Method for preparing chloroethane from chlorination by-product hydrogen chloride

A technology of chlorination reaction and ethyl chloride, which is applied in the preparation of halogenated hydrocarbons, chemical instruments and methods, dehydration of hydroxyl-containing compounds to prepare ethers, etc., can solve the problems of low recycling value, high cost of pollution control, and easy pollution of the environment , to achieve low production consumption, reduce production costs, and eliminate the effects of three wastes

Active Publication Date: 2015-01-28
HUAIYIN INSTITUTE OF TECHNOLOGY
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  • Abstract
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Problems solved by technology

Dilute sulfuric acid, dilute hydrochloric acid and waste lye in production contain a large amount of organic substances, which have low recycling value and high cost of pollution control
The application number is 201310018197.7, which discloses a haloalkanization process and system for the preparation of ethyl chloride, which uses a dedicated ethyl chloride reactor to replace multiple reactors, realizes large-scale equipment and automatic control, and improves the conversion rate of raw materials; the process There are two disadvantages: one is that the ethyl chloride coming out of the reactor is first condensed by the condenser and then rectified in the rectification tower, which consumes a lot of energy; the other is the treatment and discharge of acidic water, which is easy to pollute the environment

Method used

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  • Method for preparing chloroethane from chlorination by-product hydrogen chloride

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Example 1: Hydrogen chloride, by-product of chlorination reaction, was prepared by following steps to prepare ethyl chloride

[0015] (1) Reaction: add 30% mass concentration of zinc chloride aqueous solution in reactor 1, zinc chloride is used as a catalyst, and the heating temperature rises to 120 ° C, and the mass concentration of 30% hydrochloric acid and mass concentration of 95% ethanol are molar The ratio of 1:0.70 is passed into the reactor to react;

[0016] (2) Rectification: the reacted gaseous mixture enters the first rectification tower 2, and the water containing 7% HCl flows out and reused from the bottom of the tower, and uses it to absorb the by-product hydrogen chloride of the chlorination reaction; the tower of the first rectification tower 2 The overhead steam is condensed 3 through the first condenser, the condensing temperature is 25 ° C, the reflux ratio is 1.5, the extraction content of 95% ethanol enters the storage tank for reuse, and the non-c...

Embodiment 2

[0017] Embodiment 2: Chlorination reaction by-product hydrogen chloride prepares chloroethane according to the following steps

[0018] (1) Reaction: add 40% aqueous zinc chloride solution by mass concentration in reactor 1, zinc chloride is used as a catalyst, and the heating temperature rises to 135 ° C, and the hydrochloric acid that mass concentration is 33% and the mass concentration of 95% ethanol are molar The ratio of 1:0.75 is passed into the reactor to react;

[0019] (2) Rectification: the reacted gaseous mixture enters the first rectification tower 2, and the water containing 9% HCl flows out and reused from the bottom of the tower, and uses it to absorb the by-product hydrogen chloride of the chlorination reaction; the tower of the first rectification tower 2 The overhead steam is condensed 3 through the first condenser, the condensing temperature is 26 ℃, the reflux ratio is 1.5, the ethanol of the extraction content 95% enters the storage tank for reuse, and the...

Embodiment 3

[0020] Embodiment 3: Chlorination reaction by-product hydrogen chloride prepares chloroethane according to the following steps

[0021] (1) Reaction: adding 50% mass concentration of zinc chloride aqueous solution in reaction kettle 1, zinc chloride is used as a catalyst, the heating temperature rises to 140 ° C, and the mass concentration of 35% hydrochloric acid and 95% mass concentration of ethanol are molar The ratio of 1:0.80 is passed into the reactor to react;

[0022] (2) Rectification: the reacted gaseous mixture enters the first rectification tower 2, and the water containing 11% HCl flows out and reused from the bottom of the tower, and uses it to absorb the by-product hydrogen chloride of the chlorination reaction; the tower of the first rectification tower 2 The top steam is condensed through the first condenser 3, the condensing temperature is 27 ° C, the reflux ratio is 1.5, the extraction content 95% ethanol enters the storage tank for reuse, and the non-conden...

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Abstract

The invention discloses a method for preparing chloroethane from chlorination by-product hydrogen chloride. The method adopts a reaction rectification technology. According to the method, a reactor is connected to a first rectifying tower, water in the first rectifying tower flows out the first rectifying tower from tower bottom and then is recycled, a tower overhead fraction of the first rectifying tower goes through a first condenser, a part of ethanol is returned, a part of the ethanol is collected and then is fed into a storage tank for recycle, chloroethane and a less amount of ether mixed vapor are fed into a second rectifying tower, a tower overhead fraction of the second rectifying tower goes through a second condenser, a part of chloroethane is returned, a part of chloroethane is collected and then is fed into a storage tank for recycle, and the by-product ether is obtained by a reboiler. The method realizes timely removal of produced chloroethane and water from a system, effectively accelerates a positive reaction speed, realizes effective recovery and recycle of unreacted hydrochloric acid and ethanol, has simple processes, a high ethanol conversion rate, low production consumption and good income and realizes zero discharge.

Description

technical field [0001] The invention belongs to the field of chemical industry, and relates to the preparation technology of chloroethane, in particular to a method for preparing chloroethane by reactive distillation from hydrogen chloride, a by-product of a chlorination reaction. Background technique [0002] With the rapid development of organochlorine products in my country, a large amount of by-product hydrogen chloride is produced, and the total amount of by-product hydrogen chloride is increasing year by year. When the process system cannot be reused, the most common way to utilize by-product hydrogen chloride is by-product hydrochloric acid. The output of hydrochloric acid in my country has always been dominated by by-products, and it is increasing year by year. The market for hydrochloric acid exceeds demand. The pressure to produce hydrochloric acid from by-product hydrogen chloride is increasing. The reaction of hydrochloric acid and ethanol to prepare ethyl chlori...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/16C07C19/043C07C41/09C07C43/06
CPCY02P20/10
Inventor 钱运华李东杨勇吴彩金周伟杜卫刚固旭周苏闽方慧敏张雪
Owner HUAIYIN INSTITUTE OF TECHNOLOGY
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