CN106633915A - Highly flame-retardant halogen-free environment-friendly silicone rubber and preparation method thereof - Google Patents

Highly flame-retardant halogen-free environment-friendly silicone rubber and preparation method thereof Download PDF

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Publication number
CN106633915A
CN106633915A CN201611217540.0A CN201611217540A CN106633915A CN 106633915 A CN106633915 A CN 106633915A CN 201611217540 A CN201611217540 A CN 201611217540A CN 106633915 A CN106633915 A CN 106633915A
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silicon rubber
free
parts
flame
retardanthalogen
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罗晓锋
查若愚
黄强
王有治
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CHENGDU GUIBAO SCIENCE AND TECHNOLOGY INDUSTRIAL Co Ltd
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CHENGDU GUIBAO SCIENCE AND TECHNOLOGY INDUSTRIAL Co Ltd
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Priority to CN201611217540.0A priority Critical patent/CN106633915A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00Compositions 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
    • C08L83/04Polysiloxanes
    • 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
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/006Additives being defined by their surface area
    • 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
    • C08K2201/00Specific properties of additives
    • C08K2201/014Additives containing two or more different additives of the same subgroup in C08K
    • 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
    • C08L2201/22Halogen free composition
    • 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

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses highly flame-retardant halogen-free environment-friendly silicone rubber and a preparation method thereof. The silicone rubber comprises the following raw materials in parts by mass: 100 parts of silicone rubber, 20-60 parts of white carbon black, 20-150 parts of fillers, 10-60 parts of flame retardants, 3-7 parts of hydroxyl silicone oil, 2-5 parts of a silane coupling agent and 0.5-1.5 parts of a vulcanizing agent. Due to actual detection, the product disclosed by the invention has excellent flame-retardant property, has a limit oxygen index of more than 48% and a vertical burning level of FV-0 and is free of halogen and environmentally friendly.

