CN105542476A - Heat-conducting silicone rubber with high electric dielectric strength and preparation method of heat-conducting silicone rubber - Google Patents
Heat-conducting silicone rubber with high electric dielectric strength and preparation method of heat-conducting silicone rubber Download PDFInfo
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- CN105542476A CN105542476A CN201610072584.2A CN201610072584A CN105542476A CN 105542476 A CN105542476 A CN 105542476A CN 201610072584 A CN201610072584 A CN 201610072584A CN 105542476 A CN105542476 A CN 105542476A
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- 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
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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Abstract
The invention discloses heat-conducting silicone rubber with high electric dielectric strength, belonging to the technical field of silicone rubber. The heat-conducting silicone rubber comprises a component A and a component B in a mass ratio of (1 to 0.1)-(1 to 15), wherein the component A comprises the following components in parts by weight: 100 parts of alpha-omega-terminal hydroxyl hydrogen-containing polydimethylsiloxane, 5-15 parts of a silane coupling agent, 0.05-5 parts of a catalyst I, 100-200 parts of a heat-conducting insulating filling and 5-15 parts of an anti-sedimentation agent; and the component B comprises the following components in parts by weight: 100 parts of low-molecular-weight alpha-omega-vinyl polydimethylsiloxane and 0.5-5 parts of a catalyst II. The invention further provides a preparation method of the heat-conducting silicone rubber with high electric dielectric strength. The preparation method comprises the following steps: (1) preparing the component A; (2) preparing the component B; and (C) preparing the silicone rubber. The silicone rubber has good heat-conducting property and high electric dielectric strength, and the degrading of the electric dielectric performance caused by the introduction of the heat-conducting filling is avoided.
Description
Technical field
The present invention relates to a kind of silicon rubber, be specifically related to heat-conducting silicon rubber of a kind of high electric insulation intensity and preparation method thereof, belong to silicon rubber technical field.
Background technology
Silicon rubber, as a kind of specialty elastomer, belongs to synthetic rubber, and silicon rubber is alternately arranged as the structure of main chain makes it have the stability to heat, oxygen more much higher than general organic polymer with Siliciumatom and Sauerstoffatom.Compare with General Purpose Rubber, silicon rubber has the following advantages: have the excellent properties such as high-low temperature resistant, electric insulation, resistance to ozone, radiation hardness, difficult combustion, hydrophobic, corrosion-resistant, nonpoisonous and tasteless and physiological inertia.Due to the performance of these excellences, silicon rubber is made to play irreplaceable effect in aerospace, electric, the high-tech area such as petrochemical complex, bio-medical.
Common dealcoholizing-type one component room temperature cure silicone rubber itself has good electrical insulation capability, when adding heat conductive filler to improve its heat conductivility to it, on the one hand because the insulating property of filler itself are not good, on the other hand, filler add the formation also bringing out silicon rubber internal electrical branch, the silicon rubber electrical insulation capability prepared obviously is declined, is not enough to the service requirements reaching some electronic apparatuss.
Summary of the invention
For above-mentioned prior art Problems existing, the invention provides a kind of heat-conducting silicon rubber of high electric insulation intensity, it has good heat conductivility and high electric insulation intensity concurrently, avoids the decline causing electrical insulation capability because of the introducing of heat conductive filler.Additionally provide a kind of preparation method of heat-conducting silicon rubber of above-mentioned high electric insulation intensity simultaneously.
To achieve these goals, the heat-conducting silicon rubber of a kind of high electric insulation intensity that the present invention adopts, this silicon rubber is made up of according to mass ratio 1:0.1-1:15 component A and B component;
Described component A is made up of the raw material of following mass parts:
α, the hydrogeneous polydimethylsiloxane of omega end hydroxyl 100 parts
Silane coupling agent 5-15 part
Catalyzer I 0.05-5 part
Heat-conductive insulation filling 100-200 part
Anti-sedimentation agent 5-15 part
Described B component is made up of the raw material of following mass parts:
Lower molecular weight α, ω-vinyldimethicone 100 parts
Catalyst II 0.5-5 part.
