad are weighed standby, presses Weight portion meter, the first raw material includes: liquid methacrylate class rubber 100 parts, conductive powder 100~1000 parts, (2-(2-Butoxyethoxy) ethyl) ester 10~40 parts;Second former material Material meter by weight includes vulcanizing agent 0.1~1 part;By the first raw material at 150~180 DEG C Vacuum kneading stir 2~6 hours, then by through vacuum kneading stir after the first raw material with Second raw material mixing, is stirred for 4~40 minutes obtaining sizing material, sizing material is put in mould and Hot-press vulcanization 4~15 minutes under 130~160 DEG C of vacuum conditions, then cool down to obtain finished product., liquid Acrylate rubber includes liquid methacrylate rubber, liquid ethylene acrylate elastomer and liquid At least one in state hydroxy acrylic acid rubber.Conductive powder includes aluminium oxide, aluminium hydroxide, nitrogen Change one or more in boron, carborundum, metal powder.Vulcanizing agent is isocyanates hydroxy systems, Phenolic and epoxy and the one in hydroxy systems, soap sulfur system, TCY vulcanizing system.TCY For trithiocyanuric acid.
Liquid methacrylate resin has good mobility, can preferably coated powder, increase is led Fusion between hot powder body and colloid, thus improve the heat conductivity of product.Add (2-(2- Butoxyethoxy) ethyl) ester improves pliability.Conductive powder improves heat-conducting pad Heat conductivility.The addition of antioxidant adds the service life of pad.Vulcanizing agent is hot pressing sulfur The important source material of change process.
Further, the first raw material is counted by weight and is also included: 0~2 part of pigment, 0~2 Part antioxidant.Pigment includes any one in barba hispanica, iron oxide red, iron oxide yellow and white carbon black, anti- Oxygen agent be double (bis (alpha, alpha-dimethylbenzyl) base) diphenylamines of 4,4'-, 4,4'-bis-(propyloxy phenyl base) diphenylamines, In double (A, the A-dimethyl benzyl) diphenylamines of two [4-(1-methyl isophthalic acid-phenethyl) benzene] amine, 4,4'-one Kind.
The addition of pigment makes to present different colors, thus meets the client's different need to product Ask.The addition of antioxidant can reduce the oxidized rate of no-silicon type heat-conducting pad, increases no-silicon type and leads The service life of hot pad
Further, the second raw material is counted by weight and is also included: 0~3 part of catalyst.Urge Agent includes at least one in organotin, organo-bismuth and triethylamine.
The addition of catalyst accelerates vulcanizing agent and the reaction rate of liquid methacrylate resin.
The present invention proposes prepared by any of the above-described preparation method that a kind of present invention of employing proposes No-silicon type heat-conducting pad.
Embodiment 1
The preparation method of a kind of no-silicon type heat-conducting pad that the present embodiment provides, its concrete operations walk Suddenly it is:
Step A, will prepare the raw material of no-silicon type heat-conducting pad: liquid propene acid resin 100 Part, alumina powder 400 parts, (2-(2-Butoxyethoxy) ethyl) ester 10 parts, 4,4'- Double (bis (alpha, alpha-dimethylbenzyl) base) diphenylamines 1.8 parts, iron oxide yellow 0.1 part, organotin 0.3 part, Isocyanates 0.15 part, weighs standby.
Step B, by liquid propene acid resin 100 in load weighted for step step A raw material Part, alumina powder 400 parts, (2-(2-Butoxyethoxy) ethyl) ester 10 parts, 4,4'- Double (bis (alpha, alpha-dimethylbenzyl) base) diphenylamines 1.8 parts, iron oxide yellow 0.1 part add high-temperature vacuum and mediate Stir 2 hours at 180 DEG C in blender.
Step C, is cooled to when 100 DEG C add organotin 0.3 part, isocyanates 0.15 part, Double planetary mixer is used to obtain sizing material after stirring 15 minutes.
Step D, pours into gained sizing material in 200mm*400mm*2.0mm mould, with four At a temperature of column hydraulic machine 160 DEG C, hot-press vulcanization 5 minutes, obtains no-silicon type heat-conducting pad.
