CN103739507A - Preparation method of beta-crystal-form lysine hydrochloride - Google Patents
Preparation method of beta-crystal-form lysine hydrochloride Download PDFInfo
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- CN103739507A CN103739507A CN201310465242.3A CN201310465242A CN103739507A CN 103739507 A CN103739507 A CN 103739507A CN 201310465242 A CN201310465242 A CN 201310465242A CN 103739507 A CN103739507 A CN 103739507A
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Abstract
The invention discloses a preparation method of a beta-crystal-form lysine hydrochloride. The preparation method comprises the steps: under a condition that a ratio of a feed-grade lysine hydrochloride to purified water is 1:0.4-0.6, heating to 80-90 DEG C to dissolve, adding 1%-3% of activated carbon for decolorization, filtering, then carrying out direct cooling crystallization of the solution, centrifuging, firstly drying the product by using a boiling bed until the moisture content is 2-4%, then blowing saturated steam into a hopper of the boiling bed for 30-50 minutes, followed by drying the product, and thus obtaining the beta-crystal-form lysine hydrochloride having high product purity and having the quality according with national pharmacopoeia requirements. The preparation method abandons defects of high energy consumption and destruction of high temperature concentration to the amino acid quality in a traditional concentration crystallization method, and ensures the purity of the product; and at the same time, by adopting the boiling bed to be externally added with the saturated steam for combination drying, an alpha-crystal-form or alpha-beta mixed crystal form lysine hydrochloride is effectively allowed to be converted into the beta-crystal-form high-purity product.
Description
Technical field
The invention belongs to compound preparation field, particularly, relate to a kind of lysine hydrochloride preparation method of highly purified beta crystal.
Background technology
Methionin is that human body can not self synthetic but one of eight seed amino acid of extremely needing, be called as the necessary propylhomoserin of human body first, Methionin is increased to the utilization ratio that can improve protein in food, thereby the nutrition of nutrient fortified food greatly, enhancing development, whet the appetite, reduce disease, the effect such as build up health, particularly the childhood development phase, after being ill decubation, gestation institute's lactation essential.
Existing lysine hydrochloride manufacture method mostly is the rear condensing crystal of decolouring, and concentrated rear product is destroyed by high temperature, and product exists transmittance low more, and content is lower, and other heteroacid are many etc., consume energy high simultaneously; Traditional technology is product utilization ebullated bed or vacuum drying oven oven dry after crystallization, and after drying, product is the crystallization of α type, and the β type of the infared spectrum of product and standard-required has very big-difference.People are more and more higher to the requirement of lysine hydrochloride quality product in recent years, and particularly American-European countries is higher to the specification of quality of product.Therefore, we improve the refining drying production process of existing lysine hydrochloride, on the basis reducing costs, have improved the quality of product.
Summary of the invention
The object of this invention is to provide a kind of preparation method of beta crystal lysine hydrochloride.
For achieving the above object, technical scheme of the present invention provides a kind of preparation method of high purity hydrochloric acid Methionin of beta crystal, uses feed grade lysine hydrochloride to mix with purified water, heating for dissolving, then add activated carbon decolorizing, solution crystallisation by cooling after filtering; Centrifugal, centrifugal rear product is dried with ebullated bed, then blast saturation steam in ebullated bed hopper, then product is dried, obtain the lysine hydrochloride of beta crystal.
Preparation method of the present invention, the mass ratio that feeds intake of wherein said feed grade lysine hydrochloride and purified water is 1:0.4～1:0.6.Be preferably 1:0.5.
Preparation method of the present invention, heating for dissolving temperature is 80～90 ℃.Be preferably 85 ℃.
Preparation method of the present invention, activated carbon dosage is 1%～3% of feed grade lysine hydrochloride quality.Be preferably 2%.
Preparation method of the present invention, the direct crystallisation by cooling of solution after filtering.Cooling temperature is 20～30 ℃.
In preparation method of the present invention, centrifugal condition is 800～1000r/min, and centrifugation time is 10～20min.
Wherein, centrifugal rear product is first dried to 2～4% with ebullated bed by moisture content.Be preferably 3%.
Preparation method of the present invention blasts saturated steam 30～50min in ebullated bed.
Preferably, in ebullated bed, blast saturated steam 40min.
The invention provides the beta crystal lysine hydrochloride product that aforesaid method prepares.
