High-strength fluorinated silicone rubber gross rubber and preparation method thereof

A technology of fluorosilicone rubber and mixed rubber, which is applied in the field of rubber, and can solve problems such as unstable product performance and uneven vinyl distribution, and achieve high elongation at break, improved mechanical properties, and good tear strength.

Active Publication Date: 2011-10-19
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Aiming at the problem that the performance of the existing fluorosilicone raw rubber is unstable due to uneven distribution of vinyl groups, the present invention provides a high-strength fluorosilicone rubber compound and its preparation method. First, the fluorosilicone raw rubber passes through D 3 F is prepared by ring-opening under an anionic ring-opening catalyst. The main chain does not contain vinyl groups. The cross-linking of the vulcanized rubber is carried out by adding polyvinyl fluorine-containing silicone oil. Secondly, in order to ensure that the vinyl groups are on the main chain of the cross-linking agent Uniform distribution, select the methyl trifluoropropyl siloxane chain link and methyl vinyl siloxane chain link prepared by cohydrolysis and cracking of methyl vinyl dichlorosilane and methyl trifluoropropyl dichlorosilane ring body and D 3 F is prepared by ring-opening copolymerization under an anionic ring-opening catalyst

Method used

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  • High-strength fluorinated silicone rubber gross rubber and preparation method thereof
  • High-strength fluorinated silicone rubber gross rubber and preparation method thereof
  • High-strength fluorinated silicone rubber gross rubber and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Preparation of fluorosilicone rubber crosslinking agent:

[0029] Mix 375g of 3,3,3-trifluoropropylmethyldichlorosilane and 125g of methylvinyldichlorosilane and slowly drop them into a reactor filled with 2000g of distilled water. Remove the water layer, wash the hydrolyzate with saturated sodium bicarbonate solution until neutral, dry it with anhydrous calcium chloride, add it to a four-necked flask, then add 10 g of potassium hydroxide, raise the temperature to 160°C, and collect fractions under a reduced pressure of 13.3 to 200 Pa. A ring body containing a methyltrifluoropropylsiloxane chain unit and a methylvinylsiloxane chain unit is obtained, which may be one or more of a tricyclic body, a tetracyclic body or a pentacyclic body, and the yield is 70% %.

[0030] Put 100g of the cyclic body obtained by cracking into the polymerization reactor for dehydration. The dehydration conditions are -0.01~-0.02MPa, 60~80℃, 0.5~2h, dry nitrogen and ventilate, then raise the ...

Embodiment 2

[0032] Preparation of fluorosilicone rubber crosslinking agent:

[0033] Mix 375g of 3,3,3-trifluoropropylmethyldichlorosilane and 125g of methylvinyldichlorosilane and slowly drop them into a reactor filled with 2000g of distilled water. Remove the water layer, wash the hydrolyzate with saturated sodium bicarbonate solution until neutral, dry it with anhydrous calcium chloride, add it to a four-necked flask, then add 10 g of potassium hydroxide, raise the temperature to 160°C, and collect fractions under a reduced pressure of 13.3 to 200 Pa. A ring body containing a methyltrifluoropropylsiloxane chain unit and a methylvinylsiloxane chain unit is obtained, which may be one or more of a tricyclic body, a tetracyclic body or a pentacyclic body, and the yield is 70% %.

[0034] The ring body 100g obtained by cleavage, D 3 F 200g is added to the polymerization reactor for dehydration. The dehydration conditions are -0.01~-0.02MPa, 60~80℃, 0.5~2h, dry nitrogen and ventilate, then...

Embodiment 3

[0036] Preparation of fluorosilicone rubber crosslinking agent:

[0037] Mix 375g of 3,3,3-trifluoropropylmethyldichlorosilane and 125g of methylvinyldichlorosilane and slowly drop them into a reactor filled with 2000g of distilled water. Remove the water layer, wash the hydrolyzate with saturated sodium bicarbonate solution until neutral, dry it with anhydrous calcium chloride, add it to a four-necked flask, then add 10 g of potassium hydroxide, raise the temperature to 160°C, and collect fractions under a reduced pressure of 13.3 to 200 Pa. A ring body containing a methyltrifluoropropylsiloxane chain unit and a methylvinylsiloxane chain unit is obtained, which may be one or more of a tricyclic body, a tetracyclic body or a pentacyclic body, and the yield is 70% %.

[0038] The ring body 50g obtained by cleavage, D 3F 200g is added to the polymerization reactor for dehydration. The dehydration conditions are -0.01~-0.02MPa, 60~80°C, 0.5~2h, dry nitrogen and ventilate, then ...

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PUM

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Abstract

The invention relates to high-strength fluorinated silicone rubber gross rubber and a preparation method thereof. The gross rubber is composed of the following raw materials in parts by mass: 100 parts of fluorinated silicone raw rubber, 30-80 parts of white carbon black, 0.5-15 parts of fluorinated silicone rubber cross-linking agent, 1-5 parts of reinforcing additive and 0.5-1.5 parts of vulcanizing agent; the raw materials of the high-strength fluorinated silicone rubber gross rubber are uniformly mixed on a mill mixer or an internal mixer and then the materials are discharged to obtain the fluorinated silicone rubber gross rubber. The main chain of the fluorinated silicone raw rubber which is utilized by the invention does not contain vinyl and the concentrated cross-linking is formedin a fluorinated silicone rubber vulcanizing system through utilizing the fluorinated silicone rubber cross-linking agent with a higher vinyl content to mix the fluorinated silicone rubber so that the mechanical property of the fluorinated silicone gross rubber is greatly improved.

Description

technical field [0001] The invention relates to a high-strength fluorosilicone rubber compound and a preparation method thereof, belonging to the technical field of rubber. Background technique [0002] In the preparation process of fluorosilicone raw rubber, in order to facilitate the vulcanization of the rubber, a small amount of vinyl groups will be introduced into the main chain, mainly through the methyl trifluoropropyl cyclotrisiloxane monomer (D 3 F) The method of copolymerization with a small amount of vinyl cyclosiloxane, the vinyl ring used is generally tetramethyltetravinyl cyclotetrasiloxane. However, due to the difference in the ring-opening rate of fluorosilicone monomer and vinyl monomer, the vinyl group is unevenly distributed on the polymer main chain, which seriously affects the performance of vulcanized rubber. [0003] In the mixing process of dimethyl silicone rubber, the performance of silicone rubber can be significantly improved by adding polyvinyl s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L83/08C08K3/36C08K5/14C08K3/22C08G77/24
Inventor 冯圣玉刘月涛周传健卢海峰
Owner SHANDONG UNIV
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