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Regeneration method for acylation-reaction mother liquor of paracetamol

A technology of paracetamol and acylation reaction, applied in chemical instruments and methods, carboxylic acid amide separation/purification, organic chemistry, etc., can solve the problems of reduced effect of application, impact on product quality, etc., and achieve the effect of reducing production costs

Active Publication Date: 2014-01-15
ANHUI BBCA LIKANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

With the increase of application times, the content of organic impurities and inorganic impurities in the application solution will increase, and the application effect will be significantly reduced and even affect product quality.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The regeneration method of the acylation mother liquor of embodiment 1 paracetamol

[0019] The specific steps are:

[0020] (1) Concentration and crystallization. 500 kg of paracetamol acylation with an acidity of about 56% was applied to the mother liquor, and concentrated in vacuum at 70°C. About one-half of the volume of water is evaporated, and the acidity of the evaporated water is about 42%, which is put into the acid tank for later use. The temperature of the remaining mother liquor was lowered to 0-5°C and allowed to stand for 12 hours to crystallize. The obtained crystals were crude paracetamol with a content of 98.2%, of which p-aminophenol was 0.98%. The paracetamol crude product obtained is applied to the next pot of reaction kettle. The remaining mother liquor enters the resin adsorption process.

[0021] (2) Macroporous adsorption resin adsorption. The resin column is 5m high and has an inner diameter of 200mm. About 230kg of the remaining mother li...

Embodiment 2

[0024] The regeneration method of the acylation reaction mother liquor of embodiment 2 paracetamol

[0025] The specific steps are:

[0026] (1) Concentration and crystallization. 500 kg of paracetamol acylation with an acidity of about 52% was applied to the mother liquor, and concentrated in vacuum at 68°C. Evaporate about three-fifths of the volume of water, and the acidity of the evaporated water is about 45%, and put it into the acid tank for later use. The remaining mother liquor was cooled to 0-5°C and allowed to stand for 12 hours to crystallize. The obtained crystals were crude paracetamol with a content of 98.6%, including 0.82% p-aminophenol. The paracetamol crude product obtained is applied to the next pot of reaction kettle. The remaining mother liquor enters the resin adsorption process.

[0027] (2) Macroporous adsorption resin adsorption. The resin column is 5m high and has an inner diameter of 200mm. About 235 kg of the remaining mother liquor is put int...

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Abstract

The invention provides a regeneration method for acylation-reaction mother liquor of paracetamol. The method comprises the following steps of concentration, crystallization, resin adsorption, reverse osmosis ultrafiltration and activated carbon adsorption on the acylation-reaction mother liquor of the paracetamol. The method can recycle and imitate the crude paracetamol product in acylated and imitated mother liquor and effectively removes organic impurities and inorganic salt in the mother liquor. An acidic aqueous solution is subjected to reverse osmosis ultrafiltration treatment and activated carbon adsorption to obtain a neutral aqueous solution which reaches an emission standard, so that the complete separation of the imitated mother liquor is realized, the purposes of circulation and imitation are achieved, and meanwhile the production cost of paracetamol is reduced.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for regenerating acetaminophen acylation reaction mother liquor. Background technique [0002] At present, the synthesis of paracetamol is mainly generated by acylation reaction of p-aminophenol and acetic acid under reflux state. The mother liquor after the crystallization of the acylation reaction contains a considerable amount of p-aminophenol, crude paracetamol, organic impurities and some inorganic salts. In order to reduce costs, the mother liquor after crystallization can be applied to the next pot of acylation liquor. With the increase of application times, the content of organic impurities and inorganic impurities in the application solution is also more, and the application effect is obviously reduced and even the product quality will be affected. Therefore, the removal of impurities and regeneration of the acylation mechanically applied mother liquor can eff...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C233/25C07C231/24C02F9/04C02F1/42C02F1/28C02F1/44
Inventor 韦亚峰汪洪湖杨杰陈文婕江立新
Owner ANHUI BBCA LIKANG PHARMA