As improvement, the α in described component A, the hydrogeneous polydimethylsiloxane of omega end hydroxyl, its hydrogen content is 0.12-1.65%.
As improvement, silane coupling agent in described component A adopt in tetramethoxy-silicane, methyltrimethoxy silane, tetraethoxy, tetraethoxysilane one or more.
As improvement, the catalyzer I in described component A adopt in 2-ethyl hexyl oxy titanic acid ester, two (acetylacetone based) isopropoxy titanic acid ester, two (methyl aceto acetate base) diisopropoxy titanic acid ester, titanium isopropylate one or more.
As improvement, heat-conductive insulation filling in described component A adopt in the micron order magnesium oxide of different-grain diameter, aluminium nitride, aluminum oxide one or more.
As improvement, the anti-sedimentation agent in described component A is one or more in micron order zinc oxide, nano titanium oxide, nano silicon or nano aluminium oxide.
As improvement, the lower molecular weight α in described B component, ω-vinyldimethicone, its number-average molecular weight is 186-2000.
As improvement, the catalyst II in described B component adopts Platinic chloride-tetramethyl divinyl disiloxane complex compound.
In addition, present invention also offers the preparation method of the heat-conducting silicon rubber of high electric insulation intensity described in a kind of above-mentioned any one, specifically comprise the following steps:
(1) preparation of component A: by mass parts, take 100 parts of above-mentioned α, the hydrogeneous polydimethylsiloxane of omega end hydroxyl, 100-200 part heat-conductive insulation filling mix 0.5-1h in dispersion machine, after dewatered drying, add 5-15 part silane coupling agent, 0.05-5 part catalyzer I, 5-15 part anti-sedimentation agent under anhydrous condition again, mix;
(2) preparation of B component: take mass parts 100 parts of lower molecular weight α, ω-vinyldimethicone, 0.5-5 part catalyst II, mix;
(3) preparation of silicon rubber: the B component that component A step (1) obtained respectively and step (2) obtain is the ratio of 1:0.1-1:15 in mass ratio, mix rear deaeration in anhydrous conditions and obtain first product, by first product at room temperature through the condensation cured 2-5h of moisture, further at room temperature addition curing 3-7h or at 50-120 DEG C addition curing 0.5-2h, the heat-conducting silicon rubber of high electric insulation intensity.
The present invention adopts by α, the hydrogeneous polydimethylsiloxane of omega end hydroxyl, silane coupling agent, catalyzer I, the component A of heat-conductive insulation filling and anti-sedimentation agent composition, by lower molecular weight α, ω-vinyldimethicone and catalyst II composition B component, component A is mixed according to proper ratio with B component, with only adopt compared with condensed type or add-on type solidify in conventional art, A after the inventive method will mix, B component is through condensed type and add-on type two kinds of solidification processs, the crosslinking degree of effective raising silicon rubber, under the silicon rubber ensureing to add heat conductive filler has good heat conductivility prerequisite, effectively improve its electrical insulation capability, avoid in prior art the problem causing electrical insulation capability to decline due to the introducing of heat conductive filler, and preparation method is simple, processing condition easily realize, preparing product quality is good, efficiency is high.
Embodiment
For making the object, technical solutions and advantages of the present invention clearly understand, below by embodiment, the present invention is further elaborated.But should be appreciated that, specific embodiment described herein, only in order to explain the present invention, is not limited to scope of the present invention.
Embodiment one
Take the α that hydrogen content is 0.12%, the hydrogeneous polydimethylsiloxane of omega end hydroxyl 100 parts of (quality, lower same), median size is 20 parts, the magnesium oxide of 10 μm, median size is the aluminium nitride 40 parts of 3 μm, median size is 40 parts, the aluminum oxide of 15 μm, add dispersion machine respectively and mix 0.6h in dispersion machine, after dewatered drying under guarantee anhydrous condition, methyltrimethoxy silane 6 parts is added again in dispersion machine, two (methyl aceto acetate base) diisopropoxy titanic acid ester 0.3 part, median size is 5 parts, the zinc oxide of 1 μm, component A is obtained for subsequent use after mixing,
Take the α that number-average molecular weight is 186, ω-vinyldimethicone 100 parts and Platinic chloride-3 parts, tetramethyl divinyl disiloxane complex compound, obtain B component after mixing for subsequent use;
Taking mass ratio is that the component A of 1:0.13 mixes rear deaeration in anhydrous conditions with B component, at room temperature after moisture solidification 2.5h, then heats 0.8h at 60 DEG C, can obtain the heat-conducting silicon rubber of high electric insulation intensity.
