阅读说明：本技术 一种回收β-氨基丙酸的精制方法 (Refining method for recovering beta-aminopropionic acid ) 是由 王兵 王淑霞 王丽敏 米红杰 朱庆林 史宇浩 于 2020-06-21 设计创作，主要内容包括：本发明公开了一种回收β-氨基丙酸的精制方法,它包括以下步骤：(1)溶解：将粗β-氨基丙酸投入反应釜中,加入3-5倍质量的50-58％甲醇水溶液,反应温度控制在45-55℃,搅拌溶解25-35min；(2)浓缩析晶：离心去除甲醇溶液中的硫酸钠,收集母液进行减压浓缩蒸馏甲醇,蒸馏残液搅拌至浆状,冷却降温至15-25℃,β-氨基丙酸晶体析出；(3)离心干燥：离心得到β-氨基丙酸湿品,对其进行干燥,制得精制β-氨基丙酸。该方法操作简单、重结晶效率高、成本廉价,为β-氨基丙酸的纯化提供了一种高效的方法。(The invention discloses a refining method for recovering beta-aminopropionic acid, which comprises the following steps: (1) dissolving: putting the crude beta-aminopropionic acid into a reaction kettle, adding 50-58% methanol aqueous solution with the mass of 3-5 times of that of the crude beta-aminopropionic acid, controlling the reaction temperature at 45-55 ℃, and stirring and dissolving for 25-35 min; (2) concentrating and crystallizing: centrifuging to remove sodium sulfate in the methanol solution, collecting mother liquor, concentrating under reduced pressure, distilling methanol, stirring the distillation residual liquor to be slurry, cooling to 15-25 ℃, and separating out beta-aminopropionic acid crystals; (3) centrifugal drying: centrifuging to obtain wet beta-aminopropionic acid, and drying to obtain refined beta-aminopropionic acid. The method is simple to operate, high in recrystallization efficiency and low in cost, and provides an efficient method for purifying the beta-aminopropionic acid.)

1. A refining process for recovering beta-aminopropionic acid, comprising the steps of:

(1) dissolving: putting the crude beta-aminopropionic acid into a reaction kettle, adding 50-58% methanol aqueous solution with the mass of 3-5 times of that of the crude beta-aminopropionic acid, controlling the reaction temperature at 45-55 ℃, and stirring and dissolving for 25-35 min;

(2) concentrating and crystallizing: centrifuging to remove sodium sulfate in the methanol solution, collecting mother liquor, concentrating under reduced pressure, distilling methanol, stirring the distillation residual liquor to be slurry, cooling to 15-25 ℃, and separating out beta-aminopropionic acid crystals;

(3) centrifugal drying: centrifuging to obtain wet beta-aminopropionic acid, and drying to obtain refined beta-aminopropionic acid.

2. The refining process for recovering β -alanine according to claim 1, wherein: it comprises the following steps:

(1) dissolving: putting the crude beta-aminopropionic acid into a reaction kettle, adding 56% methanol aqueous solution with the mass of 3.6 times of that of the crude beta-aminopropionic acid, controlling the reaction temperature at 50 ℃, and stirring for dissolving for 30 min;

(2) concentrating and crystallizing: centrifuging to remove sodium sulfate in the methanol solution, collecting mother liquor, concentrating under reduced pressure, distilling methanol, stirring the distillation residual liquor to be slurry, cooling to 20 ℃, and separating out beta-aminopropionic acid crystals;

(3) centrifugal drying: centrifuging to obtain wet beta-aminopropionic acid, and drying to obtain refined beta-aminopropionic acid.

3. The refining process for recovering β -aminopropionic acid according to claim 1 or 2, wherein: in the step (2), the distillation is carried out under reduced pressure until the mass of the residual distillation liquid is 18 to 22 percent of the total input solution.

Technical Field

The invention belongs to the technical field of chemical pharmacy, and particularly relates to a refining method for recovering beta-aminopropionic acid.

Background

Calcium D-pantothenate (vitamin B5) is mainly used in medicine, food additive and feed additive, and is an indispensable trace substance for maintaining normal physiology of human body and animals. Beta-aminopropionic acid is an important raw material for synthesizing the D-calcium pantothenate, and meanwhile, in the production process, the recovered beta-aminopropionic acid is obtained by recovering and treating the D-calcium pantothenate mother liquor.

Because sulfuric acid and sodium hydroxide are added in the process of recovering the D-calcium pantothenate mother liquor, the recovered crude beta-aminopropionic acid contains a large amount of sodium sulfate. Therefore, the crude β -aminopropionic acid needs to be further purified to remove sodium sulfate.

Disclosure of Invention

The invention aims to provide a refining method for recovering beta-aminopropionic acid, which mainly solves the problems that the content of beta-aminopropionic acid is low and sodium sulfate cannot be removed in the existing beta-aminopropionic acid recovery process.

The present invention solves the above problems by the following technical solutions,

a refining process for recovering beta-aminopropionic acid, comprising the steps of:

(1) dissolving: putting the crude beta-aminopropionic acid into a reaction kettle, adding 50-58% methanol aqueous solution with the mass of 3-5 times of that of the crude beta-aminopropionic acid, controlling the reaction temperature at 45-55 ℃, and stirring and dissolving for 25-35 min;

(2) concentrating and crystallizing: centrifuging to remove sodium sulfate in the methanol solution, collecting mother liquor, concentrating under reduced pressure, distilling methanol, stirring the distillation residual liquor to be slurry, cooling to 15-25 ℃, and separating out beta-aminopropionic acid crystals;

(3) centrifugal drying: centrifuging to obtain wet beta-aminopropionic acid, and drying to obtain refined beta-aminopropionic acid.

Preferably, a refining process for recovering beta-aminopropionic acid comprises the steps of:

(1) dissolving: putting the crude beta-aminopropionic acid into a reaction kettle, adding 56% methanol aqueous solution with the mass of 3.6 times of that of the crude beta-aminopropionic acid, controlling the reaction temperature at 50 ℃, and stirring for dissolving for 30 min;

(2) concentrating and crystallizing: centrifuging to remove sodium sulfate in the methanol solution, collecting mother liquor, concentrating under reduced pressure, distilling methanol, stirring the distillation residual liquor to be slurry, cooling to 20 ℃, and separating out beta-aminopropionic acid crystals;

(3) centrifugal drying: centrifuging to obtain wet beta-aminopropionic acid, and drying to obtain refined beta-aminopropionic acid.

Preferably, in the step (2), the distillation is carried out under reduced pressure until the mass of the remaining distillation residue is 18 to 22% of the total amount of the charged solution.

The invention has the beneficial effects that:

the crude beta-aminopropionic acid is obtained by recycling the D-calcium pantothenate mother liquor, the crude beta-aminopropionic acid contains sodium sulfate, and the content of the crude beta-aminopropionic acid is about 50 to 80 percent generally; the method of the invention carries out recrystallization purification on crude beta-aminopropionic acid with unqualified content and purity, and the content of the beta-aminopropionic acid can be improved to more than 93.7 percent by controlling parameters such as recrystallization solvent selection, dosage, crystallization temperature and the like in the recrystallization process, and the recrystallization yield reaches 73 to 95 percent. In actual production, technological parameters in the recrystallization method can be flexibly selected according to the purity requirement of the crude beta-aminopropionic acid, and the purification cost is controlled;

the method has the advantages of simple operation, high recrystallization efficiency and low cost, and provides an efficient way for purifying the beta-aminopropionic acid.

Detailed Description

The technical solution of the present invention will be further specifically described below by way of examples.