CN105440693A - One-component dealcoholization type heat-conducting fixing sealant and preparation method thereof - Google Patents
One-component dealcoholization type heat-conducting fixing sealant and preparation method thereof Download PDFInfo
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- CN105440693A CN105440693A CN201511009446.1A CN201511009446A CN105440693A CN 105440693 A CN105440693 A CN 105440693A CN 201511009446 A CN201511009446 A CN 201511009446A CN 105440693 A CN105440693 A CN 105440693A
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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
- C08L83/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-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
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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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
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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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
- 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
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- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
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- Adhesives Or Adhesive Processes (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention discloses a one-component dealcoholization type heat-conducting fixing sealant. The sealant comprises components in parts by weight as follows: 100 parts of 107 silicone oil, 3-8 parts of 201 silicone oil, 100-180 parts of heat-conducting filler, 0.3-2.5 parts of a silane coupling agent, 0.01-0.5 parts of a catalyst and 4-6 parts of a cross-linking agent, wherein the heat-conducting filler is a mixture of calcium carbonate, fumed silica and zinc oxide, calcium carbonate and zinc oxide are powder with the grain size of 3,000-5,000 meshes, the water content of calcium carbonate and zinc oxide is lower than 0.1%, the fumed silica is silica synthesized with a gas phase method, the water content of the fumed silica is lower than 0.6%, and zinc oxide accounts for not less than 50% of the heat-conducting filler in percentage by mass. The one-component dealcoholization type heat-conducting fixing sealant has higher hardness and higher heat-conducting coefficient while keeping the good construction performance, and further has certain flame retardance.
Description
Technical field
The present invention relates to a kind of seal gum and preparation method thereof, particularly relate to a kind of single-component dealcoholization-type heat conduction fixing seal glue and preparation method thereof.
Background technology
Single-component room-temperature-vulsilicone silicone rubber (RTV) refers to the composition at room temperature being solidify to form rubber-like elastic body by the contact with moisture in air.Depickling type, de-oxime type, dealcoholizing-type, deacetone etc. is divided into according to the micromolecular difference of release.Dealcoholizing-type low price and little to the component corrosion of electronic apparatus, therefore dealcoholizing-type RTV usage quantity and scope are progressively developing.Along with developing rapidly of integrated technology and package technique, reducing of thousands of times of the volume of electronic component, logical circuit, has higher requirement to the thermal diffusivity of material.
As thermally conductive material, US8796190 discloses heat-conducting silicon rubber composition, but it relates to is the joint sealant of heat curing-type, does not relate to room temperature vulcanized silicone rubber.The combination of traditional silicon-dioxide, magnesium oxide can make product have certain thermal conductivity, but a large amount of interpolation must increase the rising of system viscosity, causes workability to decline.And along with the development of electron trade, while the heat conduction of inevitable requirement height, good application property can be had.
Summary of the invention
For above-mentioned the deficiencies in the prior art, the object of this invention is to provide a kind of single-component dealcoholization-type heat conduction fixing seal glue and preparation method thereof, solve room temperature vulcanized silicone rubber heat conductivility and promote the problem promoting with workability and mutually restrict.
Technical scheme of the present invention is such: a kind of single-component dealcoholization-type heat conduction fixing seal glue, be made up of the component of following parts by weight: 107 silicone oil 100 parts, 201 silicone oil 3-8 parts, heat conductive filler 100-180 part, silane coupling agent 0.3-2.5 part, catalyzer 0.01-0.5 part and linking agent 4-6 part, described heat conductive filler is calcium carbonate, the mixture of gas-phase silica and zinc oxide, the particle diameter of described calcium carbonate and zinc oxide is 3000-5000 object powder and water content is less than 0.1%, described gas-phase silica is synthesized by vapor phase process and the water content silicon-dioxide that is less than 0.6%, described zinc oxide accounts for heat conductive filler by mass percentage and is not less than 50%.
Further, described 107 silicone oil are two hydroxyl-terminated injecting two methyl siloxanes of 2000-20000CP.
Further, described 201 silicone oil are 201 methyl-silicone oils of 100-1000CP.
Preferably, described silane coupling agent is at least one in KH540, KH550 and KH792.
Preferably, described catalyzer comprises etheric acid second fat inner complex and the dibutyl tin laurate of metatitanic acid isopropyl ester.
Preferably, described linking agent is at least one in methyltrimethoxy silane, vinyltrimethoxy silane and tetramethoxy-silicane.
A kind of preparation method of single-component dealcoholization-type heat conduction fixing seal glue; comprise the following steps: first 107 silicone oil, 201 silicone oil, heat conductive filler, linking agent are metered into respectively in kneader and mediate 20-30min under room temperature; vacuum state dewaters and mediates 1-1.5 hour at 100-120 DEG C; be cooled to room temperature material to be added in planet dispersion machine; add coupling agent and catalyzer respectively again; dispersing and mixing 20-30min in planet dispersion machine, finally filters under the protection of rare gas element.
