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A kind of improved recovery method of phenylacetic acid waste liquid in 6-apa production

A technology of 6-APA and a recovery method is applied in the field of recovery of phenylacetic acid waste liquid in the production of 6-APA, and can solve the problems of large solvent loss, heavy pollution, high toxicity and the like

Active Publication Date: 2021-06-15
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 present invention relates to pharmaceutical field, be specifically related to the recovery method of phenylacetic acid waste liquid in a kind of improved 6-APA production, described method comprises the following: (1) extraction; (2) degreasing; (3) insulation; (4) decolorization Impurity removal; (5) crystallization; (6) sulfate radical treatment in mother liquor and other steps. The method for recovering phenylacetic acid provided by the invention is decolorized under the condition of water phase without using a solvent, and has obvious cost saving advantages. The recovery rate of phenylacetic acid is above 90%, the product color is white, and the purity is above 99%. The present invention also relates to The treatment and recovery of sulfate radicals in the mother liquor are eliminated, thereby producing less inorganic salts and less environmental pollution, and can be applied to the fermentation of penicillin.

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 Patents(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