Novel method for L-phenylglycine precursor phenylhydantoin by MIC reactor

A technology of L-phenylglycine and reactor, which is applied in organic chemistry and other fields, can solve problems such as hidden safety hazards and high environmental risks, excessive unorganized waste gas, leakage of sealing surface materials, etc., and achieve slow amplification effect, significant economic benefits, and economic benefits obvious effect

Active Publication Date: 2019-05-21
ZHEJIANG YUNTAO BIOTECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, the process adopts intermittent production in reactors, and there is a lot of unorganized waste gas. During the material transfer process, there may be material leakage on the sealing surface, which poses high safety hazards and environmental risks.

Method used

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  • Novel method for L-phenylglycine precursor phenylhydantoin by MIC reactor
  • Novel method for L-phenylglycine precursor phenylhydantoin by MIC reactor
  • Novel method for L-phenylglycine precursor phenylhydantoin by MIC reactor

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Embodiment 1: 820kg ammonium bicarbonate (converting pure), 1580kg sodium cyanide (30% aqueous solution), 1000kg benzaldehyde are pumped into the MIC reactor that has been preheated to 60 ℃ by metering pump respectively, note The ammonium bicarbonate aqueous solution is first pumped into about 500kg, and then the benzaldehyde, the ammonium bicarbonate aqueous solution and 30% sodium cyanide are pumped in at the same time. The flow rate setting is based on the simultaneous pumping of the three raw materials. The preparation solution was hydrolyzed to obtain 1644 kg of derbiphenylglycine, and the test results were: loss on drying: 19.23%; sulfate radical: 2 ppm; alkali absorbance value: 0.277AU.

Embodiment 2

[0019] Ammonium bicarbonate aqueous solution, 30% sodium cyanide, and benzaldehyde are continuously pumped into the MIC reactor preheated to 60°C at the flow rate of 2800L / h, 940L / h, and 600L / h respectively, and the preparation that meets the requirements can be obtained continuously Liquid, the prepared liquid can be hydrolyzed to obtain qualified DL-phenylglycine. Note that during the continuous preparation process, always pay attention to whether the reaction solution turns blue. If it turns blue, it means that there is too much sodium cyanide in the reaction system, and it is necessary to reduce the feeding amount of 30% sodium cyanide in time.

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Abstract

The invention relates to a novel method for an L-phenylglycine precursor phenylhydantoin by an MIC reactor. An existing process carries out intermittent production by using a reaction kettle, is morein tissue-free exhaust gas, has the probability that materials on a sealing face in a material transfer process leak and is relatively high in potential safety hazard and environmental protection risks. Ammonium hydrogen carbonate (converted in purity), sodium cyanide (30% aqueous solution) and benzaldehyde are pumped into the MIC reactor preheated to 60 DEG C in a mass ratio of 8.2: 15.8: 10 fora mixed reaction, and a prepared liquid is hydrolyzed to obtain a dl-phenylglycine. The discharge port of the MIC reactor is connected to a gas-liquid separating tank, the gas outlet of the gas-liquidseparating tank is connected to a pressure gauge to display the system pressure, and the gas-liquid separating tank is also connected to a back pressure value to back-press the whole system. By replacing solid ammonium hydrogen carbonate with an ammonium hydrogen carbonate aqueous solution, dust and tissue-free exhaust gas generated in inputting the solid ammonium hydrogen carbonate are avoided successfully. In addition, the dosage of ammonium hydrogen carbonate is reduced from 1.5 equivalent weight to 1.1 equivalent weight, so that the economical benefit is obvious.

Description

technical field [0001] The invention relates to a new method for preparing L-phenylglycine precursor dihydantoin with an MIC reactor. Background technique [0002] At present, manufacturers at home and abroad basically use the Bucherer–Bergs method to produce L-phenylglycine. This method uses benzaldehyde as a starting material, and reacts with excessive ammonium bicarbonate (or ammonium carbonate) under the action of sodium cyanide (or potassium cyanide). Dihydantoin is obtained, and L-phenylglycine is obtained through hydrolysis and resolution. The yield of dihydantoin (in terms of benzaldehyde) is about 80%, and the wastewater treatment is difficult. [0003] The Bucherer–Bergs method uses a large amount of highly toxic sodium cyanide (or potassium cyanide), a small amount of hydrogen cyanide gas is produced in the reaction, and CN- exists in the reaction liquid, which is harmful to equipment safety operation, occupational health control measures, and environmental protec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/74
Inventor 林韦康江晓明钱程良朱运涛归晨秋
Owner ZHEJIANG YUNTAO BIOTECH
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