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Method for preparing isooctyl thioglycolate by adopting tail liquid in the production process of O-alkyl-N-alkyl sulfide expelling carbamate

A technology of alkylthiocarbamate and isooctyl thioglycolate, which is applied in the chemical industry, can solve problems such as environmental pollution, increased production costs, low content of thioglycolic acid and esters, and achieve environmental pollution and reduce the use of Quantity, the effect of short production cycle

Active Publication Date: 2010-03-10
WEIFANG JIAHUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Utilize this method to produce isooctyl thioglycolate, the content of thioglycolic acid and ester in the crude ester obtained after extraction is low, and must add the thioglycolic acid of high concentration in the organic phase of loading thioglycolic acid before esterification, increased production cost; Moreover, when removing organic substances in the acidification solution, volatile organic solvents such as petroleum ether and ether are used, which has caused repeated pollution to the environment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Get 1000ml of tail liquid containing thioglycolic acid 9.5wt% and acidify it with hydrochloric acid until PH=2, let it stand for 2 days, then filter the acidified tail liquid with a three-stage activated carbon column, remove the suspended organic matter, and obtain the acidified The liquid is a transparent solution, containing 9.3wt% of thioglycolic acid.

[0025] (2) Take 200ml of acidified solution at a temperature of 25°C, first extract with isooctyl alcohol, the volume ratio of isooctyl alcohol to acidified solution is 1:1, then add 0.5wt% of the extract to the extracted extract Use p-toluenesulfonic acid as a catalyst, and perform esterification at 100°C; then take 200ml of new acidification solution, use the organic mixture obtained after esterification as an extraction agent, and perform extraction and esterification at the same temperature; Use the organic mixture obtained after extraction and esterification as the extractant to carry out the process of ext...

Embodiment 2

[0028] (1) Get 1000ml of tail liquid containing thioglycolic acid 8.2wt% and acidify it with sulfuric acid until PH=2, let it stand for 1 day, then filter the acidified tail liquid with a three-stage activated carbon column, remove the suspended organic matter, and obtain the acidified The liquid is a transparent solution containing 8.0 wt% of thioglycolic acid.

[0029] (2) Take 200ml of acidified solution at a temperature of 40°C, first extract with isooctyl alcohol, the volume ratio of isooctyl alcohol to acidified solution is 1:3, then add 0.01wt% of the extract to the extracted extract Use p-toluenesulfonic acid as a catalyst, and perform esterification at 150°C; then take 200ml of new acidification solution, use the organic mixture obtained after esterification as an extraction agent, and perform extraction and esterification at the same temperature; Use the organic mixture obtained after extraction and esterification as the extractant to carry out the process of extract...

Embodiment 3

[0032] (1) Get 2000ml of tail liquid containing thioglycolic acid 11.2wt%, acidify with hydrochloric acid, to PH=1.5, leave standstill for 3 days, then filter the tail liquid after acidification with a three-stage activated carbon column, remove suspended organic matter, and obtain the acidified The liquid is a transparent solution containing 10.9 wt% of thioglycolic acid.

[0033] (2) Take 300ml of acidified solution at a temperature of 30°C, first extract with isooctyl alcohol, the volume ratio of isooctyl alcohol to acidified solution is 1:1, then add 0.6wt% of the extract to the extracted extract Use p-toluenesulfonic acid as a catalyst, and perform esterification at 120°C; then take 300ml of new acidification solution, use the organic mixture obtained after esterification as an extraction agent, and perform extraction and esterification at the same temperature; Use the organic mixture obtained after extraction and esterification as the extractant to repeat the process of ...

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Abstract

The invention discloses a method for preparing isooctyl thioglycolate by adopting tail liquid in the production process of O-alkyl-N-alkyl sulfide expelling carbamate, comprising the following steps:a. acidifying and purifying tail liquid, removing separated suspending organic matters; b. extracting the acidified liquid by an extracting agent, esterifying to obtain rough ester; c. carrying out reduced pressure distillation on the rough ester and obtaining the isooctyl thioglycolate. The method is characterized in that: in the extraction and esterification processes, isooctane is firstly takenas the extracting agent to extract and esterify the acidified liquid to obtain organic mixture; the organic mixture is taken as an extracting agent to extract and esterify the new acidified liquid; and the obtained organic mixture after extraction and esterification is taken as an extracting agent to extract and esterify the new acidified liquid at least once. The invention has the advantages ofreasonable production process, raw material saving, low production cost and high product quality and is a reasonable method for recycling the tail liquid in the production process of the O-alkyl-N-alkyl sulfide expelling carbamate.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for recycling thioglycolic acid in the tail liquid of O-alkyl-N-alkylthiocarbamate production. Background technique [0002] Isooctyl thioglycolate is a new type of non-toxic plastic additive. It is a heat stabilizer widely used in the processing of PVC and other plastic products. In recent years, with the rapid development of the field of polymer materials, thioglycolate isoct The demand for octyl esters also increases accordingly. The current preparation methods of isooctyl thioglycolate all have problems such as high raw material cost, complex production process, and long production cycle. And the production technology and market have been controlled by foreign developed countries. [0003] O-alkyl-N-alkylthiocarbamate is a kind of thiocarbamate, in the production of thiocarbamate such as O-alkyl-N-alkylthiocarbamate, a large amount of The ratio of waste water (tai...

Claims

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Application Information

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IPC IPC(8): C07C323/52C07C319/12
Inventor 张华帮姜淑珍
Owner WEIFANG JIAHUA CHEM
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