After tested, its thermal conductivity is 0.88(W/ (mk)), electric simulation strength represents with breaking down field strength, is 24.3(kV/mm).
Embodiment two
Take the α that hydrogen content is 0.37%, the hydrogeneous polydimethylsiloxane of omega end hydroxyl 100 parts of (quality, lower with), median size 20 parts, the magnesium oxide that is 10 μm, the median size aluminium nitride 75 parts that is 3 μm, median size be 45 parts, the aluminum oxide of 15 μm, add dispersion machine respectively and mix 0.8h in dispersion machine, after dewatered drying under guarantee anhydrous condition, in dispersion machine, add tetraethoxy 10 parts again, 2-ethyl hexyl oxy titanic acid ester 0.25 part, median size be 5 parts, zinc oxide, the nano titanium oxide 3 parts of 1 μm, after mixing component A is for subsequent use;
Take the α that number-average molecular weight is 186, ω-vinyldimethicone 100 parts and Platinic chloride-3.5 parts, tetramethyl divinyl disiloxane complex compound, obtain B component after mixing for subsequent use;
Taking mass ratio is that the component A of 1:0.35 mixes rear deaeration in anhydrous conditions with B component, at room temperature after moisture solidification 2.5h, more at room temperature solidifies 5h further, the heat-conducting silicon rubber of high electric insulation intensity.
After tested, its thermal conductivity is 0.92(W/ (mk)), electric simulation strength represents with breaking down field strength, is 26.0(kV/mm).
Embodiment three
Take the α that hydrogen content is 0.59%, the hydrogeneous polydimethylsiloxane of omega end hydroxyl takes 100 parts of (quality, lower same), median size is 20 parts, the magnesium oxide of 10 μm, median size is the aluminium nitride 120 parts of 3 μm, median size is 60 parts, the aluminum oxide of 15 μm, add dispersion machine respectively and mix 1h in dispersion machine, after dewatered drying, in anhydrous conditions, tetramethoxy-silicane 6 parts is added again in dispersion machine, two (acetylacetone based) isopropoxy titanic acid ester 0.4 part, median size is 6 parts, the zinc oxide of 1 μm, nano aluminium oxide 2 parts, nano titanium oxide 2 parts, component A is obtained for subsequent use after mixing,
Take the α that number-average molecular weight is 1888, ω-vinyldimethicone 100 parts and Platinic chloride-3.7 parts, tetramethyl divinyl disiloxane complex compound, obtain B component after mixing for subsequent use;
Take component A and B component that mass ratio is 1:13, mix rear deaeration in anhydrous conditions, at room temperature after moisture solidification 4h, then heat 1h at 70 DEG C, the heat-conducting silicon rubber of high electric insulation intensity.
After tested, its thermal conductivity is 1.23(W/ (mk)), electric simulation strength represents with breaking down field strength, is 26.4(kV/mm).
Embodiment four
Take the α that hydrogen content is 0.91%, the hydrogeneous polydimethylsiloxane of omega end hydroxyl takes 100 parts of (quality, lower with), median size 5 parts, the magnesium oxide that is 5 μm, median size 20 parts, the magnesium oxide that is 10 μm, median size be the aluminium nitride 137 parts of 3 μm, add dispersion machine respectively and mix 0.6h in dispersion machine, after dewatered drying under guarantee anhydrous condition, in dispersion machine, add tetraethoxysilane 18 parts again, titanium isopropylate 0.35 part, median size be 3 parts, zinc oxide, the nano silicon 4 parts of 1 μm, after mixing component A is for subsequent use;
Take the α that number-average molecular weight is 482, ω-vinyldimethicone 100 parts and Platinic chloride-4.2 parts, tetramethyl divinyl disiloxane complex compound, obtain B component after mixing for subsequent use;
Take component A and B component that mass ratio is 1:3.7, mix rear deaeration in anhydrous conditions and obtain first product, by first product at room temperature after moisture solidification 2.5h, then heat 1h at 100 DEG C, the heat-conducting silicon rubber of high electric insulation intensity.
