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In-situ carbonylation method straight-through liquid sodium phenylacetate synthesis method and application

A technology of sodium phenylacetate and a synthetic method, which is applied in chemical instruments and methods, preparation of organic compounds, separation/purification of carboxylic acid compounds, etc., can solve problems such as difficult industrial production, strong odor of phenylacetic acid, and adverse environmental effects. Achieve the effects of mild synthesis conditions, low price, and low waste water treatment cost

Active Publication Date: 2021-03-02
INNER MONGOLIA CHANGSHENG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are dozens of synthetic methods for sodium phenylacetate, but most of them are difficult to apply to industrial production due to their complex operations and high raw material prices.
In addition, the sodium phenylacetate treatment process actually used for the fermentation of penicillin includes a phenylacetic acid operation unit, which has a strong odor and is difficult to treat; and the process of synthesizing phenylacetic acid produces a large amount of acidic wastewater, and a large amount of alkali is required to treat the waste acid water, which makes the process economical. , prone to adverse effects on the environment

Method used

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  • In-situ carbonylation method straight-through liquid sodium phenylacetate synthesis method and application
  • In-situ carbonylation method straight-through liquid sodium phenylacetate synthesis method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Such as figure 1 As shown, add industrial cobalt chloride (CoCl 2 ·6H 2 O) 476g, sodium thiosulfate (Na 2 S 2 o 3 ) 25g, metal manganese (200 mesh) 222g, sodium sulfide (Na 2 S) 48g, methanol 19.2L, and then use CO gas to replace 3 times, adjust the pressure to 0.08Mpa, control the reaction temperature to 35°C, adjust the speed to 800rad / min, and react for 5h.

[0045] In the reaction system of the synthetic catalyst, 24 kg of sodium hydroxide solution with a mass fraction of 40% and 15.2 kg of benzyl chloride were added dropwise, and the sodium hydroxide solution and benzyl chloride were added in about 3.5 hours (sodium hydroxide solution and chlorine Add benzyl chloride synchronously, without strictly controlling the pH during the process, then keep the temperature at 55°C and the pressure at 0.08MPa, and react for 6h.

[0046] After the reaction, the product in the reactor was aerated in situ for 2 hours; then filtered and separated, the filter cake was washed ...

Embodiment 2

[0056] The synthetic process of sodium phenylacetate is basically the same as in Example 1, the difference being that methanol and a small amount of organic phase are distilled out, and after the distilled concentrate obtained, nanofiltration decolorization and nanofiltration desalination are not carried out. The calculated yield is 95.9%, and the detected purity is 88.1%.

[0057] Carry out penicillin fermentation shake flask experiment according to embodiment 1 method:

[0058] The potency of the sodium phenylacetate shake flask prepared in this example is 15600 U / mL, which is more than 5% different from the result of the control group in Example 1, which does not meet the requirements of the fermentation experiment. It can be seen that the direct synthesis of sodium phenylacetate used for penicillin fermentation must be decolorized by nanofiltration and desalted by nanofiltration.

Embodiment 3

[0060] The synthesis process of sodium phenylacetate is the same as in Example 1, the difference is that the concentration of sodium phenylacetate is directly detected without using a nanofiltration membrane to desalinate after decolorization, and the calculated yield is 94.4%, and the detected purity is 98.1%.

[0061] Carry out penicillin fermentation shake flask experiment according to embodiment 1 method:

[0062] The potency of the sodium phenylacetate shake flask prepared in this example is 18000U / mL, which is more than 5% different from the result of the control group in Example 1, which does not meet the requirements of the fermentation experiment. It can be seen that the sodium phenylacetate used for direct synthesis of penicillin fermentation must be desalted by nanofiltration.

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Abstract

The invention discloses an in-situ carbonylation method straight-through liquid sodium phenylacetate synthesis method, which comprises the following steps of adopting cobalt salt and carbon monoxide as raw materials, adopting methanol as a solvent, adopting sodium thiosulfate, sodium sulfide and manganese metal as auxiliary materials, and carrying out low pressure synthesis under a stirring condition to obtain a cobalt carbonyl catalyst, introducing carbon monoxide into the catalyst system, adding benzyl chloride and liquid caustic soda in situ, and carrying out low-pressure synthesis under astirring condition to obtain sodium phenylacetate, carrying out in-situ aeration, cobalt and manganese precipitation and solid-liquid separation in a synthesis system, collecting a separation solution, and distilling to obtain a distilled concentrated solution, and performing decoloration, salt leaching and concentration on the distilled concentrated solution to obtain a sodium phenylacetate concentrated solution which can be directly used for penicillin fermentation. The synthesis method disclosed by the invention is simple to operate, continuous in process unit, free of repeated process units in the process and in accordance with atom economy, and the prepared sodium phenylacetate is high in purity and high in yield. No acidic wastewater is generated in the process treatment process, nophenylacetic acid containing peculiar smell is generated, the wastewater treatment cost is low, and the process is environmentally friendly.

Description

technical field [0001] The invention relates to the technical field of sodium phenylacetate synthesis, and more specifically relates to a synthesis method and application of in-situ carbonylation through liquid sodium phenylacetate. Background technique [0002] As an intermediate in organic synthesis, sodium phenylacetate is mainly used in the production of penicillin. There are dozens of synthetic methods for sodium phenylacetate, but most of them are difficult to apply to industrial production due to their complicated operation and high raw material prices. In addition, the sodium phenylacetate treatment process actually used for the fermentation of penicillin includes a phenylacetic acid operation unit, which has a strong odor and is difficult to treat; and the process of synthesizing phenylacetic acid produces a large amount of acidic wastewater, which requires a large amount of alkali to treat waste acid water, and the process is economical. , likely to cause adverse ...

Claims

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Application Information

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IPC IPC(8): C07C51/41C07C51/15C07C51/44C07C51/47C07C51/42C07C57/32B01J31/20
CPCC07C51/41C07C51/15C07C51/44C07C51/47C07C51/42B01J31/20B01J2531/845C07C57/32Y02P20/584
Inventor 郭建明陈顺记张鸿宾陈英新徐德芳袁晓明白雪峰朱兆华郝海涛高建成
Owner INNER MONGOLIA CHANGSHENG PHARMA
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