Description

High-flame-retardanthalogen-free halogen-free environmental protection silicon rubber and preparation method thereof
Technical field
The invention belongs to high-temperature silicon disulfide rubber Material Field, and in particular to a kind of high-flame-retardanthalogen-free halogen-free environmental protection silicon rubber and its Preparation method.
Background technology
Silicon rubber be it is a kind of have inorganic and organic nature macromolecular elastomer material concurrently, its main chain is former by silicon atom and oxygen Son is alternately constituted, and the silicon oxygen bond (- Si-O-) bond energy for being formed is very big, bigger than the carbon-carbon bond (- C-C-) bond energy of traditional rubber It is many, with very high heat endurance and extraordinary weatherability, while silicon rubber also has, HRR is low, charring rate is high, Nontoxic, smokeless the characteristics of, possesses relatively good fire resistance.Therefore silicon rubber is that the application of the fields such as Aero-Space is extremely wide resistance to Hot material.
But, silicon rubber can be in itself burning, and in atmosphere silicon rubber can glow phenomenon.Silicon rubber it is a lot Use environment requires that it has to possess good fire resistance, therefore research high flame retardancy silicon rubber material is very important.
Although the anti-flammability of silicon rubber, such as platinum compounds, deca-BDE or hexichol can be improved using some means Ethane makees fire retardant, Application No. CN200410077503.5, CN201310626801.4, CN201510064816.5, CN201310461092.9、CN200810196197.5、CN200910185447.X.But these fire retardants are being manufactured or made Can bring very big pollution to environment with during, and silicon rubber many use occasions be requirement halogen-free environmental (for example Subway, automobile, building, hospital, Aero-Space etc.).Therefore, not only fire-retardant but also Halogen silicon rubber is very necessary for research.
Although the patent of application number CN201410826700.6 discloses a kind of halogen-free flameproof heat vulcanized silicone rubber, its limit Oxygen index (OI) can exceed that 40%, and vertical combustion can reach FV-0 levels, but use isocyanates in that patent, the body to people Health has very big harm.Although the patent of Application No. CN201210257988.0 discloses a kind of Environment-friendlyflame-retardant flame-retardant silicone rubber Vertical combustion can reach FV-0 levels, but oxygen index (OI) is not described, and wherein with the addition of melamine, and melamine Generation cyanide severe toxicity gas can be decomposed at high temperature.Other Environment-friendlyflame-retardant flame-retardant silicone rubber patents (CN201110348676.6, CN201310265272.X, CN201310267082.1, CN201310267097.8) fire resistance of silicon rubber is not all carried out Description.Therefore develop a kind of both with very high fire resistance, again will not be to the healthy fire-retardant Halogen for working the mischief of people Environmentally friendly silicon rubber is very necessary.
The content of the invention
It is an object of the invention to provide a kind of excellent fireproof performance and the high-flame-retardanthalogen-free halogen-free of environmental protection environmental protection silicon rubber;
It is a further object to provide a kind of preparation method of high-flame-retardanthalogen-free halogen-free environmental protection silicon rubber.
In order to reach above-mentioned technique effect, the present invention takes technical scheme below:
A kind of high-flame-retardanthalogen-free halogen-free environmental protection silicon rubber, including the raw material of following mass parts:
100 parts of silicon rubber;
20~60 parts of white carbon;
20~150 parts of filler;
10~60 parts of fire retardant;
3~7 parts of hydroxy silicon oil;
2~5 parts of silane coupler;
0.5~1.5 part of vulcanizing agent.
Further technical scheme is that described silicon rubber is the methyl vinyl silicone rubber of molecular weight 350,000~700,000, Wherein contents of ethylene is 0.07%~4%.
Further technical scheme is that described white carbon is 150~400m selected from specific surface area2The vapor phase method hard charcoal of/g Black or specific surface area is 150~200m2The precipitated silica of/g.
Further technical scheme is, described hydroxy silicon oil is α, alpha, omega-dihydroxy dimethione, and dynamic viscosity is 30~40mPa.s.
Further technical scheme is that described filler is at least one in aluminium hydroxide, magnesium hydroxide.
Further technical scheme is, described fire retardant is selected from Firebrake ZB, mica powder, silicon powder, expansible graphite, poly- Two kinds in ammonium phosphate two or more.
Further technical scheme is, described silane coupler selected from γ-methacryloxy trimethoxy silane, At least one of γ-glycidyl ether oxygen propyl trimethoxy silicane, vinyltrimethoxy silane.
Further technical scheme is, described vulcanizing agent is 2,5- dimethyl -2,5- bis- (t-butylperoxy) hexane One kind in (referred to as double 2,5), peroxidating two (2,4 dichloro benzene formyl) (referred to as double 2,4).
Present invention also offers the preparation method of described high-flame-retardanthalogen-free halogen-free environmental protection silicon rubber, comprises the following steps successively:
Step A:Silicon rubber, hydroxy silicon oil, silane coupler are stirred 2~5 minutes in kneader;
Step B:By the multiple batches of addition of white carbon point, stir after adding every time;
Step C:By filler, the multiple batches of addition of fire retardant point, stir after adding every time;
Step D:150~180 DEG C are warming up to, are vacuumized, stirred 1~2 hour, plastic emitting obtains silicon rubber gross rubber;
Step E:Treat that silicon rubber gross rubber is cooled to room temperature, vulcanizing agent is added on a mill, thin logical 4~6 times, lower glue is cold But to room temperature, place more than 16 hours;
Step F:Elastomeric compound is carried out into compression molding, compression molding condition is as follows:160 DEG C of temperature, 10 minutes time, pressure 15~20MPa.
The present invention is made further explanation and description below.
