Method for synthesizing ethyl chloride by using gas phase hydrogen chloride and ethanol

A synthesis method and hydrogen chloride technology, applied in chemical instruments and methods, chemical industry, organic chemistry, etc., can solve the problems of many by-products, low product yield, harsh reaction conditions, etc., to improve equipment production capacity and reduce wastewater treatment capacity. , the effect of saving energy

Inactive Publication Date: 2013-01-02
JIANGSU ZHENFANG BIO CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] There are three synthesis methods of ethyl chloride: the addition of ethylene and hydrogen chloride, the chlorination of ethane, and the synthesis by the reaction of hydrochloric acid and ethanol; the first method uses ethylene, because ethylene has high requirements for transportation and storage equipment, and the reaction Harsh conditions require high temperature and high pressure; the second method, the ethane chlorination method, has mild reaction conditions, but there are many by-products. While the chlorination reaction generates ethyl chloride, dichloroethane and trichloroethane are also generated. Such a product separation and purification system is relatively complicated, and the product yield is low; at present, the third synthetic method is mainly adopted in China, and hydrochloric acid and ethanol synthesize ethyl chloride at a reaction temperature of 110-145 ° C and anhydrous zinc chloride as a catalyst. During the reaction process, hydrochloric acid is brought into the water in the reaction system, and the water in the reactor needs to be steamed out with steam. For every ton of ethyl chloride produced, 3.5 tons of steam are consumed. In addition, the amount of waste water produced is large, and each ton of product produces 2.05 tons of ethanol-containing wastewater

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Example 1: Put anhydrous zinc chloride into the reaction kettle, and slowly raise the temperature to 85°C with steam; the hydrogen chloride gas in the buffer tank enters the reaction kettle through the flowmeter through the bottom pipe, and continuously adds ethanol into the reaction kettle with a pump , the molar ratio of hydrogen chloride and ethanol is controlled to be 1.02:1 by the flow meter respectively, the temperature of the reactor is regulated by the jacket steam, the steam pressure of the jacket of the reactor is controlled at 5KG / cm2, and the temperature in the reactor is 135°C; the ethyl chloride gas produced by the reaction , water, and unreacted ethanol are condensed by the condenser, the water and alcohol are recovered to the liquid receiving tank, and transported to the raw material tank of the alcohol rectification tower by a pump, and ≥92% ethanol is recovered from the top of the tower, which is applied mechanically; the gaseous ethyl chloride is washed...

Embodiment 2

[0011] Example 2: Put anhydrous zinc chloride into the reaction kettle, and slowly raise the temperature to 85°C with steam; the hydrogen chloride gas in the buffer tank enters the reaction kettle through the flowmeter through the bottom pipe, and continuously adds ethanol into the reaction kettle with a pump , the molar ratio of hydrogen chloride and ethanol is controlled to be 1.025:1 by the flow meter respectively, the temperature of the reactor is regulated by the jacket steam, the steam pressure of the jacket of the reactor is controlled at 5.25KG / cm2, and the temperature in the reactor is 128°C; the ethyl chloride produced by the reaction The gas, water, and unreacted ethanol are condensed by the condenser, the water and alcohol are recovered to the liquid receiving tank, and transported to the raw material tank of the alcohol rectification tower by a pump, and ≥92% ethanol is recovered at the top of the tower, which is applied mechanically; the gaseous ethyl chloride pass...

Embodiment 3

[0012] Example 3: Put anhydrous zinc chloride into the reaction kettle, and slowly raise the temperature to 85°C with steam; the hydrogen chloride gas in the buffer tank enters the reaction kettle through the flowmeter through the bottom pipe, and continuously adds ethanol into the reaction kettle with a pump , the molar ratio of hydrogen chloride and ethanol is controlled by a flow meter to be 1.03:1, the temperature of the reactor is regulated by the jacket steam, the steam pressure of the jacket of the reactor is controlled at 5.5KG / cm2, and the temperature in the reactor is 120°C; the ethyl chloride produced by the reaction The gas, water, and unreacted ethanol are condensed by the condenser, the water and alcohol are recovered to the liquid receiving tank, and transported to the raw material tank of the alcohol rectification tower by a pump, and ≥92% ethanol is recovered at the top of the tower, which is applied mechanically; the gaseous ethyl chloride passes through Washi...

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PUM

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Abstract

The invention discloses a method for synthesizing ethyl chloride by using gas phase hydrogen chloride and ethanol. The synthesis method is as below: adding anhydrous zinc chloride to a reaction kettle; slowly heating to 85 DEG C by steam; passing the hydrogen chloride gas through a flowmeter, and introducing hydrogen chloride gas to the reaction kettle through an inserting tube in a buffer tank; and at the same time, continuously adding ethanol into the reaction kettle by a pump, respectively controlling a molar ratio of hydrogen chloride to ethanol at 1.02-1.03:1 by the flowmeter; regulating the temperature of the reaction kettle by jacket steam, and controlling the reaction kettle jacket steam pressure at 5-5.5 KG / cm<2>, and the temperature of the reaction kettle at 120-135 DEG C; condensing ethyl chloride gas and water generated by the reaction and unreacted ethanol by a condenser; recovering water and alcohol to a liquid receiving tank, and pumping the water and alcohol to a material groove of an alcohol distillation column for indiscriminate application; successively subjecting the ethyl chloride gas to water washing, alkaline washing and concentrated sulfuric acid drying; and finally condensing by frozen brine to obtain a liquid ethyl chloride product. The invention has advantages of simple process, easy operation, reduced treatment amount of waste water, energy saving and improved efficiency.

Description

technical field [0001] The invention relates to a synthesis method, in particular to a method for synthesizing ethyl chloride by utilizing gas phase hydrogen chloride and ethanol. Background technique [0002] There are three synthesis methods of ethyl chloride: the addition of ethylene and hydrogen chloride, the chlorination of ethane, and the synthesis by the reaction of hydrochloric acid and ethanol; the first method uses ethylene, because ethylene has high requirements for transportation and storage equipment, and the reaction Harsh conditions require high temperature and high pressure; the second method, the ethane chlorination method, has mild reaction conditions, but there are many by-products. While the chlorination reaction generates ethyl chloride, dichloroethane and trichloroethane are also generated. Such a product separation and purification system is relatively complicated, and the product yield is low; at present, the third synthetic method is mainly a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C19/043C07C17/16
CPCY02P20/10
Inventor 张保宏钱喜方邵建良
Owner JIANGSU ZHENFANG BIO CHEM CO LTD
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