CN113801627A - Organic silicon adhesive sealant and preparation method thereof - Google Patents

Organic silicon adhesive sealant and preparation method thereof Download PDF

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Publication number
CN113801627A
CN113801627A CN202111283580.6A CN202111283580A CN113801627A CN 113801627 A CN113801627 A CN 113801627A CN 202111283580 A CN202111283580 A CN 202111283580A CN 113801627 A CN113801627 A CN 113801627A
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parts
adhesive sealant
organosilicon
heat
flame retardant
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任天斌
刘新
石祥凯
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Suzhou Datong Advanced Material Co ltd
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Suzhou Datong Advanced Material Co ltd
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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
    • C09J11/08Macromolecular additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2217Oxides; Hydroxides of metals of magnesium
    • C08K2003/222Magnesia, i.e. magnesium oxide
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2227Oxides; Hydroxides of metals of aluminium
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2296Oxides; Hydroxides of metals of zinc
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/20Applications use in electrical or conductive gadgets
    • C08L2203/206Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention discloses an organosilicon adhesive sealant and a preparation method thereof, wherein the organosilicon adhesive sealant comprises 30-50 parts of alkoxy-terminated polydimethylsiloxane, 60-100 parts of vinyl polydimethylsiloxane, 4-10 parts of organosilicon cross-linking agent, 1-5 parts of silane coupling agent, 1-3 parts of organosilicon flame retardant, 10-20 parts of heat-conducting filler, 2-5 parts of softener, 0-10 parts of color paste and 1-3 parts of platinum catalyst. After the heat-conducting filler is added, the local concentration of heat can be avoided, and further the yellowing of the sealant caused by over-heating is avoided; and due to the addition of the heat-conducting filler, the local too fast aging of the sealant can be avoided, and the tensile strength and the elongation at break are improved.

