CN102924312B - Lysine hydrochloride crystal and production method thereof - Google Patents
Lysine hydrochloride crystal and production method thereof Download PDFInfo
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- CN102924312B CN102924312B CN201210429780.2A CN201210429780A CN102924312B CN 102924312 B CN102924312 B CN 102924312B CN 201210429780 A CN201210429780 A CN 201210429780A CN 102924312 B CN102924312 B CN 102924312B
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Abstract
The invention provides a production method of a lysine hydrochloride crystal, which comprises the following steps: preparing a lysine hydrochloride feed liquid; sequentially performing concentration crystallization and cooling crystallization on the lysine hydrochloride feed liquid; and performing solid-liquid separation on the crystal slurry obtained after cooling crystallization, wherein the cooling crystallization condition includes controlling the difference between the temperature of a cooling medium and the temperature of the lysine hydrochloride feed liquid not to be higher than 13 DEG C. The invention also provides a lysine hydrochloride crystal produced by the method. According to the method provided by the invention, the lysine hydrochloride crystal product having high quality and satisfactory crystal form can be obtained.
Description
Technical field
The present invention relates to a kind of production method of Lysine hydrochloride crystal, and Lysine hydrochloride crystal obtained by this method.
Background technology
The continuous production method of current industrial Lysine hydrochloride crystal product comprises: be first separated through membrane filtration by lysine fermentation liquor and obtain Methionin clear liquid, Methionin clear liquid exchanges after (ISEP) purifies through continuous ionic and concentrates, lysine hydrochloride feed liquid is obtained afterwards with salt acid for adjusting pH, lysine hydrochloride feed liquid is injected evaporative crystallizer continuously, maintaining Tc is within the scope of 43-60 DEG C, then the magma of advantages of good crystallization is carried out centrifugal and dry and obtain Lysine hydrochloride crystal product.The percent crystallization in massecuite of Lysine hydrochloride crystal product obtained is like this lower and second-rate (namely in product, the content of lysine hydrochloride is lower).
Summary of the invention
The object of this invention is to provide a kind of production method can improving the quality of products and obtain the Lysine hydrochloride crystal of better crystalline form, and Lysine hydrochloride crystal obtained by this method.
The present inventor finds, decrease temperature crystalline is carried out to the lysine hydrochloride feed liquid through condensing crystal, if the not temperature head of controlled cooling model medium and lysine hydrochloride feed liquid, when speed particularly in order to accelerate decrease temperature crystalline adopts with the heat-eliminating medium that the temperature head of lysine hydrochloride feed liquid is larger, such as, when temperature head is more than 13 DEG C, can cause the second-rate of the Lysine hydrochloride crystal obtained, and the more crystalline form that causes of glomerocryst is poor.
The present inventor is surprised to find that by a large amount of experiments, carry out in decrease temperature crystalline process in lysine hydrochloride feed liquid, the temperature head of controlled cooling model medium and lysine hydrochloride feed liquid within the specific limits, can obtain that quality is higher, the good Lysine hydrochloride crystal product of crystalline form.This may owing to controlling the temperature head of heat-eliminating medium and lysine hydrochloride feed liquid, avoids that Local cooling is too fast causes pseudo-brilliant, the glomerocryst of the too high easy generation of degree of supersaturation, thus obtain that quality is higher, the good product of crystalline form.
To achieve these goals, the invention provides a kind of production method of Lysine hydrochloride crystal, wherein, the method comprises prepares lysine hydrochloride feed liquid, by described lysine hydrochloride feed liquid successively through condensing crystal and decrease temperature crystalline, again the magma that decrease temperature crystalline obtains is carried out solid-liquid separation, wherein, the condition of decrease temperature crystalline comprises: the temperature of controlled cooling model medium and the temperature head of lysine hydrochloride feed liquid are not more than 13 DEG C.
Present invention also offers a kind of Lysine hydrochloride crystal obtained by aforesaid method.
Pass through technique scheme, decrease temperature crystalline is continued on the basis of condensing crystal, be not more than 13 DEG C only by the temperature of heat-eliminating medium and the temperature head of lysine hydrochloride feed liquid in control decrease temperature crystalline process, effectively can improve the quality of Lysine hydrochloride crystal and obtain good crystalline form.
Other features and advantages of the present invention are described in detail in embodiment part subsequently.
Accompanying drawing explanation
Accompanying drawing is used to provide a further understanding of the present invention, and forms a part for specification sheets, is used from explanation the present invention, but is not construed as limiting the invention with embodiment one below.In the accompanying drawings:
Fig. 1 is the optical microscope photograph of the Lysine hydrochloride crystal according to the embodiment of the present invention 4 gained;
Fig. 2 is the optical microscope photograph of the Lysine hydrochloride crystal according to comparative example 1 gained of the present invention.
