CN111662199A - Refining method for recovering beta-aminopropionic acid - Google Patents
Refining method for recovering beta-aminopropionic acid Download PDFInfo
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- CN111662199A CN111662199A CN202010608763.XA CN202010608763A CN111662199A CN 111662199 A CN111662199 A CN 111662199A CN 202010608763 A CN202010608763 A CN 202010608763A CN 111662199 A CN111662199 A CN 111662199A
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- aminopropionic acid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/38—Separation; Purification; Stabilisation; Use of additives
- C07C227/40—Separation; Purification
Abstract
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.
Description
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.
Example 1: putting 65% crude beta-aminopropionic acid into a reaction kettle, and adding 50% methanol aqueous solution with the mass being 3 times that of the crude beta-aminopropionic acid; controlling the reaction temperature at 50 ℃, and stirring for dissolving for 25 min; centrifuging to remove sodium sulfate in the methanol solution, carrying out reduced pressure concentration on the mother solution to distill methanol, stirring the residual distillation liquid with the mass accounting for 18 percent of the total input solution amount to be pulpous, cooling to about 15 ℃, separating out beta-aminopropionic acid crystals, centrifuging to obtain a wet beta-aminopropionic acid product, and drying to obtain a finished beta-aminopropionic acid product. The content of the beta-aminopropionic acid is 79.4 percent by test.
Example 2: putting the crude beta-aminopropionic acid with the content of 72% into a reaction kettle, and adding 52% methanol aqueous solution with the mass 5 times that of the crude beta-aminopropionic acid; controlling the reaction temperature at 45 ℃, and stirring and dissolving for 28 min; centrifuging to remove sodium sulfate in the methanol solution, carrying out reduced pressure concentration on the mother solution to distill methanol, stirring the residual distillation liquid with the mass accounting for 19 percent of the total input solution amount to be pulpous, cooling to about 25 ℃, separating out beta-aminopropionic acid crystals, centrifuging to obtain a wet beta-aminopropionic acid product, and drying to obtain a finished beta-aminopropionic acid product. The content of the beta-aminopropionic acid is 81.3 percent by test.
Example 3: putting 75% crude beta-aminopropionic acid into a reaction kettle, and adding 58% methanol aqueous solution with the mass being 3.6 times that of the crude beta-aminopropionic acid; controlling the reaction temperature at 52 ℃, and stirring and dissolving for 30 min; centrifuging to remove sodium sulfate in the methanol solution, carrying out reduced pressure concentration on the mother solution to distill methanol, stirring the residual distillation liquid with the mass accounting for 20% of the total input solution amount to be in a slurry state, cooling to about 20 ℃, separating out beta-aminopropionic acid crystals, centrifuging to obtain a wet beta-aminopropionic acid product, and drying to obtain a finished beta-aminopropionic acid product. The content of the beta-aminopropionic acid is 91.7 percent by test.
Example 4: putting the crude beta-aminopropionic acid with the content of 76% into a reaction kettle, and 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 48 ℃, and stirring for dissolving for 35 min; centrifuging to remove sodium sulfate in the methanol solution, carrying out reduced pressure concentration on the mother solution to distill methanol, stirring the residual distillation liquid with the mass being 21% of the total input solution amount to be in a slurry state, cooling to about 20 ℃, separating out beta-aminopropionic acid crystals, centrifuging to obtain a wet beta-aminopropionic acid product, and drying to obtain a finished beta-aminopropionic acid product. The content of the beta-aminopropionic acid is 92.8 percent through test and measurement.
Example 5: putting the crude beta-aminopropionic acid with the content of 76% into a reaction kettle, and 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; centrifuging to remove sodium sulfate in the methanol solution, carrying out reduced pressure concentration on the mother solution to distill methanol, stirring the residual distillation liquid with the mass accounting for 20% of the total input solution amount to be in a slurry state, cooling to about 20 ℃, separating out beta-aminopropionic acid crystals, centrifuging to obtain a wet beta-aminopropionic acid product, and drying to obtain a finished beta-aminopropionic acid product. The content of the beta-aminopropionic acid is 93.9 percent by test.
Example 6: putting 53 percent crude beta-aminopropionic acid into a reaction kettle, and adding 3.6 times of 56 percent methanol aqueous solution by mass; controlling the reaction temperature at 50 ℃, and stirring for dissolving for 30 min; centrifuging to remove sodium sulfate in the methanol solution, carrying out reduced pressure concentration on the mother solution to distill methanol, stirring the residual distillation liquid with the mass accounting for 20% of the total input solution amount to be in a slurry state, cooling to about 20 ℃, separating out beta-aminopropionic acid crystals, centrifuging to obtain a wet beta-aminopropionic acid product, and drying to obtain a finished beta-aminopropionic acid product. The content of the beta-aminopropionic acid is 93.7 percent by test.
Claims (3)
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.
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| CN202010608763.XA CN111662199A (en) | 2020-06-21 | 2020-06-21 | Refining method for recovering beta-aminopropionic acid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113979879A (en) * | 2021-09-26 | 2022-01-28 | 万华化学集团股份有限公司 | Method for efficiently preparing beta-aminopropionic acid |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110903207A (en) * | 2019-12-16 | 2020-03-24 | 江苏兄弟维生素有限公司 | Method for producing aminopropionic acid and sodium sulfate by using β -formylaminopropionitrile and application of aminopropionic acid and sodium sulfate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110903207A (en) * | 2019-12-16 | 2020-03-24 | 江苏兄弟维生素有限公司 | Method for producing aminopropionic acid and sodium sulfate by using β -formylaminopropionitrile and application of aminopropionic acid and sodium sulfate |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113979879A (en) * | 2021-09-26 | 2022-01-28 | 万华化学集团股份有限公司 | Method for efficiently preparing beta-aminopropionic acid |
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Application publication date: 20200915 |