A method for crystallizing beta-alanine
Patent Information
- Application Number
- CN202611241506.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-08-17
- Publication Date
- 2026-11-03
AI Technical Summary
β-alanine crystallization has a low yield and high production cost, and existing technologies make it difficult to achieve a high-quality and efficient crystallization process.
The β-alanine mother liquor was treated with cationic and anionic resins. Through filtration, concentration, crystallization and drying steps, combined with specific conditions such as flow rate, temperature and reagent ratio, high-purity β-alanine crystals were obtained.
This method improves the crystallization yield of β-alanine, reduces production costs, and yields high-quality β-alanine crystals. The operation is simple and the finished product has high purity.
Abstract
Description
Technical Field
[0001] This invention relates to the field of pharmaceutical chemistry, and more particularly to a method for crystallizing β-alanine. Background Technology
[0002] β-Alanine has various physiological functions, such as regulating metabolism, combating fatigue, and improving physical performance. As a synthetic raw material, β-alanine is used to manufacture pantothenic acid and its derivatives, and is used as a flavoring agent, adjuvant, and nutritional supplement. β-alanine is polymerized into polyβ-alanine, which is widely used in cosmetics, water purification, and construction.
[0003] β-Alanine, a non-protein amino acid, can be synthesized in microorganisms, plants, and insects. In the laboratory, it can be produced by the decarboxylation reaction of succinimide with potassium hypobromide upon heating. Chemical synthesis is the main method for large-scale production of β-alanine. β-alanine can also be prepared through enzymatic conversion and microbial fermentation.
[0004] β-alanine crystallization has a low yield and high production cost. Therefore, developing a high-yield, high-quality crystallization method has significant market value. Summary of the Invention
[0005] The purpose of this invention is to overcome the deficiencies in the prior art and provide a method for crystallizing β-alanine.
[0006] To achieve the above-mentioned objectives, the present invention provides the following technical solution: This invention provides a method for crystallizing β-alanine, comprising the following steps: (1) Pass the β-alanine mother liquor through a cation exchange resin and an anion exchange resin in sequence to obtain a β-alanine feed solution; (2) The β-alanine solution is filtered, concentrated, crystallized and dried in sequence to obtain β-alanine crystals.
[0007] Preferably, the cationic resin in step (1) is a hydrogen-form resin; The volume ratio of β-alanine mother liquor to cation exchange resin is 10~20:1~3.
[0008] Preferably, the anion exchange resin in step (1) is a hydroxyl resin; The volume ratio of β-alanine mother liquor to anion exchange resin is 10~20:2.5~3.5.
[0009] Preferably, the flow rate of the feed liquid through the cation exchange resin in step (1) is 200~400mL / h; The flow rate of the feed solution through the anion exchange resin is 200~400mL / h.
[0010] Preferably, the pore size of the filter membrane used in step (2) is 0.4~0.5μm.
[0011] Preferably, the concentration temperature in step (2) is 50~80℃, and the mass concentration of β-alanine in the concentrate is 50~65%.
[0012] Preferably, the reagent used for crystallization in step (2) is one or more of acetone, methanol, ethanol and isopropanol.
[0013] Preferably, the ratio of β-alanine to crystallization reagent in the concentrate is 1g:1~5mL.
[0014] Preferably, the crystallization temperature in step (3) is 5~15℃ and the time is ≥1h.
[0015] Preferably, the drying temperature in step (3) is 60~80℃ and the vacuum degree is -0.08~-0.1MPa.
[0016] This invention provides a method for crystallizing β-alanine, comprising the following steps: (1) passing the β-alanine mother liquor sequentially through a cation exchange resin and an anion exchange resin to obtain a β-alanine feed solution; (2) sequentially filtering, concentrating, crystallizing, and drying the β-alanine feed solution to obtain β-alanine crystals. The raw materials for this invention are widely available, inexpensive, and readily available. The β-alanine mother liquor is adsorbed by a cation exchange resin to remove ammonium ions from the system, and then passed through an anion exchange resin to remove iminodipropionic acid. The ammonium sulfate and sodium iminodipropionate obtained from the regeneration of the ion exchange resin are used; the ammonium sulfate can be used as a fertilizer, and the sodium iminodipropionate can be used as a chemical intermediate. After purification, β-alanine crystal powder is obtained by crystallization using a solvent. The advantages of this invention are high crystallization yield, simple process, convenient operation, and high-quality finished product. Detailed Implementation
[0017] This invention provides a method for crystallizing β-alanine, comprising the following steps: (1) Pass the β-alanine mother liquor through a cation exchange resin and an anion exchange resin in sequence to obtain a β-alanine feed solution; (2) The β-alanine solution is filtered, concentrated, crystallized and dried in sequence to obtain β-alanine crystals.
