CN111205816A - Gray organic silicon rubber and preparation process thereof - Google Patents

Gray organic silicon rubber and preparation process thereof Download PDF

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Publication number
CN111205816A
CN111205816A CN202010186567.8A CN202010186567A CN111205816A CN 111205816 A CN111205816 A CN 111205816A CN 202010186567 A CN202010186567 A CN 202010186567A CN 111205816 A CN111205816 A CN 111205816A
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vinyl
gray
silicone rubber
carbon black
trimethoxy silane
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Inventor
罗清婵
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Huizhou Sandao New Material Co ltd
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Huizhou Sandao New Material Co ltd
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Priority to CN202010186567.8A priority Critical patent/CN111205816A/en
Publication of CN111205816A publication Critical patent/CN111205816A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00Adhesives based on 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; Adhesives based on derivatives of such polymers
    • C09J183/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/06Non-macromolecular additives organic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08Macromolecular additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer 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

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention relates to the technical field of sealants, in particular to gray organic silicon rubber and a preparation process thereof, wherein the gray organic silicon rubber comprises the following raw materials in percentage by weight: 39-40% of base rubber; 12-13% of a cross-linking agent; 0.5 to 3 percent of silane coupling agent; 45-46% of filler; 1.0-1.5% of carbon black, 0.1-0.3% of inhibitor and 0.5-1.0% of platinum catalyst, wherein the gray organic silicon rubber is a single-component room temperature curing quick-drying type silicon rubber sealant, is specially designed for application requiring good adhesion, has excellent physical properties and is free from corrosion; the oxime-removed product has excellent physical property and adhesive property, and particularly has good adhesive property to plastics and a plurality of other substrates; the glue is ready-to-use glue, and the tube package can be subjected to manual glue dispensing or pneumatic glue dispensing. Can also provide a general barrel package on the dispensing equipment, and has wide application; the adhesive has the advantages of good adhesion without primer, no pungent smell, simple preparation and low cost.

