CN105086466B - The preparation method of acid and alkali-resistance molded silicon rubber - Google Patents
The preparation method of acid and alkali-resistance molded silicon rubber Download PDFInfo
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- CN105086466B CN105086466B CN201510485805.4A CN201510485805A CN105086466B CN 105086466 B CN105086466 B CN 105086466B CN 201510485805 A CN201510485805 A CN 201510485805A CN 105086466 B CN105086466 B CN 105086466B
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Abstract
The present invention provides the preparation method of acid and alkali-resistance molded silicon rubber, and its step is as follows：(1) oleic acid is dissolved in ethanol and stirred to being completely dissolved, addition deionized water, which is stirred to being uniformly dispersed, obtains modified solution, nano zirconium oxide powder is added into ultrasonic disperse in deionized water, move in constant temperature water bath, modified solution stirring is added simultaneously, sediment is taken out after ageing, is dried, sieved after grinding, obtain modified Nano zirconium oxide；(2) silicon rubber is added and PTFE micro mists, modified Nano zirconium oxide is added after mill mixing, bag roller, it is thin logical after mixing is uniform, slice, park, obtain base-material；(3) filler, coupling agent and base-material are added in vacuum kneader and mediated, heating adds vulcanizing agent, polymerization inhibitor, accelerator, fire retardant, plasticizer and age resistor and mediated, vacuumizes, plastic emitting after 1 hour obtains acid and alkali-resistance molded silicon rubber.The molded silicon rubber that the present invention is prepared has preferable acid-proof alkaline, it is adaptable to acid or alkalescence workplace.
Description
Technical field：
The present invention relates to the preparation method of silicon rubber, more particularly to acid and alkali-resistance molded silicon rubber.
Background technology：
Silicon rubber (Hong Kong ＆ Taiwan areas is referred to as mastic) is a kind of quite varied mould proprietary material of purposes, and silicon rubber has it
Premium properties and extensive use that his mold materials can not compare：(1) silicon rubber has good simulation quality, intensity and extremely low
Shrinkage factor；(2) mould making method is simple and easy to apply, can solidify at normal temperatures, and silicon rubber mould has good elasticity, to convex
It can be directly taken out after recess point moulding by casting；(3) silicon rubber mould is amenable to reuse, and keeps product prototype, can small lot
Product is produced, mould modification is also very convenient；(4) parts such as metal inserted piece can also be added in mould, product finished product can also enter
Row plating and spray painting processing；(5) releasing agent is not needed, cost is reduced；(6) resistance to elevated temperatures is very good.Therefore, built in decoration
Material, industrial art, hot investment casting, fiberglass industry, gypsum cement product and hot-water heating sealing, the hard foaming decoration product of polyurethane etc.
The industry of mould, which need to be used, to make mould with silicon rubber.
For example, Publication No. CN104744943A, publication date are 2015.07.01, apply for that sharp chemical industry industry is opened up in artificial Chengdu
The Chinese patent of Co., Ltd is disclosed " one kind injection machine-shaping bi-component addition type molded silicon rubber ", solid by A, B component
Chemical conversion type；Described component A includes the basic mass parts of silica gel 100, platinum complex catalyst 0.10-0.30 mass parts, alkynol class
And vinyl ring body compound polymerization inhibitor 0.1-2.0 mass parts, hydroxyl polysiloxane 0.001-0.01 mass parts；Described B groups
Dividing includes basis silica gel 0-100 mass parts, preferably one or more hydrogen-based polysiloxanes 4-15 mass parts, 5-10 mass parts, second
Alkenyl silicone oil 0-20 mass parts.The molded silicon rubber curing molding speed is fast, and easy mold release after shaping, shrinkage factor is small, and resilience is good,
Not deformation, easy mold release, but there is the bad defect of acid-proof alkaline as existing molded silicon rubber in it, in acid or alkali
Easily there are quality problems in the workplace of property.
The content of the invention：
The technical problem to be solved in the present invention is to provide a kind of preparation method of acid and alkali-resistance molded silicon rubber, the mould prepared
Tool silicon rubber has preferable acid-proof alkaline, it is adaptable to acid or alkalescence workplace.