The present invention is directed to silicon rubber and non halogen flame-retardant system, according to the interaction between fire retardant, can have at high temperature Effect ground absorbs and dilutes heat, forms carbon-coating etc., chooses suitable flame retardant combination proportioning, plays between fire retardant and fire-retardant Cooperative effect between agent and filler;Simultaneously according to white carbon and the species and consumption of filler, suitable silane coupler is chosen Improve the interface compatibility of filler and fire retardant and silicon rubber, and realize that filler exists with fire retardant by appropriate calendering process Respectively disperseing in silicon rubber, in the calendering process, by substep repeatedly charging, it is possible to reduce the group of filler and fire retardant It is poly-, improve its dispersiveness in silicon rubber, and by thin logical shearing on a mill, can further promote filler and Fire retardant is dispersed in silicon rubber so as to which the maximum performance of flame retardant effect, the silicon rubber gross rubber for obtaining has fine Fire resistance.
In the present invention, silicon rubber is the methyl vinyl silicone rubber that molecular weight is 35~700,000, wherein contents of ethylene For 0.07%~4%.Contents of ethylene is too low, can affect silicon rubber vulcanization speed and the degree of cross linking, contents of ethylene too Gao Huiying Ring the heat endurance of silicon rubber.
In the present invention, fire retardant is selected from two kinds in Firebrake ZB, mica powder, silicon powder, expansible graphite, APP Or two or more arbitrarily compounded.According to one embodiment of the invention, described fire retardant is Firebrake ZB and silicon powder Mixture, and both mass ratioes are 15~20:10~15, it is preferred that mass ratio is 15:10.A reality of the invention Example is applied, described fire retardant is silicon powder, mica powder, the mixture of expansible graphite, and the mass ratio of three is 15~20:15 ~20:3~6;Preferably, the mass ratio of three is 20:20:5.According to one embodiment of present invention, described fire retardant is The mixture of Firebrake ZB and APP, and both mass ratioes are 15~20:15~20;Preferably, mass ratio is 1:1.Root According to one embodiment of the present of invention, fire retardant is Firebrake ZB, mica powder, the mixture of silicon powder, the mass ratio of three is 10~ 15:15~20:3~5, it is preferred that the mass ratio of three is 15:20:5.According to one embodiment of present invention, it is described fire-retardant Agent is Firebrake ZB, APP, the mixture of mica powder, and the mass ratio of three is 15~20:15~20:15~20;Preferably It is that mass ratio is 1:1:1.
In the present invention, silane coupler is selected from γ-methacryloxy trimethoxy silane (KH570), γ-shrink One or more of glycerine ether oxygen propyl trimethoxy silicane (KH560), vinyltrimethoxy silane (A-171).According to white The species of carbon black is different with consumption, and the consumption of filler is different, and the consumption of silane coupler is different.Generally, hard charcoal Black and filler is more, and the consumption of silane coupler used is more;It is silane coupled used by fume colloidal silica in the case of same amount The amount ratio precipitated silica of agent is more.
The oxygen index (OI) and vertical combustion level estimate method of high-flame-retardanthalogen-free halogen-free environmental protection silicon rubber adopts GB/T10707-2008.
The present invention compared with prior art, with following beneficial effect:
Through actually detected with good fire resistance, limited oxygen index is more than 48% to the product of the present invention, vertical combustion Grade FV-0 level is burnt, while the product halogen-free environmental.
Specific embodiment
With reference to embodiments of the invention, the invention will be further elaborated.
The preparation method of high-flame-retardanthalogen-free halogen-free environmental protection silicon rubber is as follows:
(1) silicon rubber, hydroxy silicon oil, silane coupler are stirred 4 minutes in kneader;
(2) by 5 additions of white carbon point, stir 15 minutes after adding every time;
(3) by filler, 4 additions of fire retardant point, stir 30 minutes after adding every time;
(4) 160 DEG C are warming up to, are vacuumized, stirred 2 hours, plastic emitting obtains silicon rubber gross rubber;
(5) treat that silicon rubber gross rubber is cooled to room temperature, vulcanizing agent is added on a mill, thin logical 5 times, lower glue is cooled to room Temperature, placed more than 16 hours;
(6) elastomeric compound is carried out into compression molding, compression molding condition is as follows:160 DEG C of temperature, 10 minutes time, pressure 20MPa。
Embodiment 1-5 is prepared according to above-mentioned preparation method, and it is as shown in the table for the mass parts of its raw material:
Table 1:The component and mass parts of embodiment 1-5
Note:The molecular weight of silicon rubber is " 650,000 in embodiment 4 in above table:350000=9:1 " implication for representing is to divide The mol ratio of the silicon rubber that son amount is 650,000 silicon rubber and molecular weight is 350,000 is 9:1.
The contents of ethylene of silicon rubber is " 0.16% in embodiment 1 and 2 in above table:0.07%=9:1 " represent Implication is 9 for the mol ratio of the silicon rubber that contents of ethylene is 0.16% and the silicon rubber that contents of ethylene is 0.07%:1.
Silicon rubber contents of ethylene is " 0.15% in embodiment 5 in above table:4%=9.5:0.5 " implication for representing It is 9 for silicon rubber and the mol ratio of the silicon rubber that contents of ethylene is 4% that contents of ethylene is 0.15%:1.
The oxygen index (OI) and vertical combustion grade of embodiment 1-5 silicon rubber are tested using GB/T 10707-2008, its As a result it is as shown in table 2.
Table 2:The fire resistance test result of embodiment 1-5
Project Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5
Oxygen index (OI) % 47 47 > 48 48 45
Vertical combustion grade FV-0 FV-0 FV-0 FV-0 FV-0
Tensile strength MPa 6.1 5.5 5.2 6.3 6.1
Elongation at break % 235 205 217 220 223
Although reference be made herein to invention has been described for explanatory embodiment of the invention, and above-described embodiment is only this Bright preferably embodiment, embodiments of the present invention are simultaneously not restricted to the described embodiments, it should be appreciated that people in the art Member can be designed that a lot of other modification and embodiment, and these modifications and embodiment will fall in principle disclosed in the present application Within scope and spirit.

