CN109369434B - Crystal washing treatment process of ornithine - Google Patents
Crystal washing treatment process of ornithine Download PDFInfo
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- CN109369434B CN109369434B CN201811553829.9A CN201811553829A CN109369434B CN 109369434 B CN109369434 B CN 109369434B CN 201811553829 A CN201811553829 A CN 201811553829A CN 109369434 B CN109369434 B CN 109369434B
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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
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A crystal washing treatment process of ornithine belongs to the technical field of product refining. The method is characterized in that: placing the crude product or the unqualified product in a crystal washing tank, adding an ethanol water solution with the mass concentration of 75-90% which is 0.8-1.2 times of the mass of the crude product or the unqualified product, stirring and washing crystals at the washing temperature of 5-15 ℃, stirring for 20-80 min, then carrying out solid-liquid separation, and drying the solid obtained by solid-liquid separation to obtain the crystal washing agent. The invention adopts ethanol with certain concentration as the washing liquid to wash and wash the crystal of the unqualified product, and washes away impurities around the crystal, the selected washing liquid can quickly remove the impurities without dissolving excessive ornithine, and simultaneously the product and the washing liquid are easy to separate and recycle, thereby achieving the purposes of improving the product quality and improving the yield and reducing the cost.
Description
Technical Field
A crystal washing treatment process of ornithine belongs to the technical field of product refining.
Background
Ornithine of formula H2NCH2CH2CH2CH(NH2) COOH, a basic amino acid. Although not found in common proteins (not belonging to 20 amino acids constituting proteins), delta-N-acetylornithine is found in antibacterial peptides such as tyrocidin and gramicidin S, and in corydalis atrophica root. Is produced by decomposing arginine as base or arginase. In organisms, ornithine mainly participates in uric acid circulation and plays an important role in discharging ammonia nitrogen in the bodies. Ornithine is used medicinally in addition to being an agent and an injection, often together with arginine, in the preparation of a foaming beverage for fatigue recovery. In recent years, ornithine has been used in the food industry and pharmaceutical industry increasingly.
The existing process adopts a recrystallization mode generally for unqualified product quality, the recrystallization mode and yield are generally about 80%, the yield is low, and the production cost can be increased by adopting the process.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcomes the defects of the prior art, and provides a simple and quick crystal washing treatment process of ornithine with high recovery rate.
The technical scheme adopted by the invention for solving the technical problems is as follows: the crystal washing treatment process of ornithine is characterized by comprising the following steps: placing the crude product or the unqualified product into a crystal washing tank, then adding an ethanol water solution with the mass concentration of 75-90% which is 0.8-1.2 times of the mass of the crude product or the unqualified product, stirring and washing crystals at the washing temperature of 5-15 ℃, stirring for 20-80 min, then carrying out solid-liquid separation, and drying the solid obtained by the solid-liquid separation.
The invention has the advantages of simple operation, reasonable and convenient process, and can improve the product quality and yield as much as possible and reduce the production cost. The invention adopts ethanol with certain concentration as the washing liquid to wash and wash the crystal of the unqualified product, and washes away impurities around the crystal, the selected washing liquid can quickly remove the impurities without dissolving excessive ornithine, and simultaneously the product and the washing liquid are easy to separate and recycle, thereby achieving the purposes of improving the product quality and improving the yield and reducing the cost.
Preferably, the adding amount of the ethanol water solution is 0.95-1.05 times of the quality of the crude product or the unqualified product. Preferably, the amount used to remove the impurities is more thorough.
Preferably, the mass concentration of the ethanol water solution is 79-85%. The impurities are separated more rapidly at the preferred mass concentrations.
Preferably, the washing temperature is 8-10 ℃. The impurities are separated more quickly and removed more thoroughly at the preferred washing temperature.
Preferably, the stirring time is 20 min-25 min. The crystal washing time can be shortened under the optimal conditions.
The combination of preferred washing conditions can simultaneously improve the quality and yield of the product.
Preferably, the solid-liquid separation is performed by centrifugal separation.
Preferably, the solid after solid-liquid separation is dried after repeating the stirring crystal washing process at least twice. The quality of the product is better after repeated washing.
Preferably, after the liquid separated by the solid-liquid separation is distilled and refined to obtain ethanol, the mass concentration is adjusted to 75-90% and then the ethanol is reused.