[0018] In this invention, the cationic resin in step (1) is a hydrogen-form resin.
[0019] In this invention, the volume ratio of β-alanine mother liquor to cation exchange resin is preferably 10-20:1-3. More preferably, it is 12-18:1.5-2.5, and even more preferably, it is 14-16:1.8-2.2.
[0020] In this invention, the cation exchange resin can adsorb ammonium ions, thereby effectively removing ammonium salts. The cation exchange resin can be regenerated using hydrochloric acid and / or sulfuric acid.
[0021] In this invention, the anion exchange resin in step (1) is a hydrogen-oxygen type resin.
[0022] In this invention, the volume ratio of β-alanine mother liquor to anion exchange resin is preferably 10~20:2.5~3.5, more preferably 12~18:2.6~3.4, and even more preferably 14~16:2.8~3.2.
[0023] In this invention, the anion exchange resin can remove iminodipropionic acid, and the reagent used for regenerating the anion exchange resin is sodium hydroxide and / or ammonia.
[0024] In this invention, the cationic resin is ZGC650L, purchased from Ningbo Zhengguang Resin Co., Ltd.; the anionic resin is 335 weakly basic anionic resin.
[0025] In this invention, the flow rate of the cation exchange resin in step (1) is preferably 200~400mL / h, more preferably 250~350mL / h, and even more preferably 280~340mL / h.
[0026] In this invention, the flow rate of the anion exchange resin is preferably 200-400 mL / h, more preferably 250-350 mL / h, and even more preferably 280-340 mL / h.
[0027] In this invention, the pore size of the filter membrane used in step (2) is preferably 0.4~0.5μm, more preferably 0.42~0.48μm, and even more preferably 0.44~0.46μm; the filter membrane is a fiber resin water-based membrane, which is commercially available.
[0028] In this invention, the concentration temperature in step (2) is preferably 50~80℃, more preferably 55~75℃, and even more preferably 60~70℃; the mass concentration of β-alanine in the concentrate is preferably 50~65%, more preferably 55~60%, and even more preferably 57~58%.
[0029] In this invention, the reagent used for crystallization in step (2) is one or more of acetone, methanol, ethanol and isopropanol.
[0030] In this invention, the preferred ratio of β-alanine to crystallization reagent in the concentrate is 1g:1~5mL, more preferably 1g:2~4mL, and even more preferably 1g:2.5~3mL.
[0031] In this invention, the crystallization temperature in step (3) is preferably 5~15℃, more preferably 6~14℃, and even more preferably 8~12℃; the time is preferably ≥1h, more preferably ≥1.5h, and even more preferably ≥2h; stirring is maintained during the crystallization process.
[0032] In this invention, after crystallization in step (3), the solid is obtained by filtration and then washed with methanol.
[0033] In this invention, the drying temperature in step (3) is preferably 60~80℃, more preferably 65~75℃, and even more preferably 68~72℃; the vacuum degree is preferably -0.08~-0.1MPa, more preferably -0.085~-0.095MPa, and even more preferably -0.088~-0.092MPa.
[0034] The technical solutions provided by the present invention will be described in detail below with reference to the embodiments, but they should not be construed as limiting the scope of protection of the present invention.
[0035] Example 1
[0036] 1400 ml of β-alanine mother liquor was taken, and the ammonia content was found to be 2.78 g / L. The solution was passed through 200 ml of hydrogen-form resin, and 1450 mL of the column runoff was collected. The iminodiapropionic acid content was found to be 14.23 g / L. The solution was then passed through 270 mL of hydroxyl-form resin. The flow rate of the solution was 300 ml / h for both resins. The concentration of β-alanine in the anion exchange resin runoff was 342.5 g / L. The volume was 1460 mL. The solution was filtered through a 0.45 μm microporous membrane and concentrated at 65 °C to a β-alanine concentration of 60%. Methanol was added to the β-alanine solution at a ratio of 1 g: 2 mL of β-alanine to crystallization reagent. After the methanol was added, the temperature was lowered to 5 °C, and the solution was stirred for 1 h. The crystals were separated by filtration and washed with 0.5 times the volume of methanol. The crystalline material was dried at 75℃ under a vacuum of -0.095 MPa, yielding 470.05 g of β-alanine crystals. Analysis showed a product content of 99.55%, a moisture content of 0.15 wt%, and a yield of 93.57%. The yield of β-alanine was calculated as (mass of β-alanine crystals × β-alanine crystal content) / mass of β-alanine in the anion column flow solution × 100%.