The beneficial effect of technical scheme provided by the present invention is: single-component dealcoholization-type heat conduction fixing seal glue has higher hardness, thermal conductivity, also has certain fire retardancy simultaneously.Add 201 a small amount of silicone oil and adopt zinc oxide and calcium carbonate and gas-phase silica mixture as heat conductive filler, solving the problem that heat conductivility restricts mutually with workability.Dealcoholizing-type heat conduction fixing seal glue of the present invention can be widely used as in cpu heat, thyristor, heat radiation between wafer and radiator element, and iron plate dispels the heat, and the heat conduction of transformer and electronic component are fixed and filled.
Embodiment
Below in conjunction with embodiment, the invention will be further described, but not as a limitation of the invention.
Embodiment 1
Be two hydroxyl-terminated injecting two methyl siloxanes 100 parts of 8000CP by viscosity, viscosity is 201 methyl-silicone oil 4 parts of 200CP, particle diameter is 30000-5000 object powder and water content is less than 20 parts, 0.1% calcium carbonate, particle diameter is 3000-5000 object powder and water content is less than 70 parts, 0.1% zinc oxide, vapor phase process synthesis and the water content silica 10 part that is less than 0.6%, methyltrimethoxy silane 4 parts is put into kneader and mediate 20min under room temperature, vacuum degree control to be dewatered kneading 1 hour at-0.1MPA at 100 DEG C, be cooled to room temperature material is added in planet dispersion machine.Add the etheric acid second fat inner complex 0.03 part of KH5500.5 part and metatitanic acid isopropyl ester more respectively, dispersing and mixing 20min in planet dispersion machine, finally filters under the protection of rare gas element, obtains single-component dealcoholization-type heat conduction fixing seal glue.
Embodiment 2
Be two hydroxyl-terminated injecting two methyl siloxanes 100 parts of 2000CP by viscosity, viscosity is 201 methyl-silicone oil 8 parts of 100CP, particle diameter is 3000-5000 object powder and water content is less than 50 parts, 0.1% calcium carbonate, particle diameter is 3000-5000 object powder and water content is less than 100 parts, 0.1% zinc oxide, vapor phase process synthesis and water content are less than 0.6% silicon-dioxide 30 parts, vinyltrimethoxy silane 5 parts are put into kneader and mediate 25min under room temperature, vacuum state dewaters kneading 1.5 hours at 110 DEG C, is cooled to room temperature and is added in planet dispersion machine by material.Add the etheric acid second fat inner complex 0.03 part of KH5500.7 part and metatitanic acid isopropyl ester more respectively, dispersing and mixing 25min in planet dispersion machine, finally filters under the protection of rare gas element, obtains single-component dealcoholization-type heat conduction fixing seal glue.
Embodiment 3
Be two hydroxyl-terminated injecting two methyl siloxanes 100 parts of 20000CP by viscosity, viscosity is 201 methyl-silicone oil 3 parts of 1000CP, particle diameter is 3000-5000 object powder and water content is less than 25 parts, 0.1% calcium carbonate, particle diameter is 3000-5000 object powder and water content is less than 85 parts, 0.1% zinc oxide, vapor phase process synthesis and water content are less than 0.6% silicon-dioxide 27 parts, methyltrimethoxy silane 6 parts are put into kneader and mediate 30min under room temperature, vacuum state dewaters kneading 1.2 hours at 120 DEG C, is cooled to room temperature and is added in planet dispersion machine by material.Add the etheric acid second fat inner complex 0.03 part of KH5500.5 part and metatitanic acid isopropyl ester more respectively, dispersing and mixing 30min in planet dispersion machine, finally filters under the protection of rare gas element, obtains single-component dealcoholization-type heat conduction fixing seal glue.
Embodiment 4
Except tetramethoxy-silicane replaces vinyltrimethoxy silane, other technique and composition add-on are with embodiment 2.
Embodiment 5
Except KH792 replaces KH550, other technique and composition add-on are with embodiment 2.
Comparative example 1
Except do not add vapor phase process synthesis and water content is less than except the silicon-dioxide of 0.6%, other technique and composition add-on are with embodiment 2.
Single-component dealcoholization-type heat conduction fixing seal glue prepared by aforesaid method, tests its surface drying time by GB/T-13477; Extrudability test (air pressure of 0.3MPA, 3mm Jiao Zui, the quality that record 15S extrudes); UL-94 standard testing flame retardant rating; 23 ± 2 DEG C and 50 ± 5% condition under sulfuration 7 days, use conductometer test thermal conductivity; Stability in storage testing method: airtight good unvulcanized glue is put into 80 DEG C of baking oven 168h, takes out to be cooled to room temperature, test surface drying time, rate of extrusion.