Description

Gray organic silicon rubber and preparation process thereof
Technical Field
The invention relates to the technical field of sealants, in particular to gray organic silicon rubber and a preparation process thereof.
Background
Silicone rubber is one of the most important silicone products, and its excellent properties are mainly derived from the chemical structure of linear polysiloxane, i.e., excellent thermal oxidation stability, weather resistance, and good electrical properties due to the main chain consisting of Si-O-Si bonds. Silicone rubbers are mainly classified into two types, a condensation reaction type silicone rubber and an addition reaction type silicone rubber, according to the vulcanization mechanism. The condensed silicone rubber is prepared by using hydroxy-terminated polydimethylsiloxane as a basic polymer, mixing with a multifunctional cross-linking agent, a catalyst, a filler and an additive, and then performing moisture absorption and cross-linking at room temperature to obtain an elastomer; the addition type silicone rubber takes polysiloxane containing vinyl as a basic polymer, takes hydrogen-containing polysiloxane as a cross-linking agent, and generates hydrosilation reaction under the action of a platinum catalyst to be cross-linked into an elastomer. Compared with condensed silicone rubber, the addition type vulcanized silicone rubber has the advantages of no byproduct generated in curing and crosslinking reaction, deep vulcanization, controllable operation time, allowance of large-scale continuous operation construction, excellent dielectric property, low linear shrinkage rate and the like. Therefore, the epoxy resin is often used as a packaging material for electrical components to prevent moisture, dust, vibration and the like from damaging electronic components.
The addition type silicone rubber has single-component and multi-component components, and compared with the multi-component silicone rubber, the single-component silicone rubber is simple to operate and does not need special mechanical equipment for mixing and gluing. However, the single-component addition type silicone rubber has poor storage stability and generally needs low-temperature storage and transportation, so the storage and transportation cost requirement is higher. At present, the research aiming at the storage stability mainly aims at selecting a proper inhibitor to investigate the inhibition effect of the inhibitor on the hydrosilylation in the storage process, and reports on the optimization of a filler system and the change of the adhesiveness before and after storage are very rare.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the gray organic silicon rubber which has the advantages of good sealing property, strong adhesion, excellent physical property, no corrosion, good adhesion without primer coat, no pungent smell, simple preparation and low required cost and the preparation process thereof.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a gray silicone rubber comprises the following raw materials in percentage by weight: 39-40% of base rubber; 12-13% of a cross-linking agent; 0.5 to 3 percent of silane coupling agent; 45-46% of filler; 1.0 to 1.5 percent of carbon black, 0.1 to 0.3 percent of inhibitor and 0.5 to 1.0 percent of platinum catalyst.
Further, the base gum is vinyl-terminated polydialkylsiloxane, wherein the alkyl group comprises hydroxyl, methyl, vinyl, phenyl and trifluoropropyl.
Further, the viscosity of the vinyl silicone oil is 8000-10000mPa.s, and the vinyl content is 0.5-1.0%.
Furthermore, the cross-linking agent is hydrogen-terminated polydialkylsiloxane, wherein alkyl comprises hydroxyl, methyl, vinyl, phenyl and trifluoropropyl, and the hydrogen content is 0.02-0.8% or 0.4-1.2% of one of branched-chain type hydrogen-containing silicone oil.
Further, the silane coupling agent comprises vinyltrimethoxysilane and/or 3- (2, 3-glycidoxy) propyltrimethoxysilane and/or r-aminopropyltriethoxysilane and/or r-methacryloxypropyltrimethoxysilane.
Further, the inhibitor comprises ethynylcyclohexanol and/or vinyl ring and/or 1.3 methylbutynol.
Further, the filler is silica micropowder and/or precipitated white carbon black and/or hydrophobic gas-phase white carbon black and/or kaolin and/or mica powder.
Further, the platinum catalyst is chloroplatinic acid propanol solution and/or vinyl double-sealed platinum complex.
A preparation process of gray silicone rubber comprises the following steps:
s1, uniformly mixing and kneading the base rubber vinyl silicone oil, the filler silicon dioxide and the carbon black into a dough in a planetary stirrer according to the proportion, performing vacuum kneading for 4-8 hours, discharging and cooling for later use;
s2, mixing a silane coupling agent of vinyl trimethoxy silane, an adhesion promoter of 3- (2, 3-epoxypropoxy) propyl trimethoxy silane and an inhibitor into the base material for 15-30 min;
and S3, adding hydrogen-containing silicone oil and a platinum catalyst, mixing uniformly for 15-30min, and filling.
