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Preparation process of structure control agent

A structure control agent and a technology for preparation process, applied in the chemical industry, can solve the problems of the unfavorable influence of the mechanical properties and aging resistance of vulcanized silicone rubber, the difficulty of uniform distribution of vinyl and vinyl, etc., so as to increase the mechanical properties and aging resistance, Solving the effect of uneven distribution of vinyl content

Active Publication Date: 2022-04-12
HUBEI XINGRUI SILICON MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the most commonly used structure control agent is hydroxy silicone oil (low viscosity α, ω-dihydroxy polydimethylsiloxane), which can effectively improve the processing performance and storage stability of the rubber compound, but α, ω-dihydroxy polydimethylsiloxane There is no active group in the middle of the molecular chain of dimethyl siloxane, and the addition will adversely affect the mechanical properties and aging resistance of vulcanized silicone rubber. Therefore, hydroxyl-terminated polysiloxane with active groups in the middle of the molecular chain is especially necessary.
[0005] At present, the domestic synthesis method of hydroxyl silicone oil is mainly the acetic anhydride method, that is, DMC (octamethylcyclotetrasiloxane) is used as the raw material. If this method is used to synthesize hydroxyl-terminated methyl vinyl silicone oil, DMC and VMC ( Tetramethyltetravinyl cyclotetrasiloxane) copolymerization, it is easy to cause multiple vinyl groups on a hydroxyl-terminated methyl vinyl silicone oil, and the vinyl groups are difficult to distribute evenly

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Dimethyldichlorosilane and methylvinyldichlorosilane are dropped into water at a molar ratio of 20:1, and the reacted materials are layered, and potassium dihydrogen phosphate is added to neutralize until the pH is 7.1. After neutralization, The material was centrifuged under the condition of 15000r / min to obtain a hydroxyl-terminated methyl vinyl silicone oil with a viscosity of 20cs, a ring body content of 30%, a hydroxyl content of 10%, and a vinyl content of 5%. The molecular formula is HO(SiMeViO) a (SiMe 2 O) b H, a=1~3, 5≤b≤20.

[0025] Knead 140g of 110-2 type methyl vinyl silicone rubber, 70g of white carbon black, and 5g of the above-mentioned hydroxyl-terminated methyl vinyl silicone oil on an open mill for 10 minutes, and after thinning, treat it in a blast drying oven at 190°C for 3 hours, add vulcanization The test performance after the agent is vulcanized, the tensile strength is 10.5MPa, and the tear strength is 25.2KN / m.

Embodiment 2

[0027] Dimethyldichlorosilane and methylvinyldichlorosilane were dripped into excess hydrochloric acid solution at a molar ratio of 40:1, wherein the mass concentration of hydrochloric acid solution was 22%, and the reacted materials were layered, adding Potassium dihydrogen phosphate was neutralized to a pH of 7.0, and the neutralized material was centrifuged at 15,000 r / min to obtain a hydroxyl-terminated methyl vinyl silicone oil with a viscosity of 18cs, a ring content of 27%, and a hydroxyl content of 9%. Vinyl content 2.5%, molecular formula HO(SiMeViO) a (SiMe 2 O) b H, a=1~3, 5≤b≤30.

[0028] Knead 140g of 110-2 type methyl vinyl silicone rubber, 70g of white carbon black, and 5g of the above-mentioned hydroxyl-terminated methyl vinyl silicone oil on an open mill for 10 minutes, and after thinning, treat it in a blast drying oven at 190°C for 3 hours, add vulcanization The test performance after the agent is vulcanized, the tensile strength is 10.7MPa, and the tear ...

Embodiment 3

[0030] Dimethyldichlorosilane and methylvinyldichlorosilane were dropped into excess calcium chloride aqueous solution at a molar ratio of 30:1, the reacted materials were layered, and sodium bicarbonate was added to neutralize until the pH was 7.1. Centrifuge the neutralized material at 17000r / min to obtain hydroxyl-terminated methylvinyl silicone oil with a viscosity of 21cs, a ring body content of 26%, a hydroxyl content of 10%, and a vinyl content of 3%. The molecular formula is HO( SiMeViO) a (SiMe 2 O) b H, a=1~3, 5≤b≤20.

[0031] Knead 140g of 110-2 type methyl vinyl silicone rubber, 70g of white carbon black, and 5g of the above-mentioned hydroxyl-terminated methyl vinyl silicone oil on an open mill for 10 minutes, and after thinning, treat it in a blast drying oven at 190°C for 3 hours, add vulcanization The test performance after the agent is vulcanized, the tensile strength is 10.4MPa, and the tear strength is 24.8KN / m.

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Abstract

The invention relates to a preparation process of a structure control agent, the structure control agent is alpha, omega-dihydroxy polydimethyl vinyl siloxane, which is called hydroxyl-terminated methyl vinyl silicone oil for short, the preparation process of the structure control agent comprises the following steps: (1) taking methyl vinyl dichlorosilane and dimethyl dichlorosilane as raw materials, and reacting at the temperature of 60-80 DEG C for 1-2 hours; carrying out hydrolysis reaction in a hydrolysis medium; (2) adjusting the hydrolysate obtained in the step (1) to be neutral by adopting a separation or neutralization method; and (3) dehydrating the hydrolysate obtained in the step (2) to obtain the hydroxyl-terminated methyl vinyl silicone oil. The process disclosed by the invention is high in production efficiency, low in energy consumption and low in production cost. Compared with traditional hydroxyl silicone oil, the obtained hydroxyl-terminated methyl vinyl silicone oil is more suitable for being used as a structure control agent, the phenomena that a rubber material is sticky in the mixing process and adheres to a film in the vulcanization process can be effectively reduced, meanwhile, the mechanical property of vulcanized silicone rubber can be improved, and the aging resistance of the vulcanized silicone rubber can be improved.

Description

technical field [0001] The invention relates to a destructure control agent and a preparation process thereof, in particular to a hydroxyl-terminated methyl vinyl silicone oil and a preparation process thereof, belonging to the technical field of chemical engineering. Background technique [0002] High temperature vulcanized silicone rubber is kneaded into mixed silicone rubber by high molar mass linear polysiloxane (referred to as raw silicone rubber) and reinforcing filler, extender filler, structure control agent, anti-yellowing agent and other fillers at a certain temperature. Then add a vulcanizing agent to vulcanize and form under certain temperature and pressure conditions. It has excellent stability, weather resistance, physiological inertness and many other characteristics. It has been widely used in the fields of electronic appliances, aerospace, automobiles and food daily chemicals. [0003] During the storage process, the mixed rubber gradually hardens, its plast...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/20C08L83/07
Inventor 陈泽雨孙刚李岩松彭靖杜宏伟田丽君詹欢欢
Owner HUBEI XINGRUI SILICON MATERIAL CO LTD
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