Table one performance test
Single-component dealcoholization-type heat conduction fixing seal glue of the present invention, has the thermal conductivity of adjustable, good thixotropy and flame retardant resistance, is applicable to single-component packaged form.
Claims (7)
1. a single-component dealcoholization-type heat conduction fixing seal glue, it is characterized in that, sealing glue is made up of the component of following parts by weight: 107 silicone oil 100 parts, 201 silicone oil 3-8 parts, heat conductive filler 100-180 part, silane coupling agent 0.3-2.5 part, catalyzer 0.01-0.5 part and linking agent 4-6 part, described heat conductive filler is calcium carbonate, the mixture of gas-phase silica and zinc oxide, the particle diameter of described calcium carbonate and zinc oxide is 3000-5000 object powder and water content is less than 0.1%, described gas-phase silica is synthesized by vapor phase process and the water content silicon-dioxide that is less than 0.6%, described zinc oxide accounts for heat conductive filler by mass percentage and is not less than 50%.
2. single-component dealcoholization-type heat conduction fixing seal glue according to claim 1, is characterized in that: described 107 silicone oil are two hydroxyl-terminated injecting two methyl siloxanes of 2000-20000CP.
3. single-component dealcoholization-type heat conduction fixing seal glue according to claim 1, is characterized in that: described 201 silicone oil are 201 methyl-silicone oils of 100-1000CP.
4. single-component dealcoholization-type heat conduction fixing seal glue according to claim 1, is characterized in that: described silane coupling agent is at least one in KH540, KH550 and KH792.
5. single-component dealcoholization-type heat conduction fixing seal glue according to claim 1, is characterized in that: described catalyzer comprises etheric acid second fat inner complex and the dibutyl tin laurate of metatitanic acid isopropyl ester.
6. single-component dealcoholization-type heat conduction fixing seal glue according to claim 1, is characterized in that: described linking agent is at least one in methyltrimethoxy silane, vinyltrimethoxy silane and tetramethoxy-silicane.
7. the preparation method of a single-component dealcoholization-type heat conduction fixing seal glue according to claim 1; it is characterized in that comprising the following steps: first 107 silicone oil, 201 silicone oil, heat conductive filler, linking agent are metered into respectively in kneader and mediate 20-30min under room temperature; vacuum state dewaters and mediates 1-1.5 hour at 100-120 DEG C; be cooled to room temperature material to be added in planet dispersion machine; add coupling agent and catalyzer respectively again; dispersing and mixing 20-30min in planet dispersion machine, finally filters under the protection of rare gas element.
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| CN201511009446.1A CN105440693A (en) | 2015-12-29 | 2015-12-29 | One-component dealcoholization type heat-conducting fixing sealant and preparation method thereof |
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| CN201511009446.1A CN105440693A (en) | 2015-12-29 | 2015-12-29 | One-component dealcoholization type heat-conducting fixing sealant and preparation method thereof |
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106497069A (en) * | 2016-11-09 | 2017-03-15 | 金锚电力控股有限公司 | Electric insulation silicone grease |
| CN106700556A (en) * | 2016-12-26 | 2017-05-24 | 广州市白云化工实业有限公司 | Heat-dissipation silicone rubber and preparation method thereof |
| CN106833504A (en) * | 2017-02-10 | 2017-06-13 | 深圳市森日有机硅材料股份有限公司 | A kind of heat conduction single-component dealcoholization-type RTV fluid sealants and preparation method thereof |
| CN107141807A (en) * | 2017-06-22 | 2017-09-08 | 江苏赛凯诺环保科技有限公司 | A kind of organic silicone heat conduction network chain and preparation method thereof |
| CN108192349A (en) * | 2017-12-13 | 2018-06-22 | 天永诚高分子材料（常州）有限公司 | A kind of dealcoholized type room temperature vulcanized silicone rubber and preparation method thereof |
| JP2019524934A (en) * | 2016-08-03 | 2019-09-05 | ダウ シリコーンズ コーポレーション | Elastomer compositions and their uses |
| CN110305620A (en) * | 2019-07-16 | 2019-10-08 | 杭州之江新材料有限公司 | A kind of dealcoholized type heat conduction organosilicon sealant and preparation method thereof |
