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Method for processing acetaminophen refined mother liquid

A technology of paracetamol and a treatment method, which is applied in the field of removing impurities and recycling of paracetamol refining mother liquor, can solve the problems of consuming large heat energy, increasing coal-burning air pollution, energy waste and the like, and achieving the effect of saving energy

Active Publication Date: 2011-07-13
浙江康乐药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the increase of heat-decomposed impurities in the mother liquor and the concentration of impurities and inorganic salts, the quality of acetaminophen recovered in the mother liquor is poor, and it often needs to be refined two to three times to meet the qualified requirements, and the process is relatively cumbersome.
Moreover, the process of concentrating and refining the mother liquor consumes a lot of heat energy, resulting in waste of energy and increasing air pollution caused by coal burning

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] The refined mother liquor of acetaminophen (containing sodium sulfate and sodium sulfite, with a conductivity of about 4000μs / CM) is desalted through the DSAⅣ-1×1 / 100 electrodialyzer according to the conventional method, and is repeatedly circulated until the conductivity of the mother liquor drops to 300μs / CM. Below CM, stop the electrodialysis desalination operation. Take 250ml of the desalted mother liquor, add 50g of crude acetaminophen to be refined and 5g of activated carbon, heat to boiling under stirring, then filter to remove the activated carbon, put the filtrate into a flask with 0.5g of sodium pyrosulfite added in advance, and filter after cooling , the filter cake was washed with a small amount of purified water and drained, and dried in an oven at 100°C until dry to obtain white crystals of paracetamol.

Embodiment 2

[0014] Take 001×7 strongly acidic styrene-based cation exchange resin and treat it to H type according to conventional methods; take D301 macroporous weakly basic anion exchange resin and treat it to OH type according to conventional methods. Mix the two resins according to the volume ratio of cation exchange resin: anion exchange resin = 1:4, and put them into a glass resin column with a diameter of 45mm according to the conventional method, so that the height of the resin in the column reaches 50cm. Slowly pass the refined paracetamol solution into the resin column at a flow rate of about 50ml per minute, discard the aqueous solution containing no paracetamol in the previous section, and collect the purified paracetamol solution after desalination (conductivity≤5μs / CM ). Take 250ml of the desalted mother liquor, add 50g of crude acetaminophen to be refined and 5g of activated carbon, heat to boiling under stirring, then filter to remove the activated carbon, put the filtrate...

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PUM

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Abstract

The invention discloses an energy-saving environment-friendly method for processing acetaminophen refined mother liquid, comprising the following steps: removing inorganic salt in the mother liquid by carrying out electrodialysis method processing or cation exchange resinion exchange resin and anion exchange resin mixed ion exchange resin processing on acetaminophen refined aqueous mother liquid and lowering the electrical conductivity of the mother liquid below 300mus / CM; and using the acetaminophen refined aqueous mother liquid processed by desalting for refining an acetaminophen crude product again. The acetaminophen refined aqueous mother liquid processed by the method can be recycled, and acetaminophen contained in the mother liquid needs not to be separated out; compared with a technology for processing the mother liquid in the prior art, a concentration process is removed, and a large number of energy resources are saved; and because impurities which are carried in the mother liquid and are concerned to the acetaminophen have consistent sources and properties with impurities in the acetaminophen crude product which needs refining, the refining process of a product is not influenced.

Description

technical field [0001] The invention relates to a method for removing impurities and recycling paracetamol refined mother liquor. Background technique [0002] Acetaminophen is currently the most widely used antipyretic and analgesic drug. The crude acetaminophen synthesized by various methods must be refined to obtain products whose quality meets the requirements of the Pharmacopoeia. Due to the large difference in solubility between hot water and cold water, the product is generally refined in water (U.S. Pat. No. 3,042,719, U.S. Pat. No. 3,748,358, U.S. Pat. No. 3,781,354, U.S. Pat. No. 5,981,799) . [0003] The refining process is generally to dissolve the crude acetaminophen in hot water, add an appropriate amount of activated carbon to decolorize it, filter to remove the activated carbon, and precipitate acetaminophen crystals after cooling the filtrate, filter, wash the crystals with water, and dry to obtain the finished product of acetaminophen. [0004] Because t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C233/25C07C231/24A61P29/00
Inventor 姚元海陈经伟
Owner 浙江康乐药业股份有限公司
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