In order to solve the above technical problems, the technical scheme is that：
The preparation method of acid and alkali-resistance molded silicon rubber, its step is as follows：
(1) oleic acid is dissolved in ethanol and stirred to being completely dissolved, addition deionized water, which is stirred to being uniformly dispersed, to be modified
Solution, adds ultrasonic disperse 30 minutes in deionized water by nano zirconium oxide powder, moves in constant temperature water bath, change while adding
Property 90 DEG C of solution at stir 3 hours, ageing takes out sediment after 24 hours, be placed in vacuum desiccator at 100 DEG C dry it is 2 small
When, sieved after grinding, obtain modified Nano zirconium oxide, wherein oleic acid, the weight ratio of nano zirconium oxide powder are 1:4；
(2) 100 parts by weight of silicone rubber are added into mill to knead under the conditions of roll spacing is 1mm, 16-21 weights is added after bag roller
The modified Nano zirconium oxide that amount part PTFE micro mists, 6-9 parts by weight step (1) are obtained, it is thin logical 3 times after mixing is uniform, roll spacing is adjusted
Save as 3mm, slice, park, obtain base-material；
(3) base-material obtained by 10-16 parts of filler material by weight, 0.5-1 parts by weight coupling agent and step (2) is added into vacuum kneading
Mediated 20 minutes in machine, be warming up to 180 DEG C, added 3-5 parts by weight vulcanizing agent, 0.5-1 parts by weight polymerization inhibitor, 1-2 parts by weight and promote
Enter agent, 5-8 parts by weight of flame retardant, 6-7 parts by weight of plasticizer and 1-1.5 parts by weight age resistor to mediate 2 hours, be evacuated to true
Reciprocal of duty cycle is 0.08MPa, and plastic emitting after 1 hour obtains acid and alkali-resistance molded silicon rubber.
Preferably, silicon rubber of the present invention is methyl vinyl phenyl silicon rubber.
Preferably, filler of the present invention is glass microsphere or aluminum oxide.
Preferably, coupling agent of the present invention is KH560.
Preferably, vulcanizing agent of the present invention is 2,4- dichlorobenzoperoxides.
Preferably, polymerization inhibitor of the present invention is alkynol.
Preferably, accelerator of the present invention is dibenzothiazyl disulfide.
Preferably, fire retardant of the present invention is nano-sized magnesium hydroxide.
Preferably, plasticizer of the present invention is dimethicone.
Preferably, age resistor of the present invention is antioxidant 4010NA.
Compared with prior art, the invention has the advantages that：
1) nano zircite is a kind of amphoteric oxide inorganic particle, its surface not oleophylic, with silicone rubber matrix compatibility
It is not good, therefore the present invention is modified the carboxyl in processing, oleic acid and the active hydroxyl on nano zircite surface to it by oleic acid
Covalent bonding together occurs for base, and the long-chain molecule of oleic acid grafts on the surface formation monolayer of nano zircite, effectively blocked
The hydrophily on nano zircite surface is changed into lipophile by the reunion of nano zircite, organic oleic acid, makes itself and silicon rubber
Compatibility between matrix and interface cohesion therebetween have obtained larger improvement, due to nano oxygen in silicone rubber matrix
Change zirconium is amphoteric oxide, so nano zircite can react with acid or alkali respectively when silicon rubber runs into acid or alkali environment,
The soda acid destruction that silicone rubber matrix is subject to is greatly reduced, so as to effectively improve the acid-proof alkaline of silicon rubber.
2) PTFE is the English abbreviation of polytetrafluoroethylene (PTFE), and it is polymerized by tetrafluoroethylene monomer, with high-melting-point, Gao Jie
Brilliant degree, and in molecular structure by fluorine atom constitute outer " shell " can resistance to various soda acids, therefore formed with silicone rubber matrix
After blending structure, the acid-proof alkaline of silicon rubber can be further improved.
Embodiment：
Describe the present invention in detail below in conjunction with specific embodiment, herein illustrative examples and explanation of the invention
For explaining the present invention, but it is not as a limitation of the invention.
