CN103739507B - Preparation method of beta-crystal-form lysine hydrochloride - Google Patents
Preparation method of beta-crystal-form lysine hydrochloride Download PDFInfo
- Publication number
- CN103739507B CN103739507B CN201310465242.3A CN201310465242A CN103739507B CN 103739507 B CN103739507 B CN 103739507B CN 201310465242 A CN201310465242 A CN 201310465242A CN 103739507 B CN103739507 B CN 103739507B
- Authority
- CN
- China
- Prior art keywords
- product
- lysine hydrochloride
- preparation
- crystal
- beta
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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
A kind of the invention belongs to field of compound preparation, in particular it relates to the lysine hydrochloride preparation of highly purified beta crystal
Method.
Background technology
Lysine is that human body can not itself synthesize but one of eight kinds of highly desirable aminoacid, and being referred to as human body first must
Must propylhomoserin, lysine is increased to the utilization rate that can improve protein in food, thus the nutrition of condensed food significantly, promotes
The effects such as growth promoter, appetite strengthening, minimizing disease, health invigorating, particularly childhood development phase, after being ill convalescent period, pregnant suckling
Phase, institute was required.
Existing lysine hydrochloride manufacture method mostly is condensing crystallizing after decolouring, and after concentration, product is subject to high temperature, product
There is light transmittance is low, and content is relatively low, and other heteroacid are many etc. more, consume energy high simultaneously；Traditional handicraft product utilization boiling after crystallisation
Bed or vacuum drying oven are dried, and after drying, product crystallizes for α type, and the β type that the infared spectrum of product is required with standard has very big difference.
The requirement more and more higher to lysine hydrochloride product quality for the people in recent years, particularly American-European countries, the prescription to product
Higher.Therefore, we refine drying production process to existing lysine hydrochloride and are improved, on the basis of reduces cost
On, improve the quality of product.
Content of the invention
It is an object of the invention to provide a kind of preparation method of beta crystal lysine hydrochloride.
For reaching above-mentioned purpose, technical scheme provides a kind of preparation side of the high purity hydrochloric acid lysine of beta crystal
Method, is mixed with purified water with feed grade lysine hydrochloride, heating for dissolving, then plus activated carbon decolorizing, solution crystallisation by cooling after filtration；
Centrifugation, after being centrifuged, product ebullated bed dries, then blasts saturated vapor in ebullated bed hopper, then product is dried, and obtains β brilliant
The lysine hydrochloride of type.
The preparation method of the present invention, wherein said feed grade lysine hydrochloride is 1:0.4 with the mass ratio that feeds intake of purified water
～1:0.6.It is preferably 1:0.5.
The preparation method of the present invention, heating for dissolving temperature is 80～90 DEG C.It is preferably 85 DEG C.
The preparation method of the present invention, activated carbon dosage is the 1%～3% of feed grade lysine hydrochloride quality.It is preferably 2%.
The preparation method of the present invention, the direct crystallisation by cooling of solution after filtration.Chilling temperature is 20～30 DEG C.
In the preparation method of the present invention, centrifugal condition is 800～1000r/min, and centrifugation time is 10～20min.
Wherein, after centrifugation, moisture content is first dried to 2～4% with ebullated bed by product.It is preferably 3%.
The preparation method of the present invention, blasts the steam 30～50min of saturation in ebullated bed.
Preferably, blast the steam 40min of saturation in ebullated bed.
The invention provides the beta crystal lysine hydrochloride product that said method prepares.
The present invention is to be innovated on the basis of traditional handicraft, has searched out a kind of high-purity salt of beta crystal of simple possible
The preparation method of sour lysine, it is important that being optimized to parameters such as direct bleaching crystallization, product drying, this method yield can
Reach 95%, improve 20% compared with traditional method, reduce production cost；During condensing crystallizing has been abandoned using direct bleaching crystallization
High temperature concentrates destruction to aminoacid quality, improves product quality, and the power consumption during overcoming condensing crystallizing is high
Defect, reduces energy consumption；Employ the additional saturated vapor of ebullated bed simultaneously and combine drying, β monocrystalline type high-purity hydrochloric acid can be formed
Lysine product, makes alpha-crystal form or the lysine hydrochloride of α β mixing crystal formation be converted into beta crystal product, superior, product effectively
Quality meets Chinese Pharmacopoeia requirement.
Brief description
Fig. 1 absorbs collection of illustrative plates (beta crystal) for standard IR.
Fig. 2 is sample 1 infrared absorption pattern.
Fig. 3 is sample 2 infrared absorption pattern.
Fig. 4 is sample 3 infrared absorption pattern.
Fig. 5 is sample 4 infrared absorption pattern.
Fig. 6 is sample 5 infrared absorption pattern.
