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
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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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