Embodiment 1
The preparation method of acid and alkali-resistance molded silicon rubber, its step is as follows：
(1) oleic acid is dissolved in ethanol and stirred to being completely dissolved, addition deionized water, which is stirred to being uniformly dispersed, to be modified
Solution, adds ultrasonic disperse 30 minutes in deionized water by nano zirconium oxide powder, moves in constant temperature water bath, change while adding
Property 90 DEG C of solution at stir 3 hours, ageing takes out sediment after 24 hours, be placed in vacuum desiccator at 100 DEG C dry it is 2 small
When, sieved after grinding, obtain modified Nano zirconium oxide, wherein oleic acid, the weight ratio of nano zirconium oxide powder are 1:4；
(2) 100 parts by weight methyl vinyl phenyl silicon rubber are added into mill to knead under the conditions of roll spacing is 1mm, bag
18 parts by weight PTFE micro mists are added after roller, the modified Nano zirconium oxide that 7.5 parts by weight steps (1) are obtained, it is thin by logical 3 after mixing is uniform
It is secondary, roll spacing is adjusted to 3mm, slice, parked, base-material is obtained；
(3) base-material obtained by 10 parts by weight of glass microballoons, 0.6 parts by weight KH560 and step (2) is added into vacuum kneader
It is interior to mediate 20 minutes, 180 DEG C are warming up to, 5 parts by weight 2,4- dichlorobenzoperoxides, 0.6 parts by weight alkynol, 1.4 weights are added
Measure part dibenzothiazyl disulfide, 5.5 parts by weight nano-sized magnesium hydroxides, 6.6 parts by weight dimethicones and 1.2 parts by weight anti-
Old agent 4010NA is mediated 2 hours, is evacuated to vacuum for 0.08MPa, plastic emitting after 1 hour obtains acid and alkali-resistance molded silicon rubber.
Embodiment 2
The preparation method of acid and alkali-resistance molded silicon rubber, its step is as follows：
(1) oleic acid is dissolved in ethanol and stirred to being completely dissolved, addition deionized water, which is stirred to being uniformly dispersed, to be modified
Solution, adds ultrasonic disperse 30 minutes in deionized water by nano zirconium oxide powder, moves in constant temperature water bath, change while adding
Property 90 DEG C of solution at stir 3 hours, ageing takes out sediment after 24 hours, be placed in vacuum desiccator at 100 DEG C dry it is 2 small
When, sieved after grinding, obtain modified Nano zirconium oxide, wherein oleic acid, the weight ratio of nano zirconium oxide powder are 1:4；
(2) 100 parts by weight methyl vinyl phenyl silicon rubber are added into mill to knead under the conditions of roll spacing is 1mm, bag
20 parts by weight PTFE micro mists are added after roller, the modified Nano zirconium oxide that 7 parts by weight steps (1) are obtained, it is thin by logical 3 after mixing is uniform
It is secondary, roll spacing is adjusted to 3mm, slice, parked, base-material is obtained；
(3) base-material obtained by 12 parts by weight of glass microballoons, 0.8 parts by weight KH560 and step (2) is added into vacuum kneader
It is interior to mediate 20 minutes, 180 DEG C are warming up to, 3.5 parts by weight 2,4- dichlorobenzoperoxides, 0.9 parts by weight alkynol, 1.2 are added
Parts by weight dibenzothiazyl disulfide, 8 parts by weight nano-sized magnesium hydroxides, 7 parts by weight dimethicones and 1.4 parts by weight are anti-old
Agent 4010NA is mediated 2 hours, is evacuated to vacuum for 0.08MPa, plastic emitting after 1 hour obtains acid and alkali-resistance molded silicon rubber.