Fig. 7 is that the xrd of sample 4 schemes (alpha-crystal form).
Fig. 8 is that the xrd of sample 5 schemes (beta crystal).
Specific embodiment
With reference to embodiment, the specific embodiment of the present invention is described in further detail.Following examples are used for
The present invention is described, but is not limited to the scope of the present 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, be subsequently adding 0.6 ton of purified water, 80 DEG C of heating are molten
Solution, adds 30 kilograms of activated carbon；
(2) above-mentioned solution is filtered hot in crystallization kettle, 20 DEG C of crystallisation by cooling.
(3) 900r/min centrifugation 10min, the product after centrifugation is dried to moisture content 2% in ebullated bed；
(4) directly blast steam 50min in the hopper of ebullated bed；
(5) close the steam that blasts, with hot blast by drying materials.
Gained lysine hydrochloride (sample 1) meets Chinese Pharmacopoeia standard regulation, and wherein product light transmittance is 99.5%, content
For 99.7%, the standard diagram of infrared absorption pattern and beta crystal product is completely the same.As shown in accompanying drawing 1,2.
The preparation method of the lysine hydrochloride of embodiment 2 beta crystal
(1) 1.0 tons of feed grade lysine hydrochlorides are added in dissolution kettle, be subsequently adding 0.5 ton of purified water, 85 DEG C of heating are molten
Solution, adds 20 kilograms of activated carbon；
(2) above-mentioned solution is taken advantage of heat filtering to crystallization kettle, 25 DEG C of crystallisation by cooling.
(3) 800r/min centrifugation 20min, the product after centrifugation is dried to moisture content 3% in ebullated bed；
(4) directly blast steam 40min in the hopper of ebullated bed；
(5) close the steam that blasts, with hot blast by drying materials.
Gained lysine hydrochloride (sample 2) meets Chinese Pharmacopoeia standard regulation, and wherein product light transmittance is 99.4%, content
For 99.8%, the standard diagram of infrared absorption pattern and beta crystal product is completely the same.As shown in Figure 3.
The preparation method of the lysine hydrochloride of embodiment 3 beta crystal
(1) 1.0 tons of feed grade lysine hydrochlorides are added in dissolution kettle, be subsequently adding 0.4 ton of purified water, 90 DEG C of heating are molten
Solution, adds 10 kilograms of activated carbon；
(2) above-mentioned solution is taken advantage of heat filtering to crystallization kettle, 25 DEG C of crystallisation by cooling.
(3) 1000r/min centrifugation 15min, the product after centrifugation is dried to moisture content 5% in ebullated bed；
(4) directly blast steam 30min in the hopper of ebullated bed；
(5) close the steam that blasts, with hot blast by drying materials.
Gained lysine hydrochloride (sample 3) meets Chinese Pharmacopoeia standard regulation, and wherein product light transmittance is 99.5%, content
For 99.8%, the standard diagram of infrared absorption pattern and beta crystal product is completely the same.As shown in Figure 4.
The lysine hydrochloride of embodiment 4 alpha-crystal form is converted into beta crystal product
(1) 1.0 tons of feed grade lysine hydrochlorides are added in dissolution kettle, be subsequently adding 0.4 ton of purified water, 90 DEG C of heating are molten
Solution, adds 10 kilograms of activated carbon；
(2) above-mentioned solution is taken advantage of heat filtering to crystallization kettle, 25 DEG C of crystallisation by cooling.
(3) 1000r/min centrifugation 15min, the product after centrifugation is dried to moisture content 0.2% in ebullated bed；
Gained lysine hydrochloride (sample 4) physical and chemical index meets Chinese Pharmacopoeia standard regulation, and wherein product light transmittance is
99.5%, content is 99.7%, and infrared absorption pattern is inconsistent with standards of pharmacopoeia collection of illustrative plates, and that is, this product is alpha-crystal form product.Infrared suction
Receive collection of illustrative plates as shown in Figure 5, xrd collection of illustrative plates is as shown in Figure 7.
(4) the lysine hydrochloride 200kg of the alpha-crystal form of above-mentioned drying is added in ebullated bed；
(5) directly blast steam 50min in the hopper of ebullated bed；
(6) close the steam that blasts, with hot blast by drying materials.
Gained lysine hydrochloride (sample 5) meets Chinese Pharmacopoeia standard regulation, and wherein product light transmittance is 99.5%, content
For 99.7%, the standard diagram of infrared absorption pattern and beta crystal product is completely the same.Infrared absorption pattern as shown in Figure 6, xrd
Collection of illustrative plates is as shown in Figure 8.
The above is only the preferred embodiment of the present invention it is noted that ordinary skill people for the art
For member, on the premise of without departing from the technology of the present invention principle, some improvements and modifications can also be made, these improvements and modifications
Also should be regarded as protection scope of the present invention.