Compared with the prior art, the invention has the beneficial effects that: the ethanol with a certain concentration is used as a washing liquid to wash (wash crystal) unqualified products, so that loss caused by recrystallization of dissolved unqualified products is avoided, and the product quality is improved by washing (washing crystal) impurities around the crystal. The operation is simpler and faster, and the recovery rate reaches more than 95%.
Detailed Description
The invention is further illustrated by the following specific examples, of which example 1 is the best mode of practice.
Example 1
Placing the unqualified product in a crystal washing tank, adding an ethanol aqueous solution with the mass concentration of 82% of that of the crude product or the unqualified product being 1 time of that of the crude product or the unqualified product, stirring and washing crystals at the washing temperature of 9 ℃, stirring for 20min, performing solid-liquid separation in a centrifugal separation mode, distilling the liquid obtained by the solid-liquid separation to obtain ethanol, adjusting the mass concentration, reusing the liquid obtained by the solid-liquid separation, and drying the solid obtained by the solid-liquid separation after repeating the stirring and crystal washing process at least twice.
Example 2
Placing the unqualified product in a crystal washing tank, adding ethanol water solution with the mass concentration of 85% and the stirring time of 1.05 times of the mass of the crude product or the unqualified product, washing the crystal at the washing temperature of 8 ℃, stirring for 22min, performing solid-liquid separation in a centrifugal separation mode, distilling the liquid obtained after the solid-liquid separation to obtain ethanol, adjusting the mass concentration, reusing, and drying the solid obtained after the solid-liquid separation after repeating the stirring crystal washing process at least twice.
Example 3
Placing the unqualified product in a crystal washing tank, adding an ethanol water solution with the mass concentration of 79% and the stirring time of 25min, wherein the mass concentration of the ethanol water solution is 0.95 times of that of the crude product or the unqualified product, stirring and washing the crystal at the washing temperature of 10 ℃, then performing solid-liquid separation in a centrifugal separation mode, distilling the liquid obtained by the solid-liquid separation to obtain ethanol, adjusting the mass concentration, then repeatedly using the ethanol, and drying the solid obtained by the solid-liquid separation after repeating the stirring and crystal washing process at least twice.
Example 4
Placing the unqualified product in a crystal washing tank, adding ethanol water solution with the mass concentration of 75% and the quality of the crude product or the unqualified product being 0.8 times of the quality of the crude product or the unqualified product, stirring and washing the crystal at the washing temperature of 15 ℃, stirring for 65 min, then performing solid-liquid separation in a centrifugal separation mode, distilling the liquid obtained after the solid-liquid separation to refine the ethanol, adjusting the mass concentration, then reusing the liquid obtained after the solid-liquid separation, and drying the solid obtained after the solid-liquid separation is repeated for at least two times by the stirring and crystal washing process to obtain the crystal.
Example 5
Placing the unqualified product in a crystal washing tank, adding ethanol water solution with the mass concentration of 90% and the quality of 1.2 times of that of the crude product or the unqualified product, stirring and washing the crystal at the washing temperature of 5 ℃, stirring for 80min, performing solid-liquid separation in a centrifugal separation mode, distilling the liquid obtained after the solid-liquid separation to obtain ethanol, adjusting the mass concentration, reusing the liquid obtained after the solid-liquid separation, repeating the stirring and crystal washing process at least twice, and drying to obtain the crystal washing liquid.
Comparative example 1
The basic process was the same as in example 1, except that the aqueous ethanol solution used had a mass concentration of 50%.
Comparative example 2
The basic procedure is as in example 1, except that anhydrous ethanol is used instead of the aqueous ethanol solution.
Comparative example 3
The basic procedure is as in example 1, except that the washing temperature is 25 ℃.
The detection method of the products obtained in the examples and the comparative examples comprises the following steps: a detection instrument: 721 visible spectrophotometer
Table 1 results of performance testing
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (5)
1. A crystal washing treatment process of ornithine is characterized by comprising the following steps: placing the crude product or the unqualified product into a crystal washing tank, adding an ethanol water solution with the mass concentration of 79-85% which is 0.95-1.05 times of the mass of the crude product or the unqualified product, stirring and washing crystals at the washing temperature of 8-10 ℃ for 20-80 min, then carrying out solid-liquid separation, and drying the solid obtained by the solid-liquid separation.