After tested, its thermal conductivity is 1.04(W/ (mk)), electric simulation strength represents with breaking down field strength, is 28.3(kV/mm).
Embodiment five
Take the α that hydrogen content is 1.38%, the hydrogeneous polydimethylsiloxane of omega end hydroxyl takes 100 parts of (quality, lower with), median size 15 parts, the magnesium oxide that is 10 μm, median size 160 parts, the aluminum oxide that is 15 μm, add dispersion machine respectively and mix 0.6h in dispersion machine, after dewatered drying under guarantee anhydrous condition, add methyltrimethoxy silane 9 parts, two (methyl aceto acetate base) diisopropoxy titanic acid ester 0.35 part, nano silicon 7 parts again, obtain component A after mixing for subsequent use;
Take the α that number-average molecular weight is 334, ω-vinyldimethicone 100 parts and Platinic chloride-5 parts, tetramethyl divinyl disiloxane complex compound, obtain B component after mixing for subsequent use;
Take component A and B component that mass ratio is 1:9.6, mix rear deaeration in anhydrous conditions, at room temperature after moisture solidification 2.5h, more at room temperature solidify 7h further, the heat-conducting silicon rubber of high electric insulation intensity.
After tested, its thermal conductivity is 1.19(W/ (mk)), electric simulation strength represents with breaking down field strength, is 28.6(kV/mm).
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement or improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. a heat-conducting silicon rubber for high electric insulation intensity, is characterized in that, this silicon rubber is made up of according to mass ratio 1:0.1-1:15 component A and B component;
Described component A is made up of the raw material of following mass parts:
α, the hydrogeneous polydimethylsiloxane of omega end hydroxyl 100 parts
Silane coupling agent 5-15 part
Catalyzer I 0.05-5 part
Heat-conductive insulation filling 100-200 part
Anti-sedimentation agent 5-15 part
Described B component is made up of the raw material of following mass parts:
Lower molecular weight α, ω-vinyldimethicone 100 parts
Catalyst II 0.5-5 part.
2. the heat-conducting silicon rubber of a kind of high electric insulation intensity according to claim 1, is characterized in that, the α in described component A, the hydrogeneous polydimethylsiloxane of omega end hydroxyl, and its hydrogen content is 0.12-1.65%.
3. the heat-conducting silicon rubber of a kind of high electric insulation intensity according to claim 1, it is characterized in that, silane coupling agent in described component A adopt in tetramethoxy-silicane, methyltrimethoxy silane, tetraethoxy, tetraethoxysilane one or more.
4. the heat-conducting silicon rubber of a kind of high electric insulation intensity according to claim 1, it is characterized in that, the catalyzer I in described component A adopt in 2-ethyl hexyl oxy titanic acid ester, two (acetylacetone based) isopropoxy titanic acid ester, two (methyl aceto acetate base) diisopropoxy titanic acid ester, titanium isopropylate one or more.
5. the heat-conducting silicon rubber of a kind of high electric insulation intensity according to claim 1, is characterized in that, heat-conductive insulation filling in described component A adopt in the micron order magnesium oxide of different-grain diameter, aluminium nitride, aluminum oxide one or more.
6. the heat-conducting silicon rubber of a kind of high electric insulation intensity according to claim 1, is characterized in that, the anti-sedimentation agent in described component A is one or more in micron order zinc oxide, nano titanium oxide, nano silicon or nano aluminium oxide.