Description

Organic silicon adhesive sealant and preparation method thereof
Technical Field
The invention relates to the technical field of sealant processing, in particular to an organosilicon adhesive sealant and a preparation method thereof.
Background
With the progress and development of material science and technology, the organic silicon adhesive sealant is widely applied to electronic plates in products such as electronic appliances, automobiles, mobile phones, homes, lamp illumination, aerospace and the like.
The organosilicon adhesive sealant is sometimes in a high-temperature state in the application process, so the sealant needs to meet the requirements of high temperature resistance and yellowing resistance, and if the performance of the organosilicon sealant is not upgraded, the application and popularization of organosilicon sealing in the industries of electronic appliances, lamp illumination and the like can be limited, and the development of the industries is influenced.
Disclosure of Invention
The invention aims to provide an organic silicon adhesive sealant and a preparation method thereof, which aim to solve the problems in the background technology.
In order to achieve the purpose, the invention adopts the technical scheme that: the organosilicon adhesive sealant comprises, by weight, 30-50 parts of alkoxy-terminated polydimethylsiloxane, 60-100 parts of vinyl polydimethylsiloxane, 4-10 parts of organosilicon crosslinking agent, 1-5 parts of silane coupling agent, 1-3 parts of organosilicon flame retardant, 10-20 parts of heat-conducting filler, 2-5 parts of softener, 0-10 parts of color paste and 1-3 parts of platinum catalyst.
As a further optimization, the viscosity of the vinyl polydimethylsiloxane is 1000-5000 mPa.s.
As a further optimization, the organosilicon crosslinking agent is one or more of methyltrimethoxysilane, vinyltrimethoxysilane, methyltriethoxysilane, methyl orthosilicate and ethyl orthosilicate.
As a further optimization, the silane coupling agent is a silane coupling agent KH550 or KH 570.
As a further optimization, the organosilicon flame retardant is a polyborosiloxane flame retardant.
As a further optimization, the heat-conducting filler is one or more of multi-particle-size spherical alumina, zinc oxide and magnesium oxide; the particle size of the heat-conducting filler is 1-100 mu m. The heat-conducting filler also has excellent insulating property, mechanical property, high-temperature resistance, chemical corrosion resistance and the like.
As a further optimization, the softener is one or more of dibutyl phthalate, dioctyl phthalate and tricresyl phosphate.
As further optimization, the color paste is one or more of black color paste, white color paste and silver color paste.
The invention also provides a preparation method of the organosilicon adhesive sealant, which comprises the following steps,
s1) accurately weighing each component;
s2) adding alkoxy-terminated polydimethylsiloxane, vinyl polydimethylsiloxane, an organic silicon flame retardant, a heat-conducting filler, a softening agent and color paste into a reaction kettle, mixing and uniformly stirring to obtain a base material;
s3) adding an organosilicon crosslinking agent, a silane coupling agent and a platinum catalyst into the base material, mixing and stirring to obtain the organosilicon adhesive sealant.
As further optimization, the reaction temperature in S2 is 100-150 ℃, and the reaction time is 1-6 h; the reaction temperature in S3 is 60-100 ℃, and the reaction time is 0.5-5 h.
Compared with the prior art, the invention has the beneficial effects that:
1. by adding the heat-conducting filler, the heat conduction of the sealant can be accelerated when the sealant is heated, the heat accumulation at a certain position is avoided, and the overall heat resistance and yellowing resistance are improved;
2. by adding the organic silicon flame retardant, the compatibility of the flame-retardant raw material and the organic silicon component is better on the basis of improving the flame-retardant performance of the sealant, and the compatibility of the raw material is improved.
Detailed Description
The following are specific examples of the present invention and further describe the technical solutions of the present invention, but the present invention is not limited to these examples.
Example 1
The organic silicon adhesive sealant comprises, by weight, 38 parts of alkoxy-terminated polydimethylsiloxane, 85 parts of vinyl polydimethylsiloxane, 8 parts of methyltrimethoxysilane, 2 parts of silane coupling agent KH 5502 parts, 2 parts of polyborosiloxane flame retardant, 16 parts of alumina, 2 parts of dibutyl phthalate, 5 parts of white slurry and 1 part of platinum catalyst.
The preparation method comprises the following steps: s1) accurately weighing each component; s2) adding alkoxy-terminated polydimethylsiloxane, vinyl polydimethylsiloxane, polyborosiloxane flame retardant, aluminum oxide, dibutyl phthalate and white slurry into a reaction kettle, mixing and uniformly stirring, wherein the reaction temperature is 100 ℃ and 150 ℃, and the reaction time is 1-6h to obtain a base material; s3) adding methyltrimethoxysilane, a silane coupling agent KH550 and a platinum catalyst into the base material, mixing and stirring, wherein the reaction temperature is 60-100 ℃, and the reaction time is 0.5-5h, thus obtaining the organosilicon adhesive sealant.
Example 2
