Method and device for producing liquid polycarbosilane precursor material

Abstract

The invention discloses a method and a device for producing a liquid polycarbosilane precursor material. Chloromethyl trichlorosilane and methanol are used as raw materials, chloromethyl alkoxy chlorosilane is synthesized by an alcoholysis method through a packed tower reactor, the chloromethyl trichlorosilane is quantitatively sprayed into a packed tower through a sprayer from the tower top, and after being gasified, methanol is divided into three paths according to a certain molar mass ratio to enter the packed tower, and is subjected to contact reaction with the sprayed chloromethyl trichlorosilane in three steps in a packing part, so that the molar mass ratio of chloromethyl methoxydichlorosilane to chloromethyl dimethoxychlorosilane to chloromethyl trimethoxysilane which are products is strictly controlled; the liquid polycarbosilane is synthesized by using the finally obtained chloromethyl alkoxy chlorosilane with an ideal ratio, the number-average molecular weight of the obtained liquid polycarbosilane is 700-1000, the oxygen content is lower than 1.5%, and the ceramic yield is as high as 70-80%; and the production process is relatively simple, the reaction rate is high, the energy consumption is relatively low, the content of byproducts in the product is low, and continuous production can be realized.

Description

technical field [0001] The invention relates to the technical field of ceramic precursor materials, in particular to a production method and device for a liquid polycarbosilane precursor material. Background technique [0002] Liquid polycarbosilane (LPCS) is an ideal precursor for the preparation of silicon carbide (SiC) ceramic matrix composites. The Grignard coupling method is the main method for synthesizing liquid polycarbosilanes. The raw material for synthesizing liquid polycarbosilane by Grignard coupling method is chloromethyltrichlorosilane and its analogues, which are polymerized by head-to-tail polymerization through Grignard reagent coupling reaction. [0003] Chloromethyltrichlorosilane (Cl 3 SiCH 2 Cl) and methanol carry out alkoxylation reaction in a certain proportion, and a certain ratio of chloromethyltrimethoxysilane with 1 functional group degree, chloromethyldimethoxychlorosilane with 2 functional group degree and 3 functional group can be obtained b...

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Problems solved by technology

[0005] The existing device used to prepare methylated chlorosilane is to add chloromethyltrichlorosilane to the reaction kettle, then drop methanol at a controlled rate, use nitrogen or dry air to bubble, and react at room temperature to obtain chloromethyl alkane Oxychlorosilane, then there will be the following problems: 1. The process route for preparing chloromethylalkoxychlorosilane in a tank reactor is to drop into chloromethyltrichlorosilane first, and then control a certain rate to drop quantitative Methanol, this kind of one-p

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