CN102584613B - Crystallization method for L-serine in stable crystal form - Google Patents
Crystallization method for L-serine in stable crystal form Download PDFInfo
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- CN102584613B CN102584613B CN201110455353.7A CN201110455353A CN102584613B CN 102584613 B CN102584613 B CN 102584613B CN 201110455353 A CN201110455353 A CN 201110455353A CN 102584613 B CN102584613 B CN 102584613B
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Abstract
The invention discloses a crystallization method for L-serine in a stable crystal form. The method comprises the following steps of: 1) dissolving, namely weighing L-serine powder, adding water and heating to 90 to 95 DEG C to dissolve, decolorizing by using activated carbon, filtering and colleting filtrate; 2) crystallizing and centrifuging, namely pumping the filtrate into a crystallization kettle, when cooling to 55 to 60 DEG C and generating fine crystals, and dripping ethanol in an amount which is 40 to 50 based on the volume of the filtrate; stirring at speed of 150 to 300 revolutions/minute, after the temperature of a solution is reduced to 12 to 15 DEG C, stopping stirring, standing at the temperature of between 12 and 15 DEG C, ageing and crystallizing for 4 to 5 hours, and filtering and spin-drying to obtain a crystal, namely a L-serine wet product; and 3) drying and packaging. The L-serine in the stable crystal form has the advantages of stable form and stable quality, and hardly absorbs moisture to be deteriorated at normal temperature.
Description
Technical field
The present invention relates to Serine synthetic method technical field, be specifically related to a kind of crystallization method of Serine stable crystal form.
Background technology
Serine is a kind of in the 20 common seed amino acids of constitutive protein matter, is mammiferous non-essential amino acid, is also ketogenic amino acid.It is bringing into play and is acting in fat and the metabolism of lipid acid and the growth of muscle, because it contributes to the generation of immunoglobulin and antibody, maintaining healthy immunity system also needs Serine.Serine is all being brought into play and is being acted in the sheath of manufacture processing, muscle tissue and the encirclement neurocyte of cytolemma synthetic, and its purposes is roughly divided into following several:
1, medical material: Serine is widely used in configuration third generation Hausmam Amin 20 and accessory substance, and for the synthesis of multiple silk amino acid derivative, if cardiovascular, anticancer, AIDS new drug and genetically engineered are with protected amino acid etc.;
2, food: Serine is for sports beverages, amino acid weight-reducing drinks etc.;
3, feed: Serine, for animal-feed, can promote animal growth.
But at present, Serine on the market exists mainly with pulverous form, and this pulverous Serine is extremely unstable under normal conditions, thereby the moisture being easy in absorbed air degenerates the quality of product, and quality stability is poor.
Summary of the invention
The above-mentioned deficiency that the present invention is directed to prior art, provides a kind of form stable, is difficult under normal conditions the moisture absorption, rotten, the crystallization method of stay-in-grade Serine stable crystal form.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: a kind of crystallization method of Serine stable crystal form, and the crystallisation step of the method comprises:
(1) dissolve
Taking Powdered Serine is Serine crude product, adds purified water (deionized water), is then heated to 90～95 ℃ and makes it to dissolve, in solution after dissolving, add gac to decolour, the add-on of gac is 2～5% of Serine crude product weight, then filters, and collects filtrate;
(2) crystallization, centrifugal
Filtrate is pumped into crystallization kettle, be cooled to 55～60 ℃ while having tiny crystallization, drip ethanol, amount of alcohol added is filtrate volume 40～50%; Then stir, controlling stirring velocity is 150～300 revs/min, after solution temperature is down to 12～15 ℃, stops stirring, and then standing at 12～15 ℃ is aging crystallization 4～5 hours, then filters, dries that to obtain xln be the wet product of Serine;
(3) dry, packing
The wet product of Serine after step (2) is dried, packs spray-drier into, and dry 2～3 hours, discharging, cooling, sub-sieve, packing.
As preferably, it is 95 ℃ that the described solvent temperature of step (1) is controlled, and maintains the solvent Serine crude product that this temperature can be quick and complete.
As preferably, the described ethanol of step (2) is the ethanol of volumetric concentration 65%～80%.
Advantage of the present invention and beneficial effect:
1. to adopt commercially available Powdered Serine be raw material in the present invention, after simple processes, can obtain form stable, be difficult for the moisture absorption, rotten, the Serine that stay-in-grade crystal habit exists under normal conditions.The transmittance of the Serine that this crystal habit exists can reach 99.0%, and crystal habit is good.
2. to take commercially available Powdered Serine be raw material in the present invention, sufficient raw, and preparation technology is simple, easily operation, product yield is high; Add ethanol as precipitation agent and play the stabilization to product, by changing crystallization mode, obtaining many ribs type xln, thereby strengthened the stability of product.
Embodiment
Below by specific embodiment, the present invention is described in further detail, but the present invention is not only confined to following examples, any modification within the scope of the claims in the present invention, all thinks and falls within the scope of protection of the present invention.