The present invention is innovated on the basis of traditional technology, searched out a kind of preparation method of beta crystal high purity hydrochloric acid Methionin of simple possible, emphasis is that the parameters such as direct bleaching crystallization, product oven dry are optimized, present method yield can reach 95%, compared with traditional method, improved 20%, reduced production cost; Adopt direct bleaching crystallization to abandon the concentrated destruction to amino acid quality of high temperature in condensing crystal process, improved quality product, and overcome the high defect of power consumption in condensing crystal process, reduced energy consumption; Adopted the additional saturation steam of ebullated bed to combine oven dry simultaneously, can form β monocrystalline type high-purity hydrochloric acid lysine product, effectively make the lysine hydrochloride of alpha-crystal form or α β mixing crystal formation be converted into beta crystal product, superior, quality product meets Chinese Pharmacopoeia requirement.
Accompanying drawing explanation
Fig. 1 is standard infrared absorption pattern (beta crystal).
Fig. 2 is sample 1 infrared absorption pattern.
Fig. 3 is sample 2 infrared absorption patterns.
Fig. 4 is sample 3 infrared absorption patterns.
Fig. 5 is sample 4 infrared absorption patterns.
Fig. 6 is sample 5 infrared absorption patterns.
Fig. 7 is the XRD figure (alpha-crystal form) of sample 4.
Fig. 8 is the XRD figure (beta crystal) of sample 5.
Embodiment
Below in conjunction with embodiment, the specific embodiment of the present invention is described in further detail.Following examples are used for illustrating the present invention, but are not used for limiting the scope of the invention.
The preparation method of the lysine hydrochloride of embodiment 1 beta crystal
(1) 1.0 tons of feed grade lysine hydrochlorides are added in dissolution kettle, then add 0.6 ton of purified water, 80 ℃ of heating for dissolving, add 30 kilograms of gacs;
(2) above-mentioned solution is filtered hot in crystallization kettle to 20 ℃ of crystallisation by cooling.
(3) the centrifugal 10min of 900r/min is dried to moisture content 2% by the product after centrifugal in ebullated bed;
(4) in the hopper of ebullated bed, directly blast steam 50min;
(5) close the steam blasting, with hot blast by drying materials.
Gained lysine hydrochloride (sample 1) meets Chinese Pharmacopoeia standard regulation, and wherein product transmittance is 99.5%, and content is 99.7%, and the standard diagram of infrared absorption pattern and beta crystal product is in full accord.As shown in accompanying drawing 1,2.
The preparation method of the lysine hydrochloride of embodiment 2 beta crystals
(1) 1.0 tons of feed grade lysine hydrochlorides are added in dissolution kettle, then add 0.5 ton of purified water, 85 ℃ of heating for dissolving, add 20 kilograms of gacs;
(2) take advantage of heat filtering to crystallization kettle above-mentioned solution, 25 ℃ of crystallisation by cooling.
(3) the centrifugal 20min of 800r/min is dried to moisture content 3% by the product after centrifugal in ebullated bed;
(4) in the hopper of ebullated bed, directly blast steam 40min;
(5) close the steam blasting, with hot blast by drying materials.
Gained lysine hydrochloride (sample 2) meets Chinese Pharmacopoeia standard regulation, and wherein product transmittance is 99.4%, and content is 99.8%, and the standard diagram of infrared absorption pattern and beta crystal product is in full accord.As shown in Figure 3.
The preparation method of the lysine hydrochloride of embodiment 3 beta crystals
(1) 1.0 tons of feed grade lysine hydrochlorides are added in dissolution kettle, then add 0.4 ton of purified water, 90 ℃ of heating for dissolving, add 10 kilograms of gacs;
(2) take advantage of heat filtering to crystallization kettle above-mentioned solution, 25 ℃ of crystallisation by cooling.
(3) the centrifugal 15min of 1000r/min is dried to moisture content 5% by the product after centrifugal in ebullated bed;
(4) in the hopper of ebullated bed, directly blast steam 30min;
(5) close the steam blasting, with hot blast by drying materials.
Gained lysine hydrochloride (sample 3) meets Chinese Pharmacopoeia standard regulation, and wherein product transmittance is 99.5%, and content is 99.8%, and the standard diagram of infrared absorption pattern and beta crystal product is in full accord.As shown in Figure 4.
The lysine hydrochloride of embodiment 4 alpha-crystal forms is converted into beta crystal product
(1) 1.0 tons of feed grade lysine hydrochlorides are added in dissolution kettle, then add 0.4 ton of purified water, 90 ℃ of heating for dissolving, add 10 kilograms of gacs;
(2) take advantage of heat filtering to crystallization kettle above-mentioned solution, 25 ℃ of crystallisation by cooling.
(3) the centrifugal 15min of 1000r/min is dried to moisture content 0.2% by the product after centrifugal in ebullated bed;
Gained lysine hydrochloride (sample 4) physical and chemical index meets Chinese Pharmacopoeia standard regulation, and wherein product transmittance is 99.5%, and content is 99.7%, and infrared absorption pattern and standards of pharmacopoeia collection of illustrative plates are inconsistent, and this product is alpha-crystal form product.Infrared absorption pattern as shown in Figure 5, compose as shown in Figure 7 by XRD figure.