Embodiment 3
The preparation method of acid and alkali-resistance molded silicon rubber, its step is as follows：
(1) oleic acid is dissolved in ethanol and stirred to being completely dissolved, addition deionized water, which is stirred to being uniformly dispersed, to be modified
Solution, adds ultrasonic disperse 30 minutes in deionized water by nano zirconium oxide powder, moves in constant temperature water bath, change while adding
Property 90 DEG C of solution at stir 3 hours, ageing takes out sediment after 24 hours, be placed in vacuum desiccator at 100 DEG C dry it is 2 small
When, sieved after grinding, obtain modified Nano zirconium oxide, wherein oleic acid, the weight ratio of nano zirconium oxide powder are 1:4；
(2) 100 parts by weight methyl vinyl phenyl silicon rubber are added into mill to knead under the conditions of roll spacing is 1mm, bag
16 parts by weight PTFE micro mists are added after roller, the modified Nano zirconium oxide that 9 parts by weight steps (1) are obtained, it is thin by logical 3 after mixing is uniform
It is secondary, roll spacing is adjusted to 3mm, slice, parked, base-material is obtained；
(3) base-material obtained by 16 parts by weight of alumina, 0.5 parts by weight KH560 and step (2) is added in vacuum kneader
Mediate 20 minutes, be warming up to 180 DEG C, add 3 parts by weight 2,4- dichlorobenzoperoxides, 1 parts by weight alkynol, 1.6 parts by weight
Dibenzothiazyl disulfide, 7 parts by weight nano-sized magnesium hydroxides, 6.5 parts by weight dimethicones and 1 parts by weight age resistor
4010NA is mediated 2 hours, is evacuated to vacuum for 0.08MPa, plastic emitting after 1 hour obtains acid and alkali-resistance molded silicon rubber.
Embodiment 4
The preparation method of acid and alkali-resistance molded silicon rubber, its step is as follows：
(1) oleic acid is dissolved in ethanol and stirred to being completely dissolved, addition deionized water, which is stirred to being uniformly dispersed, to be modified
Solution, adds ultrasonic disperse 30 minutes in deionized water by nano zirconium oxide powder, moves in constant temperature water bath, change while adding
Property 90 DEG C of solution at stir 3 hours, ageing takes out sediment after 24 hours, be placed in vacuum desiccator at 100 DEG C dry it is 2 small
When, sieved after grinding, obtain modified Nano zirconium oxide, wherein oleic acid, the weight ratio of nano zirconium oxide powder are 1:4；
(2) 100 parts by weight methyl vinyl phenyl silicon rubber are added into mill to knead under the conditions of roll spacing is 1mm, bag
21 parts by weight PTFE micro mists are added after roller, the modified Nano zirconium oxide that 8 parts by weight steps (1) are obtained, it is thin by logical 3 after mixing is uniform
It is secondary, roll spacing is adjusted to 3mm, slice, parked, base-material is obtained；
(3) base-material obtained by 14 parts by weight of alumina, 0.7 parts by weight KH560 and step (2) is added in vacuum kneader
Mediate 20 minutes, be warming up to 180 DEG C, add 4.5 parts by weight 2,4- dichlorobenzoperoxides, 0.5 parts by weight alkynol, 2 weight
Part dibenzothiazyl disulfide, 6.6 parts by weight nano-sized magnesium hydroxides, 6 parts by weight dimethicones and 1.5 parts by weight age resistor
4010NA is mediated 2 hours, is evacuated to vacuum for 0.08MPa, plastic emitting after 1 hour obtains acid and alkali-resistance molded silicon rubber.
Embodiment 5
The preparation method of acid and alkali-resistance molded silicon rubber, its step is as follows：
(1) oleic acid is dissolved in ethanol and stirred to being completely dissolved, addition deionized water, which is stirred to being uniformly dispersed, to be modified
Solution, adds ultrasonic disperse 30 minutes in deionized water by nano zirconium oxide powder, moves in constant temperature water bath, change while adding
Property 90 DEG C of solution at stir 3 hours, ageing takes out sediment after 24 hours, be placed in vacuum desiccator at 100 DEG C dry it is 2 small
When, sieved after grinding, obtain modified Nano zirconium oxide, wherein oleic acid, the weight ratio of nano zirconium oxide powder are 1:4；
(2) 100 parts by weight methyl vinyl phenyl silicon rubber are added into mill to knead under the conditions of roll spacing is 1mm, bag
17 parts by weight PTFE micro mists are added after roller, the modified Nano zirconium oxide that 6.5 parts by weight steps (1) are obtained, it is thin by logical 3 after mixing is uniform
It is secondary, roll spacing is adjusted to 3mm, slice, parked, base-material is obtained；
(3) base-material obtained by 15 parts by weight of alumina, 0.9 parts by weight KH560 and step (2) is added in vacuum kneader
Mediate 20 minutes, be warming up to 180 DEG C, add 4 parts by weight 2,4- dichlorobenzoperoxides, 0.8 parts by weight alkynol, 1.5 weight
Part dibenzothiazyl disulfide, 5 parts by weight nano-sized magnesium hydroxides, 6.4 parts by weight dimethicones and 1.3 parts by weight age resistor
4010NA is mediated 2 hours, is evacuated to vacuum for 0.08MPa, plastic emitting after 1 hour obtains acid and alkali-resistance molded silicon rubber.
