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Novel beta-aminopropanoic acid synthesis technology

A kind of technology of aminopropionic acid and synthesis process, which is applied in the preparation of organic compounds, organic chemistry, chemical instruments and methods, etc., can solve the problems of β-alanine acid destruction, unqualified finished product quality, long production time, etc., and achieve concentration The effect of short cycle, shortened recovery cycle and high yield

Active Publication Date: 2014-07-30
江苏兄弟维生素有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] 1. A large amount of mother liquor needs to be recycled and concentrated, and the production time is long, which leads to the destruction of part of β-alanine during the recycling process, and the yield is low
[0011] 2. Recycling leads to the accumulation of impurities, and the quality of the finished product will be unqualified if it is applied more than 5 times per cycle. In the end, the residual liquid of methanol distillation has to be discarded (commonly known as batch killing), and the finished product is washed and reworked, resulting in low yield. Big pollution

Method used

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  • Novel beta-aminopropanoic acid synthesis technology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) Hydrolysis, temperature-controlled dropwise addition of β-aminopropionitrile in the β-aminopropionitrile metering tank 1 to the hydrolysis kettle 2 in which liquid caustic soda has been added to carry out the hydrolysis reaction;

[0036] (2) Neutralization, using hydrochloric acid to neutralize the hydrolyzed solution in the neutralization tank 3;

[0037] (3) Concentrate and concentrate in the concentration kettle 4 while maintaining a certain temperature and vacuum;

[0038] (4) Heat filtration, adding a salting-out agent and using a centrifuge 5 for direct heat filtration, and the filtrate is cooled and filtered to obtain the crude product of β-alanine;

[0039] (5) Synchronous operation, the filtrate obtained by filtering the crude product of β-alanine is returned to the concentrated and filtered cycle operation through the salt washing tank 6; at the same time, the crude product of β-alanine is dissolved to enter the next step;

[0040] (6) Recrystallization,...

Embodiment 2

[0044] hydrolysis:

[0045] 1. Add 211.2g of liquid caustic soda to the three-necked flask, raise the temperature to 80°C with a water bath, slowly open the 88g β-aminopropionitrile drop valve, and control the dropwise addition in 5-6 hours, the temperature is 80-90°C;

[0046] 2. At the end of the dropwise addition, keep warm for 30 minutes at a temperature of 90-95°C and a pressure of -0.02MPa;

[0047] 3. After the heat preservation is completed, the ammonia is driven by vacuum.

[0048] neutralize:

[0049] 1. Cool down to about 40°C and add 230g of hydrochloric acid dropwise, and the neutralization temperature is below 50°C;

[0050] 2. When adding dropwise until 10g of hydrochloric acid remains, check the pH, continue to add dropwise until the pH is 7, and retest the pH value after half an hour.

[0051] Concentration: Keep the decompression outlet water temperature at 85-100°C and the vacuum degree above -0.09MPa.

[0052] Hot Filtration: After adding salting-out ag...

Embodiment 3

[0063] hydrolysis:

[0064] 1. Add 105.6g of liquid caustic soda into the three-necked flask, raise the temperature to 80°C with a water bath, slowly open the 44g aminopropionitrile drop valve, control the dropwise addition within 2-3 hours, and the temperature is 80-90°C;

[0065] 2. At the end of the dropwise addition, keep warm for 30 minutes at a temperature of 90-95°C and a pressure of -0.02MPa;

[0066] 3. After the heat preservation is completed, the ammonia is driven by vacuum.

[0067] neutralize:

[0068] 1. Cool down to about 40°C and prepare to add 115g of hydrochloric acid dropwise, and the neutralization temperature is below 50°C;

[0069] 2. When adding dropwise until 10g of hydrochloric acid remains, check the pH, continue to add dropwise until the pH is 7, and retest the pH value after half an hour.

[0070] Concentration: Keep the decompression outlet water temperature at 85-100°C and the vacuum degree above -0.09MPa.

[0071] Hot Filtration: After adding...

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Abstract

The invention discloses a novel beta-aminopropanoic acid synthesis technology, which comprises the following steps: hydrolyzing beta-aminopropionitrile under an alkali solution condition, neutralizing, concentrating for a while and adding a salting-out agent for direct hot filtration, cooling a filtrate and filtering to obtain the aminopropanoic acid crude product, returning the filtrate for concentrating, filtering and performing a cycle operation, dissolving the beta-aminopropanoic acid crude product, adding a novel recrystallization solvent for recrystallization, filtering a recrystallization mixture to obtain the beta-aminopropanoic acid refine product, drying to obtain the finished product, rectifying a crystallization mother liquor, recovering the solvent for application, performing spray drying on rectification raffinate to obtain the aminopropanoic acid, and recovering the aminopropanoic acid and washing through the novel solvent and dissolving for a recrystallization cycle operation. The synthesis technology has the advantages of high efficiency, short concentration period and high yield, and the refined yield can reach 95% by refining process.

Description

technical field [0001] The invention relates to a synthesis method of organic compounds, in particular to a synthesis process of an organic chemical intermediate β-alanine. Background technique [0002] Nitrile compounds are a class of chemical substances (R-CN) containing cyano functional groups, and are important synthetic raw materials. Starting from nitrile compounds, a class of compounds with higher value and wider application range such as amides, amino acids, and carboxylic acids can be obtained. They can be used as chemical raw materials, pharmaceutical intermediates, and vitamin precursors. [0003] β-alanine is a multipurpose organic raw material and an important intermediate for the preparation of calcium pantothenate, which is widely used in medicine, food and feed industries. my country consumes a lot of β-alanine and its related products. At present, there are many domestic units producing β-alanine, but its industrial production methods are mainly acrylonitri...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C229/08C07C227/26C07C227/40
Inventor 李健平李来成陈英明崔胜凯
Owner 江苏兄弟维生素有限公司
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