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Method for high-valued utilization of thiourethane production tail liquid

A thiourethane, high-value technology, applied in the field of separating thiourethane tail liquid to obtain high-purity thioglycolic acid, can solve the problems of excessive extraction times, high operating conditions, complicated processes, etc., and achieves simple process, guaranteed purity, high purity effect

Inactive Publication Date: 2020-03-13
SHANDONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method avoids the problems caused by the use of extractant, the process is relatively complicated and the operating conditions are high.
Xu Qinghua [Shandong Chemical Industry, 2015, 44 (12): 10-11; Shandong Chemical Industry, 2015, 44 (21): 40-41] used ethyl acetate as the extraction agent to recover thioglycolic acid from the thiourethane tail liquid, but the extraction Too many times, complex process and high energy consumption
Zheng Hong et al. [Nonferrous Mining and Metallurgy, 2006, 22 (6): 17-18] used a mixed extractant of dichloromethane and ether to recover thioglycolic acid from thiourethane tail liquid, which has complicated process and low purity

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The invention discloses a method for separating thioglycolic acid from a thiourethane tail liquid. The thioglycolic acid in the tail liquid is enriched by one-time extraction, and the impurity in the primary extract is removed by adding the reaction liquid to one-step reaction to precipitate sodium thioglycolate, and then filtering to obtain Sodium thioglycolate is formulated into a solution for acidification, and after secondary extraction, high-purity thioglycolic acid product is obtained by vacuum distillation. Wherein, the content of thioglycolic acid in the tail liquid is 10 wt%, and the treatment process includes the following steps:

[0023] (1) The tail liquid containing 10 wt% thioglycolic acid was extracted for the first time with a quantitative ester extractant, and the thioglycolic acid was extracted and enriched to obtain a primary extract with a content of 9.5 wt% thioglycolic acid. Wherein, the extractant used is isobutyl acetate, and the volume ratio of ...

Embodiment 2

[0028] The invention discloses a method for separating thioglycolic acid from a thiourethane tail liquid. The thioglycolic acid in the tail liquid is enriched by one-time extraction, and the impurity in the primary extract is removed by adding the reaction liquid to one-step reaction to precipitate sodium thioglycolate, and then filtering to obtain Sodium thioglycolate is formulated into a solution for acidification, and after secondary extraction, high-purity thioglycolic acid product is obtained by vacuum distillation. Wherein, the content of thioglycolic acid in the tail liquid is 5 wt%, and the treatment process includes the following steps:

[0029] (1) The tail liquid containing 5 wt% thioglycolic acid was extracted for the first time with quantitative ester extractant, and the primary extract was obtained by extracting and enriching thioglycolic acid. The content of thioglycolic acid was 4.9 wt%. Wherein, the extractant used is isopropyl acetate, and the volume ratio of...

Embodiment 3

[0034] The invention discloses a method for separating thioglycolic acid from thiourethane tail liquid. The thioglycolic acid in the tail liquid is enriched by one-time extraction, and the impurity in the primary extract is removed by adding the reaction liquid to one-step reaction to precipitate sodium thioglycolate, and then filtering to obtain Sodium thioglycolate is formulated into a solution for acidification, and after secondary extraction, high-purity thioglycolic acid product is obtained by vacuum distillation. Wherein, the content of thioglycolic acid in the tail liquid is 15 wt%, and the treatment process includes the following steps:

[0035] (1) The tail liquid containing 15 wt% thioglycolic acid was extracted for the first time with quantitative ester extractant, and the primary extract was obtained by extracting and enriching thioglycolic acid, the content of thioglycolic acid was 14.2 wt%. Wherein, the extractant used is butyl acetate, and the volume ratio of th...

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Abstract

The invention discloses a method for high-valued utilization of a thiourethane production tail liquid. A high-purity mercaptoacetic acid product can be obtained through separation. The method comprises the following steps: extracting mercaptoacetic acid in the enriched tail liquid by using a small amount of an extractant, removing impurities in the obtained primary extract in the mode that a reaction liquid is added for a one-step reaction to separate out an intermediate sodium thioglycolate, then preparing a solution from sodium thioglycolate obtained through filtration, acidizing the solution, performing secondary extraction, and then carrying out reduced pressure distillation to obtain a high-purity thioglycolic acid product. The method solves the problem of difficulty in treatment of the thiourethane production tail liquid, realizes high-value utilization of wastes, simplifies the production process, and reduces the production cost.

Description

technical field [0001] The invention relates to a high-value utilization method of chemical production waste liquid, in particular to a method for obtaining high-purity thioglycolic acid by separating thiourethane tail liquid. Background technique [0002] Thiocarbamate refers to a class of compounds with the general formula ROCSNHR, which is a derivative of xanthate (xanthate). It is usually an oily liquid with low solubility in water and a special smell. It is an excellent flotation agent for sulfide ore. Thiurethane has a strong ability to collect copper sulfide, sphalerite and gold activated by copper ions, but has a weak ability to collect sulfide minerals such as iron sulfide. exhibited good selectivity in the separation. It is characterized by less dosage and easy foaming, so it is widely used in the flotation of various copper ore, gold ore, lead-zinc ore. A large amount of tail liquid containing thioglycolic acid will be produced in the production process of thio...

Claims

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Application Information

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IPC IPC(8): C07C319/12C07C319/28C07C323/52
CPCC07C319/12C07C319/28C07C323/52
Inventor 张连正高军徐冬梅马艺心赵萍萍李傲徐鑫
Owner SHANDONG UNIV OF SCI & TECH
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