CN111909519A - Flexible heat-conducting silicon rubber and preparation method and application thereof - Google Patents

Flexible heat-conducting silicon rubber and preparation method and application thereof Download PDF

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CN111909519A
CN111909519A CN202010731948.XA CN202010731948A CN111909519A CN 111909519 A CN111909519 A CN 111909519A CN 202010731948 A CN202010731948 A CN 202010731948A CN 111909519 A CN111909519 A CN 111909519A
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modified
parts
flexible heat
conducting
calcium carbonate
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蒋冲
黄计锋
闻明
徐华斌
练志良
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Shenzhen Sunyes New Material Co ltd
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Shenzhen Sunyes New Material Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/04—Polysiloxanes
    • C08L83/06—Polysiloxanes containing silicon bound to oxygen-containing groups
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K7/00—Constructional details common to different types of electric apparatus
    • H05K7/20—Modifications to facilitate cooling, ventilating, or heating
    • H05K7/2039—Modifications to facilitate cooling, ventilating, or heating characterised by the heat transfer by conduction from the heat generating element to a dissipating body
    • 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
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2217—Oxides; Hydroxides of metals of magnesium
    • C08K2003/222—Magnesia, i.e. magnesium oxide
    • 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
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2217—Oxides; Hydroxides of metals of magnesium
    • C08K2003/2224—Magnesium hydroxide
    • 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
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • 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
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2296—Oxides; Hydroxides of metals of zinc
    • 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
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C08K2003/265—Calcium, strontium or barium carbonate
    • 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
    • C08K3/38—Boron-containing compounds
    • C08K2003/387—Borates
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/20—Applications use in electrical or conductive gadgets
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure

Abstract

The invention discloses a flexible heat-conducting silicone rubber and a preparation method and application thereof, wherein the raw materials of the flexible heat-conducting silicone rubber comprise 100 parts of base rubber, 100-500 parts of diluent, 300-800 parts of heat-conducting filler, 100-600 parts of flame retardant, 100-400 parts of calcium carbonate, 0.05-5 parts of cross-linking agent and 0.05-5 parts of catalyst.