The product defect rate that the present embodiment produces is less than 1%, and human cost is low, the present embodiment The heat conductivity of conducting strip without silicon of preparation can reach 1.0-1.5W/mK, has surface microviscosity, 100 DEG C of continuous work 1000 hours without fuel-displaced, without catabiosis, be mainly used in silicone oil sensitive Occasion thermal conductive gap.
Embodiment 2
The preparation method of a kind of no-silicon type heat-conducting pad that the present embodiment provides, its concrete operations walk Suddenly it is:
Step A, will prepare the raw material of no-silicon type heat-conducting pad: liquid propene acid resin 100 Part, alumina powder 500 parts, (2-(2-Butoxyethoxy) ethyl) ester 20 parts, 4,4'- Double (bis (alpha, alpha-dimethylbenzyl) base) diphenylamines 1.8 parts, white carbon black 0.1 part, organotin 0.25 part, isocyanide Acid esters 0.13 part, weighs standby.
Step B, by liquid propene acid resin 100 in load weighted for step step A raw material Part, alumina powder 500 parts, (2-(2-Butoxyethoxy) ethyl) ester 20 parts, 4,4'- Double (bis (alpha, alpha-dimethylbenzyl) base) diphenylamines 1.8 parts, white carbon black 0.1 part add high-temperature vacuum and mediate stirring Stir 4 hours at 175 DEG C in machine.
Step C, is cooled to when 100 DEG C add organotin 0.25 part, isocyanates 0.13 Part, use double planetary mixer to obtain sizing material after stirring 15 minutes.
Step D, pours into gained sizing material in 200mm*400mm*2.0mm mould, with four At a temperature of column hydraulic machine 150 DEG C, hot-press vulcanization 6 minutes, obtains no-silicon type heat-conducting pad.
The product defect rate that the present embodiment produces is less than 1%, and human cost is low, the present embodiment The heat conductivity of conducting strip without silicon of preparation can reach 2.0-2.5W/mK, has surface microviscosity, 100 DEG C of continuous work 1000 hours without fuel-displaced, without catabiosis, be mainly used in silicone oil sensitive Occasion thermal conductive gap, heat conduction requires height, has certain insulating requirements to require occasion.
Embodiment 3
The preparation method of a kind of no-silicon type heat-conducting pad that the present embodiment provides, its concrete operations walk Suddenly it is:
Step A, will prepare the raw material of no-silicon type heat-conducting pad: liquid propene acid resin 100 Part, boron nitride part 600 parts, aluminium powder 400 parts, (2-(2-Butoxyethoxy) ethyl) Ester 10 parts, isocyanates 0.13 part, weigh standby.
Step B, by liquid propene acid resin 100 in load weighted for step step A raw material Part, boron nitride part 600 parts, aluminium powder 400 parts, (2-(2-Butoxyethoxy) ethyl) Stir 6 hours at 175 DEG C in ester 10 parts, addition high-temperature vacuum Kneeding stirrer.
Step C, is cooled to when 100 DEG C add isocyanates 0.1 part, uses double-planet to stir Mix after machine stirs 40 minutes and obtain sizing material.
Step D, pours into gained sizing material in 200mm*400mm*2.0mm mould, with four At a temperature of column hydraulic machine 130 DEG C, hot-press vulcanization 15 minutes, obtains no-silicon type heat-conducting pad.
The product defect rate that the present embodiment produces is less than 1%, and human cost is low, the present embodiment The heat conductivity of conducting strip without silicon of preparation can reach 4.5-6.0W/mK, has surface microviscosity, 100 DEG C of continuous work 1000 hours without fuel-displaced, without catabiosis, be mainly used in silicone oil sensitive Occasion thermal conductive gap, heat conduction requires high, but the application blind that naked requires.
Embodiment 4
The preparation method of a kind of no-silicon type heat-conducting pad that the present embodiment provides, its concrete operations walk Suddenly it is:
Step A, will prepare the raw material of no-silicon type heat-conducting pad: liquid propene acid resin 100 Part, alumina powder 500 parts, (2-(2-Butoxyethoxy) ethyl) ester 20 parts, 4,4'- Double (bis (alpha, alpha-dimethylbenzyl) base) diphenylamines 2 parts, white carbon black 2 parts, organotin 3 parts, isocyanates 1 Part, weigh standby.
