Method for compositing trialkoxysilanes by adopting multistage fluidized bed

A technology of trialkoxysilane and fluidized bed, which is applied in the field of synthesis of trialkoxysilane, can solve the problems of low productivity of silicon-copper contacts, easy hydrolysis of products, and difficult recovery of catalysts, etc., so as to improve the utilization rate of raw materials, The effect of reducing production cost and improving the utilization rate of alcohol

Active Publication Date: 2010-03-17
WUXI HAITE NEW MATERIAL RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to solve the problem of difficulty in catalyst recovery, low reaction efficiency, difficult separation of products, poor contact between silicon powder and copper catalysts, low productivity of silicon-copper contacts and low re

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  • Method for compositing trialkoxysilanes by adopting multistage fluidized bed
  • Method for compositing trialkoxysilanes by adopting multistage fluidized bed
  • Method for compositing trialkoxysilanes by adopting multistage fluidized bed

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specific Embodiment approach 1

[0021] Specific implementation mode 1: In this embodiment, a method for synthesizing trialkoxysilane in a multi-stage fluidized bed is achieved through the following steps:

[0022] 1. Preparation of silicon-copper contact: a. Place 100-350 mesh metallurgical-grade silicon powder in a mixed acid of hydrofluoric acid and nitric acid for etching under the action of ultrasound. The etching time is 0.5-2min, then The etched silicon powder is rinsed to neutrality and then dried, wherein the ratio of the amount of hydrofluoric acid and nitric acid is (1 / 10-10):1;

[0023] b. Add the silicon powder etched in step a to the copper-based catalyst pre-precipitation solution, vacuum, and then under the action of ultrasound, add precipitation initiator to the mixture of silicon powder and copper-based catalyst pre-precipitation solution until there is no The precipitate is formed, then filtered, and vacuum-dried to obtain a copper-based catalyst-coated silicon powder composite, and then pretrea...

specific Embodiment approach 2

[0031] Specific embodiment two: This embodiment is different from the specific embodiment one in that the preparation method of the cuprous chloride catalyst pre-precipitation liquid in step b of step one is: adopting a wet method to combine copper chloride, copper powder, sodium chloride and Concentrated hydrochloric acid is mixed to prepare a cuprous chloride pre-precipitation solution, the precipitation initiator is deionized water, the mass ratio of copper chloride to copper powder is 1:1 to 1.5, and the ratio of copper chloride to sodium chloride is 1: 1.5~2.5, the mass ratio of copper chloride to concentrated hydrochloric acid is 1:5~8. Other steps and parameters are the same as in the first embodiment.

[0032] The mass concentration of the cuprous chloride pre-precipitation solution prepared in this embodiment is 2%-10%. In this embodiment, a copper-silicon contact body coated with cuprous chloride is obtained.

specific Embodiment approach 3

[0033] Specific embodiment three: this embodiment is different from specific embodiment one in the preparation method of the copper hydroxide catalyst pre-precipitation solution in step b of step one: copper sulfate is dissolved in deionized water and configured to have a mass fraction of 10%~ The 20% copper sulfate solution is the copper hydroxide catalyst pre-precipitation solution for preparing the copper hydroxide catalyst, and the precipitation initiator is sodium hydroxide.

[0034] In this embodiment, a copper hydroxide-coated silicon copper contact body is obtained.

[0035] In this embodiment, acetic acid or nonanoic acid is used instead of the precipitation initiator sodium hydroxide to obtain a copper-silicon contact body coated with copper acetate or copper nonanoate catalyst.

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Abstract

A method for compositing trialkoxysilanesby adopting a multistage fluidized bed relates to a composite method of trialkoxysilanesby. The composite method solves the problems that in the existing composite technology of trialkoxysilanesby, catalytic agent is difficult to be recycled, reactive efficiency is low, products are difficult to be separated, silica powder and copper-based catalytic agent have poor contact, copper silicon contacts have slow productivity and low reactive activity, the catalytic agent loses effectiveness easily after meeting water, and the products are easily hydrolyzed after meeting water. The composite method of trialkoxysilanesby comprises the following steps: 1. preparing copper silicon contacts containing different cuprous chloride mass percents; 2. charging copper silicon contacts obtained in the step one to a reactor of the multistage fluidized bed in stages; and 3. introducing alcohol gas dried by ethyl orthosilicate into the reactor of the multistage fluidized bed to obtain trialkoxysilanesby after reaction and composition. By adopting the method for compositing trialkoxysilanes by adopting the multistage fluidized bed, the selectivity of trialkoxysilanesby reaches 95% and reactive transformation ratio reaches 95%.

Description

Technical field [0001] The invention relates to a method for synthesizing trialkoxysilane. Background technique [0002] At present, the synthesis method of trialkoxysilane mainly adopts the direct method. In the direct method, a kettle-type slurry reactor is mostly used. The reaction process requires a solvent as a suspending agent. The problems that this brings are: ① Increase the operating cost of the reaction. ② It is difficult to recover the catalyst and the remaining silicon powder after the reaction. ③ It hinders the direct contact between the silicon powder and the alcohol vapor. ④ It is not conducive to product separation and purification. Moreover, during the reaction process, a silicon dioxide film is formed due to the oxidation of the silicon powder surface, resulting in poor contact between the silicon powder and the copper-based catalyst, low silicon-copper contacts, low reactivity, and the presence of trace water in the reaction system. Catalyst failure, product h...

Claims

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Application Information

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IPC IPC(8): C07F7/18B01J27/128B01J23/72
Inventor 杨春晖张磊李季杨恺胡成发葛士彬
Owner WUXI HAITE NEW MATERIAL RES INST
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