Description

Flexible heat-conducting silicon rubber and preparation method and application thereof
Technical Field
The invention belongs to the technical field of rubber materials, and particularly relates to flexible heat-conducting silicone rubber as well as a preparation method and application thereof.
Background
With the rapid development of electronic technology of electronic products, components tend to be densified and miniaturized, and the temperature of the working environment rises rapidly, so that the service life of the components can be greatly shortened if the temperature of the components cannot be rapidly dissipated. The heat conduction silicon rubber can effectively and quickly dissipate heat generated by the components, and the service life and the working efficiency of the components are improved. The filling type heat-conducting silicone rubber is a compound consisting of a high polymer material and a high heat-conducting filler, wherein when the amount of the heat-conducting filler is increased to a certain degree, the silicone rubber generally has the phenomena of high hardness, large interface stress and certain adhesiveness, so that the silicone rubber cannot be repaired in the construction process, and components and parts are easily scrapped, thereby increasing the production cost and reducing the production efficiency.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the first purpose of the present invention is to provide a flexible heat-conducting silicone rubber, which has good flexibility, is easy to repair, and has good mechanical properties.
The technical scheme adopted by the invention for realizing the purpose is as follows:
the flexible heat-conducting silicone rubber comprises the following raw materials in parts by mass:
100 portions of base rubber
100-500 parts of diluent
300-800 parts of heat-conducting filler
100-600 parts of flame retardant
100-400 parts of calcium carbonate
0.05-5 parts of cross-linking agent
0.05-5 parts of catalyst
The base adhesive is one or more of hydroxyl silicone oil, alkoxy silicone oil, vinyl silicone oil and MQ silicone resin.
At 25 ℃, the viscosity range of the hydroxyl silicone oil is 500-55000 mPa.s, the viscosity range of the alkoxy silicone oil is 500-50000 mPa.s, the viscosity range of the vinyl silicone oil is 300-12000 mPa.s, and the viscosity range of the MQ silicone resin is 200-10000 mPa.s.
The diluent is one or more of dimethyl silicone oil, MDT type silicone oil, white oil, mineral oil and phenyl silicone oil.
The heat conducting filler is one or more of aluminum oxide, modified aluminum oxide, zinc oxide, modified zinc oxide, magnesium oxide, modified magnesium oxide, silicon micropowder, modified silicon micropowder, aluminum powder, modified aluminum powder, silver powder, modified silver powder, silicon carbide, modified silicon carbide, boron nitride, modified boron nitride, aluminum nitride, modified aluminum nitride, graphene and modified graphene.
The flame retardant is one or more of melamine cyanurate, polyphosphate, aluminum hydroxide, modified aluminum hydroxide, magnesium hydroxide, modified magnesium hydroxide, zinc borate and modified zinc borate.
The calcium carbonate is one or more of heavy calcium carbonate, light calcium carbonate, nano calcium carbonate, hydrophobic heavy calcium carbonate, hydrophobic light calcium carbonate and hydrophobic nano calcium carbonate.
The cross-linking agent is methyl orthosilicate, ethyl orthosilicate, propyl orthosilicate, ethyl polysilicate, methyltrimethoxysilane, methyltriethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, isobutyl triethoxysilane, isooctyltriethoxysilane, vinylmethyldimethoxysilane, vinyltriisopropenoxysilane, tetraisopropoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane, methyltriacetoxysilane, modified methyltriacetoxysilane, ethyltriacetoxysilane, propyltriacetoxysilane, methylpropyltriacetoxysilane, methylethyltriacetoxysilane, di-tert-butoxydiacetoxysilane, methyltributanonoximesilane, vinyltributonoximosilane, phenyltributonoximosilane, tetrabutoximinosilane, methyltripropoximinosilane, ethyl trisiloximosilane, methyl-tri-butoximosilane, methyl-ethyl-triethoximidosilane, methyl-ethyl-tri, One or more of diethylaminomethyltrimethoxysilane, 3-diethylaminopropyltriethoxysilane, dichloromethyltriethoxysilane, aniline methyltriethoxysilane, 3-chloropropyltrimethoxysilane, and hydrogen-containing silicone oil.
The catalyst is one or more of dibutyltin dilaurate, dibutyltin diacetate, chelated tin, diisopropyl di (ethyl acetoacetate) titanate, tetrabutyl titanate, tetraisopropyl titanate, di (acetylacetone) -1, 3-propylenedioxytitanium, diisopropyl di (acetylacetone) titanate, titanate chelate, titanate complex, 3-diethylaminopropyltrimethoxysilane, 3-diethylaminopropyltriethoxysilane and platinum catalyst.
The second purpose of the invention is to provide a preparation method of the flexible heat-conducting silicone rubber.
A preparation method of flexible heat-conducting silicone rubber comprises the following steps:
(1) blending base glue, a diluent, a heat-conducting filler, a flame retardant and calcium carbonate for reaction;
(2) adding a cross-linking agent and a catalyst, and stirring to obtain the flexible heat-conducting silicon rubber.
In the step (1), the temperature of the reactants is 80-140 ℃, and the reaction time is 60-150 min.
In the step (1), the reaction is carried out under vacuum condition, and the vacuum degree is-0.06 MPa to-0.1 MPa.
In step (2), the crosslinking agent and the catalyst are added under the same vacuum conditions as in step (1).