Embodiment
Below the specific embodiment of the present invention is described in detail.Should be understood that, embodiment described herein, only for instruction and explanation of the present invention, is not limited to the present invention.
The production method of Lysine hydrochloride crystal provided by the invention comprises prepares lysine hydrochloride feed liquid, by described lysine hydrochloride feed liquid successively through condensing crystal and decrease temperature crystalline, again the magma that decrease temperature crystalline obtains is carried out solid-liquid separation, wherein, the condition of decrease temperature crystalline comprises: the temperature of controlled cooling model medium and the temperature head of lysine hydrochloride feed liquid are not more than 13 DEG C.
According to method of the present invention, the temperature head of heat-eliminating medium and lysine hydrochloride feed liquid can realize object of the present invention in above-mentioned scope, under preferable case, when the temperature head of heat-eliminating medium and lysine hydrochloride feed liquid is 5-13 DEG C, the quality of the Lysine hydrochloride crystal obtained is higher, crystalline form is better.
In the present invention, by the temperature head of controlled cooling model medium and lysine hydrochloride feed liquid in above-mentioned scope, avoid that Local cooling is too fast causes pseudo-brilliant, the glomerocryst of the too high easy generation of degree of supersaturation, thus can obtain that purity is higher, the good product of crystalline form.But in order to better realize the present invention further, under preferable case, it is 1-9 DEG C/h that the condition of described decrease temperature crystalline comprises rate of temperature fall, is more preferably 4-7 DEG C/h.The temperature head of heat-eliminating medium and lysine hydrochloride feed liquid can be made to reach 1-9 DEG C/h by the amount of controlled cooling model medium, be more preferably within the scope of the rate of temperature fall of 4-7 DEG C/h.The present inventor finds, when the temperature head of controlled cooling model medium and lysine hydrochloride feed liquid is not more than 13 DEG C, and control rate of temperature fall in above-mentioned preferable range time, the outburst nucleation of crystal can be avoided further, reduce glomerocryst, pseudo-brilliant formation, be more conducive to obtaining the better product of crystalline form.
In the present invention, heat-eliminating medium can be the various material that can realize cooling down effect well known by persons skilled in the art, such as water coolant or cooling air.The preferred heat-eliminating medium of the present invention is water coolant.
In the present invention, the crystallizer carrying out decrease temperature crystalline can be well known to a person skilled in the art jacketed type or coil pipe type crystallizer.In order to carry out in the process of decrease temperature crystalline at use heat-eliminating medium, keep the temperature head of heat-eliminating medium and lysine hydrochloride feed liquid in above-mentioned scope, various method well known by persons skilled in the art can be adopted, such as can pass into water coolant continuously in the chuck of the crystallizer of decrease temperature crystalline or in circulation tube or in chuck and circulation tube, regulate the temperature head of the temperature of water coolant and lysine hydrochloride feed liquid in above-mentioned scope.
In addition, in order to prevent in decrease temperature crystalline process, cause owing to passing into heat-eliminating medium in the chuck of crystallizer occurring the temperature difference near the lysine hydrochloride feed liquid of jacket portion and the lysine hydrochloride feed liquid of middle body in crystallizer, preferably stir in decrease temperature crystalline process, be tending towards even with the temperature of the lysine hydrochloride feed liquid making whole crystallizer.The mode of concrete stirring can be any-mode well known by persons skilled in the art.
According to method of the present invention, the temperature of described condensing crystal can be selected in relative broad range, and as being 40-60 DEG C, under preferable case, the temperature of described condensing crystal is 43-60 DEG C.
According to method of the present invention, the time terminating condensing crystal can be selected in relative broad range, in order to guarantee output while taking into account quality product, under preferable case, in described condensing crystal process, when the crystalline content in feed liquid reaches 50-55 % by weight, terminate condensing crystal and start decrease temperature crystalline.The present inventor finds can enhance productivity better like this.
In the present invention, described condensing crystal can step mode carry out, and also can carry out in a continuous manner.When described condensing crystal carries out in step mode, the condensing crystal product that directly crystalline content in the feed liquid of acquisition can be met above-mentioned condition carries out decrease temperature crystalline at crystallizer or injection decrease temperature crystalline tank.When described condensing crystal carries out in a continuous manner, the condensing crystal product that the crystalline content in the feed liquid of acquisition can be met above-mentioned condition injects crystallizer, carries out decrease temperature crystalline.
In the present invention, the temperature of carrying out the magma of solid-liquid separation can be 10-25 DEG C, preferred 10-15 DEG C
In the present invention, in the lysine hydrochloride feed liquid of preparation, the concentration of lysine hydrochloride is not particularly limited, and can select in relative broad range, and the present invention is preferably 50-55 % by weight.