Embodiment 6
The preparation method of acid and alkali-resistance molded silicon rubber, its step is as follows：
(1) oleic acid is dissolved in ethanol and stirred to being completely dissolved, addition deionized water, which is stirred to being uniformly dispersed, to be modified
Solution, adds ultrasonic disperse 30 minutes in deionized water by nano zirconium oxide powder, moves in constant temperature water bath, change while adding
Property 90 DEG C of solution at stir 3 hours, ageing takes out sediment after 24 hours, be placed in vacuum desiccator at 100 DEG C dry it is 2 small
When, sieved after grinding, obtain modified Nano zirconium oxide, wherein oleic acid, the weight ratio of nano zirconium oxide powder are 1:4；
(2) 100 parts by weight methyl vinyl phenyl silicon rubber are added into mill to knead under the conditions of roll spacing is 1mm, bag
19 parts by weight PTFE micro mists are added after roller, the modified Nano zirconium oxide that 6 parts by weight steps (1) are obtained, it is thin by logical 3 after mixing is uniform
It is secondary, roll spacing is adjusted to 3mm, slice, parked, base-material is obtained；
(3) base-material obtained by 11 parts by weight of glass microballoons, 1 parts by weight KH560 and step (2) is added in vacuum kneader
Mediate 20 minutes, be warming up to 180 DEG C, add 4.4 parts by weight 2,4- dichlorobenzoperoxides, 0.7 parts by weight alkynol, 1.8 weights
Measure part dibenzothiazyl disulfide, 6 parts by weight nano-sized magnesium hydroxides, 6.3 parts by weight dimethicones and 1.1 parts by weight anti-old
Agent 4010NA is mediated 2 hours, is evacuated to vacuum for 0.08MPa, plastic emitting after 1 hour obtains acid and alkali-resistance molded silicon rubber.
After tested, molded silicon rubber made from embodiment 1-6 and the acid-proof alkaline of comparative example are as shown in the table, its
In：Comparative example is Publication No. CN104744943A patent；Acid-proof alkaline is tested by GB/T 1690-2006:First claim
Go out the aerial quality of silicon rubber to be measured, silicon rubber to be measured is then soaked in the sodium hydroxide that mass fraction is 0.1 respectively
Solution, volume fraction is in 0.2 dilute sulfuric acid, soak 3 days, table in the heat and moisture preserving case that temperature is 25 DEG C, humidity is 50%
Face cleaned with distilled water, dry up after claim its quality, mass change be after silicon rubber to be measured soaks with before immersion it is of poor quality with
The percentage of quality before immersion, the numerical value is smaller, it was demonstrated that acid-proof alkaline is better.
As seen from the above table, molded silicon rubber made from 1-6 of the embodiment of the present invention soaks in sodium hydroxide and dilution heat of sulfuric acid
Mass change after bubble is significantly lower than comparative example, with preferable acid-proof alkaline.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
Know the personage of this technology all can carry out modifications and changes under the spirit and scope without prejudice to the present invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete without departing from disclosed spirit and institute under technological thought such as
Into all equivalent modifications or change, should by the present invention claim be covered.