In conclusion, the invention has the advantages that:
1. the gray organic silicon rubber is a single-component room temperature curing quick-drying type silicon rubber sealant, is specially designed for application requiring good adhesion, has excellent physical properties and is free from corrosion;
2. the oxime-removed product has excellent physical property and adhesive property, and particularly has good adhesive property to plastics and a plurality of other substrates;
3. the glue is ready-to-use glue, and the tube package can be subjected to manual glue dispensing or pneumatic glue dispensing. Can also provide a general barrel package on the dispensing equipment, and has wide application;
4. the adhesive has the advantages of good adhesion without primer, no pungent smell, simple preparation and low required cost.
Detailed Description
The invention will be further described with reference to specific embodiments:
the first embodiment is as follows:
a gray silicone rubber comprises the following raw materials in percentage by weight: 39% of base rubber; 13% of a cross-linking agent; 1.3% of a silane coupling agent; 45% of filler; 1.0% of carbon black, 0.1% of inhibitor and 0.6% of platinum catalyst.
Wherein the base adhesive is vinyl-terminated polydialkylsiloxane, wherein the alkyl comprises hydroxyl, methyl, vinyl, phenyl and trifluoropropyl.
Wherein the viscosity of the vinyl silicone oil is 8000-10000mPa.s, and the vinyl content is 0.5-1.0%.
Wherein the cross-linking agent is hydrogen-terminated polydialkylsiloxane, wherein alkyl comprises hydroxyl, methyl, vinyl, phenyl and trifluoropropyl, and the hydrogen content is 0.02-0.8% or 0.4-1.2% of one of branched-chain type hydrogen-containing silicone oil.
Wherein the silane coupling agent comprises vinyl trimethoxy silane and/or 3- (2, 3-epoxypropoxy) propyl trimethoxy silane and/or r-aminopropyl triethoxy silane and/or r-methacryloxypropyl trimethoxy silane.
Wherein the inhibitor comprises ethynylcyclohexanol and/or vinyl ring and/or 1.3 methylbutynol.
Wherein, the filler is silica micropowder and/or precipitation white carbon black and/or hydrophobic gas phase white carbon black and/or kaolin and/or mica powder.
Wherein the platinum catalyst is chloroplatinic acid propanol solution and/or vinyl double-sealed platinum complex.
A preparation process of gray silicone rubber comprises the following steps:
s1, uniformly mixing and kneading the base rubber vinyl silicone oil, the filler silicon dioxide and the carbon black into a dough in a planetary stirrer according to the proportion, performing vacuum kneading for 4-8 hours, discharging and cooling for later use;
s2, mixing a silane coupling agent of vinyl trimethoxy silane, an adhesion promoter of 3- (2, 3-epoxypropoxy) propyl trimethoxy silane and an inhibitor into the base material for 30 min;
and S3, adding hydrogen-containing silicone oil and a platinum catalyst, mixing uniformly for 30min, and filling.
Example two:
a gray silicone rubber comprises the following raw materials in percentage by weight: 39.5 percent of base rubber; 12.5% of a cross-linking agent; 1.4% of a silane coupling agent; 45% of filler; 1.0% of carbon black, 0.1% of inhibitor and 0.5% of platinum catalyst.
Wherein the base adhesive is vinyl-terminated polydialkylsiloxane, wherein the alkyl comprises hydroxyl, methyl, vinyl, phenyl and trifluoropropyl.
Wherein the viscosity of the vinyl silicone oil is 8000-10000mPa.s, and the vinyl content is 0.5-1.0%.
Wherein the cross-linking agent is hydrogen-terminated polydialkylsiloxane, wherein alkyl comprises hydroxyl, methyl, vinyl, phenyl and trifluoropropyl, and the hydrogen content is 0.02-0.8% or 0.4-1.2% of one of branched-chain type hydrogen-containing silicone oil.
Wherein the silane coupling agent comprises vinyl trimethoxy silane and/or 3- (2, 3-epoxypropoxy) propyl trimethoxy silane and/or r-aminopropyl triethoxy silane and/or r-methacryloxypropyl trimethoxy silane.
Wherein the inhibitor comprises ethynylcyclohexanol and/or vinyl ring and/or 1.3 methylbutynol.
Wherein, the filler is silica micropowder and/or precipitation white carbon black and/or hydrophobic gas phase white carbon black and/or kaolin and/or mica powder.
Wherein the platinum catalyst is chloroplatinic acid propanol solution and/or vinyl double-sealed platinum complex.
A preparation process of gray silicone rubber comprises the following steps:
s1, uniformly mixing and kneading the base rubber vinyl silicone oil, the filler silicon dioxide and the carbon black into a dough in a planetary stirrer according to the proportion, performing vacuum kneading for 4-8 hours, discharging and cooling for later use;
s2, mixing a silane coupling agent of vinyl trimethoxy silane, an adhesion promoter of 3- (2, 3-epoxypropoxy) propyl trimethoxy silane and an inhibitor into the base material for 30 min;
and S3, adding hydrogen-containing silicone oil and a platinum catalyst, mixing uniformly for 30min, and filling.
Example three:
a gray silicone rubber comprises the following raw materials in percentage by weight: 40% of base rubber; 12% of a cross-linking agent; 1.1% of a silane coupling agent; 45% of filler; 1.0% of carbon black, 0.1% of inhibitor and 0.8% of platinum catalyst.
Wherein the base adhesive is vinyl-terminated polydialkylsiloxane, wherein the alkyl comprises hydroxyl, methyl, vinyl, phenyl and trifluoropropyl.
Wherein the viscosity of the vinyl silicone oil is 8000-10000mPa.s, and the vinyl content is 0.5-1.0%.
Wherein the cross-linking agent is hydrogen-terminated polydialkylsiloxane, wherein alkyl comprises hydroxyl, methyl, vinyl, phenyl and trifluoropropyl, and the hydrogen content is 0.02-0.8% or 0.4-1.2% of one of branched-chain type hydrogen-containing silicone oil.
Wherein the silane coupling agent comprises vinyl trimethoxy silane and/or 3- (2, 3-epoxypropoxy) propyl trimethoxy silane and/or r-aminopropyl triethoxy silane and/or r-methacryloxypropyl trimethoxy silane.
Wherein the inhibitor comprises ethynylcyclohexanol and/or vinyl ring and/or 1.3 methylbutynol.
Wherein, the filler is silica micropowder and/or precipitation white carbon black and/or hydrophobic gas phase white carbon black and/or kaolin and/or mica powder.
Wherein the platinum catalyst is chloroplatinic acid propanol solution and/or vinyl double-sealed platinum complex.
A preparation process of gray silicone rubber comprises the following steps:
s1, uniformly mixing and kneading the base rubber vinyl silicone oil, the filler silicon dioxide and the carbon black into a dough in a planetary stirrer according to the proportion, performing vacuum kneading for 4-8 hours, discharging and cooling for later use;
s2, mixing a silane coupling agent of vinyl trimethoxy silane, an adhesion promoter of 3- (2, 3-epoxypropoxy) propyl trimethoxy silane and an inhibitor into the base material for 30 min;
and S3, adding hydrogen-containing silicone oil and a platinum catalyst, mixing uniformly for 30min, and filling.
Example four:
a gray silicone rubber comprises the following raw materials in percentage by weight: 39.7 percent of base rubber; 12.3% of a cross-linking agent; 1.1% of a silane coupling agent; 45.3 percent of filler; 1.0% of carbon black, 0.1% of inhibitor and 0.5% of platinum catalyst.
Wherein the base adhesive is vinyl-terminated polydialkylsiloxane, wherein the alkyl comprises hydroxyl, methyl, vinyl, phenyl and trifluoropropyl.
Wherein the viscosity of the vinyl silicone oil is 8000-10000mPa.s, and the vinyl content is 0.5-1.0%.
Wherein the cross-linking agent is hydrogen-terminated polydialkylsiloxane, wherein alkyl comprises hydroxyl, methyl, vinyl, phenyl and trifluoropropyl, and the hydrogen content is 0.02-0.8% or 0.4-1.2% of one of branched-chain type hydrogen-containing silicone oil.
Wherein the silane coupling agent comprises vinyl trimethoxy silane and/or 3- (2, 3-epoxypropoxy) propyl trimethoxy silane and/or r-aminopropyl triethoxy silane and/or r-methacryloxypropyl trimethoxy silane.
Wherein the inhibitor comprises ethynylcyclohexanol and/or vinyl ring and/or 1.3 methylbutynol.
Wherein, the filler is silica micropowder and/or precipitation white carbon black and/or hydrophobic gas phase white carbon black and/or kaolin and/or mica powder.
Wherein the platinum catalyst is chloroplatinic acid propanol solution and/or vinyl double-sealed platinum complex.
A preparation process of gray silicone rubber comprises the following steps:
s1, uniformly mixing and kneading the base rubber vinyl silicone oil, the filler silicon dioxide and the carbon black into a dough in a planetary stirrer according to the proportion, performing vacuum kneading for 4-8 hours, discharging and cooling for later use;
s2, mixing a silane coupling agent of vinyl trimethoxy silane, an adhesion promoter of 3- (2, 3-epoxypropoxy) propyl trimethoxy silane and an inhibitor into the base material for 30 min;
and S3, adding hydrogen-containing silicone oil and a platinum catalyst, mixing uniformly for 30min, and filling.
In conclusion, the gray organic silicon rubber is a single-component room temperature curing quick-drying type silicon rubber sealant, is specially designed for application requiring good adhesion, has excellent physical properties and is non-corrosive;
the oxime-removed product has excellent physical property and adhesive property, and particularly has good adhesive property to plastics and a plurality of other substrates;
the glue is ready-to-use glue, and the tube package can be subjected to manual glue dispensing or pneumatic glue dispensing. Can also provide a general barrel package on the dispensing equipment, and has wide application;
the adhesive has the advantages of good adhesion without primer, no pungent smell, simple preparation and low required cost.
Various other changes and modifications to the above embodiments and concepts will become apparent to those skilled in the art, and all such changes and modifications are intended to be included within the scope of the present invention as defined in the appended claims.