In the present invention, described method can also comprise carries out dry step by the crystal that solid-liquid separation obtains.The mode of described drying can be various drying mode well known to those skilled in the art, and such as, the drying mode of the various routines such as seasoning, forced air drying, vacuum-drying, does not repeat them here.Dry temperature and time does not specially require, as long as the crystal of acquisition can be made fully dry.
Present invention also offers the Lysine hydrochloride crystal obtained by aforesaid method.The quality of the Lysine hydrochloride crystal obtained by aforesaid method is higher, crystalline form is better.
In the present invention, the fermentation method of purification that the method preparing lysine hydrochloride feed liquid can use for this area routine, such as, the ripe seed liquor of preparation can be comprised, preparation fermention medium, fermentation, carries out solid-liquid separation by the fermented liquid of acquisition, and fermentation clear liquid solid-liquid separation obtained contacts with hydrochloric acid through concentrated after ISEP purifies again.Described ISEP method of purification also can be the ordinary method of this area, therefore does not repeat them here.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characteristic described in above-mentioned embodiment, in reconcilable situation, can be combined by any suitable mode, in order to avoid unnecessary repetition, the present invention illustrates no longer separately to various possible array mode.
In addition, also can carry out arbitrary combination between various different embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Below will be described the present invention by embodiment.
In following examples, crystalline content refers to that the Lysine hydrochloride crystal of actual crystallization accounts for the mass percent of feed liquid or magma total mass; Lysine hydrochloric acid salts contg refers to the mass percent of lysine hydrochloride in Lysine hydrochloride crystal product, lysine hydrochloride content value is higher, illustrate that the foreign matter content in product is lower, quality product is higher, lysine hydrochloric acid salts contg adopts conventional perchloric acid method to measure, concrete operations can see feed grade L-Lysine hydrochloride GB GB8245-87, wherein, feed grade L-Lysine hydrochloride demand fulfillment content >=98.5%(quality) requirement; The optical microscope photograph of gained crystal adopts Olympus Optical microscope (OLIMPUS Cx31 type) to obtain.
Embodiment 1
By 22m
3lysine hydrochloride feed liquid (lysine hydrochloric acid salts contg is 50 % by weight) inject crystallizer, crystallization control temperature is 45 DEG C, carry out condensing crystal, when the crystalline content in feed liquid reaches 55 % by weight, be injected in crystallizer and carry out decrease temperature crystalline, the temperature controlling the water coolant passed in crystallizer chuck makes the temperature head of lysine hydrochloride feed liquid in itself and crystallizer be 10 DEG C, controlling rate of temperature fall is 7 DEG C/h, when being cooled to 10 DEG C, the lysine hydrochloride magma obtained is carried out centrifugation, and the crystal that will wet was 105 DEG C of dryings 40 minutes, obtain Lysine hydrochloride crystal product.In gained crystal product, lysine hydrochloric acid salts contg is 99.5%.
Embodiment 2
By 22m
3lysine hydrochloride feed liquid (lysine hydrochloric acid salts contg is 55 % by weight) inject crystallizer, crystallization control temperature is 60 DEG C, carry out condensing crystal, when the crystalline content in feed liquid reaches 55 % by weight, be injected in crystallizer and carry out decrease temperature crystalline, the temperature controlling the water coolant passed in crystallizer chuck makes the temperature head of lysine hydrochloride feed liquid in itself and crystallizer be 8 DEG C, controlling rate of temperature fall is 4 DEG C/h, when being cooled to 15 DEG C, the lysine hydrochloride magma obtained is carried out centrifugation, and the crystal that will wet was 105 DEG C of dryings 40 minutes, obtain Lysine hydrochloride crystal product.In gained crystal product, lysine hydrochloric acid salts contg is 99.7%.
Embodiment 3
By 22m
3lysine hydrochloride feed liquid (lysine hydrochloric acid salts contg is 52 % by weight) inject crystallizer, crystallization control temperature is 50 DEG C, carry out condensing crystal, when the crystalline content in feed liquid reaches 50 % by weight, be injected in crystallizer and carry out decrease temperature crystalline, the temperature controlling the water coolant passed in crystallizer chuck makes the temperature head of lysine hydrochloride feed liquid in itself and crystallizer be 5 DEG C, controlling rate of temperature fall is 5 DEG C/h, when being cooled to 15 DEG C, the lysine hydrochloride magma obtained is carried out centrifugation, and the crystal that will wet was 105 DEG C of dryings 40 minutes, obtain Lysine hydrochloride crystal product.In gained crystal product, lysine hydrochloric acid salts contg is 99.8%.
