Preparation method of ethyl silicate

A preparation process, a technology of ethyl silicate, applied in the directions of silicon organic compounds, chlorine/hydrogen chloride, etc., can solve the problems of low economic efficiency of hydrochloric acid, multiple operating costs, and reduced yield, and achieve clean production, significant economic and social Benefit, the effect of improving yield

Inactive Publication Date: 2014-12-31
TAICANG GOLDEN ANCHOR CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The market sales volume of this part of silicon tetrachloride is very little. In order to ensure production and prevent environmental pollution at the same time, the usual practice of enterprises is: first, absorb silicon tetrachloride with water to produce hydrochloric acid, but the economic efficiency of producing hydrochloric acid by this method is low; Ethyl silicate is produced after purification, but if the purification is carried out, more operating costs need to be increased, the cost is high, and the yield will also decrease

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Be 80% silicon tetrachloride and 95% ethanol 1:0.8 mass ratio batching by 200g content, put into reactor after silicon tetrachloride is measured, then add silicon tetrachloride amount 0.1% Active copper powder 0.2g. Add 95% ethanol to the specified liquid level in the ethanol high level tank, and set aside. Then turn on the vacuum pump to evacuate, control the vacuum degree of 0.01-0.05MPa, and gradually add ethanol to the reaction kettle dropwise. Slowly raise the temperature of the kettle to reflux. The HCl produced during the reaction is absorbed by water to produce hydrochloric acid by-product. After reflux for about 0.5 hours, the temperature is raised to evaporate unreacted ethanol. After the distillation, the solution was cooled down, a certain amount of activated carbon was added, stirred and precipitated for one hour, and then filtered, the filtrate was distilled to remove ethanol, and the fraction at 160-180°C was collected to obtain ethyl silicate 206 with a...

Embodiment 2

[0022] Be 80% silicon tetrachloride and 95% ethanol 1:1 mass ratio batching by 100g content, put into reactor after silicon tetrachloride is metered, then add the active copper of silicon tetrachloride amount 0.8% Powder 0.8g. Add 95% ethanol to the specified liquid level in the ethanol high level tank, and set aside. Then turn on the vacuum pump to evacuate, control the vacuum degree of 0.01-0.05MPa, and gradually add ethanol to the reaction kettle dropwise. Slowly raise the temperature of the kettle to reflux. The HCl produced during the reaction is absorbed by water to produce hydrochloric acid by-product. After reflux for about 0.5 hours, the temperature is raised to evaporate unreacted ethanol. After the distillation, the solution was cooled down, a certain amount of activated carbon was added, stirred and precipitated for one hour, and then filtered, the filtrate was distilled to remove ethanol, and the fraction at 160-180°C was collected to obtain ethyl silicate 105 wi...

Embodiment 3

[0024] Be 90% silicon tetrachloride and 95% ethanol 1:1.2 mass ratio batching by 150g content, put into reactor after silicon tetrachloride is measured, then add the active zinc of silicon tetrachloride amount 0.2% Powder 0.3g. Add 95% ethanol to the specified liquid level in the ethanol high level tank, and set aside. Then turn on the vacuum pump to evacuate, control the vacuum degree of 0.01-0.05MPa, and gradually add ethanol to the reaction kettle dropwise. Slowly raise the temperature of the kettle to reflux. The HCl produced during the reaction is absorbed by water to produce hydrochloric acid by-product. After about 1 hour of reflux, the temperature is raised to evaporate unreacted ethanol. After the distillation, the solution was cooled down, a certain amount of activated carbon was added, stirred and precipitated for one hour, then filtered, the filtrate was distilled to remove ethanol, and the fraction at 160-180°C was collected to obtain ethyl silicate 158 with a yi...

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PUM

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Abstract

The invention relates to a preparation method of ethyl silicate, and the preparation method comprises the following preparation process: (1) first, adding a weighed silicon tetrachloride crude product and an active metal catalyst into a reactor, and adding an ethanol solution into an elevated tank; (2) in a certain vacuum degree, gradually dripping the ethanol into the reactor, after the dripping, rapidly reacting, regulating the reaction speed through control of the amount of the dripped ethanol; after the ethanol is completely dripped, slowly heating the reactor for reflux, using water to absorb HC1 produced during the reaction to produce by-product hydrochloric acid, after about 0.5 to 1 hour of reflux, heating to evaporate out unreacted ethanol; and (3) at the end of the reaction, cooling to room temperature, decolorizing with activated carbon, distilling to remove the ethanol, and collecting 160-180 DEG C fractions. The method can effectively solve and use the silicon tetrachloride crude product, avoids environmental pollution, achieves cleaner production, reduces production cost, improves yield, and has significant economic and social benefits.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation process of ethyl silicate. Background technique [0002] 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 certain amount of silicon tetrachloride will inevitably be produced as a side reaction. The market sales volume of this part of silicon tetrachloride is very little. In order to ensure pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/04C01B7/01
Inventor 施兆武
Owner TAICANG GOLDEN ANCHOR CHEM CO LTD
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