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Preparation method of vinyl silicone oil with low hydroxyl content

A technology of vinyl silicone oil and low hydroxyl group, which is applied in the field of preparation of vinyl silicone oil with low hydroxyl content, can solve the problems of high silicon hydroxyl content in vinyl silicone oil, and achieve the effects of simplifying production steps, reducing consumption and improving efficiency

Pending Publication Date: 2021-04-06
HUBEI XINGRUI SILICON MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to solve the problem of high silanol content in vinyl silicone oil and simplify the production process, the present invention removes the steps of dehydration and capping agent adsorption, uses a silanol remover to remove silanol, and introduces vinyl groups at the same time. Does not introduce other impurities

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024]DMC (100 ppm) was added to the reaction kettle with stirring and heated, tetramethyl di silicone is added, and the amount of DMC is 4.1% in the reactor; the NCK-9 cation exchange resin is added, and the amount is added. The DMC is 8%, reacted at 80 ° C for 3 hours; the vinylethoxysilane is added, and the amount of the amount of material in the reactor is 0.05%, the reaction is 1H; the resin catalyst; at 160 ° C, vacuum decentralized 3 hours, cooling Filter and get a finished product. The viscosity is 96 cp, the vinyl content of 0.816%, and the aliquot of the silicon hydroxy group is 1.2.

Embodiment 2

[0026]D4 (water content 60 ppm) was added to the reaction kettle with stirring and heated, and the low viscosity end vinyl silicone oil was added, and the amount of D4 mass in the reaction vessel was added; the potassium hydroxide silachydrate was added such that the base in the reaction system was added. The content was 40 ppm, reacted at 85 ° C for 1 hour; reaction at 105 ° C for 3 hours; the vinylmethoxysilane was added, and the amount of vinylmethoxysilane was added to 0.10% of the mass of the material in the reactor, and the reaction was 0.5 h; in phosphoric acid; at 165; The vacuum at ° C was degraded for 3 hours, and filtered, and the finished product was obtained. The viscosity of 375 cp, a vinyl content of 0.518%, and the silicon hydroxy group relative value 1.15.

Embodiment 3

[0028]DMC (water content 120 ppm) was added to the reaction kettle with stirring and heated, and tetramethyl diethylene siloxane was added, and the amount of DMC mass was 0.42% in the reactor; the tetramethylammonium oxide silicate is added. The alkali content in the reaction system was 25 ppm, reacted at 90 ° C for 1 hour; at 110 ° C for 3 hours; add vinylethoxysilane, 0.5% by weight of the material mass in the reactor, reaction 0.5 h; heating 160 ° C for 30 minutes; vacuum decentralized at 170 ° C for 4 hours, cooling filtration, and obtained product. The viscosity is 9875 cp, the vinyl content of 0.128%, and the silicon hydroxy group is resistant to 1.1.

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Abstract

The invention discloses a preparation method of vinyl silicone oil with low hydroxyl content, which comprises the following steps: (1) adding a dimethyl siloxane ring body and an end capping agent into a reaction kettle with stirring and heating functions; (2) adding a catalyst, and reacting for 25 hours at the temperature of 80-110 DEG C; (3) adding a silicon hydroxyl eliminating agent, and reacting for 0.5-1.5 h; (4) breaking enzyme for 30-60 minutes; and (5) at the temperature of 160-180 DEG C and the vacuum degree of greater than 0.095, removing the solvent for 3-5 hours, cooling and filtering to obtain a finished product. Silicon hydroxyl in the vinyl silicone oil is eliminated by adopting the silicon hydroxyl eliminating agent, so that the process is simplified, the energy is saved, the efficiency is improved, the content of silicon hydroxyl in the vinyl silicone oil is reduced, and the quality of the vinyl silicone oil is improved.

Description

Technical field[0001]The present invention relates to a method for preparing a low hydroxyl content of vinyl silicone oil.Background technique[0002]Vinyl silicone oil, is a modifier such as a main raw material of liquid silicone rubber, a reinforcement such as a mixed rubber, an elastomer and emulsion modifier, polyurethane temperature resistant flame retardant, acrylate, high low temperature, hand sense Modified agents, other materials modifiers, and applications are very wide.[0003]The dimethylsiloxane ring used in the preparation of vinyl silicone oil is in production, and the water is inevitable during storage. In general, the dimethylsiloxane ring contains about 100 ppm, when the weather is When moist, the moisture content will increase while synthesizing the head of the vinyl silicone oil, which is also a micro moisture.[0004]During the synthesis of vinyl silicone oil, due to the water itself, the reaction system will contain a trace amount of water in the reaction system beca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/16C08G77/20C08G77/06
CPCC08G77/16C08G77/20C08G77/06
Inventor 李少平杜斌李书兵徐小刚陈海平王明亮李磊
Owner HUBEI XINGRUI SILICON MATERIAL CO LTD
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