Claims (5)
1. a kind of preparation method of beta crystal lysine hydrochloride it is characterised in that
With feed grade lysine hydrochloride with purified water with the mass ratio that feeds intake as 1:0.4～0.6 mix；
80～90 DEG C of heating for dissolving；Again plus 1% activated carbon that mass percent is feed grade lysine hydrochloride carries out activated carbon
Decolouring；After filtration, solution direct cools to 20-30 DEG C of crystallization；Centrifugation, centrifugal condition is 800～1000r/min, and centrifugation time is
10～20min；Moisture content is first dried to 2～4% by product ebullated bed after centrifugation；Blast saturation again to steam in ebullated bed hopper
Vapour, the time blasting the steam of saturation in ebullated bed is 30～50min；Reusable heat wind is by drying materials；Obtain the hydrochloric acid of beta crystal
Lysine；
The xrd figure of described beta crystal lysine hydrochloride is as shown in Figure 8.
2. preparation method as claimed in claim 1 is it is characterised in that the quality that feeds intake of feed grade lysine hydrochloride and purified water
Than for 1:0.5.
3. preparation method as claimed in claim 1 is it is characterised in that heating for dissolving temperature is 85 DEG C.
4. preparation method as claimed in claim 1 it is characterised in that centrifugation after product ebullated bed first moisture content is dried to 3%.
5. preparation method as claimed in claim 1 it is characterised in that the time blasting the steam of saturation in ebullated bed be
40min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310465242.3A CN103739507B (en) | 2013-10-08 | 2013-10-08 | Preparation method of beta-crystal-form lysine hydrochloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310465242.3A CN103739507B (en) | 2013-10-08 | 2013-10-08 | Preparation method of beta-crystal-form lysine hydrochloride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103739507A CN103739507A (en) | 2014-04-23 |
| CN103739507B true CN103739507B (en) | 2017-01-25 |
Family
ID=50496598
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310465242.3A Active CN103739507B (en) | 2013-10-08 | 2013-10-08 | Preparation method of beta-crystal-form lysine hydrochloride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103739507B (en) |
Families Citing this family (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 |
| CN112679371B (en) * | 2020-12-11 | 2022-11-18 | 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)
| 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 |
-
2013
- 2013-10-08 CN CN201310465242.3A patent/CN103739507B/en active Active
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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103739507A (en) | 2014-04-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103435518B (en) | Preparation method of metformin hydrochloride | |
| CN104788345B (en) | A kind of production method of high-purity hydrochloric acid metformin | |
| BR112019018873A2 (en) | process for producing fuel ethanol using corn starch as a raw material. | |
| CN101914054B (en) | Comprehensive method for extracting L-tryptophan from fermentation liquor | |
| CN102775340A (en) | Method for synthesizing pyroglutamic calcium glutamate with shells serving as calcium sources | |
| CN102311450B (en) | Preparation method for Azlocillin sodium | |
| CN103739507B (en) | Preparation method of beta-crystal-form lysine hydrochloride | |
| CN106834402A (en) | A kind of preparation method of sunflower seed dregs complex polypeptide | |
| CN101156675A (en) | Glutamic acid abstraction technics combining rotation crystal | |
| CN105331751A (en) | Method for preparing medicinal waterless crystallized fructose by taking sugarcane as raw material | |
| CN103275047B (en) | Preparation method of griseofulvin | |
| CN107779351A (en) | A kind of production method of black glutinous rice wine | |
| CN110003295A (en) | A kind of preparation method of erythromycin thiocyanate | |
| CN106748847A (en) | A kind of extracting method of L alanine | |
| CN106473147B (en) | Purple yam anti-digestion starch and preparation method thereof | |
| CN105061289A (en) | Preparation method of pharmaceutical grade L-tryptophan | |
| WO2024119732A1 (en) | Method for extracting high-purity xylose liquid and cellulose from corn straw | |
| CN111410627A (en) | production method of pharmaceutical-grade L-tryptophan | |
| CN105949111A (en) | Preparation process of high-purity high-transmittance L-tryptophan | |
| BR112012011635B1 (en) | METHOD FOR THE PRODUCTION OF WHITE SUGAR, SUGAR | |
| CN105111247B (en) | A kind of preparation method of wild jujube nucleocapsid xylose and silica | |
| CN103641886B (en) | A kind of process for purification of glutamine dipeptide | |
| CN105503630A (en) | Method for purifying lysine hydrochloride | |
| CN106336366A (en) | Method for synthesizing 4-(2-aminoethyl)benzsulfamide | |
| CN102775453A (en) | Method for crystallizing and separating stevioside A3 from stevia total glycoside mixture |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |