A kind of method that utilizes organosilicon azeotrope to produce ethyl orthosilicate

A technology of tetraethyl orthosilicate and azeotrope, which is applied in the field of reuse of by-products in the synthesis and production of organic silicon monomers in the chemical industry, to achieve the effects of sufficient supply, stable process and high yield

Active Publication Date: 2016-03-30
HOSHINE SILICON IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The invention provides a method for producing tetraethyl orthosilicate by using organosilicon azeotrope, which can effectively solve the by-product trimethylchlorosilane- Recycling and Utilization of Tetrachlorosilane-Hydrochlorosilane Azeotrope

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] (1) By-product azeotrope [(CH 3 ) 3 SiCl: 51.27wt%, SiCl 4 : 40.23wt%, CH 3 SiHCl 2 : 5.67wt%, HSiCl 3 : 1.12wt%, (CH 3 ) 2 SiHCl: 1.54wt%] was added to a still-type device with a packed tower for heating and distillation. Control the temperature at the bottom of the tower to 70-80°C, and the temperature at the top of the tower to about 40°C, and sequentially separate light components such as methylhydrogendichlorosilane, trichlorosilane, and dimethylhydrogenchlorosilane with a boiling point lower than 40°C. Obtain the intermediate mixture of silicon tetrachloride and trimethylchlorosilane in the kettle;

[0046] (2) Put the intermediate mixture obtained in step (1) into the esterification reaction kettle. At 25°C, first drop 1 / 3 of the ethanol used in this step into the intermediate mixture at 200L / h. Reflux reaction at 40°C for 2 hours, and then at 40°C, drop 2 / 3 of the ethanol used in this step into the partial esterification reaction solution at 300L / h, and ...

Embodiment 2

[0051] (1) By-product azeotrope [(CH 3 ) 3 SiCl: 50.12wt%, SiCl 4 : 40.77wt%, CH 3 SiHCl 2 : 6.37wt%, HSiCl 3 : 1.31wt%, (CH 3 ) 2 SiHCl: 1.43wt%] was added to a still-type device with a packed tower for heating and distillation. Control the temperature of the tower kettle at 70-80°C, and the temperature at the top of the tower at about 40°C, and sequentially separate light components such as methyldichlorosilane, trichlorosilane, and dimethylhydrochlorosilane with boiling points lower than 40°C. Obtain the intermediate mixture of silicon tetrachloride and trimethylchlorosilane in;

[0052] (2) Put the intermediate mixture obtained in step (1) into the esterification reaction kettle. At 30°C, first drop 1 / 2 of the ethanol used in this step into the intermediate mixture at 250L / h. Reflux reaction at 45°C for 1 hour, and then at 45°C, drop 1 / 2 of the ethanol used in this step into the partial esterification reaction solution at 350L / h, and raise the temperature to 50°C f...

Embodiment 3

[0057] (1) By-product azeotrope [(CH 3 ) 3 SiCl: 53.41wt%, SiCl 4 : 38.59wt%, CH 3 SiHCl 2 : 5.37wt%, HSiCl 3 : 1.31wt%, (CH 3 ) 2 SiHCl: 1.16wt%] was added to a still-type device with a packed tower for heating and distillation. Control the temperature of the tower kettle at 70-80°C, and the temperature at the top of the tower at about 40°C, and sequentially separate light components such as methyldichlorosilane, trichlorosilane, and dimethylhydrochlorosilane with boiling points lower than 40°C. Obtain the intermediate mixture of silicon tetrachloride and trimethylchlorosilane in;

[0058] (2) Put the intermediate mixture obtained in step (1) into the esterification reaction kettle. At 25°C, first drop 1 / 2 of the ethanol used in this step into the intermediate mixture at 250L / h. Reflux reaction at 40°C for 2 hours, and then at 40°C, drop 1 / 2 of the ethanol used in this step into the partial esterification reaction solution at 300L / h, and then raise the temperature to ...

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Abstract

The invention discloses a method for producing tetraethyl orthosilicate by use of organic silicon azeotrope, which comprises the following steps of: (1) heating to distill organic silicon azeotrope, and removing the fraction with a boiling point lower than 40 DEG C to obtain an intermediate mixture; (2) mixing the intermediate mixture and ethanol for the first two-step intermittent esterification reaction; heating to distill the reaction liquid; and collecting the fraction with a boiling point not lower than 80 DEG C; and (3) mixing the fraction with a boiling point not lower than 80 DEG C and ethanol for the second esterification reaction; and separating and purifying to obtain tetraethyl orthosilicate. According to the method disclosed by the invention, the raw material azeotrope is cheap, and the supply is sufficient; a toxic and harmful solvent is not needed in the reaction process, the reaction conditions are mild, the technology is stable, and the continuous production efficiency is high; and the content of the obtained finished product of tetraethyl orthosilicate is over 99%, and the content of chloride ions is less than 100ppm.

Description

technical field [0001] The invention relates to the technical field of recycling by-products in the synthesis and production of organosilicon monomers in the chemical industry, in particular to a method for producing ethyl orthosilicate by using organosilicon azeotropes. Background technique [0002] Organosilicon materials are mainly a kind of polymer compound with Si-O bond as the main chain, and then introduce organic groups as side chains on Si. It has excellent performance and unique functions, and is widely used in military industry, aerospace, medical treatment, chemical industry, etc. field, where (CH 3 ) 2 SiCl 2 It is the most important organosilicon monomer. Since American Luo Qiao (US2380995) invented the method of directly synthesizing organochlorosilane by using methyl chloride and silicon powder under the catalysis of copper powder in 1941, the synthesis technology of methyl chlorosilane has been developed for more than half a century and has been perfected...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): C07F7/18
Inventor方红承彭金鑫刘国旺毛利俊陈浪涛谭军欧阳玉霞
OwnerHOSHINE SILICON IND CO LTD