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Treatment process for leftover materials generated in glycine ethyl ester hydrochloride preparation process

A technology for treating ethyl glycine hydrochloride, which is applied in the recycling field of reaction waste, and can solve the problems such as the increase of impurities in the scrap mother liquor

Active Publication Date: 2021-02-19
江苏优普生物化学科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After many times of treatment, the impurities in the scrap mother liquor increase, usually at 140°C, vacuum degree -0.098MPa, still contains a large amount of water that cannot be evaporated, because glycine ethyl ester hydrochloride is very soluble in water, the scrap in this state It is difficult to process the raw materials to obtain products, which can only be treated as solid waste

Method used

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  • Treatment process for leftover materials generated in glycine ethyl ester hydrochloride preparation process
  • Treatment process for leftover materials generated in glycine ethyl ester hydrochloride preparation process

Examples

Experimental program
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Effect test

Embodiment 1

[0036](1) To a glass-lined kettle a with a stirring volume of 3000L, pump 800L of the mother liquor after distillation and recovery of ethanol, stir, pump 1600L of absolute ethanol, stir for half an hour, press filter to a volume with stirring and reflux 3000L glass-lined kettle b;

[0037](2) Slowly pour ammonia gas into the glass-lined kettle b, and control the aeration speed to 1.5~2.0m3 / min, after reaching the pH value of 8, keep the pH value around 8 and keep the temperature at 55~65℃ for 2 hours, observe that a large number of white crystals appear in the kettle;

[0038](3) Pass cooling water to the jacket of the glass-lined kettle b, cool it to room temperature, keep it for 2 hours, centrifuge it, and after spin-drying, take a sample to detect that the chloride ion content in the filter cake is 0.9%, and use 95% ethanol. After washing the filter cake once, the chloride ion content in the filter cake was detected to be 0.4%. The filter cake was vacuum-dried to obtain 342.9 kg of cr...

Embodiment 2

[0041](1) To a glass-lined kettle a with a stirring volume of 3000L, pump 800L of the mother liquor after distillation and recovery of ethanol, stir, pump in 1600L of 95% ethanol, stir for half an hour, and filter to a volume with stirring and reflux. 3000L glass-lined kettle b.

[0042](2) Slowly pour ammonia gas into the glass-lined kettle b, and control the aeration speed to 1.5~2.0m3 / min, after reaching the pH value of 8, keep the pH value around 8 and keep the temperature at 55~65℃ for 2 hours, observe that a large number of white crystals appear in the kettle;

[0043](3) Pass cooling water to the jacket of the glass-lined kettle b, cool it down to normal temperature, keep it for 2 hours, centrifuge it, and after spinning dry, take a sample and check that the chloride ion content in the filter cake is 0.6%. Use 95% ethanol. After washing the filter cake once, the chloride ion content in the filter cake was detected to be 0.35%. The filter cake was vacuum-dried to obtain 316.3kg of c...

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Abstract

The invention discloses a treatment process for leftover materials generated in a glycine ethyl ester hydrochloride preparation process. The process comprises the steps of reacting glycine with absolute ethyl alcohol in the presence of hydrogen chloride, crystallizing and separating a reaction product to obtain mother liquor, and adding alkali to hydrolyze the mother liquor. The treatment method provided by the scheme for the leftover materials generated in the glycine ethyl ester hydrochloride preparation process is particularly suitable for treating the leftover materials after repeated treatment and recovery. Through the treatment, residual glycine ethyl ester hydrochloride, glycine hydrochloride and other hydrolyzable byproducts are hydrolyzed into glycine and the like by adding alkali, then the pH value is adjusted to be close to an isoelectric point of glycine, glycine is separated out, glycine is obtained through separation, and ethanol generated through hydrolysis is recycled through distillation. By means of the scheme, the generation amount of leftover solid waste can be greatly reduced.

Description

Technical field[0001]The invention relates to the technical field of the recovery of reaction wastes, and in particular to a process for treating the waste produced in the process of preparing glycine ethyl ester hydrochloride.Background technique[0002]The chemical name of ethyl glycinate hydrochloride is ethyl aminoacetate hydrochloride, a widely used pesticide and pharmaceutical intermediate, and can also be used in biochemical research and as a feed additive. In the synthesis of pesticides, ethyl glycinate hydrochloride is the key intermediate for many pyrethroid pesticides such as permethrin, allethrin, furfurthrin, tetramethrin, and fenthrin. Pyrethroid insecticides are the most widely used insecticides in the world. They are widely used in agriculture, storage, and sanitation. It can also be used to synthesize pesticides such as iprodione. In medical synthesis, it can be used to synthesize anti-inflammatory drugs such as gemifloxacin, such as Chinese patent CN104725294A, which...

Claims

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Application Information

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IPC IPC(8): C07C227/18C07C227/40C07C229/08C07C29/09C07C31/04C07C29/80
CPCC07C227/18C07C227/40C07C29/095C07C29/80C07C229/08C07C31/04
Inventor 张继钱马成龙徐莹莹邱历施云云
Owner 江苏优普生物化学科技股份有限公司
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