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Addition type liquid fluorinated silicone rubber base rubber and preparation method thereof

A technology of liquid fluorosilicone and base rubber, applied in the field of addition type liquid fluorosilicone rubber base rubber and its preparation, can solve the problems of affecting vinyl crosslinking activity, impairing oil resistance of fluorosilicone rubber, product turbidity, etc. Steric hindrance effect, reducing shielding effect, ensuring the effect of cross-linking activity

Active Publication Date: 2016-07-20
新元化学(山东)股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The structure of fluorosilicone rubber base rubber prepared in the industry is usually: Vi(Me) 2 SiO-[Si(Me) 2 O] n -[Si(Rf)(Me)O] m -[Si(Vi)(Me)O] q -Si(Me) 2 Vi, where Me represents CH 3 -, Vi stands for CH 2 =CH-, Rf represents CF 3 CH 2 CH 2 -, when more dimethylsiloxane chains or methyl vinylsiloxane chains are introduced into the molecular chain of the base rubber, it will damage the oil resistance of fluorosilicone rubber; when the molecular chain of the base rubber does not contain dimethyl silicon Oxygen chains and methyl vinyl siloxane chains (n=0, q=0), due to the larger spatial structure of the trifluoropropyl group, will cause a shielding effect on the Si-Vi directly connected to the end of the molecular chain, The steric hindrance effect will seriously affect the cross-linking activity of the vinyl group, resulting in incomplete vulcanization and affecting the mechanical properties of the product
[0005] A fluorosilicone copolymer base rubber is prepared in the Chinese patent document CN101250266A; however, the copolymer base rubber has poor oil resistance and cannot be used in harsh oil and gas environments
However, this process is not easy to control the molecular weight. When the molecular weight of the base rubber is small, it is necessary to add an excessive amount of lithium vinyl silicon alkoxide to catalyze the reaction and end-capping, and the corresponding amount of dimethyl vinyl chlorosilane must also be increased, resulting in There is a large amount of lithium chloride salt, which causes the product to be cloudy and affects the vulcanization performance
[0008] In addition, the basic rubber molecular chains in Chinese patent documents such as CN102225997B, CN103725199B, and CN103642046B are directly connected to the Si-Vi at the end of the chain with trifluoropropylmethylsiloxane chains, causing steric hindrance to the terminal vinyl group. Affects the crosslinking activity of vinyl

Method used

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  • Addition type liquid fluorinated silicone rubber base rubber and preparation method thereof
  • Addition type liquid fluorinated silicone rubber base rubber and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] An addition-type liquid fluorosilicone rubber base rubber has the following structural formula:

[0040] Vi(Me) 2 SiO-Si(Me) 2 O-[Si(Rf)(Me)O] 35 -Si(Me) 2 O-Si(Me) 2 Vi

[0041] The preparation steps are as follows:

[0042] (1) Add 600g trifluoropropylmethylcyclotrisiloxane (D 3 F), 37.5g 1-vinyl-3-hydroxyl-1,1,3,3-tetramethyldisiloxane (purity 96%) and 0.5g sodium hydroxide silicon alkoxide (NaOH content 4.05%), stirring uniform;

[0043] (2) At room temperature, vacuumize the reactor to -0.04MPa, turn on the heating, raise the temperature to 120-130°C to initiate the reaction of the system and maintain it for 2.5h, maintain the pressure of -0.04MPa to -0.08MPa throughout the reaction, and the water vapor generated by the polymerization, As the reaction proceeds, it is continuously sucked away by negative pressure;

[0044](3) After the reaction is complete, add silicon-based phosphate to neutralize the catalyst and keep it for 0.5h;

[0045] (4) Under the ...