Claims (9)

1. a kind of high-flame-retardanthalogen-free halogen-free environmental protection silicon rubber, it is characterised in that including the raw material of following mass parts:
100 parts of silicon rubber;
20~60 parts of white carbon;
20~150 parts of filler;
10~60 parts of fire retardant;
3~7 parts of hydroxy silicon oil;
2~5 parts of silane coupler;
0.5~1.5 part of vulcanizing agent.
2. high-flame-retardanthalogen-free halogen-free according to claim 1 environmental protection silicon rubber, it is characterised in that described silicon rubber is molecular weight 350000~700,000 methyl vinyl silicone rubber, wherein contents of ethylene are 0.07%~4%.
3. high-flame-retardanthalogen-free halogen-free according to claim 1 environmental protection silicon rubber, it is characterised in that described white carbon is selected from than table Area is 150~400m2The fume colloidal silica or specific surface area of/g is 150~200m2The precipitated silica of/g.
4. high-flame-retardanthalogen-free halogen-free according to claim 1 environmental protection silicon rubber, it is characterised in that described hydroxy silicon oil is α, ω- Dihydroxy dimethione, dynamic viscosity is 30~40mPa.s.
5. high-flame-retardanthalogen-free halogen-free according to claim 1 environmental protection silicon rubber, it is characterised in that described filler be aluminium hydroxide, At least one in magnesium hydroxide.
6. high-flame-retardanthalogen-free halogen-free according to claim 1 environmental protection silicon rubber, it is characterised in that described fire retardant is selected from boric acid Two kinds in zinc, mica powder, silicon powder, expansible graphite, APP two or more.
7. high-flame-retardanthalogen-free halogen-free according to claim 1 environmental protection silicon rubber, it is characterised in that described silane coupler is selected from γ-methacryloxy trimethoxy silane, γ-glycidyl ether oxygen propyl trimethoxy silicane, vinyl trimethoxy At least one of silane.
8. high-flame-retardanthalogen-free halogen-free according to claim 1 environmental protection silicon rubber, it is characterised in that described vulcanizing agent is 2,5- bis- One kind in methyl -2,5- two (t-butylperoxy) hexane, peroxidating two (2,4 dichloro benzene formyl).
9. the preparation method of the environmentally friendly silicon rubber of high-flame-retardanthalogen-free halogen-free described in any one of claim 1-8, it is characterised in that wrap successively Include following steps:
Step A:Silicon rubber, hydroxy silicon oil, silane coupler are stirred 2~5 minutes in kneader;
Step B:By the multiple batches of addition of white carbon point, stir after adding every time;
Step C:By filler, the multiple batches of addition of fire retardant point, stir after adding every time;
Step D:150~180 DEG C are warming up to, are vacuumized, stirred 1~2 hour, plastic emitting obtains silicon rubber gross rubber;
Step E:Treat that silicon rubber gross rubber is cooled to room temperature, vulcanizing agent is added on a mill, thin logical 4~6 times, lower glue is cooled to Room temperature, placed more than 16 hours;
Step F:Elastomeric compound is carried out into compression molding, compression molding condition is as follows:160 DEG C of temperature, 10 minutes time, pressure 15~ 20MPa。
CN201611217540.0A 2016-12-26 2016-12-26 Highly flame-retardant halogen-free environment-friendly silicone rubber and preparation method thereof Pending CN106633915A (en)