7. the heat-conducting silicon rubber of a kind of high electric insulation intensity according to claim 1, is characterized in that, the lower molecular weight α in described B component, ω-vinyldimethicone, and its number-average molecular weight is 186-2000.
8. the heat-conducting silicon rubber of a kind of high electric insulation intensity according to claim 1, is characterized in that, the catalyst II in described B component adopts Platinic chloride-tetramethyl divinyl disiloxane complex compound.
9. a preparation method for the heat-conducting silicon rubber of high electric insulation intensity described in any one of claim 1-8, is characterized in that, specifically comprise the following steps:
(1) preparation of component A: by mass parts, take 100 parts of above-mentioned α, the hydrogeneous polydimethylsiloxane of omega end hydroxyl, 100-200 part heat-conductive insulation filling mix 0.5-1h in dispersion machine, after dewatered drying, add 5-15 part silane coupling agent, 0.05-5 part catalyzer I, 5-15 part anti-sedimentation agent under anhydrous condition again, mix;
(2) preparation of B component: take mass parts 100 parts of lower molecular weight α, ω-vinyldimethicone, 0.5-5 part catalyst II, mix;
(3) preparation of silicon rubber: the B component that component A step (1) obtained respectively and step (2) obtain is the ratio of 1:0.1-1:15 in mass ratio, mix rear deaeration in anhydrous conditions and obtain first product, by first product at room temperature through the condensation cured 2-5h of moisture, further at room temperature addition curing 3-7h or at 50-120 DEG C addition curing 0.5-2h, the heat-conducting silicon rubber of high electric insulation intensity.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106189255A (en) * | 2016-07-22 | 2016-12-07 | 江阴市驰誉电力科技有限公司 | Electrically insulating silicone rubber and jumper clamp insulation protective hood prepared therefrom |
| CN107022101A (en) * | 2017-06-01 | 2017-08-08 | 广州新诚生物科技有限公司 | Massage unit and its preparation method and application |
| CN109054392A (en) * | 2018-05-28 | 2018-12-21 | 佛山市三水铠潮材料科技有限公司 | A kind of high thermal conductive silicon rubber composition |
| CN109912979A (en) * | 2019-01-28 | 2019-06-21 | 深圳市博恩实业有限公司 | Heat conductive flame-retarding foaming sealing material and preparation method thereof for 5G communication |
| CN110719939A (en) * | 2017-05-31 | 2020-01-21 | 迈图高新材料日本合同公司 | Thermally conductive silicone composition |
| CN111620998A (en) * | 2020-06-09 | 2020-09-04 | 黎哲华 | High-insulation silicone oil-boron nitride modified polyurethane material and preparation method thereof |
| CN113604051A (en) * | 2021-08-20 | 2021-11-05 | 凤阳加松新型材料科技有限公司 | Vulcanized silica gel pad and manufacturing method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106189255A (en) * | 2016-07-22 | 2016-12-07 | 江阴市驰誉电力科技有限公司 | Electrically insulating silicone rubber and jumper clamp insulation protective hood prepared therefrom |
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| CN107022101A (en) * | 2017-06-01 | 2017-08-08 | 广州新诚生物科技有限公司 | Massage unit and its preparation method and application |
| CN109054392A (en) * | 2018-05-28 | 2018-12-21 | 佛山市三水铠潮材料科技有限公司 | A kind of high thermal conductive silicon rubber composition |
| CN109912979A (en) * | 2019-01-28 | 2019-06-21 | 深圳市博恩实业有限公司 | Heat conductive flame-retarding foaming sealing material and preparation method thereof for 5G communication |
| CN111620998A (en) * | 2020-06-09 | 2020-09-04 | 黎哲华 | High-insulation silicone oil-boron nitride modified polyurethane material and preparation method thereof |
| CN113604051A (en) * | 2021-08-20 | 2021-11-05 | 凤阳加松新型材料科技有限公司 | Vulcanized silica gel pad and manufacturing method thereof |
| CN113604051B (en) * | 2021-08-20 | 2022-09-16 | 凤阳加松新型材料科技有限公司 | Vulcanized silica gel pad and manufacturing method thereof |
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