An organic silicon adhesive sealant comprises, by weight, 46 parts of alkoxy-terminated polydimethylsiloxane, 76 parts of vinyl polydimethylsiloxane, 6 parts of methyltrimethoxysilane, 3 parts of a silane coupling agent KH 5503 parts of a polyborosiloxane flame retardant, 18 parts of alumina, 3 parts of dioctyl phthalate, 8 parts of white slurry and 2 parts of a platinum catalyst.
The preparation method comprises the following steps: s1) accurately weighing each component; s2) adding alkoxy-terminated polydimethylsiloxane, vinyl polydimethylsiloxane, polyborosiloxane flame retardant, aluminum oxide, dioctyl phthalate and white slurry into a reaction kettle, mixing and uniformly stirring, wherein the reaction temperature is 100-150 ℃, and the reaction time is 1-6h to prepare a base material; s3) adding methyltrimethoxysilane, a silane coupling agent KH550 and a platinum catalyst into the base material, mixing and stirring, wherein the reaction temperature is 60-100 ℃, and the reaction time is 0.5-5h, thus obtaining the organosilicon adhesive sealant.
Example 3
An organosilicon adhesive sealant comprises, by weight, 32 parts of alkoxy-terminated polydimethylsiloxane, 82 parts of vinyl polydimethylsiloxane, 10 parts of vinyl trimethoxy silane, 3 parts of silane coupling agent KH 5503 parts of polyborosiloxane flame retardant, 12 parts of zinc oxide, 3 parts of tricresyl phosphate and 1 part of platinum catalyst.
The preparation method comprises the following steps: s1) accurately weighing each component; s2) adding alkoxy-terminated polydimethylsiloxane, vinyl polydimethylsiloxane, a polyborosiloxane flame retardant, zinc oxide and tricresyl phosphate into a reaction kettle, mixing and uniformly stirring, wherein the reaction temperature is 100-150 ℃, and the reaction time is 1-6h to obtain a base material; s3) adding vinyl trimethoxy silane, a silane coupling agent KH550 and a platinum catalyst into the base material, mixing and stirring, wherein the reaction temperature is 60-100 ℃, and the reaction time is 0.5-5h, so as to obtain the organosilicon adhesive sealant.
Example 4
An organosilicon adhesive sealant comprises, by weight, 48 parts of alkoxy-terminated polydimethylsiloxane, 72 parts of vinyl polydimethylsiloxane, 8 parts of methyltriethoxysilane, KH 5702 parts of a silane coupling agent, 2 parts of a polyborosiloxane flame retardant, 15 parts of zinc oxide, 3 parts of tricresyl phosphate, 3 parts of silver paste and 1 part of a platinum catalyst.
The preparation method comprises the following steps: s1) accurately weighing each component; s2) adding alkoxy-terminated polydimethylsiloxane, vinyl polydimethylsiloxane, a polyborosiloxane flame retardant, zinc oxide, tricresyl phosphate and silver paste into a reaction kettle, mixing and uniformly stirring, wherein the reaction temperature is 100-150 ℃, and the reaction time is 1-6h to prepare a base material; s3) adding methyl triethoxysilane, a silane coupling agent KH570 and a platinum catalyst into the base material, mixing and stirring, wherein the reaction temperature is 60-100 ℃, and the reaction time is 0.5-5h, so as to obtain the organosilicon adhesive sealant.
Example 5
An organic silicon adhesive sealant comprises, by weight, 35 parts of alkoxy-terminated polydimethylsiloxane, 80 parts of vinyl polydimethylsiloxane, 8 parts of methyl orthosilicate, KH 5702 parts of a silane coupling agent, 2 parts of a polyborosiloxane flame retardant, 15 parts of magnesium oxide, 3 parts of tricresyl phosphate, 3 parts of silver paste and 1 part of a platinum catalyst.
The preparation method comprises the following steps: s1) accurately weighing each component; s2) adding alkoxy-terminated polydimethylsiloxane, vinyl polydimethylsiloxane, polyborosiloxane flame retardant, magnesium oxide, tricresyl phosphate and silver paste into a reaction kettle, mixing and uniformly stirring, wherein the reaction temperature is 100-150 ℃, and the reaction time is 1-6h to prepare a base material; s3) adding methyl orthosilicate, a silane coupling agent KH570 and a platinum catalyst into the base material, mixing and stirring, wherein the reaction temperature is 60-100 ℃, and the reaction time is 0.5-5h, so as to obtain the organosilicon adhesive sealant.
Comparative example 1
It differs from the embodiment in that no thermally conductive filler is added.
Comparative example 2
It differs from the examples in that no silicone flame retardant was added.
Application examples
The silicone adhesive sealants of examples 1 to 5 and comparative examples 1 to 2 were tested for deep-cure rate, yellowing resistance, and strength properties, wherein: the deep curing rate is tested according to JB/T10900-2016 standard;
yellowing resistance testing procedure: 1. uniformly coating the sealant in the glass cover and at the opening, and bonding and sealing the opening and the glass plate; 2. immediately putting the mixture into a high-temperature oven for baking, controlling the temperature to be 120-150 ℃ and the time to be 24 hours; 3. and taking out the glass after baking, cooling to normal temperature, observing whether the transparent glass cover is yellowed or not, and judging whether the sealed part is 100% cohesive failure or not to be qualified.
The test data are shown in the following table,
Figure BDA0003332174040000061
according to experimental data, after the heat-conducting filler is added, the local concentration of heat can be avoided, and further the yellowing of the sealant caused by excessive heating is avoided; and due to the addition of the heat-conducting filler, the local too fast aging of the sealant can be avoided, and the tensile strength and the elongation at break are improved.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.