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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107400364A (en) * 2017-08-02 2017-11-28 安徽宜德电子有限公司 A kind of high porcelain Ceramic silicon rubber formula of high fire-retardance
CN107760039A (en) * 2017-11-02 2018-03-06 广东聚合科技股份有限公司 A kind of ceramic flame-retardant silicon rubber and preparation method thereof
CN107880562A (en) * 2017-12-11 2018-04-06 中国人民武装警察部队学院 Expandable flame retardant silicon rubber composite material and preparation method thereof
CN108795057A (en) * 2018-06-25 2018-11-13 淄博泰康轻工制品有限公司 A kind of glass silica gel sheath
CN108795302A (en) * 2018-06-28 2018-11-13 丹阳市沃德立电工材料有限公司 A kind of silicon rubber self-adhesive tape that novel fire-resistant is fire-retardant
CN109401321A (en) * 2018-09-27 2019-03-01 唐山师范学院 Expandable flame retardant room temperature vulcanized silicone rubber formula and expandable flame retardant room temperature vulcanized silicone rubber
CN109912976A (en) * 2019-01-21 2019-06-21 佛山市美捷远电器实业有限公司 A kind of environmental-protection fireproof type silicon rubber and preparation method thereof
CN110791105A (en) * 2019-09-26 2020-02-14 无锡市华美电缆有限公司 Low-temperature flame-retardant silica gel outer sheath for cable and preparation method thereof
CN110982276A (en) * 2019-12-23 2020-04-10 成都硅宝科技股份有限公司 Silicone rubber vibration damping pad with low dynamic-static stiffness ratio and preparation method thereof
CN111040455A (en) * 2019-12-31 2020-04-21 长缆电工科技股份有限公司 Corrosion-resistant self-adhesive low-smoke halogen-free fireproof wrapping tape material and preparation method thereof
CN113061342A (en) * 2021-03-26 2021-07-02 浙江百朗士橡塑科技有限公司 Low-hardness flame-retardant silica gel and preparation process thereof
CN113355047A (en) * 2021-06-25 2021-09-07 上海珏晟新材料科技有限公司 Flame-retardant liquid silica gel for bonding electrical elements and preparation method thereof
CN114958000A (en) * 2022-06-06 2022-08-30 华容县丰硕硅材料有限公司 High-flame-retardant weather-resistant silicone rubber composition and preparation method thereof
CN115746796A (en) * 2022-12-16 2023-03-07 中国科学技术大学 Preparation method of flexible flame-retardant shape-stabilized phase-change material

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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107400364A (en) * 2017-08-02 2017-11-28 安徽宜德电子有限公司 A kind of high porcelain Ceramic silicon rubber formula of high fire-retardance
CN107760039A (en) * 2017-11-02 2018-03-06 广东聚合科技股份有限公司 A kind of ceramic flame-retardant silicon rubber and preparation method thereof
CN107880562A (en) * 2017-12-11 2018-04-06 中国人民武装警察部队学院 Expandable flame retardant silicon rubber composite material and preparation method thereof
CN108795057A (en) * 2018-06-25 2018-11-13 淄博泰康轻工制品有限公司 A kind of glass silica gel sheath
CN108795302A (en) * 2018-06-28 2018-11-13 丹阳市沃德立电工材料有限公司 A kind of silicon rubber self-adhesive tape that novel fire-resistant is fire-retardant
CN109401321A (en) * 2018-09-27 2019-03-01 唐山师范学院 Expandable flame retardant room temperature vulcanized silicone rubber formula and expandable flame retardant room temperature vulcanized silicone rubber
CN109912976A (en) * 2019-01-21 2019-06-21 佛山市美捷远电器实业有限公司 A kind of environmental-protection fireproof type silicon rubber and preparation method thereof
CN110791105A (en) * 2019-09-26 2020-02-14 无锡市华美电缆有限公司 Low-temperature flame-retardant silica gel outer sheath for cable and preparation method thereof
CN110982276A (en) * 2019-12-23 2020-04-10 成都硅宝科技股份有限公司 Silicone rubber vibration damping pad with low dynamic-static stiffness ratio and preparation method thereof
CN111040455A (en) * 2019-12-31 2020-04-21 长缆电工科技股份有限公司 Corrosion-resistant self-adhesive low-smoke halogen-free fireproof wrapping tape material and preparation method thereof
CN113061342A (en) * 2021-03-26 2021-07-02 浙江百朗士橡塑科技有限公司 Low-hardness flame-retardant silica gel and preparation process thereof
CN113355047A (en) * 2021-06-25 2021-09-07 上海珏晟新材料科技有限公司 Flame-retardant liquid silica gel for bonding electrical elements and preparation method thereof
CN114958000A (en) * 2022-06-06 2022-08-30 华容县丰硕硅材料有限公司 High-flame-retardant weather-resistant silicone rubber composition and preparation method thereof
CN115746796A (en) * 2022-12-16 2023-03-07 中国科学技术大学 Preparation method of flexible flame-retardant shape-stabilized phase-change material

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Application publication date: 20170510