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Method for treating chloroacetic acid heavy component based on chloroacetic acid recovery

A treatment method, the technology of chloroacetic acid, applied in the preparation of carboxylate/lactone, organic chemistry, etc., can solve the problems of long capital occupation period, harmful gas generation, greenhouse effect, etc., to reduce the generation of three wastes and reduce the pressure on environmental protection , the effect of reducing production costs

Active Publication Date: 2018-03-23
山东民基新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 1. Alkali neutralization first and then biological method: Alkali neutralization requires a large amount of lye, the cost is high, the waste liquid stays for a long time, the treatment tank covers a large area, and the treatment effect is unstable, which is affected by natural factors such as seasons, temperature, and light Big
[0005] 2. As combustible heavy oil for sale or steam incineration treatment: the sale of combustible heavy oil is relatively narrow; the incineration method requires a large investment and takes a long period of capital, and incineration has certain requirements for the calorific value of waste, generally not less than 5000kJ / kg, It limits its application range, and incineration will also produce harmful gases, emit carbon dioxide, cause environmental pollution and greenhouse effects and other problems
[0006] 3. Utilize the main components contained in the production of downstream products: the separation of products and impurities is the main problem in the production of downstream products, and the utilization rate of raw materials is low. Therefore, the waste liquid of chloroacetic acid recombination is not conducive to the production of downstream products

Method used

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  • Method for treating chloroacetic acid heavy component based on chloroacetic acid recovery

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Take 150g of the stock solution of the heavy fraction of chloroacetic acid and put it into a 500mL three-neck flask, add 150g of water, add 3g of beryllium chloride, gradually heat up to 80°C under magnetic stirring, keep the hydrolysis reaction at 80°C for 20h, filter, and keep for use.

[0026] Take 300g of the heavy component solution of chloroacetic acid after hydrolysis and filtration and add it to a 500mL three-necked flask, heat it in an oil bath at 185°C, and distill under a pressure of -0.095MPa under a pressure of -0.095MPa under a pressure of magnetic force. At 138°C, when the top temperature dropped to 90°C, the reaction was stopped, and the distillate was weighed, that is, the quality of the chloroacetic acid aqueous solution was 243.3g, and the content of chloroacetic acid in the chloroacetic acid aqueous solution was 92.83g. At this time, the temperature of the oil bath was kept constant, the raffinate was stirred in vacuum for 30 minutes, and then the tem...

Embodiment 2

[0028] Take 100g of the stock solution of the heavy fraction of chloroacetic acid and add it to a 500mL three-neck flask, add 60g of water, add 1g of aluminum chloride, gradually heat up to 90°C under magnetic stirring, keep the hydrolysis reaction at 90°C for 7h, filter, and keep for use.

[0029] Take 160g of the heavy component solution of chloroacetic acid after hydrolysis and filtration and add it to a 500mL three-necked flask, heat it in an oil bath at 185°C, and distill under a pressure of -0.095MPa under a pressure of -0.095MPa under a pressure of magnetic force. At 130°C, when the top temperature dropped to 90°C, the reaction was stopped, and the weight of the distillate, chloroacetic acid aqueous solution, was weighed to be 111.1g, wherein the content of chloroacetic acid in the chloroacetic acid aqueous solution was 53.33g. At this time, the temperature of the oil bath was kept constant, the raffinate was stirred in vacuum for 30 minutes, and then the temperature was...

Embodiment 3

[0031] Take 100g of the stock solution of the heavy fraction of chloroacetic acid and add it to a 500mL three-neck flask, add 80g of water, add 2g of magnesium nitrate, gradually heat up to 90°C under magnetic stirring, keep the hydrolysis reaction at 90°C for 7h, filter, and keep for use.

[0032] Take 180g of the heavy component solution of chloroacetic acid after hydrolysis and filtration and add it to a 500mL three-necked flask, heat it in an oil bath at 185°C, and distill it under a pressure of -0.095MPa under a pressure of -0.095MPa under a pressure of magnetic force. At 130°C, when the top temperature dropped to 90°C, the reaction was stopped, and the distillate was weighed, that is, the quality of the chloroacetic acid aqueous solution was 132.3g, and the content of chloroacetic acid in the chloroacetic acid aqueous solution was 54.00g. At this time, the temperature of the oil bath was kept constant, the raffinate was stirred in vacuum for 30 minutes, and then the tempe...

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Abstract

The invention belongs to the technical field of chemical industry, and in particular relates to a method for treating a chloroacetic acid heavy component based on chloroacetic acid recovery. The method comprises the following steps: adding water into the chloroacetic acid heavy component, heating, performing hydrolysis reaction, performing reduced-pressure distillation to obtain a chloroacetic acid aqueous solution, adding water into the residual liquid after reduced-pressure distillation to dissolve, and performing incineration or alkali neutralizing treatment. Ethyl chloroacetate in the chloroacetic acid heavy component is hydrolyzed into chloroacetic acid successfully by controlling the hydrolysis temperature and hydrolysis time and adding a hydrolysis aid, and reduced-pressure distillation is conducted to obtain the chloroacetic acid aqueous solution. The utilization rate of the raw materials is increased, three wastes are reduced, the environmental protection pressure of enterprises is reduced, and the production cost of products is reduced.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a treatment method for heavy components of chloroacetic acid based on recovery of chloroacetic acid. Background technique [0002] Chloroacetic acid is an important fine chemical intermediate, which is widely used in pesticides, medicines, dyes, daily chemicals, chemical reagents, food additives and other fields. However, the heavy component of chloroacetic acid produced in the production process is a volatile, highly toxic and viscous waste liquid, which has a great destructive effect on the environment and poses a great threat to human life and health. [0003] At present, there are three main ways to deal with the distillation raffinate of the heavy fraction of chloroacetic acid as follows: [0004] 1. Alkali neutralization first and then biological method: Alkali neutralization requires a large amount of lye, the cost is high, the waste liquid stays for...

Claims

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Application Information

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IPC IPC(8): C07C51/09C07C53/16
CPCC07C51/09C07C53/16
Inventor 韦兵陈衍坤李建军张海朋罗汉金张红梅王国亮高丽霞肖勇胡广霞胡永嘉
Owner 山东民基新材料科技有限公司
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