Method for preparing hydroxy terminated high-boiling silicone oil through low-temperature continuous hydrolysis technology

A hydroxyl-terminated, high-boiling silicone oil technology, which is applied in the field of silicone production, can solve the problems of easy emulsification of high-boiling silicone oil, easy product return to acid, alcohol-containing waste acid, and inability to properly handle waste neutralizer flux, etc. No three wastes discharge, stable product quality, avoid excessive cross-linking effect

Inactive Publication Date: 2017-02-22
TANGSHAN SANYOU SILICON IND
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  • Abstract
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Problems solved by technology

[0004] The object of the present invention is to provide a production method for preparing hydroxyl-terminated high-boiling silicone oil by a continuous hydrolysis process of methyl chlorosilane high-boiling matter, so as to solve the problem of alcohol-containing waste acid, alcohol-containing waste acid, The problem that was

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  • Method for preparing hydroxy terminated high-boiling silicone oil through low-temperature continuous hydrolysis technology

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Embodiment 1

[0034] A method for preparing hydroxyl-terminated high-boiling silicone oil by a low-temperature continuous hydrolysis process, the process steps are as follows:

[0035] ①Pretreatment of high boilers: Use a rectification device to rectify the by-product high-boiling chlorosilane mixtures (substances with a boiling point greater than 70.5°C under standard conditions) in the process of direct synthesis of methyl chlorosilanes, and collect them under standard conditions The fraction with a boiling range between 70.5°C and 160°C is used in the hydrolysis process to prepare hydroxyl-terminated high-boiling silicone oil.

[0036] ②Preparation of aqueous solution for hydrolysis: prepare the hydrolysis aid ferric chloride and production water to prepare an aqueous solution for hydrolysis with a catalyst mass concentration of 0.5%.

[0037] ③Hydrolysis: The methyl chlorosilane high boiler with a boiling range of 70.5℃~160℃ and the aqueous solution for hydrolysis are continuously pumpe...

Embodiment 2

[0043] A method for preparing hydroxyl-terminated high-boiling silicone oil by a low-temperature continuous hydrolysis process, the process steps are as follows:

[0044] ①Pretreatment of high boilers: Use a rectification device to rectify the by-product high-boiling chlorosilane mixtures (substances with a boiling point greater than 70.5°C under standard conditions) in the process of direct synthesis of methyl chlorosilanes, and collect them under standard conditions The fraction with a boiling range between 70.5°C and 140°C is used in the hydrolysis process to prepare hydroxyl-terminated high-boiling silicone oil.

[0045] ②Preparation of aqueous solution for hydrolysis: The hydrolysis aid sodium trifluoromethanesulfonate and hydrolysis acid are prepared to prepare an aqueous solution for hydrolysis with a mass concentration of catalyst of 1%.

[0046] ③Hydrolysis: The methyl chlorosilane high boiler with a boiling range of 70.5℃~140℃ and the aqueous solution for hydrolysis ...

Embodiment 3

[0052] A method for preparing hydroxyl-terminated high-boiling silicone oil by a low-temperature continuous hydrolysis process, the process steps are as follows:

[0053] ①Pretreatment of high boilers: Use a rectification device to rectify the by-product high-boiling chlorosilane mixtures (substances with a boiling point greater than 70.5°C under standard conditions) in the process of direct synthesis of methyl chlorosilanes, and collect them under standard conditions The fraction with a boiling range between 70.5°C and 140°C is used in the hydrolysis process to prepare hydroxyl-terminated high-boiling silicone oil.

[0054] ②Preparation of aqueous solution for hydrolysis: The hydrolysis aid sodium trifluoromethanesulfonate and hydrolysis acid are prepared to prepare an aqueous solution for hydrolysis with a mass concentration of catalyst of 1%.

[0055] ③Hydrolysis: The methyl chlorosilane high boiler with a boiling range of 70.5℃~140℃ and the aqueous solution for hydrolysis ...

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Abstract

The invention belongs to the technical field of organic silicon production, and particularly relates to a method for preparing hydroxy terminated high-boiling silicone oil through a continuous hydrolysis technology in the condition of low temperature of organosilicon high-boiling components. The method comprises the following steps: performing rectifying treatment on chlorosilane compound with the boiling point of byproducts being greater than 70.5 DEG C during the synthesis of methyl chlorosilane through a rectification device and a direct method; collecting the fraction with the boiling range being 70.5 to 180 DEG C in a standard condition; performing low-temperature hydrolysis reaction through a hydrolysis assistant solution with certain concentration. According to the method, the technical problem that organosilicon high-boiling component hydrolysis is easy to cause crosslinking and emulsification through the steps of continuous hydrolysis, water washing, alkali washing, telomerization and filtering, hydroxy terminated high-boiling silicone oil products are produced, and the fact that hydrogen chloride produced through high-boiling component hydrolysis is directly applied to methyl chloride synthesis after being subjected to purification is realized. The method has the advantages that the production automation degree is high, the product quality is stable, active silicon hydroxyl at the molecular chain end of a product is wide in application range, three waste discharge does not exist in the whole technology, and clean and environment-friendly continuous production is realized.

Description

technical field [0001] The invention belongs to the technical field of organosilicon production, and in particular relates to a method for preparing hydroxyl-terminated high-boiling silicone oil by adopting a continuous hydrolysis process of organosilicon high-boilers under low temperature conditions. Background technique [0002] At present, the direct synthesis of methylchlorosilane monomer is generally adopted at home and abroad, and about 5-10% of high boiling substances are produced for every ton of crude monomer synthesized. With the rapid development of my country's organic silicon industry, by the end of 2015, the total production capacity of methyl chlorosilane in my country reached 2.8 million tons / year, the total output exceeded 1.8 million tons / year, and the by-product high boiling substances exceeded 150,000 tons / year. However, due to the complex composition of high boilers, difficulty in separation and utilization, and strong corrosiveness, it has become a prob...

Claims

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Application Information

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IPC IPC(8): C08G77/16C08G77/36C08G77/32
CPCC08G77/16C08G77/32C08G77/36
Inventor 陈春江孙长江曹鹤李献起周健张书文刘秋艳张鹏硕赵洁
Owner TANGSHAN SANYOU SILICON IND
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