| CN110317581A (en) * | 2019-06-06 | 2019-10-11 | 东莞市盛元新材料科技有限公司 | A kind of pureed thermostable heat-conductive composite material and preparation method |
| CN111218115A (en) * | 2020-02-28 | 2020-06-02 | 中国电子科技集团公司第五十八研究所 | Preparation method of high-thermal-conductivity silicone sheet and high-thermal-conductivity silicone sheet |
| US10808154B2 (en) | 2016-08-03 | 2020-10-20 | Dow Silicones Corporation | Elastomeric compositions and their applications |
| US10844177B2 (en) | 2016-08-03 | 2020-11-24 | Dow Silicones Corporation | Elastomeric compositions and their applications |
| US11090253B2 (en) | 2016-08-03 | 2021-08-17 | Dow Silicones Corporation | Cosmetic composition comprising silicone materials |
| US11254847B2 (en) | 2017-05-09 | 2022-02-22 | Dow Silicones Corporation | Lamination adhesive compositions and their applications |
| US11332581B2 (en) | 2015-01-28 | 2022-05-17 | Dow Silicones Corporation | Elastomeric compositions and their applications |
| US11479022B2 (en) | 2017-05-09 | 2022-10-25 | Dow Silicones Corporation | Lamination process |
| CN115246992A (en) * | 2021-09-01 | 2022-10-28 | 上海首孚复合材料有限公司 | High-elasticity silica gel foam and application thereof |
| US11485936B2 (en) | 2016-08-03 | 2022-11-01 | Dow Silicones Corporation | Fabric care composition comprising silicone materials |
| JP7508585B2 (en) | 2020-04-28 | 2024-07-01 | 中国石油化工股▲ふん▼有限公司 | Catalyst components for olefin polymerization or copolymerization, their preparation and use |
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11332581B2 (en) | 2015-01-28 | 2022-05-17 | Dow Silicones Corporation | Elastomeric compositions and their applications |
| US11090253B2 (en) | 2016-08-03 | 2021-08-17 | Dow Silicones Corporation | Cosmetic composition comprising silicone materials |
| US10808154B2 (en) | 2016-08-03 | 2020-10-20 | Dow Silicones Corporation | Elastomeric compositions and their applications |
| US10844177B2 (en) | 2016-08-03 | 2020-11-24 | Dow Silicones Corporation | Elastomeric compositions and their applications |
| JP2019524934A (en) * | 2016-08-03 | 2019-09-05 | ダウ シリコーンズ コーポレーション | Elastomer compositions and their uses |
| US11485936B2 (en) | 2016-08-03 | 2022-11-01 | Dow Silicones Corporation | Fabric care composition comprising silicone materials |
| US10526453B2 (en) | 2016-08-03 | 2020-01-07 | Dow Silicones Corporation | Elastomeric compositions and their applications |
| CN106497069A (en) * | 2016-11-09 | 2017-03-15 | 金锚电力控股有限公司 | Electric insulation silicone grease |
| CN106700556A (en) * | 2016-12-26 | 2017-05-24 | 广州市白云化工实业有限公司 | Heat-dissipation silicone rubber and preparation method thereof |
| CN106833504A (en) * | 2017-02-10 | 2017-06-13 | 深圳市森日有机硅材料股份有限公司 | A kind of heat conduction single-component dealcoholization-type RTV fluid sealants and preparation method thereof |
| US11479022B2 (en) | 2017-05-09 | 2022-10-25 | Dow Silicones Corporation | Lamination process |
| US11254847B2 (en) | 2017-05-09 | 2022-02-22 | Dow Silicones Corporation | Lamination adhesive compositions and their applications |
| CN107141807A (en) * | 2017-06-22 | 2017-09-08 | 江苏赛凯诺环保科技有限公司 | A kind of organic silicone heat conduction network chain and preparation method thereof |
| CN108192349A (en) * | 2017-12-13 | 2018-06-22 | 天永诚高分子材料（常州）有限公司 | A kind of dealcoholized type room temperature vulcanized silicone rubber and preparation method thereof |
| CN110317581A (en) * | 2019-06-06 | 2019-10-11 | 东莞市盛元新材料科技有限公司 | A kind of pureed thermostable heat-conductive composite material and preparation method |
| CN110305620A (en) * | 2019-07-16 | 2019-10-08 | 杭州之江新材料有限公司 | A kind of dealcoholized type heat conduction organosilicon sealant and preparation method thereof |
| CN111218115A (en) * | 2020-02-28 | 2020-06-02 | 中国电子科技集团公司第五十八研究所 | Preparation method of high-thermal-conductivity silicone sheet and high-thermal-conductivity silicone sheet |
| JP7508585B2 (en) | 2020-04-28 | 2024-07-01 | 中国石油化工股▲ふん▼有限公司 | Catalyst components for olefin polymerization or copolymerization, their preparation and use |
| CN115246992A (en) * | 2021-09-01 | 2022-10-28 | 上海首孚复合材料有限公司 | High-elasticity silica gel foam and application thereof |
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