Embodiment 1
(1) dissolve
Taking commercially available Powdered Serine is Serine crude product 100g, adds purified water (deionized water) 220ml, is then heated to 95 ℃ and makes it to dissolve, and adds 2 grams of stirrings of gac to decolour in the solution after dissolving,, then filter, collect filtrate;
(2) crystallization, centrifugal
Filtrate is pumped into crystallization kettle, be cooled to 60 ℃ while having tiny crystallization, the ethanol 100ml that dropping volumetric concentration is 70%, then stir, control stirring velocity is 200 revs/min and stops stirring after solution temperature is down to 15 ℃, then standing at 15 ℃ is aging crystallization 5 hours, then filters, dries that to obtain xln be the wet product of Serine;
(3) dry, packing
The wet product of Serine after step (2) is dried, packs in spray-drier, dry 3 hours of 70～80 ℃ of sprayings, and discharging, cooling, sub-sieve, packing.
Weigh 92.0 grams of target products, yield is 92.0%.
Adopt industry ordinary method to detect resulting lenticular Serine, its transmittance is 99.0%.
Embodiment 2
(1) dissolve
Taking commercially available Powdered Serine is Serine crude product 100g, adds purified water (deionized water) 240ml, is then heated to 90 ℃ and makes it to dissolve, and adds 4 grams of stirrings of gac to decolour in the solution after dissolving,, then filter, collect filtrate;
(2) crystallization, centrifugal
Filtrate is pumped into crystallization kettle, be cooled to 58 ℃ while having tiny crystallization, drip ethanol 120ml, then stir, control stirring velocity is 260 revs/min and stops stirring after solution temperature is down to 15 ℃, then standing at 15 ℃ is aging crystallization 5 hours, then filters, dries that to obtain xln be the wet product of Serine;
(3) dry, packing
The wet product of Serine after step (2) is dried, packs in spray-drier, and 70～80 ℃ of sprayings are dried 3 hours, and discharging is cooling, sub-sieve, packing.
Weigh 90.1 grams of target products, yield is 90.1%.
Adopt industry ordinary method to detect resulting lenticular Serine, its transmittance is 98.9%.
Embodiment 3
(1) dissolve
Taking commercially available Powdered Serine is Serine crude product 100g, adds purified water (deionized water) 240ml, is then heated to 90 ℃ and makes it to dissolve, and adds 4 grams of stirrings of gac to decolour in the solution after dissolving,, then filter, collect filtrate;
(2) crystallization, centrifugal
Filtrate is pumped into crystallization kettle, be cooled to 58 ℃ while having tiny crystallization, drip ethanol 120ml, then stir, control stirring velocity is 260 revs/min and stops stirring after solution temperature is down to 15 ℃, then standing at 15 ℃ is aging crystallization 5 hours, then filters, dries that to obtain xln be the wet product of Serine;
(3) dry, packing
The wet product of Serine after step (2) is dried, packs in spray-drier, and 70～80 ℃ of sprayings are dried 3 hours, and discharging is cooling, sub-sieve, packing.
The target product of weighing is 89.8 grams, and yield is 89.8%.
Adopt industry ordinary method to detect resulting lenticular Serine, its transmittance is 99.0%.
Claims (2)
1. a crystallization method for Serine stable crystal form, is characterized in that: the crystallisation step of the method comprises:
(1) dissolve: taking Powdered Serine is Serine crude product, adds purified water, be then heated to 90 ~ 95 ℃ and make it to dissolve, in solution after dissolving, add gac to decolour, the add-on of gac is 2 ~ 5% of Serine crude product weight, then filters, and collects filtrate;
(2) crystallization, centrifugal: filtrate is pumped into crystallization kettle, be cooled to 55 ~ 60 ℃ while having tiny crystallization, drip the ethanol of volumetric concentration 65%～80%, the amount of alcohol added of volumetric concentration 65%～80% is filtrate volume 40 ~ 50%; Then stir, controlling stirring velocity is 150 ~ 300 revs/min, after solution temperature is down to 12 ~ 15 ℃, stops stirring, and then standing at 12 ~ 15 ℃ is aging crystallization 4 ~ 5 hours, then filters, dries that to obtain xln be the wet product of Serine;
(3) dry, packing: the wet product of Serine after step (2) is dried, pack spray-drier into, dry 2 ~ 3 hours, discharging, cooling, sub-sieve, packing.
2. the crystallization method of Serine stable crystal form according to claim 1, is characterized in that: it is 95 ℃ that the solvent temperature of step (1) is controlled.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110455353.7A CN102584613B (en) | 2011-12-30 | 2011-12-30 | Crystallization method for L-serine in stable crystal form |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110455353.7A CN102584613B (en) | 2011-12-30 | 2011-12-30 | Crystallization method for L-serine in stable crystal form |
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| CN102584613A CN102584613A (en) | 2012-07-18 |
| CN102584613B true CN102584613B (en) | 2014-04-02 |
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| CN108707084A (en) * | 2018-07-02 | 2018-10-26 | 无锡晶海氨基酸股份有限公司 | A kind of preparation method of pharmaceutical grade Serine |
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| CN100491337C (en) * | 2006-07-17 | 2009-05-27 | 安徽省恒锐新技术开发有限责任公司 | Method for preparing levo-serine and dextro serine by induced crystallizing method |
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