Step B, by liquid propene acid resin 100 in load weighted for step step A raw material Part, alumina powder 500 parts, (2-(2-Butoxyethoxy) ethyl) ester 20 parts, 4,4'- Double (bis (alpha, alpha-dimethylbenzyl) base) diphenylamines 2 parts, white carbon black 2 parts add high-temperature vacuum Kneeding stirrer Interior stirring 4 hours at 160 DEG C.
Step C, is cooled to when 100 DEG C add organotin 3 parts, isocyanates 1 part, adopts Sizing material is obtained with double planetary mixer after stirring 10 minutes.
Step D, pours into gained sizing material in 200mm*400mm*2.0mm mould, with four At a temperature of column hydraulic machine 160 DEG C, hot-press vulcanization 4 minutes, obtains no-silicon type heat-conducting pad.
The product defect rate that the present embodiment produces is less than 1%, and human cost is low, the nothing of preparation Silicon conducting strip heat conductivity can reach 3.5-4.0W/mK, has surface microviscosity, 100 DEG C of companies Continuous work 1000 hours without fuel-displaced, without catabiosis, be mainly used in silicone oil sensitivity occasion and lead Temperature gap, heat conduction requires height, has certain insulating requirements to require occasion.
Embodiment 5
The preparation method of a kind of no-silicon type heat-conducting pad that the present embodiment provides, its concrete operations walk Suddenly it is:
Step A, will prepare the raw material of no-silicon type heat-conducting pad: liquid propene acid resin 100 Part, alumina powder 500 parts, (2-(2-Butoxyethoxy) ethyl) ester 20 parts, 4,4'- Double (bis (alpha, alpha-dimethylbenzyl) base) diphenylamines 1.8 parts, white carbon black 0.1 part, organotin 0.25 part, isocyanide Acid esters 0.13 part, weighs standby.
Step B, by liquid propene acid resin 100 in load weighted for step step A raw material Part, alumina powder 500 parts, (2-(2-Butoxyethoxy) ethyl) ester 20 parts, 4,4'- Double (bis (alpha, alpha-dimethylbenzyl) base) diphenylamines 1.8 parts, white carbon black 0.1 part add high-temperature vacuum and mediate stirring Stir 4 hours at 175 DEG C in machine.
Step C, is cooled to when 100 DEG C add organotin 0.25 part, isocyanates 0.13 Part, use double planetary mixer to obtain sizing material after stirring 15 minutes.
Step D, pours into gained sizing material in 200mm*400mm*2.0mm mould, with four At a temperature of column hydraulic machine 150 DEG C, hot-press vulcanization 12 minutes, obtains no-silicon type heat-conducting pad.
The product defect rate that the present embodiment produces is less than 1%, and human cost is low, the present embodiment The heat conductivity of conducting strip without silicon of preparation can reach 2.4-2.8W/mK, has surface microviscosity, 100 DEG C of continuous work 1000 hours without fuel-displaced, without catabiosis, be mainly used in silicone oil sensitive Occasion thermal conductive gap, heat conduction requires height, has certain insulating requirements to require occasion.
Embodiment 6
Step A, will prepare the raw material of no-silicon type heat-conducting pad: liquid propene acid resin 100 Part, alumina powder 400 parts, (2-(2-Butoxyethoxy) ethyl) ester 10 parts, 4,4'- Double (bis (alpha, alpha-dimethylbenzyl) base) diphenylamines 1.8 parts, iron oxide yellow 0.1 part, organotin 0.3 part, Isocyanates 0.15 part, weighs standby.
Step B, by liquid propene acid resin 100 in load weighted for step step A raw material Part, alumina powder 400 parts, (2-(2-Butoxyethoxy) ethyl) ester 10 parts, 4,4'- Double (bis (alpha, alpha-dimethylbenzyl) base) diphenylamines 1.8 parts, iron oxide yellow 0.1 part add high-temperature vacuum and mediate Stir 6 hours at 180 DEG C in blender.