The invention further aims to provide application of the flexible heat-conducting silicone rubber, and particularly provides the flexible heat-conducting silicone rubber which is used for heat dissipation of electronic components, so that interface stress is reduced, and the functions of heat dissipation and easy repair are achieved.
Compared with the prior art, the silicon rubber provided by the invention has the advantages that the cross-linking density of the silicon rubber is reduced by reasonably matching materials, so that the hardness is reduced, the silicon rubber has good flexibility and heat conductivity, is easy to repair, has good mechanical properties, and can meet the requirements of the electronic industry on heat conductivity and easy repair performance.
Detailed Description
The technical solution of the present invention is further described below with reference to specific examples.
Example 1
This example provides a flexible heat-conductive silicone rubber, the raw materials of which are shown in table 1.
The preparation method of the flexible heat-conducting silicone rubber comprises the following steps:
(1) 100 parts of hydroxyl silicone oil, 200 parts of dimethyl silicone oil, 500 parts of alumina, 120 parts of aluminum hydroxide and 120 parts of nano calcium carbonate are respectively mixed in a stirrer according to the weight for 60min, the mixture is continuously stirred for 120min under the vacuum condition and the high temperature condition of 115 ℃, and the mixture is cooled to the room temperature and then is continuously stirred for 20min under the vacuum condition.
(2) Sequentially adding 2 parts of methyltrimethoxysilane and 1 part of titanate complex, uniformly stirring, and discharging under the protection of inert gas.
Example 2
This example provides a flexible heat-conductive silicone rubber, the raw materials of which are shown in table 1.
The preparation method of the flexible heat-conducting silicone rubber comprises the following steps:
(1) 100 parts of alkoxy silicone oil, 400 parts of white oil, 500 parts of alumina, 300 parts of zinc oxide, 420 parts of magnesium hydroxide and 320 parts of hydrophobic light calcium carbonate are respectively mixed in a stirrer according to the amount for 60min, the mixture is continuously stirred for 110min under the vacuum condition and the high temperature condition of 95 ℃, and the mixture is cooled to the room temperature and then is continuously stirred for 60min under the vacuum condition.
(2) Sequentially adding 1 part of methyltrimethoxysilane and 2 parts of 3-diethylaminopropyltriethoxysilane, uniformly stirring, and discharging under the protection of inert gas.
Example 3
This example provides a flexible heat-conductive silicone rubber, the raw materials of which are shown in table 1.
The preparation method of the flexible heat-conducting silicone rubber comprises the following steps:
(1) 100 parts of hydroxyl silicone oil, 350 parts of dimethyl silicone oil, 420 parts of silicon micropowder, 50 parts of magnesium oxide, 250 parts of melamine cyanurate, 80 parts of zinc borate and 220 parts of hydrophobic heavy calcium carbonate are respectively mixed in a stirrer for 60min according to the measurement, the mixture is continuously stirred for 30min under the vacuum condition and the high temperature condition of 130 ℃, and the mixture is continuously stirred for 60min under the vacuum condition after being cooled to the room temperature.
(2) Sequentially adding 3 parts of methyl tributyl ketoxime silane, 2 parts of vinyl tributyroxime silane and 0.2 part of chelating tin, uniformly stirring, and discharging under the protection of inert gas.
Comparative example 1
This comparative example is similar to example 1 except that: calcium carbonate was omitted.
Comparative example 2
This comparative example is similar to example 2 except that: the flame retardant is omitted.
Comparative example 3
This comparative example is similar to example 3 except that: the base rubber is replaced by polyurethane.
TABLE 1 Flexible heat-conducting Silicone rubber raw material ratio
Example 1 Example 2 Example 3
Base rubber 100 100 100
Diluent 200 400 350
Heat conductive filler 500 800 470
Flame retardant 120 420 330
Calcium carbonate 120 320 220
Crosslinking agent 2 1 5
Catalyst and process for preparing same 1 2 0.2
Performance detection
The flexible heat-conducting silicone rubber is subjected to performance tests, and the results are shown in the following table 2:
wherein the tack free time is measured in accordance with GB/T13477.5-2002, the mechanical properties are measured in accordance with GBT531-1999 for hardness after 7 days of curing, the thermal conductivity is measured in accordance with ISO/DIS 22007, and the tensile strength and elongation are measured in accordance with ASTM D412.
Table 2 flexible heat-conductive silicone rubber performance test results
Figure BDA0002603482730000051
According to the test results, the flexible heat-conducting silicone rubber disclosed by the invention has the advantages of lower hardness, reduced interface stress, good flexibility, better heat conductivity coefficient and mechanical property, and capability of meeting excellent heat conductivity, low interface stress and easy repair performance required by the electronic industry. When calcium carbonate or a flame retardant is omitted from the raw materials or the base rubber is replaced by polyurethane, the mechanical property of the silicone rubber is obviously reduced although the silicone rubber still keeps better flexibility, so that the calcium carbonate, the flame retardant and the base rubber have important influence on reducing the hardness of the silicone rubber and simultaneously keeping good mechanical property.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (10)

