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Method for separating dichloropropanol from dichloropropanol hydrochloric acid solution through alkane azeotrope agent

A technology of dichloropropanol hydrochloric acid and dichloropropanol, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry and other directions, can solve the problems of pollution, waste of resources, environment, complicated operation procedures, etc., and achieves high purity, The effect of low recovery rate and simple operation

Active Publication Date: 2019-01-04
SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the problems of relatively cumbersome operation procedures, waste of resources and environmental pollution in the prior art, the present invention provides a method for separating dichloropropanol from dichloropropanol hydrochloric acid solution by using an alkane entrainer

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Add 200 g of cyclohexane and 200 g of dichloropropanol hydrochloric acid solution into a three-necked flask, and the upper part of the three-necked flask is connected to a rectification column, a condenser, a water separator and an exhaust gas absorption device in sequence, and the filler of the rectification column is glass The packing method of spring and packing is random; heat the three-necked flask through an oil bath to reflux the azeotropic system, the temperature is about 70 ℃, the azeotropic distillation time of the system is 7h, and the rectification components are separated by a water separator to obtain the mass fraction It is 125 g of 23% hydrochloric acid solution, the recovery rate is 96.15%, and the residual organic solvent is 10 ppm;

[0025] (2) The mixture of dichloropropanol and cyclohexane was distilled and separated under normal pressure at 82 ± 1°C to obtain 67.48 g of dichloropropanol, with a recovery rate of 96.4% and a purity of 99.2%;

[0...

Embodiment 2

[0028] (1) Put 200 g of n-hexane and 200 g of dichloropropanol hydrochloric acid solution in a three-necked flask, and the upper part of the three-necked flask is connected to a rectification column, a condenser, a water separator and an exhaust gas absorption device in sequence, and the packing of the rectification column is pulled West ring, spiral ring; heat the three-necked flask through an oil bath to reflux the azeotropic system, the temperature is about 62 ℃, the azeotropic distillation time of the system is 8 h, and the rectification components are separated by a water separator to obtain a mass fraction of 24 % hydrochloric acid solution 122 g, the recovery rate is 93.85%, and the residual organic solvent is 25 ppm;

[0029] (2) The mixture of dichloropropanol and n-hexane was distilled and separated under normal pressure at 70 ± 1°C to obtain 67.27 g of dichloropropanol, with a recovery rate of 96.1% and a purity of 99.1%;

[0030] (3) Combine steps (1) and (2) to se...

Embodiment 3

[0032] (1) Add 400 g of cyclohexane and 200 g of dichloropropanol hydrochloric acid solution into a three-necked flask, place the three-necked flask in an oil bath, and connect the upper part of the three-necked flask to the rectification column, condenser, water separator and tail gas in sequence The absorption device, the packing of the rectifying column is saddle-shaped, and the packing method is random; the three-necked flask is heated through an oil bath to reflux the azeotropic system at a temperature of about 70 °C, and the azeotropic distillation time of the system is 5 h. The rectification components were separated by a water separator to obtain 120 g of hydrochloric acid solution with a mass fraction of 24.1%, the recovery rate was 92.3%, and the residual organic solvent was 20 ppm;

[0033] (2) The mixture of dichloropropanol and cyclohexane was distilled and separated under normal pressure at 82 ± 1°C to obtain 67.9 g of dichloropropanol, with a recovery rate of 97....

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Abstract

The invention discloses a method for separating dichloropropanol from a dichloropropanol hydrochloric acid solution through an alkane azeotrope agent. The method specifically comprises the following steps: adding the alkane azeotrope agent which is subjected to azeotropy with water to a dichloropropanol hydrochloric acid water solution; heating until the system reaches azeotropy; rectifying and cooling to separate a hydrochloric acid solution and the alkane azeotrope agent from a rectified component; distilling the non-rectified components under normal pressure to obtain high-purity dichloropropanol; and recycling the alkane azeotrope agent. The method is simple to operate; the complicated operation of extracting in a plurality of times is avoided; the separation efficiency is high; the cost is low; all materials can be recycled; the raw material utilization rate is high; and the environmental pollution is reduced.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and in particular relates to a method for separating dichloropropanol from dichloropropanol hydrochloric acid solution by using an alkane entrainer. Background technique [0002] Epichlorohydrin, namely 3-chloro-1,2-propylene oxide, is an important organic chemical raw material and synthetic intermediate, which can be used as a solvent for cellulose esters, resins and cellulose ethers, and is also used for the production of surfactants , pharmaceuticals, pesticides, coatings, adhesives, ion exchange resins, plasticizers, glycerin derivatives and glycidol derivatives are widely used in chemical, light industry, pharmaceutical, electronics and other industries. [0003] At present, there are mainly three production methods of epichlorohydrin: propylene high-temperature chlorination method using propylene as raw material, propylene acetate method and glycerin chlorination method using glycerol as raw m...

Claims

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Application Information

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IPC IPC(8): C07C29/82C07C29/80C07C31/36
CPCC07C29/80C07C29/82C07C31/36
Inventor 赵坤程终发高灿柱周荣奇王宁宁陈树招陆久田张敏
Owner SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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