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Method for preparing hexamethyldisiloxane by using organic silicon by-product

A technology of hexamethyldisiloxane and trimethylmonochlorosilane, applied in the field of organosilicon by-product production, can solve the problems of limitation, high cost, difficult purification and recovery, etc., so as to reduce the load of the acid removal process and reduce the industrial Production cost, the effect of reducing production cost

Inactive Publication Date: 2015-11-18
HUBEI XINGRUI SILICON MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent CN101362777A has invented a method for preparing hexamethyldisiloxane, by reacting trimethylmonochlorosilicon with carbonate, and then collecting hexamethyldisiloxane by steaming. The process of this method is simple, but Due to the addition of solid salts in the preparation process, it is difficult to purify and recycle, and the cost is high, which limits the application of this technology; Chinese patent CN103951692A provides a method for preparing high-purity and high-quality hexamethyldisiloxane. Chlorotrimethylsilane is added dropwise to the hydrolysis reaction kettle pre-added with water and condensation catalyst to react. The hydrolyzate is divided into three layers after standing, and the hydrolyzate in the upper layer is washed with water, neutralized with alkali solution, dewatered, filtered, Fractional distillation obtains hexamethyldisiloxane with a higher mass fraction. This method uses a condensation catalyst to promote the efficiency of the hydrolysis reaction, and the prepared product has a higher mass fraction. However, the technical process is long, complicated, and involves operations such as filtration. , which reduces the yield of hexamethyldisiloxane to a certain extent, which limits the promotion of this technology

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 2kg of organosilicon by-product trimethyl-chlorosilane to the enamel reaction kettle, turn on the cooling device of the reaction kettle and blow back the compressed air at the bottom of the reaction kettle; add 4kg of recovered dilute hydrochloric acid to the reaction kettle dropwise to maintain the temperature in the kettle At 15±5°C; after the hydrolysis reaction is completed, the hydrolyzed product is transported to the standing tank for 30 minutes to separate the acidic water in the lower layer to obtain crude hexamethyldisiloxane; wash the product 3 times with 4.5kg of process water After the crude product is left to stand for stratification, all the dilute hydrochloric acid solution in the lower layer is collected, and the upper layer solution is transported to the rectification tower. Under normal pressure, the fraction at 99~102°C is collected to be refined hexamethyldisiloxane. Among them: yield: about 95%, refractive index (25°C): 1.3735, specific gravity (...

Embodiment 2

[0019] Other implementation conditions are the same as in 1. When 5kg of dilute hydrochloric acid produced by washing is added dropwise, when the washing process water used is 5.5kg, the yield of hexamethyldisiloxane obtained is about 93%, and the refractive index (25°C): 1.3745 , Specific gravity (25°C): 0.765, Hexamethyldisiloxane content: 99.54%.

Embodiment 3

[0021] Other implementation conditions are the same as 1. When 6kg of dilute hydrochloric acid produced by washing is added dropwise, and when the washing process water used is 6.5kg, the yield of hexamethyldisiloxane obtained is about 92%, and the refractive index (25°C): 1.3744 , Specific gravity (25°C): 0.767, Hexamethyldisiloxane content: 99.52%.

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Abstract

The invention provides a method for preparing hexamethyldisiloxane by using an organic silicon by-product. According to the method, the organic silicon by-product chlorotrimethylsilane and recycled washing diluted hydrochloric acid are subjected to hydrolysis under a certain condition, hydrogen chloride gas generated by hydrolysis is removed through reverse blowing of compressed air, after reaction is compelled, the product is left to stand for layering, and an upper solution is washed with water for multiple times for deacidification and then rectified at normal pressure, so that the hexamethyldisiloxane finished product is obtained. Practice proves hexamethyldisiloxane prepared through the method provided by the invention is stable in quality, simple in process and easy to produce industrially and the comprehensive utilization value of the organic silicon by-product chlorotrimethylsilane is increased greatly.

Description

technical field [0001] The invention belongs to the technical field of organosilicon by-product production, and in particular relates to a method for preparing hexamethyldisiloxane by utilizing organosilicon by-product trimethylmonochlorosilane. Background technique [0002] With the rapid development of the organosilicon industry, the output of organosilicon chlorosilane monomers is also increasing. It is estimated that by the end of this year, the total production capacity of domestic organosilicon monomer manufacturers will be about 2500kt / a. Trimethylchlorosilane is one of the by-products of the production of organosilylchlorosilane monomers, accounting for about 3% of monomer production capacity. The molecular structure contains Si-Cl bonds. Therefore, it is necessary to comprehensively utilize the substance from the aspects of saving production cost and safety and environmental protection. [0003] Hexamethyldisiloxane is an important primary raw material for organosi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/08
Inventor 王文金陈冠炎刘宏彬颜昌锐
Owner HUBEI XINGRUI SILICON MATERIAL CO LTD
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