Embodiment 4
By 22m
3lysine hydrochloride feed liquid (lysine hydrochloric acid salts contg is 51 % by weight) inject crystallizer, crystallization control temperature is 50 DEG C, carry out condensing crystal, when the crystalline content in feed liquid reaches 50 % by weight, be injected in crystallizer and carry out decrease temperature crystalline, the temperature controlling the water coolant passed in crystallizer chuck makes the temperature head of lysine hydrochloride feed liquid in itself and crystallizer be 13 DEG C, controlling rate of temperature fall is 5 DEG C/h, when being cooled to 15 DEG C, the lysine hydrochloride magma obtained is carried out centrifugation, and the crystal that will wet was 105 DEG C of dryings 40 minutes, obtain Lysine hydrochloride crystal product.In gained crystal product, lysine hydrochloric acid salts contg is 98.6%.The optical microscope photograph (amplifying 40 times) of this crystal product as shown in Figure 1.
Comparative example 1
According to the method production Lysine hydrochloride crystal of embodiment 4, unlike, have suffered in temperature-fall period, the temperature head passing into lysine hydrochloride feed liquid in water coolant in crystallizer chuck and crystallizer is 20 DEG C.In gained crystal product, lysine hydrochloric acid salts contg is 98.3%.The optical microscope photograph (amplifying 40 times) of this crystal product as shown in Figure 2.
As can be seen from embodiment 1-4, in the Lysine hydrochloride crystal that method provided by the invention is produced, lysine hydrochloric acid salts contg is more than 98.6%, and can up to 99.8%, higher than the criterion of acceptability 98.5% in GB 8245-87, therefore, qualified Lysine hydrochloride crystal can not only be produced by method of the present invention, and can the higher Lysine hydrochloride crystal of the quality of production; And not within the scope of method provided by the invention, lysine hydrochloric acid salts contg is 98.3% in the Lysine hydrochloride crystal of production, lower than 98.5%, qualified Lysine hydrochloride crystal can not be obtained.
In addition, as can be seen from Fig. 1 and Fig. 2, the glomerocryst of the Lysine hydrochloride crystal of producing according to method provided by the invention is less, and crystalline form is better; And not within the scope of method provided by the invention, the Lysine hydrochloride crystal glomerocryst produced is more, crystalline form is poor.As can be seen here, method provided by the invention can provide crystalline form good Lysine hydrochloride crystal.
Claims (5)
1. the production method of a Lysine hydrochloride crystal, it is characterized in that, the method comprises prepares lysine hydrochloride feed liquid, by described lysine hydrochloride feed liquid successively through condensing crystal and decrease temperature crystalline, again the magma that decrease temperature crystalline obtains is carried out solid-liquid separation, wherein, the condition of decrease temperature crystalline comprises: the temperature of controlled cooling model medium and the temperature head of lysine hydrochloride feed liquid are not more than 13 DEG C, rate of temperature fall is 1-9 DEG C/h, in described condensing crystal process, when the crystalline content in described lysine hydrochloride feed liquid reaches 50-55 % by weight, terminate condensing crystal and start decrease temperature crystalline.
2. method according to claim 1, wherein, the temperature of controlled cooling model medium and the temperature head of lysine hydrochloride feed liquid are 5-13 DEG C.
3. method according to claim 1, wherein, the rate of temperature fall of described decrease temperature crystalline is 4-7 DEG C/h.
4. method according to claim 1, wherein, the temperature of described condensing crystal is 43-60 DEG C.
5. method according to claim 1, wherein, the crystal that described method also comprises solid-liquid separation obtains carries out drying.
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| CN103739507B (en) * | 2013-10-08 | 2017-01-25 | 蚌埠丰原医药科技发展有限公司 | Preparation method of beta-crystal-form lysine hydrochloride |
| CN104230733B (en) * | 2014-07-28 | 2016-08-24 | 中粮生物化学（安徽）股份有限公司 | A kind of production method of Lysine hydrochloride crystal |
| CN111116392B (en) * | 2019-12-30 | 2021-04-23 | 海南全星制药有限公司 | Lysine hydrochloride compound and pharmaceutical composition thereof |
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| JPS60184054A (en) * | 1984-03-03 | 1985-09-19 | Ajinomoto Co Inc | Method for purifying optically active lysine |
| 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 |
| CN101665442A (en) * | 2009-10-09 | 2010-03-10 | 蚌埠丰原涂山制药有限公司 | Crystallization method of high purity DL-lysine |
| CN102875404B (en) * | 2012-10-12 | 2014-07-23 | 中粮生物化学（安徽）股份有限公司 | Production method and application of lysine hydrochloride crystals |
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