Step C, is cooled to when 100 DEG C add organotin 0.3 part, isocyanates 0.15 part, Double planetary mixer is used to obtain sizing material after stirring 15 minutes.
Step D, pours into gained sizing material in 200mm*400mm*2.0mm mould, with four At a temperature of column hydraulic machine 160 DEG C, hot-press vulcanization 5 minutes, obtains no-silicon type heat-conducting pad.
The product defect rate that the present embodiment produces is less than 1%, and human cost is low, the present embodiment The heat conductivity of conducting strip without silicon of preparation can reach 1.5-2.0W/mK, has surface microviscosity, 100 DEG C of continuous work 1000 hours without fuel-displaced, without catabiosis, be mainly used in silicone oil sensitive Occasion thermal conductive gap.
Comparative example 1
A kind of preparation method of heat-conducting pad without silicone oil, its concrete operation step is as follows:
Step A, will prepare the raw material of no-silicon type heat-conducting pad: liquid propene acid resin 100 Part, alumina powder 1200 parts, (2-(2-Butoxyethoxy) ethyl) ester 50 parts, 4,4'- Double (bis (alpha, alpha-dimethylbenzyl) base) diphenylamines 2.5 parts, iron oxide yellow 3 parts, organotin 4 parts, isocyanide Acid esters 2 parts, weighs standby.
Step B, by liquid propene acid resin 100 in load weighted for step step A raw material Part, alumina powder 1200 parts, (2-(2-Butoxyethoxy) ethyl) ester 50 parts, 4,4'- Double (bis (alpha, alpha-dimethylbenzyl) base) diphenylamines 2.5 parts, iron oxide yellow 3 parts add high-temperature vacuum kneading and stir Stir 7 hours at 200 DEG C in mixing machine.
Step C, is cooled to when 100 DEG C add organotin 4 parts, isocyanates 2 parts, adopts Sizing material is obtained with double planetary mixer after stirring 50 minutes.
Step D, pours into gained sizing material in 200mm*400mm*2.0mm mould, with four At a temperature of column hydraulic machine 180 DEG C, hot-press vulcanization 20 minutes, obtains no-silicon type heat-conducting pad.
The product defect rate that the present embodiment produces is more than 2%, and human cost is low, the nothing of preparation Silicon conducting strip heat conductivity can reach more than 4.0W/mK, but 100 DEG C of continuous work less than Fuel-displaced, catabiosis occurred in 1000 hours.
Comparative example 2
A kind of preparation method of heat-conducting pad without silicone oil, its concrete operation step is as follows:
Step A, will prepare the raw material of no-silicon type heat-conducting pad: liquid propene acid resin 100 Part, alumina powder 50 parts, (2-(2-Butoxyethoxy) ethyl) ester 5 parts, Carbimide. Ester 0.01 part, weighs standby.
Step B, by liquid propene acid resin 100 in load weighted for step step A raw material Part, alumina powder 20 parts, (2-(2-Butoxyethoxy) ethyl) ester 5 parts, addition height Stir 1 hour at 100 DEG C in temperature vacuum kneading blender.
Step C, is cooled to when 100 DEG C add isocyanates 0.01 part, uses double-planet to stir Mix after machine stirs 5 minutes and obtain sizing material.
Step D, pours into gained sizing material in 200mm*400mm*2.0mm mould, with four At a temperature of column hydraulic machine 100 DEG C, hot-press vulcanization 2 minutes, obtains no-silicon type heat-conducting pad.
The product defect rate that the present embodiment produces is more than 10%, and human cost is low, but preparation The heat conductivity of conducting strip without silicon is at below 1.0W/mK, and 100 DEG C of continuous work are less than 1000 Hour occur fuel-displaced, catabiosis.
Comparative example 3
A kind of preparation method of heat-conducting pad without silicone oil, its concrete operation step is as follows:
2 parts and 100 parts propylene liguid acid resins of 4,4'-bis-(propyloxy phenyl base) diphenylamines are added Mill carries out mill, cooked bag roller, is subsequently adding alumina powder 500 parts, (2-(2-fourth Epoxide ethyoxyl) ethyl) ester 20 parts, white carbon black 2 parts, continue mill, mixing uniformly after add Entering isocyanates 1 part, after putting through 10 times, mill terminates to obtain sizing material, sizing material is added mould and exists Molding in 3 minutes is vulcanized at 170 DEG C.
