Method for preparing beta-aminopropionic acid with high selectivity

A technology of aminopropionic acid and acrylic acid, applied in the field of chemistry, can solve the problems of low yield and selectivity, unfavorable for large-scale use, etc., and achieves the effects of improved selectivity, mild reaction conditions, and improved overall yield

Active Publication Date: 2021-11-05
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Lower yield and selectivity are not conducive to the large-scale use of this route

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Put acrylic acid and ammonia water with a concentration of 35wt% into the reactor at a molar ratio of acrylic acid:ammonia=1:7, and the addition amounts of cobalt chloride and 4,4'-dicarboxy-2,2'-bipyridine are respectively 5 mol% and 10 mol% of acrylic acid, after the reactor is sealed, the reaction temperature is controlled at 80° C., the pressure is controlled at 1.0 MPa, and the reaction is performed at a constant temperature for 3 hours. After the reaction was completed, the conversion rate of acrylic acid was detected by sampling to be greater than 99%. The excess ammonia was absorbed by an ammonia absorption pump, and then concentrated by vacuum distillation until the reaction liquid was syrupy, and then methanol was added that was 7 times the weight of the initial acrylic acid. Continue to stir and reflux at this temperature for 1 h, then cool down and crystallize. The resulting crystals are β-alanine after suction filtration and drying. The resulting crystalli...

Embodiment 2

[0018] Put acrylic acid and ammonia water with a concentration of 35% into the reactor at a molar ratio of acrylic acid:ammonia=1:10, and the addition amounts of cobalt chloride and 4,4'-dicarboxy-2,2'-bipyridine are respectively 9mol% and 15mol% of acrylic acid, after the reactor is sealed, the reaction temperature is controlled at 130°C, the pressure is controlled at 1.7MPa, and the reaction is performed at a constant temperature for 0.5h. After the reaction is completed, the conversion rate of acrylic acid is greater than 99% by sampling. The excess ammonia is absorbed by an ammonia absorption pump, and then concentrated by vacuum distillation until the reaction liquid is syrupy, and then methanol that is 8 times the weight of acrylic acid is added. Continue to stir and reflux at this temperature for 1 h, then cool down and crystallize. The resulting crystals are β-alanine after suction filtration and drying. The resulting crystalline mother liquor is recycled to remove me...

Embodiment 3

[0020] Put acrylic acid and ammonia water with a concentration of 30% into the reactor at a molar ratio of acrylic acid:ammonia=1:10, and the addition amounts of nickel chloride and 5,5'-dicarboxy-2,2'-bipyridine are respectively 8 mol% and 13 mol% of acrylic acid, after the reactor is sealed, the reaction temperature is controlled at 120° C., the pressure is controlled at 1.5 MPa, and the reaction is performed at a constant temperature for 1 hour. After the reaction was completed, the conversion rate of acrylic acid was detected to be greater than 99% by sampling. The excess ammonia was absorbed by an ammonia absorption pump, and then concentrated by vacuum distillation until the reaction liquid was in the form of syrup, and methanol 9 times the weight of acrylic acid was added. Continue to stir and reflux at this temperature for 1 h, then cool down and crystallize. The resulting crystals are β-alanine after suction filtration and drying. The resulting crystalline mother liq...

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Abstract

The invention discloses a method for preparing beta-aminopropionic acid from acrylic acid. The method comprises the step that: in a tank reactor, acrylic acid and ammonia water react in the presence of a catalyst and a ligand, and then reaction liquid is subjected to deamination, concentration and crystallization treatment to prepare beta-aminopropionic acid, wherein the catalyst is a transition metal inorganic salt, and the ligand is a pyridine ligand. The method has the advantages of good product selectivity, high yield, convenience in purification, mild process conditions and the like. Experiments show that: with the catalyst and the ligand introduced, the conversion rate of the acrylic acid is greater than 99%, the yield of the single-pass product of the reaction is greatly improved to 82%, the difficulty of later purification is greatly reduced, a mother liquor can be recycled, and the recycling yield is greater than 95%.

Description

technical field [0001] The invention belongs to the technical field of chemistry, and in particular relates to a preparation method of β-alanine. Background technique [0002] β-alanine, as the only β-type amino acid in nature, is mainly used as a key intermediate in the synthesis of calcium pantothenate (vitamin B5). In addition, it is also widely used in medicine, food and other fields, and has a good market prospect. At present, the methods for producing β-alanine mainly include acrylonitrile ammoniation hydrolysis, enzymatic method and acrylic acid ammoniation method. Among them, the route of the acrylonitrile method is relatively long, and after hydrolysis, a large amount of inorganic salts are produced, so purification is relatively difficult. The enzymatic method mainly uses L-aspartic acid as a raw material, which is catalyzed by L-aspartic acid decarboxylase, and the production cost is relatively high, and it is accompanied by the generation of a large amount of wa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/08C07C227/08C07C227/40C07C227/42
CPCC07C227/08C07C227/40C07C227/42C07C229/08
Inventor 李胜勇孔令晓张涛
Owner WANHUA CHEM GRP CO LTD
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