Claims (10)
1. the preparation method of acid and alkali-resistance molded silicon rubber, it is characterised in that comprise the following steps：
(1) oleic acid is dissolved in ethanol and stirred to being completely dissolved, addition deionized water, which is stirred to being uniformly dispersed, obtains modified solution,
Nano zirconium oxide powder is added into ultrasonic disperse 30 minutes in deionized water, moved in constant temperature water bath, while it is molten to add modification
Stirred 3 hours at 90 DEG C of liquid, ageing takes out sediment after 24 hours, be placed in vacuum desiccator at 100 DEG C and dry 2 hours, grind
Sieved after mill, obtain modified Nano zirconium oxide, wherein oleic acid, the weight ratio of nano zirconium oxide powder are 1:4；
(2) 100 parts by weight of silicone rubber are added into mill to knead under the conditions of roll spacing is 1mm, 16-21 parts by weight is added after bag roller
The modified Nano zirconium oxide that PTFE micro mists, 6-9 parts by weight step (1) are obtained, it is thin logical 3 times after mixing is uniform, roll spacing is adjusted to
3mm, slice, is parked, and obtains base-material；
(3) base-material obtained by 10-16 parts of filler material by weight, 0.5-1 parts by weight coupling agent and step (2) is added in vacuum kneader
Mediate 20 minutes, be warming up to 180 DEG C, add 3-5 parts by weight vulcanizing agent, 0.5-1 parts by weight polymerization inhibitor, 1-2 parts by weight accelerator,
5-8 parts by weight of flame retardant, 6-7 parts by weight of plasticizer and 1-1.5 parts by weight age resistor are mediated 2 hours, are evacuated to vacuum
For 0.08MPa, plastic emitting after 1 hour obtains acid and alkali-resistance molded silicon rubber.
2. the preparation method of acid and alkali-resistance molded silicon rubber according to claim 1, it is characterised in that：The silicon rubber is first
Base ethenylphenyl silicon rubber.
3. the preparation method of acid and alkali-resistance molded silicon rubber according to claim 1, it is characterised in that：The filler is glass
Microballoon or aluminum oxide.
4. the preparation method of acid and alkali-resistance molded silicon rubber according to claim 1, it is characterised in that：The coupling agent is
KH560。
5. the preparation method of acid and alkali-resistance molded silicon rubber according to claim 1, it is characterised in that：The vulcanizing agent is 2,
4- dichlorobenzoperoxides.
6. the preparation method of acid and alkali-resistance molded silicon rubber according to claim 1, it is characterised in that：The polymerization inhibitor is alkynes
Alcohol.
7. the preparation method of acid and alkali-resistance molded silicon rubber according to claim 1, it is characterised in that：The accelerator is two
Dibenzothiazyl disulfide.
8. the preparation method of acid and alkali-resistance molded silicon rubber according to claim 1, it is characterised in that：The fire retardant is to receive
Rice magnesium hydroxide.
9. the preparation method of acid and alkali-resistance molded silicon rubber according to claim 1, it is characterised in that：The plasticizer is two
Methyl-silicone oil.
10. the preparation method of acid and alkali-resistance molded silicon rubber according to claim 1, it is characterised in that：The age resistor is
Antioxidant 4010NA.
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| CN109054397A (en) * | 2018-07-31 | 2018-12-21 | 山东聚众数字医学科技开发有限公司 | A kind of people doctor teaching mode production silicon rubber and preparation method thereof |
| CN111662552A (en) * | 2020-07-10 | 2020-09-15 | 东莞市固泰有机硅有限公司 | Acid and alkali resistant silicone rubber and preparation method thereof |
| CN112940506B (en) * | 2021-02-02 | 2021-12-28 | 深圳深凯硅胶制品有限公司 | Aviation silica gel sealing element and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010059710A1 (en) * | 2008-11-19 | 2010-05-27 | Dow Corning Corporation | A silicone composition and a method for preparing the same |
| 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 |
| CN103694711A (en) * | 2013-12-23 | 2014-04-02 | 西安向阳航天材料股份有限公司 | Oil-resistant fluorinated silicone rubber and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010059710A1 (en) * | 2008-11-19 | 2010-05-27 | Dow Corning Corporation | A silicone composition and a method for preparing the same |
| 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 |
| CN103694711A (en) * | 2013-12-23 | 2014-04-02 | 西安向阳航天材料股份有限公司 | Oil-resistant fluorinated silicone rubber and preparation method thereof |
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