Claims (10)

1. The organosilicon adhesive sealant is characterized by comprising, by weight, 30-50 parts of alkoxy-terminated polydimethylsiloxane, 60-100 parts of vinyl polydimethylsiloxane, 4-10 parts of organosilicon cross-linking agent, 1-5 parts of silane coupling agent, 1-3 parts of organosilicon flame retardant, 10-20 parts of heat-conducting filler, 2-5 parts of softener, 0-10 parts of color paste and 1-3 parts of platinum catalyst.
2. The silicone adhesive sealant of claim 1 wherein the viscosity of the vinyl polydimethylsiloxane is 1000-.
3. The silicone bonding sealant of claim 1, wherein the silicone crosslinker is one or more of methyltrimethoxysilane, vinyltrimethoxysilane, methyltriethoxysilane, methyl orthosilicate, and ethyl orthosilicate.
4. The silicone adhesive sealant according to claim 1 wherein the silane coupling agent is the silane coupling agent KH550 or KH 570.
5. The silicone adhesive sealant of claim 1 wherein the silicone flame retardant is a polyborosiloxane flame retardant.
6. The silicone adhesive sealant of claim 1 wherein the thermally conductive filler is one or more of multi-particle size spherical alumina, zinc oxide, magnesium oxide; the particle size of the heat-conducting filler is 1-100 mu m.
7. The silicone adhesive sealant according to claim 1 wherein the softening agent is one or more of dibutyl phthalate, dioctyl phthalate, tricresyl phosphate.
8. The silicone adhesive sealant according to claim 1 wherein the color paste is one or more of a black paste, a white paste and a silver paste.
9. A method of preparing the silicone adhesive sealant according to any one of claims 1 to 8 comprising the steps of,
s1) accurately weighing each component;
s2) adding alkoxy-terminated polydimethylsiloxane, vinyl polydimethylsiloxane, an organic silicon flame retardant, a heat-conducting filler, a softening agent and color paste into a reaction kettle, mixing and uniformly stirring to obtain a base material;
s3) adding an organosilicon crosslinking agent, a silane coupling agent and a platinum catalyst into the base material, mixing and stirring to obtain the organosilicon adhesive sealant.
10. The method for preparing the organosilicon adhesive sealant according to claim 9, wherein the reaction temperature in S2 is 100-150 ℃, and the reaction time is 1-6 h; the reaction temperature in S3 is 60-100 ℃, and the reaction time is 0.5-5 h.
CN202111283580.6A 2021-11-01 2021-11-01 Organic silicon adhesive sealant and preparation method thereof Pending CN113801627A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102009002231A1 (en) * 2009-04-06 2010-10-07 Wacker Chemie Ag Self-adherent Pt-catalyzed addition-crosslinking silicone compositions at room temperature
CN102516928A (en) * 2011-12-20 2012-06-27 江苏明昊新材料科技有限公司 Silicone sealant used for electronic products, preparation method thereof, and application thereof
CN103146340A (en) * 2013-03-06 2013-06-12 广州市高士实业有限公司 Low-viscosity high-heat-conductivity organic silicon electronic pouring sealant and preparation method thereof
CN105086927A (en) * 2015-08-07 2015-11-25 东莞市新星有机硅科技有限公司 Inorganic nano-filler modified silicone pressure-sensitive adhesive and preparation method thereof
US20190194508A1 (en) * 2017-12-26 2019-06-27 Nano And Advanced Materials Institute Limited Room temperature curable polyoranopolysloxane silicone sealant composition, the silicone sealant and method for preparing thereof
CN112724921A (en) * 2020-12-25 2021-04-30 杭州之江新材料有限公司 Low-viscosity heat-conducting flame-retardant silicone rubber sealant and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102009002231A1 (en) * 2009-04-06 2010-10-07 Wacker Chemie Ag Self-adherent Pt-catalyzed addition-crosslinking silicone compositions at room temperature
CN102516928A (en) * 2011-12-20 2012-06-27 江苏明昊新材料科技有限公司 Silicone sealant used for electronic products, preparation method thereof, and application thereof
CN103146340A (en) * 2013-03-06 2013-06-12 广州市高士实业有限公司 Low-viscosity high-heat-conductivity organic silicon electronic pouring sealant and preparation method thereof
CN105086927A (en) * 2015-08-07 2015-11-25 东莞市新星有机硅科技有限公司 Inorganic nano-filler modified silicone pressure-sensitive adhesive and preparation method thereof
US20190194508A1 (en) * 2017-12-26 2019-06-27 Nano And Advanced Materials Institute Limited Room temperature curable polyoranopolysloxane silicone sealant composition, the silicone sealant and method for preparing thereof
CN112724921A (en) * 2020-12-25 2021-04-30 杭州之江新材料有限公司 Low-viscosity heat-conducting flame-retardant silicone rubber sealant and preparation method thereof

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编辑委员会: "《化工百科全书》", 31 August 1996 *

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