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Improved method for recycling phenylacetic acid waste liquid in 6-APA production

A 6-APA, recovery method technology, applied in the field of recovery of phenylacetic acid waste liquid in 6-APA production, can solve the problems of large solvent loss, equipment corrosion, high toxicity, etc.

Active Publication Date: 2019-03-29
UNITED LAB INNER MONGOLIA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses the organic solvent methyl isobutyl ketone, and the obtained phenylacetic acid has a yellower color, which cannot meet the requirements of penicillin fermentation
[0009] The recovery method of the above-mentioned phenylacetic acid uses solvents such as toluene and methyl isobutyl ketone, and adds concentrated sulfuric acid or hydrogen peroxide to the organic phase to oxidize.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] During the production of 6-APA by cleavage of penicillin G, the organic phase after extraction of the lysate contains phenylacetic acid. Take 155L of organic phase containing phenylacetic acid, the content of phenylacetic acid is about 60mg / ml, the temperature is controlled at 15°C, adjust the pH to 10.5 with 5% sodium hydroxide solution, stir for 5min, let stand to separate the phases, and the heavy phase (containing phenylacetic acid solution ) 87.5L, into the distillation tank. The light phase is recycled for the extraction of the lysate.

[0058] Raise the temperature of the phenylacetic acid-containing solution in the distillation tank to 95°C and keep it for 60 minutes. After removing the residual extractant, continue to raise the temperature to 121°C, keep it at 0.12MPa for 120 minutes, and reduce the pressure to normal pressure to obtain 63.6L of pretreatment liquid.

[0059] Put the pretreatment solution into the decolorization tank, add suitable purified wate...

Embodiment 2

[0063] During the production of 6-APA by cleavage of penicillin G, the organic phase after extraction of the lysate contains phenylacetic acid. Take 300L of organic phase containing phenylacetic acid, the content of phenylacetic acid is about 50mg / ml, the temperature is controlled at 20°C, adjust the pH to 11 with 10% sodium hydroxide solution, stir for 5min, let stand until the phases are separated, and the heavy phase (containing phenylacetic acid solution) 170L, poured into the distillation tank. The light phase is recycled for the extraction of the lysate.

[0064] Raise the temperature of the phenylacetic acid-containing solution in the distillation tank to 98°C and keep it for 60 minutes. After removing the residual extractant, continue to raise the temperature to 123°C, keep it at 0.12MPa for 120 minutes, and reduce the pressure to normal pressure to obtain 123L of pretreatment liquid.

[0065] Put the pretreatment solution into the decolorization tank, add suitable pu...

Embodiment 3

[0069]During the production of 6-APA by cleavage of penicillin G, the organic phase after extraction of the lysate contains phenylacetic acid. Take 500L of organic phase containing phenylacetic acid, the content of phenylacetic acid is about 58mg / ml, the temperature is controlled at 25°C, the pH is adjusted to 11.5 with 20% sodium hydroxide solution, stirred for 10min, and allowed to stand until the phases are separated to obtain the heavy phase (containing benzene Acetic acid solution) 283L, into the distillation tank. The light phase is recycled for the extraction of the lysate.

[0070] Raise the temperature of the phenylacetic acid-containing solution in the distillation tank to 100°C and keep it for 60 minutes. After removing the residual extractant, continue to raise the temperature to 125°C, keep the temperature at 0.13 MPa for 120 minutes, and reduce the pressure to normal pressure to obtain 205 L of pretreatment liquid.

[0071] Put the pretreatment solution into the...

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PUM

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Abstract

The invention relates the field of pharmacy, and specifically relates to an improved method for recycling phenylacetic acid waste liquid in 6-APA production. The method includes the following steps: (1) performing extraction; (2) performing degreasing; (3) performing heat preservation; (4) performing decolorization and impurity removal; (5) performing crystallization; and (6) processing sulfate radical in mother liquor. The method can perform decolorization under a water phase condition without using a solvent, so that costs can be obviously saved, and the recycling rate of phenylacetic acid can reach more than 90%; and the color of an obtained product is white, and the purity of the product can reach more than 99%. The processing and recycling of the sulfate radical in the mother liquor are also related, so that generated inorganic salt is less, and the pollution on environments is less, and therefore, the products obtained through the method can be applied to penicillin fermentation.

Description

technical field [0001] The invention relates to the pharmaceutical field, in particular to an improved recovery method of phenylacetic acid waste liquid in 6-APA production. Background technique [0002] Phenylacetic acid is the precursor compound of penicillin. During the synthesis of penicillin, phenylacetic acid waste liquid will be produced. The by-product of phenylacetic acid contains many harmful impurities, which cannot be reused and discarded, resulting in a large amount of sewage. Phenylacetic acid is recovered. [0003] Patent CN1227216A discloses a method for recovering phenylacetic acid. The method is to adjust the pH of the cracked waste liquid to 10-14, then add 0.3%-1% hydrogen peroxide at room temperature, oxidize, distill, and heat the still liquid to 100 ~106°C, distill off the organic solvent methyl isobutyl ketone, cool and settle the remaining part for more than 10 hours, take the supernatant and adjust the pH to 10-14, add 0.1%-0.5% hydrogen peroxide a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/42C07C57/32C01D5/06
CPCC01D5/06C07C51/42C07C57/32
Inventor 何同鹏吴艳菲王克玉李海均
Owner UNITED LAB INNER MONGOLIA CO LTD
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