Embodiment 2

[0048] An addition-type liquid fluorosilicone rubber base rubber has the following structural formula:

[0049] Vi(Me) 2 SiO-Si(Me) 2 O-[Si(Rf)(Me)O] 68 -Si(Me) 2 O-Si(Me) 2 Vi

[0050] The preparation steps are as follows:

[0051] (1) Add 600g trifluoropropylmethylcyclotrisiloxane (D 3 F), 20g 1-vinyl-3-hydroxyl-1,1,3,3-tetramethyldisiloxane (purity 96%) and 0.48g sodium hydroxide silicon alkoxide (NaOH content 4.05%), stir well ;

[0052] (2) At room temperature, vacuumize the reactor to -0.04MPa, turn on the heating, raise the temperature to 120-130°C to initiate the reaction of the system and maintain it for 2.5h, maintain the pressure of -0.04MPa to -0.08MPa throughout the reaction, and the water vapor generated by the polymerization, As the reaction proceeds, it is continuously sucked away by negative pressure;

[0053] (3) After the reaction is complete, add silicon-based phosphate to neutralize the catalyst and keep it for 0.5h;

[0054] (4) Under the pressu...

Embodiment 3

[0057] An addition-type liquid fluorosilicone rubber base rubber has the following structural formula:

[0058] Vi(Me) 2 SiO-Si(Me) 2 O-[Si(Rf)(Me)O] 170 -Si(Me) 2 O-Si(Me) 2 Vi

[0059] The preparation steps are as follows:

[0060] (1) Add 600g trifluoropropylmethylcyclotrisiloxane (D 3 F), 9g 1-vinyl-3-hydroxyl-1,1,3,3-tetramethyldisiloxane (purity 96%) and 0.49g sodium hydroxide silicon alkoxide (NaOH content 4.05%), stir well ;

[0061] (2) At room temperature, vacuumize the reactor to -0.04MPa, turn on the heating, raise the temperature to 120-130°C to initiate the reaction of the system and maintain it for 2.5h, maintain the pressure of -0.04MPa to -0.08MPa throughout the reaction, and the water vapor generated by the polymerization, As the reaction proceeds, it is continuously sucked away by negative pressure;

[0062] (3) After the reaction is complete, add silicon-based phosphate to neutralize the catalyst and keep it for 0.5h;

[0063] (4) Under the pressu...

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Abstract

The invention relates to addition type liquid fluorinated silicone rubber base rubber and a preparation method thereof. The base rubber has following structural general formula of Vi(Me)2SiO-Si(Me)2O-[Si(Rf)(Me)O]m-Si(Me)2Vi, wherein Me represents CH3-, Vi represents CH2=CH-, Rf represents CF3CH2CH2-, and m represents an integer of 18-2000. According to the preparation method, 1-vinyl-3-hydroxy-1,1,3,3-tetramethyldisiloxane is taken as an end-capping agent, and two dimethyl siloxane chains are linked with vinyl, so that the screening effect of trifluoropropyl groups on vinyl at terminals of molecular chains is reduced, the steric-hinerance effect is reduced, the crosslinking activity of vinyl is guaranteed, and the oil resistance of the fluorinated silicone rubber is not damaged.

Description

technical field [0001] The invention relates to the field of rubber preparation, in particular to an addition-type liquid fluorosilicone rubber base rubber and a preparation method thereof. Background technique [0002] Addition-type liquid fluorosilicone rubber has excellent electrical insulation properties, aging resistance, good elasticity, rapid and convenient molding, no by-products in the reaction, and a wide range of operating temperatures. It can be used for packaging or infusion of electronic components and electrical equipment. In particular, it has excellent oil resistance, low volume swelling rate, can produce gaskets, sealing rings, etc. that are in direct contact with fuel, without secondary vulcanization, and has a low compression set rate, which is very suitable for the production of oil resistance for automobiles, etc. part. [0003] The vulcanization of addition-type liquid fluorosilicone rubber is based on the vinyl group in the molecular chain of the bas...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/24C08G77/08
CPCC08G77/08C08G77/24
Inventor 解乐福于鹏飞张殿松侯志伟夏子祥王爱卿王天宇
Owner 新元化学(山东)股份有限公司
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