1. A flexible heat-conducting silicone rubber is characterized in that: the composite material comprises the following raw materials in parts by mass:
100 portions of base rubber
100-500 parts of diluent
300-800 parts of heat-conducting filler
100-600 parts of flame retardant
100-400 parts of calcium carbonate
0.05-5 parts of cross-linking agent
0.05-5 parts of catalyst
The base adhesive is one or more of hydroxyl silicone oil, alkoxy silicone oil, vinyl silicone oil and MQ silicone resin.
2. The flexible heat-conducting silicone rubber according to claim 1, wherein: at 25 ℃, the viscosity range of the hydroxyl silicone oil is 500-55000 mPa.s, the viscosity range of the alkoxy silicone oil is 500-50000 mPa.s, the viscosity range of the vinyl silicone oil is 300-12000 mPa.s, and the viscosity range of the MQ silicone resin is 200-10000 mPa.s.
3. The flexible heat-conducting silicone rubber according to claim 1, wherein: the diluent is one or more of dimethyl silicone oil, MDT type silicone oil, white oil, mineral oil and phenyl silicone oil.
4. The flexible heat-conducting silicone rubber according to claim 1, wherein: the heat conducting filler is one or more of aluminum oxide, modified aluminum oxide, zinc oxide, modified zinc oxide, magnesium oxide, modified magnesium oxide, silicon micropowder, modified silicon micropowder, aluminum powder, modified aluminum powder, silver powder, modified silver powder, silicon carbide, modified silicon carbide, boron nitride, modified boron nitride, aluminum nitride, modified aluminum nitride, graphene and modified graphene.
5. The flexible heat-conducting silicone rubber according to claim 1, wherein: the flame retardant is one or more of melamine cyanurate, polyphosphate, aluminum hydroxide, modified aluminum hydroxide, magnesium hydroxide, modified magnesium hydroxide, zinc borate and modified zinc borate.
6. The flexible heat-conducting silicone rubber according to claim 1, wherein: the calcium carbonate is one or more of heavy calcium carbonate, light calcium carbonate, nano calcium carbonate, hydrophobic heavy calcium carbonate, hydrophobic light calcium carbonate and hydrophobic nano calcium carbonate.
7. The flexible heat-conducting silicone rubber according to claim 1, wherein: the cross-linking agent is methyl orthosilicate, ethyl orthosilicate, propyl orthosilicate, ethyl polysilicate, methyltrimethoxysilane, methyltriethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, isobutyl triethoxysilane, isooctyltriethoxysilane, vinylmethyldimethoxysilane, vinyltriisopropenoxysilane, tetraisopropoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane, methyltriacetoxysilane, modified methyltriacetoxysilane, ethyltriacetoxysilane, propyltriacetoxysilane, methylpropyltriacetoxysilane, methylethyltriacetoxysilane, di-tert-butoxydiacetoxysilane, methyltributanonoximesilane, vinyltributonoximosilane, phenyltributonoximosilane, tetrabutoximinosilane, methyltripropoximinosilane, ethyl trisiloximosilane, methyl-tri-butoximosilane, methyl-ethyl-triethoximidosilane, methyl-ethyl-tri, One or more of diethylaminomethyltrimethoxysilane, 3-diethylaminopropyltriethoxysilane, dichloromethyltriethoxysilane, aniline methyltriethoxysilane, 3-chloropropyltrimethoxysilane, and hydrogen-containing silicone oil.
8. The flexible heat-conducting silicone rubber according to claim 1, wherein: the catalyst is one or more of dibutyltin dilaurate, dibutyltin diacetate, chelated tin, diisopropyl di (ethyl acetoacetate) titanate, tetrabutyl titanate, tetraisopropyl titanate, di (acetylacetone) -1, 3-propylenedioxytitanium, diisopropyl di (acetylacetone) titanate, titanate chelate, titanate complex, 3-diethylaminopropyltrimethoxysilane, 3-diethylaminopropyltriethoxysilane and platinum catalyst.
9. A preparation method of the flexible heat-conducting silicone rubber as claimed in any one of claims 1 to 8, characterized by comprising: the method comprises the following steps:
(1) blending base glue, a diluent, a heat-conducting filler, a flame retardant and calcium carbonate for reaction;
(2) adding a cross-linking agent and a catalyst, and stirring to obtain the flexible heat-conducting silicon rubber.
10. The use of the flexible heat-conducting silicone rubber of any one of claims 1 to 8 in heat dissipation of electronic components.
CN202010731948.XA 2020-07-27 2020-07-27 Flexible heat-conducting silicon rubber and preparation method and application thereof Pending CN111909519A (en)

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* Cited by examiner, † Cited by third party
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CN112521750A (en) * 2020-11-23 2021-03-19 晟大科技(南通)有限公司 Modified silicone rubber composition and preparation method and application thereof
CN113956834A (en) * 2021-10-25 2022-01-21 广州集泰化工股份有限公司 Silicone sealant and preparation method and application thereof
CN113956834B (en) * 2021-10-25 2023-01-24 广州集泰化工股份有限公司 Silicone sealant and preparation method and application thereof
CN114621511A (en) * 2022-04-18 2022-06-14 惠州量子导通新材料有限公司 Non-silicon heat-conducting grease composition and preparation method thereof
CN114621511B (en) * 2022-04-18 2024-03-12 惠州量子导通新材料有限公司 Non-silicon heat conduction grease composition and preparation method thereof

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