2. The crystal washing treatment process of ornithine according to claim 1, wherein: the stirring time is 20-25 min.
3. The crystal washing treatment process of ornithine according to claim 1, wherein: the solid-liquid separation adopts a centrifugal separation mode.
4. The crystal washing treatment process of ornithine according to claim 1, wherein: and the solid after solid-liquid separation is dried after repeating the stirring and crystal washing process at least twice.
5. The crystal washing treatment process of ornithine according to claim 1 or 4, wherein: and distilling the liquid separated by the solid-liquid separation to refine ethanol, and adjusting the mass concentration to 75-90% for reuse.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811553829.9A CN109369434B (en) | 2018-12-18 | 2018-12-18 | Crystal washing treatment process of ornithine |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811553829.9A CN109369434B (en) | 2018-12-18 | 2018-12-18 | Crystal washing treatment process of ornithine |
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| CN109369434A CN109369434A (en) | 2019-02-22 |
| CN109369434B true CN109369434B (en) | 2021-08-24 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090082594A1 (en) * | 2004-11-15 | 2009-03-26 | Kyowa Hakko Kogyo Co., Ltd. | Crystals of l-ornithine and process for producing the same |
| CN102041282A (en) * | 2009-10-14 | 2011-05-04 | 新沂市汉菱生物工程有限公司 | Method for preparing L-ornithine by utilizing enzyme method |
| CN102191291A (en) * | 2011-04-25 | 2011-09-21 | 武汉远大弘元股份有限公司 | Method for producing L-ornithine hydrochloride by genetic engineering bacteria |
| CN107325016A (en) * | 2017-08-20 | 2017-11-07 | 合肥信达膜科技有限公司 | A kind of high-quality ornithine extracting method |
| CN107916282A (en) * | 2017-12-13 | 2018-04-17 | 湖北新生源生物工程有限公司 | A kind of method that bioanalysis prepares L citrulling and L ornithines |
-
2018
- 2018-12-18 CN CN201811553829.9A patent/CN109369434B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090082594A1 (en) * | 2004-11-15 | 2009-03-26 | Kyowa Hakko Kogyo Co., Ltd. | Crystals of l-ornithine and process for producing the same |
| CN102041282A (en) * | 2009-10-14 | 2011-05-04 | 新沂市汉菱生物工程有限公司 | Method for preparing L-ornithine by utilizing enzyme method |
| CN102191291A (en) * | 2011-04-25 | 2011-09-21 | 武汉远大弘元股份有限公司 | Method for producing L-ornithine hydrochloride by genetic engineering bacteria |
| CN107325016A (en) * | 2017-08-20 | 2017-11-07 | 合肥信达膜科技有限公司 | A kind of high-quality ornithine extracting method |
| CN107916282A (en) * | 2017-12-13 | 2018-04-17 | 湖北新生源生物工程有限公司 | A kind of method that bioanalysis prepares L citrulling and L ornithines |
Non-Patent Citations (2)
| Title |
|---|
| L-鸟氨酸的制备及应用;万红贵 等;《生物加工过程》;20080131;第6卷(第1期);第12-15页 * |
| L-鸟氨酸的化学合成方法;郝永兵 等;《氨基酸和生物资源》;20071231;第29卷(第3期);第54-56页 * |
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| CN109369434A (en) | 2019-02-22 |
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Denomination of invention: A crystal washing process for ornithine Effective date of registration: 20220601 Granted publication date: 20210824 Pledgee: Zibo Branch of Bank of Communications Co.,Ltd. Pledgor: SHANDONG JINYANG PHARMACEUTICAL Co.,Ltd. Registration number: Y2022980006929 |
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Date of cancellation: 20230529 Granted publication date: 20210824 Pledgee: Zibo Branch of Bank of Communications Co.,Ltd. Pledgor: SHANDONG JINYANG PHARMACEUTICAL Co.,Ltd. Registration number: Y2022980006929 |
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| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: A crystal washing treatment process for ornithine Effective date of registration: 20230530 Granted publication date: 20210824 Pledgee: Zibo Branch of Bank of Communications Co.,Ltd. Pledgor: SHANDONG JINYANG PHARMACEUTICAL Co.,Ltd. Registration number: Y2023980042228 |