[0037] Example 2
[0038] 1400 ml of β-alanine mother liquor was taken, and the ammonia content was found to be 3.16 g / L. The solution was passed through 200 ml of hydrogen-form resin, and 1420 mL of the column runoff was collected. The iminodipropionic acid content was found to be 16.64 g / L. The solution was then passed through 270 mL of hydroxyl-form resin. The flow rate of the solution was 300 ml / h for both resins. The concentration of β-alanine in the anion exchange resin runoff was 369.76 g / L. The volume was 1400 mL. The solution was filtered through a 0.45 μm microporous membrane and concentrated at 65 °C to a β-alanine concentration of 60%. Methanol was added to the β-alanine solution at a ratio of 1 g: 2 mL of β-alanine to crystallization reagent. After the methanol was added, the temperature was lowered to 5 °C, and the solution was stirred for 1 h. The crystals were separated by filtration and washed with 0.5 times the volume of methanol. The crystalline material was dried at 75℃ under a vacuum of -0.095 MPa, yielding 487.13 g of β-alanine crystals. Analysis showed a product purity of 99.35%, a moisture content of 0.10 wt%, and a yield of 93.49%.
[0039] Example 3
[0040] 1400 ml of β-alanine mother liquor was taken, and the ammonia content was found to be 2.98 g / L. The solution was passed through 200 ml of hydrogen-form resin, and 1430 mL of the column liquid was collected. The iminodipropionic acid content was found to be 14.23 g / L. The solution was then passed through 270 mL of hydroxyl-form resin. The flow rate of the solution was 300 ml / h for both resins. The concentration of β-alanine in the anion exchange resin was 348.96 g / L. The volume was 1440 mL. The solution was filtered through a 0.45 μm microporous membrane and concentrated at 65 °C to a β-alanine concentration of 60%. Methanol was added to the β-alanine solution at a ratio of 1 g: 2 mL of β-alanine to crystallization reagent. After the methanol was added, the temperature was lowered to 5 °C, and the solution was stirred for 1 h. The crystals were separated by filtration and washed with 0.5 times the volume of methanol. The crystalline material was dried at 75℃ under a vacuum of -0.095 MPa, yielding 476.32 g of β-alanine crystals. Analysis showed a product purity of 99.7%, a moisture content of 0.13 wt%, and a yield of 94.5%.
[0041] The above description is only a preferred embodiment of the present invention. It should be noted that those skilled in the art can make several improvements and modifications without departing from the principle of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.
Claims
1. A method for crystallizing β-alanine, characterized in that, Includes the following steps: (1) Pass the β-alanine mother liquor through a cation exchange resin and an anion exchange resin in sequence to obtain a β-alanine feed solution; (2) The β-alanine solution is filtered, concentrated, crystallized and dried in sequence to obtain β-alanine crystals.
2. The crystallization method of β-alanine as described in claim 1, characterized in that, In step (1), the cation exchange resin is a hydrogen-form resin; The volume ratio of β-alanine mother liquor to cation exchange resin is 10~20:1~3.
3. The crystallization method of β-alanine as described in claim 2, characterized in that, In step (1), the anion exchange resin is a hydroxide-type resin; The volume ratio of β-alanine mother liquor to anion exchange resin is 10~20:2.5~3.
5.
4. The crystallization method of β-alanine as described in claim 3, characterized in that, In step (1), the flow rate of the feed solution through the cation exchange resin is 200~400mL / h; The flow rate of the feed solution through the anion exchange resin is 200~400mL / h.
5. The crystallization method of β-alanine as described in claim 4, characterized in that, The pore size of the filter membrane used in step (2) is 0.4~0.5μm.
6. The crystallization method of β-alanine as described in claim 5, characterized in that, In step (2), the concentration temperature is 50~80℃, and the mass concentration of β-alanine in the concentrate is 50~65%.
7. The crystallization method of β-alanine as described in claim 6, characterized in that, The reagent used for crystallization in step (2) is one or more of acetone, methanol, ethanol and isopropanol.
8. The crystallization method of β-alanine as described in claim 7, characterized in that, The ratio of β-alanine to crystallization reagent in the concentrated solution is 1g:1~5mL.
9. The crystallization method of β-alanine as described in claim 8, characterized in that, In step (3), the crystallization temperature is 5~15℃ and the time is ≥1h.
10. The crystallization method of β-alanine as described in claim 9, characterized in that, The drying temperature in step (3) is 60~80℃ and the vacuum degree is -0.08~-0.1MPa.