This comparative example gained no-silicon type heat-conducting pad heat conductivity reaches 1.0-1.5W/mK, has table Face viscosity, at 100 DEG C continuously work 1000 hours without permeability, without catabiosis, but This technique is produced defect rate and is more than 2%, and it is high to produce human cost.
Comparative example 4
A kind of preparation method of heat-conducting pad without silicone oil, its concrete operation step is as follows:
Step A, will prepare the raw material of no-silicon type heat-conducting pad: on-liquid acroleic acid resin 100 parts, alumina powder 1200 parts, (2-(2-Butoxyethoxy) ethyl) ester 50 parts, Double (bis (alpha, alpha-dimethylbenzyl) base) diphenylamines 2.5 parts of 4,4'-, iron oxide yellow 3 parts, organotin 4 parts, Isocyanates 2 parts, weighs standby.
Step B, by liquid propene acid resin 100 in load weighted for step step A raw material Part, alumina powder 1200 parts, (2-(2-Butoxyethoxy) ethyl) ester 50 parts, 4,4'- Double (bis (alpha, alpha-dimethylbenzyl) base) diphenylamines 2.5 parts, iron oxide yellow 3 parts add high-temperature vacuum kneading and stir Stir 2 hours at 200 DEG C in mixing machine.
Step C, is cooled to when 100 DEG C add organotin 4 parts, isocyanates 2 parts, adopts Sizing material is obtained with double planetary mixer after stirring 50 minutes.
Step D, pours into gained sizing material in 200mm*400mm*2.0mm mould, with four At a temperature of column hydraulic machine 180 DEG C, hot-press vulcanization 20 minutes, obtains no-silicon type heat-conducting pad.
The product defect rate that the present embodiment produces is more than 1%, and human cost is low, the present embodiment The heat conductivity of conducting strip without silicon of preparation can reach 0.8-1.3W/mK, has surface microviscosity, 100 DEG C of continuous work 1000 hours without fuel-displaced, without catabiosis, be mainly used in silicone oil sensitive Occasion thermal conductive gap.
The manpower that above-described embodiment puts into traditional heat-conducting pad production process with comparative example becomes Originally compare, draw the height of human cost.
Table 1. embodiment 1~6 and comparative example 1~4 gained end properties and produce result and see table
Comparative example 1 and comparative example 2 compared to embodiment 1-4, its every material coefficient and each Operation index is many not in the present invention, but its operating procedure still uses high-temperature vacuum kneading to stir Mixing, its comparing result can be seen that the properties of product produced are not as good as embodiment 1-4, embodiment 1 The most identical except vacuum kneading mixing time other indices different with embodiment 6, embodiment The vacuum kneading mixing time of 6 is more than embodiment 1, and its result is that embodiment 6 is produced The heat conductivity of heat-conducting pad without silicon is higher than embodiment 1, illustrates at the time range that the present invention is given The heat conductivity of heat-conducting pad without silicon of the interior the most long-living output of vacuum kneading mixing time is the best, implements Example 2 is with embodiment 5 in addition to the hot-press vulcanization time is different, and other indices are the most identical, The hot-press vulcanization time of embodiment 5 is big with the hot-press vulcanization time of embodiment 2, and its result is reality The thermal conductivity ratio embodiment 2 executing the heat-conducting pad without silicon that example 5 is produced is high, illustrates at this In the bright time range be given, the heat conduction system of the heat-conducting pad without silicon of the most long-living output of cure time Number is the highest, but its identical with the raw materials for production of embodiment 4 of comparative example 3 uses the operation of mill By contrast, technique, although can be seen that its product performance produced does not differs with embodiment 4 Too much, but its production defect rate is slightly higher, and clearance is observed and contrasted itself and traditional heat-conducting pad Human cost height in process of production, comparative example 3 is of a relatively high, and comparative example 4 is former in production Using non-liquid acroleic acid resin on material, other materials indexs and operation index are with embodiment 1 Identical, but final finished lead coefficient compared to use propylene liguid acid resin be the lower slightly of raw material, And the defect rate produced is also the slightly higher of raw material compared to propylene liguid acid resin.