Claims (9)

1. A gray silicone rubber characterized by: comprises the following raw materials in percentage by weight: 39-40% of base rubber; 12-13% of a cross-linking agent; 0.5 to 3 percent of silane coupling agent; 45-46% of filler; 1.0 to 1.5 percent of carbon black, 0.1 to 0.3 percent of inhibitor and 0.5 to 1.0 percent of platinum catalyst.
2. A silicone adhesive according to claim 1, wherein: the base glue is vinyl-terminated polydialkylsiloxane, wherein alkyl comprises hydroxyl, methyl, vinyl, phenyl and trifluoropropyl.
3. A gray silicone rubber according to claim 2, wherein: the viscosity of the vinyl silicone oil is 8000-10000mPa.s, and the vinyl content is 0.5-1.0%.
4. A gray silicone rubber according to claim 1, wherein: the cross-linking agent is hydrogen-terminated polydialkylsiloxane, wherein alkyl comprises hydroxyl, methyl, vinyl, phenyl and trifluoropropyl, and the hydrogen content is 0.02-0.8% or 0.4-1.2% of one of branched-chain type hydrogen-containing silicone oil.
5. A gray silicone rubber according to claim 1, wherein: the silane coupling agent comprises vinyl trimethoxy silane and/or 3- (2, 3-epoxypropoxy) propyl trimethoxy silane and/or r-aminopropyl triethoxy silane and/or r-methacryloxypropyl trimethoxy silane.
6. A gray silicone rubber according to claim 1, wherein: the inhibitor comprises ethynylcyclohexanol and/or vinylcyclo and/or 1.3 methylbutynol.
7. A gray silicone rubber according to claim 1, wherein: the filler is silica micropowder and/or precipitation white carbon black and/or hydrophobic gas phase white carbon black and/or kaolin and/or mica powder.
8. A gray silicone rubber according to claim 1, wherein: the platinum catalyst is chloroplatinic acid propanol solution and/or vinyl double-sealed platinum complex.
9. A process for preparing a gray silicone rubber according to any of claims 1 to 8, wherein: the method comprises the following steps:
s1, uniformly mixing and kneading the base rubber vinyl silicone oil, the filler silicon dioxide and the carbon black into a dough in a planetary stirrer according to the proportion, performing vacuum kneading for 4-8 hours, discharging and cooling for later use;
s2, mixing a silane coupling agent of vinyl trimethoxy silane, an adhesion promoter of 3- (2, 3-epoxypropoxy) propyl trimethoxy silane and an inhibitor into the base material for 15-30 min;
and S3, adding hydrogen-containing silicone oil and a platinum catalyst, mixing uniformly for 15-30min, and filling.
CN202010186567.8A 2020-03-17 2020-03-17 Gray organic silicon rubber and preparation process thereof Pending CN111205816A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113861696A (en) * 2021-10-15 2021-12-31 深圳市欧普特工业材料有限公司 Cured organic silicon rubber and preparation method thereof
WO2022140877A1 (en) * 2020-12-28 2022-07-07 广州市白云化工实业有限公司 Addition-type silicone rubber having high adhesive strength and preparation method therefor

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103305012A (en) * 2013-07-11 2013-09-18 江苏天辰硅材料有限公司 One-component addition type liquid silicone rubber and preparing method thereof
CN104725869A (en) * 2014-12-17 2015-06-24 苏州锦腾电子科技有限公司 One-component addition type liquid silicone rubber used for electronics and electrics and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103305012A (en) * 2013-07-11 2013-09-18 江苏天辰硅材料有限公司 One-component addition type liquid silicone rubber and preparing method thereof
CN104725869A (en) * 2014-12-17 2015-06-24 苏州锦腾电子科技有限公司 One-component addition type liquid silicone rubber used for electronics and electrics and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022140877A1 (en) * 2020-12-28 2022-07-07 广州市白云化工实业有限公司 Addition-type silicone rubber having high adhesive strength and preparation method therefor
CN113861696A (en) * 2021-10-15 2021-12-31 深圳市欧普特工业材料有限公司 Cured organic silicon rubber and preparation method thereof

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