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A kind of method separating dichloropropanol from dichloropropanol hydrochloric acid azeotropic liquid

A technology of dichloropropanol hydrochloride and dichloropropanol, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as cumbersome operation procedures, waste of resources, environmental pollution, etc., and reduce environmental pollution , High efficiency of carrying water, less organic residue

Active Publication Date: 2021-12-10
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 cumbersome operation procedures, resource waste, environmental pollution and high cost in the prior art, the invention provides a method for separating dichloropropanol from dichloropropanol hydrochloride azeotropic liquid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Put 200g of dichloropropanol hydrochloric acid azeotropic liquid and 200g of toluene in a three-necked flask. The upper part of the three-necked flask is connected to the rectification column, water separator, condenser and tail gas absorption device in sequence. The packing of the rectification column is Raschig ring, the packing method is random; the three-necked flask is heated by an oil bath to rectify the azeotropic system, the temperature is about 84 ° C, the azeotropic distillation time of the system is 6 hours, and the rectified components are separated by a water separator. The mass fraction is 123g of hydrochloric acid solution of 30%, the recovery rate is 83.9% (calculated as hydrogen chloride), and the residual organic solvent is 310ppm;

[0026] (2) The mixture of dichloropropanol and toluene in the three-necked flask was distilled and separated under atmospheric pressure at 90-100 °C to obtain 67.3 g of dichloropropanol, with a recovery rate of 96.1% an...

Embodiment 2

[0029] (1) Put 200g of dichloropropanol hydrochloric acid azeotropic liquid and 200g of xylene in a three-necked flask, and the upper part of the three-necked flask is connected to the rectification column, water separator, condenser and tail gas absorption device in sequence, and the packing of the rectification column is pulled In Xihuan, the packing method is random; the three-necked flask is heated by an oil bath to rectify the azeotropic system at a temperature of about 92°C, and the azeotropic distillation time of the system is 4.5 hours, and the rectified components pass through the water separator The separated mass fraction is 125g of hydrochloric acid solution of 31%, the recovery rate is 88% (in terms of hydrogen chloride), and the residual organic solvent is 280ppm;

[0030] (2) The mixture of dichloropropanol and xylene in the three-neck flask was distilled and separated under normal pressure at a temperature of 90~100°C to obtain 67.5g of dichloropropanol, with a ...

Embodiment 3

[0033] (1) Put 200g of dichloropropanol hydrochloric acid azeotropic liquid and 300g of toluene in a three-necked flask, and the upper part of the three-necked flask is connected to the rectification column, water separator, condenser and tail gas absorption device in sequence, and the packing of the rectification column is Raschig Ring, the packing method is random; heat the three-necked flask through an oil bath to reflux the azeotropic system, the temperature is about 84 ° C, the azeotropic distillation time of the system is 5 hours, and the rectified components are separated by a water separator to obtain the mass fraction It is 124g of 30.5% hydrochloric acid solution, the recovery rate is 85.9% (calculated as hydrogen chloride), and the residual organic solvent is 351ppm;

[0034] (2) The mixture of dichloropropanol and toluene in the three-neck flask was distilled and separated under normal pressure at 90-100°C to obtain 68g of dichloropropanol, with a recovery rate of 9...

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Abstract

The invention discloses a method for separating dichloropropanol from dichloropropanol hydrochloric acid azeotropic liquid. The specific operation steps are as follows: adding aromatic hydrocarbons and esters azeotropic with water to dichloropropanol hydrochloric acid azeotropic liquid Form a new azeotropic system with ethers as an organic water-carrying agent, heat the system to azeotrope, and realize the separation of hydrochloric acid and organic water-carrying agent through rectification, cooling, and water separation; unrectified components containing dichloropropanol High-purity dichloropropanol is obtained after distillation under normal pressure, and the water-carrying agent in the system can be recovered and recycled. The method has the advantages of simple operation, high separation efficiency of dichloropropanol and hydrochloric acid solution, high recovery rate, and high purity of obtained dichloropropanol and hydrochloric acid. Aromatic hydrocarbons, esters and ether organic water-carrying agents have high water-carrying efficiency, can be recycled, have low cost, and reduce environmental pollution.

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 azeotropic liquid. 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 material. The interm...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/80C07C29/82C07C31/36
CPCC07C29/80C07C29/82C07C31/36
Inventor 赵坤程终发高灿柱周荣奇陈树招陆久田杨修艳王宁宁
Owner SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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