In sum, it is good that the no-silicon type heat-conducting pad of the embodiment of the present invention has heat conductivity, work Making the time long, it is low that its preparation technology has production defect rate, advantage that human cost is low.
Embodiments described above is a part of embodiment of the present invention rather than whole enforcement Example.The detailed description of embodiments of the invention is not intended to limit the model of claimed invention Enclose, but be merely representative of the selected embodiment of the present invention.Based on the embodiment in the present invention, this It is every other that field those of ordinary skill is obtained under not making creative work premise Embodiment, broadly falls into the scope of protection of the invention.

Claims (10)

1. the preparation method of a no-silicon type heat-conducting pad, it is characterised in that described preparation method Comprise the following steps:
The first raw material and the second raw material of preparing no-silicon type heat-conducting pad are weighed standby, presses Weight portion meter, described first raw material includes: liquid methacrylate class rubber 100 parts, heat conduction Powder 100~1000 parts, (2-(2-Butoxyethoxy) ethyl) ester 10~40 parts;Described Two raw materials are counted by weight and are included vulcanizing agent 0.1~1 part;Described first raw material is existed At 150~180 DEG C, vacuum kneading stirs 2~6 hours, then will stir through described vacuum kneading After described first raw material mix with described second raw material, be stirred for 4~40 minutes glue Material, puts into described sizing material in mould and hot-press vulcanization 4~15 under 130~160 DEG C of vacuum conditions Minute, then cool down to obtain finished product.
Preparation method the most according to claim 1, it is characterised in that described hot-press vulcanization Time be 10~15 minutes.
3. according to the preparation method described in claim 1, it is characterised in that described first raw material Count by weight and also include: 0~2 part of pigment, 0~2 part of antioxidant.
Preparation method the most according to claim 3, it is characterised in that described pigment includes Any one in barba hispanica, iron oxide red, iron oxide yellow and white carbon black, described antioxidant is 4,4'- Double (bis (alpha, alpha-dimethylbenzyl) base) diphenylamines, 4,4'-bis-(propyloxy phenyl base) diphenylamines, two [4-(1-methyl -1-phenethyl) benzene] amine, at least one in double (A, the A-dimethyl benzyl) diphenylamines of 4,4'-.
Preparation method the most according to claim 2, it is characterised in that described second former material Material is counted by weight and is also included: 0~3 part of catalyst.
6. with according to the preparation method described in claim 5, it is characterised in that described catalyst bag Include at least one in organotin, organo-bismuth and triethylamine.
Preparation method the most according to claim 2, it is characterised in that described propylene liguid Acid esters rubber includes liquid methacrylate rubber, liquid ethylene acrylate elastomer and liquid hydroxyl At least one in base acrylic rubber.
Preparation method the most according to claim 2, it is characterised in that described conductive powder bag Include at least one in aluminium oxide, aluminium hydroxide, boron nitride, carborundum and metal powder.
Preparation method the most according to claim 2, it is characterised in that described vulcanizing agent is Isocyanates hydroxy systems, phenolic and epoxy and hydroxy systems, soap sulfur system and TCY sulfur Any one in change system.
10. a no-silicon type heat-conducting pad, it is characterised in that described no-silicon type heat-conducting pad by Preparation method described in any one of claim 1-9 prepares.
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CN102807754A (en) * 2011-05-31 2012-12-05 北京中石伟业技术有限公司 Heat conduction gap filling material, preparation method and application thereof
CN103319829A (en) * 2013-06-13 2013-09-25 深圳德邦界面材料有限公司 Silicon-free heat-conducting gasket and preparation method thereof
CN104497585A (en) * 2014-12-17 2015-04-08 苏州锦腾电子科技有限公司 High-thermal-conductivity silicone rubber and preparation method thereof

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CN102807754A (en) * 2011-05-31 2012-12-05 北京中石伟业技术有限公司 Heat conduction gap filling material, preparation method and application thereof
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