Method for recovering phenylacetic acid in enzymatic aqueous solution of 6-aminopenicillanic acid

A technology of aminopenicillanic acid enzymatic method and recovery method, which is applied in the separation/purification of carboxylic acid compounds, organic chemistry, etc., and can solve the problems of air, water environment and water source pollution, which are not conducive to health and high risk. To achieve a win-win situation of economy and environmental protection, simplify operation and steps, and achieve good recycling effect

Active Publication Date: 2018-10-16
SHANXI WEIQIDA PHARMA IND
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Problems solved by technology

This method uses toluene solvent extraction, which is not conducive to health first, and can cause pollution to the air, water environment and water sources; secondly, a large amount of acid and alkali are used in the process, which is not only dangerous, but also produces a large amount of inorganic salts that need to be recycled. The steps are more cumbersome and consume more energy

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  • Method for recovering phenylacetic acid in enzymatic aqueous solution of 6-aminopenicillanic acid

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preparation example Construction

[0022] In the preparation of the step (1) phenylacetate aqueous solution, the pH of the 6-APA enzymatic aqueous solution is adjusted to acidity with an inorganic acid, and then mixed solvents are used to extract the phenylacetic acid in the 6-APA enzymatic aqueous solution, which is separated to obtain 6-APA water phase and solvent phase containing phenylacetic acid; adding lye to the solvent phase containing phenylacetic acid, layering to obtain the aqueous phase containing phenylacetic acid salt, after evaporation and concentration, to obtain concentrated phenylacetic acid salt liquid.

[0023] In the step (1), the 6-APA enzymatic aqueous solution means that penicillin G is decomposed by penicillin acylase to generate 6-APA and phenylacetic acid, and the enzymatic hydrolysis solution after filtering and removing impurities, this part of the enzymatic hydrolysis solution Contains the product 6-APA, and also contains the by-product phenylacetic acid, wherein the concentration ...

Embodiment 1

[0034] (1) Preparation of sodium phenylacetate aqueous solution

[0035] Take 50L of 6-APA enzymatic aqueous solution (the content of phenylacetic acid is 22.4g / L), the pH value is 8.1, at a temperature of 10°C, use 32% (v / v) concentrated hydrochloric acid to adjust the pH to 1.0, then add 50L butyl acetate / The n-butanol mixed solvent (n-butanol accounts for 14% (volume)) was fully stirred, and the extract was collected after standing to separate 49.4L (phenylacetic acid content 20.8g / L); use 40% (w / v) sodium hydroxide The solution adjusted the pH of the extract to 10.5, stirred well and then separated and collected the heavy phase 6.6L (phenylacetic acid content 151.3g / L); then, vacuum distillation concentrated the phenylacetic acid content to 263.5g / L, volume 3.8L.

[0036] (2) preparation of purified sodium phenylacetate aqueous solution

[0037] The concentrated solution containing sodium phenylacetate obtained in step (1) is removed by a nanofiltration membrane with a m...

Embodiment 2

[0041] (1) Preparation of sodium phenylacetate aqueous solution

[0042] Take 50L of 6-APA enzymatic aqueous solution (phenylacetic acid content 22.3g / L), the pH value is 8.0, the temperature is 11°C, use 32% (v / v) concentrated hydrochloric acid to adjust the pH to 1.0, and then add 100L butyl acetate / normal Butanol mixed solvent (n-butanol accounts for 24.5% (volume)) was fully stirred, and the extract was collected after standing to separate 99.2L (11.0g / L); use 40% (w / v) sodium hydroxide solution to adjust the extract The pH was 10.5, and after being fully stirred, the heavy phase was collected by stratification at 6.8 L (154.9 g / L); then, the content of phenylacetic acid was concentrated to 297.9 g / L by vacuum distillation, and the volume was 3.5 L.

[0043] (2) preparation of purified sodium phenylacetate aqueous solution

[0044] The concentrated solution containing sodium phenylacetate obtained in step (1) is removed by a nanofiltration membrane with a molecular weight...

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Abstract

The invention relates to a method for recovering phenylacetic acid (PAA) in an enzymatic aqueous solution of 6-aminopenicillanic acid (6-APA). The method comprises the following steps: firstly, usinga mixed solvent to extract PAA from the enzymatic aqueous solution of 6-APA to a solvent phase, so as to enable 6-APA to be separated from PAA; then, performing lye stripping and evaporation concentration on the solvent phase to obtain an aqueous solution containing phenylacetate; and finally, recovering PAA in the aqueous solution in a manner of combining secondary nanofiltration with reverse osmosis. The method provided by the invention can directly separate and obtain high-quality aqueous solution of phenylacetate from the enzymatic aqueous solution of 6-APA in a manner of combining extraction, stripping, concentration and nanofiltration, can be directly used for fermentation to produce penicillin, further treats high-impurity nanofiltration concentrate in a manner of combining water dilution, nanofiltration and reverse osmosis, realize zero discharge of PAA, and minimizes discharged wastes by recycling of a solvent and water in the process.

Description

technical field [0001] The invention belongs to the technical field of pharmacy, and relates to a method for recovering phenylacetic acid in a 6-aminopenicillanic acid (hereinafter referred to as 6-APA) enzymatic aqueous solution. Recovery method of by-product phenylacetic acid in alkanoic acid process. Background technique [0002] Phenylacetic acid, referred to as PAA, has a molecular weight of 136.15 and is in the form of white shiny leaf-shaped crystals. Phenylacetic acid is chemically active and has typical reactions of carboxyl, methylene and benzene rings. It can undergo reactions such as salt formation, esterification, amidation, nitration, halogenation, sulfonation, and decarboxylation, and can participate in the conversion of many functional groups. It is an important Pharmaceutical and fine chemical intermediates. In the field of medicine, phenylacetic acid is the main precursor for the production of penicillin G by fermentation, and penicillin G is the main raw...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/42C07C57/32
CPCC07C51/42C07C57/32
Inventor 苗瑞春王雁蒋远顺岳峰贾金龙
Owner SHANXI WEIQIDA PHARMA IND
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