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Preparation method of fluorinated polysiloxane raw rubber with terminal groups containing vinyl

A technology of fluorosilicone raw rubber and tetramethyldivinyldisiloxane, which is applied in the field of preparation of fluorosilicone raw rubber containing vinyl groups at the end groups, can solve the problems affecting the quality and performance of heat vulcanized fluorosilicone rubber, raw rubber The molecular weight is not easy to control, the vinyl end-capping rate is low, etc., and the polymerization time is short, the preparation is convenient, and the product is uniform.

Inactive Publication Date: 2014-07-09
浙江恒业成有机硅有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In short, the existing fluorosilicone raw rubber preparation method has low vinyl end-capping rate, difficult control of raw rubber molecular weight, high volatile content, and wide molecular weight distribution, which directly affect the quality and performance of heat vulcanized fluorosilicone rubber.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Preparation of sodium vinyldimethylsilanol: 1kg sodium hydroxide and 30kg tetramethyldivinyldisiloxane were added to the reactor and heated to 55-60°C and dehydrated under a pressure of 130Pa for 1.5h. Then it was heated to reflux at 140°C for 8 hours, cooled and filtered, and then the filtrate was reduced under a pressure of 130 Pa to remove the water produced by the reaction and unreacted tetramethyldivinyl disiloxane, to obtain 3.0 kg of vinyl dimethyl Sodium siliconate solid powder, sealed and stored under anhydrous conditions;

[0033] (2) Preparation of sodium vinyl dimethyl silanate alkali gum: Add 2 kg of sodium dimethyl silanate prepared in step (1) and 50 kg of fluorine-containing monomer 3,3,3- to the reactor. Trifluoropropylmethyl cyclotrisiloxane, heated to 70~90℃, dehydrated under 130Pa pressure for 1.5h. Then continue to heat to 130°C and react for 3 hours under anhydrous conditions, and remove low-boiling substances under reduced pressure to prepare a ...

Embodiment 2

[0036] (1) Preparation of sodium vinyldimethylsilanol: 1kg sodium hydroxide and 9kg tetramethyldivinyldisiloxane are added to the reactor and heated to 55~60℃, dehydrated under 130Pa pressure for 1.5h. Then it was heated and refluxed at 140°C for 8 hours, cooled and filtered, and then the filtrate was reduced under a pressure of 130 Pa to remove the water produced by the reaction and unreacted tetramethyldivinyl disiloxane to obtain 2.8 kg of vinyl dimethyl Sodium siliconate solid powder, sealed and stored under anhydrous conditions;

[0037] (2) Preparation of sodium vinyl dimethyl silanate alkali gum: Add 2 kg of sodium dimethyl silanate prepared in step (1) and 78 kg of fluorine-containing monomer 3,3,3- to the reactor. Trifluoropropylmethyl cyclotrisiloxane, heated to 70~90℃, dehydrated under 130Pa pressure for 1.5h. Then continue to heat to 130°C and react for 3 hours under anhydrous conditions, and remove low-boiling substances under reduced pressure to prepare a vinyl dim...

Embodiment 3

[0040] (1) Preparation of sodium vinyldimethylsilanol: 1kg of sodium hydroxide and 99kg of tetramethyldivinyldisiloxane were added to the reactor and heated to 55-60°C and dehydrated under a pressure of 130Pa for 1.5h. Then it was heated to reflux at 140°C for 8 hours, cooled and filtered, and then the filtrate was reduced under a pressure of 130 Pa to remove the water produced by the reaction and unreacted tetramethyldivinyl disiloxane to obtain 3.05 kg of vinyl dimethyl Sodium siliconate solid powder, sealed and stored under anhydrous conditions;

[0041] (2) Preparation of sodium vinyl dimethyl silanate alkali gum: Add 2 kg of sodium dimethyl silanate prepared in step (1) and 28 kg of fluorine-containing monomer 3,3,3- to the reactor. Trifluoropropylmethyl cyclotrisiloxane, heated to 70~90℃, dehydrated under 130Pa pressure for 1.5h. Then continue to heat to 130°C and react for 3 hours under anhydrous conditions, and remove low-boiling substances under reduced pressure to prep...

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Abstract

The invention relates to a preparation method of fluorinated polysiloxane raw rubber with terminal groups containing vinyl. The preparation method comprises the following steps: (1) carrying out heating dehydration on sodium hydroxide and divinyl tetramethyl disiloxane, carrying out heating reflux, cooling, filtrating, reducing pressure of filtrate so as to remove impurities so as to obtain solid powder, sealing and storing; (2) heating vinyl dimethyl silanol sodium salt in the step (1) and a fluorine-containing monomer (3,3,3-trifluoropropyl)methylcyclotrisiloxane, dewatering, continuously heating, and carrying out reduced pressure so as to remove low-boiling-point substances; (3) adding the fluorine-containing monomer (3,3,3-trifluoropropyl)methylcyclotrisiloxane and tetravinyl tetramethyl cyelo tetrasiloxane to a polymerization reactor, heating, dewatering, adding vinyl dimethyl silanol sodium salt alkali-gel, carrying out polymerization reaction, neutralizing by using a neutralizing agent, heating and removing low-boiling-point substances to obtain the fluorinated polysiloxane raw rubber with the terminal groups containing vinyl. The preparation method is used for producing the hot vulcanized fluorinated polysiloxane raw rubber with oil resistance and solvent resistance; the hot vulcanized fluorinated polysiloxane raw rubber serving as sealing materials, coating materials, gasket materials and the like is widely applied to the fields such as aviation, aerospace, automobiles, petrochemical engineering and artificial organs.

Description

technical field [0001] The invention relates to a preparation method of fluorosilicone raw rubber containing vinyl groups at the end groups. The method is suitable for industrial production, and the prepared fluorosilicone raw rubber is suitable for the production of Properties of heat vulcanized fluorosilicone base polymers. Background technique [0002] With the rapid development of the automobile and aerospace industries in recent years, the requirements for the temperature resistance and oil resistance of materials are getting higher and higher. Silicone rubber represented by dimethyl polysiloxane has excellent high and low temperature properties, electrical properties and elastic properties, but this rubber is poor in saturated steam resistance, oil resistance and solvent resistance, making its application restricted. However, after introducing fluorine-containing groups (such as trifluoropropyl) into the carbon chain of silicone rubber to form fluorosilicone rubber, d...

Claims

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Application Information

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IPC IPC(8): C08G77/24C08G77/08
Inventor 王琼燕甘腾飞吴忆南
Owner 浙江恒业成有机硅有限公司
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