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Ethyl polysilicate synthesizing process

A polyethyl silicate and synthesis process technology, applied in the field of silicon chemical industry, can solve problems such as method disclosure, and achieve the effects of reducing production costs, significant economic and social benefits, and alleviating environmental protection pressures

Inactive Publication Date: 2011-07-06
淄博市临淄齐泉工贸有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

How to use the by-product silicon tetrachloride in the production to synthesize ethyl silicate with a certain degree of polymerization has become a widely concerned issue in related fields, but no practical method has been disclosed.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] According to the mass ratio of silicon tetrachloride and ethanol 1:0.8, the by-produced silicon tetrachloride is measured and put into the reactor, and then the active iron powder with the amount of silicon tetrachloride 0.05% is added. Add 1% ethanol containing water to the specified liquid level in the ethanol high level tank, and set it aside.

[0015] Then turn on the vacuum pump to evacuate, control the vacuum degree of 0.01-0.05MPa, and gradually add ethanol dropwise to the reaction kettle. Reflux, the HCl produced during the reaction is absorbed by water to produce hydrochloric acid by-product, and after about half an hour of reflux, the temperature is raised to evaporate unreacted ethanol. After the distillation, the solution is cooled down, a certain amount of activated carbon is added, stirred and precipitated for one hour, and then filtered. The filtrate is transferred to a finished product tank, and after passing the analysis, it is loaded into barrels to ob...

Embodiment 2

[0017] According to the mass ratio of silicon tetrachloride and ethanol 1:1.2, the by-produced silicon tetrachloride is metered and put into the reactor, and then the active iron powder with the amount of silicon tetrachloride 0.5% is added. Add water-containing 10% ethanol to the specified liquid level in the ethanol high level tank, and set it aside.

[0018] Turn on the vacuum pump to evacuate, control the vacuum degree of 0.01-0.05MPa, gradually add ethanol to the reaction kettle dropwise, the reaction will be rapid after dropping, and control the reaction speed by controlling the amount of ethanol added dropwise; after all the ethanol is added, the reaction kettle will be heated slowly Reflux, the HCl produced during the reaction is absorbed by water to produce hydrochloric acid by-product, and after about half an hour of reflux, the temperature is raised to distill unreacted ethanol. After the distillation, the solution is cooled down, a certain amount of activated carbo...

Embodiment 3

[0020] According to the mass ratio of silicon tetrachloride and ethanol 1:1, put the by-product silicon tetrachloride into the reaction kettle after metering, and then add active zinc powder with a silicon tetrachloride content of 0.25%; 5% ethanol to the specified level, set aside.

[0021] Turn on the vacuum pump to evacuate, control the vacuum degree of 0.01-0.05MPa, gradually add ethanol to the reaction kettle dropwise, the reaction will be rapid after dropping, and control the reaction speed by controlling the amount of ethanol added dropwise; after all the ethanol is added, the reaction kettle will be heated slowly Reflux, the HCl produced during the reaction is absorbed by water to produce hydrochloric acid by-product, and after about half an hour of reflux, the temperature is raised to distill unreacted ethanol. After the distillation, the solution is cooled down, a certain amount of activated carbon is added, stirred and precipitated for one hour, and then filtered. T...

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PUM

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Abstract

The present invention relates to an ethyl polysilicate synthesizing process comprising the following steps: firstly quantitative byproduct silicon tetrachloride and active metal powder are added into a kettle, alcohol is slowly dropwise added at certain negative pressure to be mixed and react, warming and refluxing are carried out after adding is finished for complete reaction, and HCL produced during reaction is absorbed by water; reaction liquid is heated for distillation after reaction is completed, unreacted alcohol is expelled, then residual liquid at the bottom of the kettle is cooled and added with active carbon for decolouration filtering, and the filtrate is the ethyl silicate. Product purity and yield of the ethyl silicate obtained by adopting the process for production can meet market requirements, production control is extremely stable, not only production cost is reduced while improving revenue, but also environmental pollution is avoided, thereby having significant economic benefit and social benefit.

Description

technical field [0001] The invention relates to a production process of polyethyl silicate, in particular to a process for directly synthesizing ethyl silicate with relatively low-purity by-product silicon tetrachloride, belonging to the technical field of silicon chemical industry. Background technique [0002] Ethyl polysilicate (often referred to as ethyl silicate) is mainly used in chemical-resistant coatings and heat-resistant coatings, organic silicon solvents, investment casting adhesives, and inorganic zinc-rich primers. At present, the production of ethyl silicate mostly adopts the following production process: pure silicon tetrachloride and ethanol are reacted in batch kettles, the synthetic liquid after reaction is rectified, and then the unreacted ethanol is distilled out to obtain ethyl silicate. Due to the low purity of the by-product silicon tetrachloride in the production of related enterprises, such as in the production of chloropropyl coupling agent, a cert...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/02
Inventor 乌洪涛齐峰全刘荣森
Owner 淄博市临淄齐泉工贸有限公司
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