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Preparation method of beta-aminopropionic acid

A technology of aminopropionic acid and acrylic acid, applied in the preparation of organic compounds, chemical instruments and methods, preparation of cyanide reaction, etc., can solve the problems of long reaction time, increased energy consumption, slow mass transfer and heat transfer, etc. The method is simple, the use amount is reduced, and the reaction efficiency is high.

Active Publication Date: 2021-01-05
安徽泰格生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the succinimide method requires high process indicators and high raw material costs; while the acrylonitrile ammoniation method has a long route, many side reactions, and a large amount of salt will be generated in the process, so the cost is also very high
[0004] A patent has reported a method for preparing β-alanine by reacting acrylic acid and ammonia water in an autoclave, but hydroquinone and p-phenylenediamine need to be added as additives, and the purification of the product is difficult, and the final yield is only 73%. And the reaction time is longer, resulting in higher cost and low yield
There are also data reports that after adding acrylic acid to the autoclave and then adding ammonia and ammonium bicarbonate to mix, the reaction time is about 6-8 hours; although the above-mentioned process prepares β-alanine, the route is short, but the acrylic acid ammoniation process is all through the autoclave Realization, the mass transfer and heat transfer of the reaction system is slow, the material back-mixing is serious, the reaction time is long, and the side reactions produce more impurities. On the other hand, the intermittent reaction also makes the product space-time yield low, energy consumption increases, and costs increased
There is also a process research on the ammonification of acrylic acid to prepare β-alanine using a microchannel reactor. The reaction time is about 40-60 minutes. Although the reported conversion rate is very high, the impurities in it are slightly higher, which will lead to overall The yield is lower and the purity is slightly lower

Method used

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  • Preparation method of beta-aminopropionic acid
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A kind of preparation method of β-alanine is as follows:

[0036] (1) Prepare mixed solution according to the ratio of 1100g 18% ammonia water plus 3.6g ammonium bicarbonate, control the flow rate of acrylic acid to 1.0mL / min, the flow rate of ammonium bicarbonate and ammonia water mixture to be 8.6mL / min, mix acrylic acid, bicarbonate The mixture of ammonium and ammonia water is pumped into the mixer of the microchannel reactor at the same time, and the mixed raw materials enter the reactor for reaction at 180°C, the reaction gauge pressure is 3.0MPa, the residence time of the reaction solution is 10min, and then cooled to obtain For the mixed solution of β-alanine, open the ammonia absorption device to absorb the remaining ammonia;

[0037] (2) Add activated carbon to the mixed solution containing β-alanine and stir for 0.5 hours. After filtering out the activated carbon, the filtrate is concentrated to a syrupy state with a water-bath scraper, and 95% methanol with t...

Embodiment 2-4

[0040] The difference from Example 1 is that in this example, the reaction temperature of step (1) is 190°C (Example 2), 200°C (Example 3), and 220°C (Example 4).

Embodiment 5

[0042] A kind of preparation method of β-alanine is as follows:

[0043] (1) Prepare a mixed solution according to the ratio of 1100g 20% ​​ammonia water plus 4g ammonium bicarbonate, control the flow rate of acrylic acid to 1.0mL / min, and the flow rate of ammonium bicarbonate and ammonia water mixture to 15mL / min, mix acrylic acid, ammonium bicarbonate and The ammonia-water mixture is pumped into the mixer of the microchannel reactor at the same time, and the mixed raw materials enter the reactor to react at 200°C, the reaction gauge pressure is 3.2MPa, the residence time of the reaction solution is 10min, and then cooled down to obtain β- For the mixed solution of GALA, open the ammonia absorption device to absorb the remaining ammonia;

[0044] (2) Add activated carbon to the mixed solution containing β-alanine and stir for 1 hour. After filtering out the activated carbon, the filtrate is concentrated to a syrupy state with a water-bath scraper, and 95% methanol with twice ...

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Abstract

The invention provides a preparation method of beta-aminopropionic acid. The preparation method comprises the following steps: mixing acrylic acid, ammonium bicarbonate and ammonia water, and reactingto obtain a mixed solution containing beta-aminopropionic acid, wherein the mass ratio of the acrylic acid to the ammonium bicarbonate to the ammonia water is 1: (0.01-0.1): (5-30). The preparation method of beta-aminopropionic acid is high in conversion efficiency of acrylic acid, and the finally obtained beta-aminopropionic acid is extremely few in impurities and relatively high in purity; themethod is short in reaction time, high in reaction efficiency, environment-friendly and safe.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and relates to a preparation method of β-alanine. Background technique [0002] β-alanine, also known as 3-alanine, is an important organic synthesis intermediate, mainly used in the synthesis of pantothenic acid, calcium pantothenate, carnosine, pamidronate sodium, balsalazide, etc., in medicine, feed , food and other fields are widely used. [0003] The existing techniques for producing β-alanine mainly include acrylonitrile ammoniation method, acrylic acid (ester) ammoniation method and succinimide method. Among them, the succinimide method requires high process indicators and high raw material costs; while the acrylonitrile ammoniation method has a long route, many side reactions, and a large amount of salt will be generated in the process, and the cost is also very high. [0004] A patent has reported a method for preparing β-alanine by reacting acrylic acid and ammonia water in ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C227/08C07C229/08
CPCC07C227/08C07C229/08
Inventor 段小瑞赵安全蔡奇峰刘伟汪洪湖
Owner 安徽泰格生物科技有限公司