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Method for efficiently preparing beta-aminopropionic acid

A technology of aminopropionic acid and liquid ammonia, applied in chemical instruments and methods, preparation of cyanide reaction, preparation of organic compounds, etc., can solve problems such as low yield and selectivity, and lack of conditions for large-scale use, and achieve The effect of simple purification, high product index and improved economic benefit

Pending Publication Date: 2022-01-28
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Low yield and selectivity make this route unsuitable for large-scale use

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Put acrylonitrile, liquid ammonia, water, isopropanol, piperazine, and ammonium carbonate into the autoclave, wherein the molar ratio of acrylonitrile and liquid ammonia is 1:10, and the addition amounts of water and isopropanol are respectively acrylonitrile The mass is 4 times and 7 times, and the addition amount of piperazine and ammonium carbonate (the molar ratio of the two is: 1:8) is 70 mol% based on acrylonitrile.

[0019] After sealing the reactor, control the reaction temperature to 190° C. and the pressure to 4.8 MPa, and react at constant temperature for 13 hours. After the reaction is completed, a sample is taken to detect that the conversion rate of acrylonitrile is greater than 99%, the ammonia absorption pump is turned on to absorb the remaining ammonia, and then the reaction mother liquor is concentrated under reduced pressure. The concentrated reaction solution is cooled to crystallize, the obtained crystal is suction filtered and dried to obtain the p...

Embodiment 2

[0021] Put acrylonitrile, liquid ammonia, water, tert-butanol, morpholine, and ammonium carbonate into the autoclave, wherein the molar ratio of acrylonitrile and liquid ammonia is 1:8, and the addition amounts of water and tert-butanol are respectively The mass is 6 times and 10 times, and the addition amount of morpholine and ammonium carbonate (the molar ratio of the two is: 1:10) is 90 mol% based on acrylonitrile.

[0022] After sealing the reactor, control the reaction temperature to 250° C. and the pressure to 7.5 MPa, and react at constant temperature for 18 hours. After the reaction is completed, a sample is taken to detect that the conversion rate of acrylonitrile is greater than 99%, the ammonia absorption pump is turned on to absorb the remaining ammonia, and then the reaction mother liquor is concentrated under reduced pressure. The concentrated reaction solution is cooled to crystallize, the obtained crystal is suction filtered and dried to obtain the product, and...

Embodiment 3

[0024] Put acrylonitrile, liquid ammonia, water, isopropanol, diphenylamine and ammonium bicarbonate into the autoclave, wherein the molar ratio of acrylonitrile and liquid ammonia is 1:12, and the addition amount of water and isopropanol is propylene The mass of nitrile is 3 times and 5 times, and the addition amount of diphenylamine and ammonium bicarbonate (the molar ratio of both is: 1:15) is 100 mol% based on acrylonitrile.

[0025] After sealing the reactor, control the reaction temperature to 120° C. and the pressure to 2.3 MPa, and react at constant temperature for 15 hours. After the reaction is completed, a sample is taken to detect that the conversion rate of acrylonitrile is greater than 99%, the ammonia absorption pump is turned on to absorb the remaining ammonia, and then the reaction mother liquor is concentrated under reduced pressure. The concentrated reaction solution is cooled to crystallize, the obtained crystal is suction filtered and dried to obtain the p...

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PUM

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Abstract

The invention discloses a method for directly preparing beta-aminopropionic acid from acrylonitrile. The method comprises the following steps: in a tank reactor, acrylonitrile and liquid ammonia are reacted in the presence of a solvent and an additive, then a reaction liquid is subjected to ammonia recovery, solvent recovery and crystallization treatment, beta-aminopropionic acid is prepared, and mother liquor is recycled; wherein the solvent is a mixed system of water and alcohol, and the additive is organic amine and / or inorganic amine salt. Beta-aminopropionic acid is synthesized in one step, generation of a large amount of inorganic salt in a two-step method is avoided, and the method has the advantages of being simple and safe in route, high in product yield, convenient to purify and the like.

Description

technical field [0001] The present invention relates to the preparation of an amino acid, in particular to a preparation method of β-alanine. Background technique [0002] D-pantothenic acid is an indispensable and irreplaceable substance for humans and animals to maintain normal physiological functions. It has broad market prospects. However, due to the instability of pantothenic acid such as deliquescence, its commercial form is calcium salt, namely calcium pantothenate. One of the key intermediates in the production of calcium pantothenate is β-alanine. [0003] At present, the production methods of β-alanine mainly include enzymatic method and acrylonitrile ammonification hydrolysis method. Among them, the cost of enzymatic production is relatively high, and it is accompanied by the generation of a large amount of waste water. In the acrylonitrile ammonification hydrolysis method, acrylonitrile is used as a raw material, and the product is prepared through two-step rea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C227/26C07C227/40C07C227/42C07C229/08
CPCC07C227/26C07C227/40C07C227/42C07C229/08
Inventor 李胜勇郑兵张涛
Owner WANHUA CHEM GRP CO LTD