(4) the lysine hydrochloride 200kg of the alpha-crystal form of above-mentioned oven dry is joined in ebullated bed;
(5) in the hopper of ebullated bed, directly blast steam 50min;
(6) close the steam blasting, with hot blast by drying materials.
Gained lysine hydrochloride (sample 5) meets Chinese Pharmacopoeia standard regulation, and wherein product transmittance is 99.5%, and content is 99.7%, and the standard diagram of infrared absorption pattern and beta crystal product is in full accord.Infrared absorption pattern as shown in Figure 6, compose as shown in Figure 8 by XRD figure.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, do not departing under the prerequisite of the technology of the present invention principle; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. a preparation method for beta crystal lysine hydrochloride, is characterized in that, uses feed grade lysine hydrochloride to mix with purified water, heating for dissolving, then add activated carbon decolorizing, solution crystallisation by cooling after filtering; Centrifugal, centrifugal rear product is dried with ebullated bed, then blast saturation steam in ebullated bed hopper, then product is dried, obtain the lysine hydrochloride of beta crystal.
2. preparation method as claimed in claim 1, is characterized in that, the mass ratio that feeds intake of feed grade lysine hydrochloride and purified water is 1:0.4～0.6, is preferably 1:0.5.
3. preparation method as claimed in claim 1, is characterized in that, heating for dissolving temperature is 80～90 ℃, and it is preferably 85 ℃.
4. preparation method as claimed in claim 1, is characterized in that, activated carbon dosage is 1%～3% of feed grade lysine hydrochloride, and it is preferably 2%, and described % is mass percent.
5. preparation method as claimed in claim 1, is characterized in that, the temperature that after filtering, solution is directly cooled to is 20～30 ℃.
6. preparation method as claimed in claim 1, is characterized in that, centrifugal condition is 800～1000r/min, and centrifugation time is 10～20min.
7. preparation method as claimed in claim 1, is characterized in that, centrifugal rear product is first dried to 2～4% by moisture content with ebullated bed, is preferably 3%.
8. preparation method as claimed in claim 1, is characterized in that, the time that blasts saturated steam in ebullated bed is 30～50min.
9. preparation method as claimed in claim 1, is characterized in that, the time that blasts saturated steam in ebullated bed is 40min.
10. the preparation method described in claim 1-9 any one prepares beta crystal lysine hydrochloride product.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104892437A (en) * | 2015-05-15 | 2015-09-09 | 南通荣泰生物科技有限公司 | Production technology for L-lysine hydrochloride |
| CN112679371A (en) * | 2020-12-11 | 2021-04-20 | 北京民康百草医药科技有限公司 | Preparation method of L-lysine hydrochloride beta crystal form |
Citations (4)
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|---|---|---|---|---|
| EP1016651A1 (en) * | 1998-12-30 | 2000-07-05 | Archer-Daniels-Midland Company | A process for simultaneous production of amino acid hydrochloride and caustic via electrodialytic water splitting |
| US20020035269A1 (en) * | 2000-03-29 | 2002-03-21 | John Soper | Method for separating a basic amino acid from fermentation broth |
| CN101712624A (en) * | 2009-06-29 | 2010-05-26 | 冀州市华阳化工有限责任公司 | Method for purifying L-lysine hydrochloride |
| CN102924312A (en) * | 2012-11-01 | 2013-02-13 | 中粮生物化学（安徽）股份有限公司 | Lysine hydrochloride crystal and production method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1016651A1 (en) * | 1998-12-30 | 2000-07-05 | Archer-Daniels-Midland Company | A process for simultaneous production of amino acid hydrochloride and caustic via electrodialytic water splitting |
| US20020035269A1 (en) * | 2000-03-29 | 2002-03-21 | John Soper | Method for separating a basic amino acid from fermentation broth |
| CN101712624A (en) * | 2009-06-29 | 2010-05-26 | 冀州市华阳化工有限责任公司 | Method for purifying L-lysine hydrochloride |
| CN102924312A (en) * | 2012-11-01 | 2013-02-13 | 中粮生物化学（安徽）股份有限公司 | Lysine hydrochloride crystal and production method thereof |
Non-Patent Citations (1)
| Title |
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| 中华人民共和国卫生部药典委员会: "《药品红外光谱集 第1卷 1995》", 31 January 1996, article "第399号光谱图" * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104892437A (en) * | 2015-05-15 | 2015-09-09 | 南通荣泰生物科技有限公司 | Production technology for L-lysine hydrochloride |
| CN112679371A (en) * | 2020-12-11 | 2021-04-20 | 北京民康百草医药科技有限公司 | Preparation method of L-lysine hydrochloride beta crystal form |
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