CN100336814C - Method for preparing spherical crystal lactochrome utilizing solvent supersonic synergetic effect - Google Patents
Method for preparing spherical crystal lactochrome utilizing solvent supersonic synergetic effect Download PDFInfo
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- CN100336814C CN100336814C CNB2005100163160A CN200510016316A CN100336814C CN 100336814 C CN100336814 C CN 100336814C CN B2005100163160 A CNB2005100163160 A CN B2005100163160A CN 200510016316 A CN200510016316 A CN 200510016316A CN 100336814 C CN100336814 C CN 100336814C
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- riboflavin
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- hydrochloric acid
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Abstract
The present invention discloses a method for preparing spherical crystal riboflavin utilizing solvent supersonic synergetic effects, which belongs to preparing technique of the riboflavin. The method comprises the following procedures that: needle crystal riboflavin is completely dissolved into prime solvent of hydrochloric solution; the temperature of the dissolution process is controlled between 0 and 80DEG C; the foreign matter of the obtained riboflavin hydrochloric mixed liquor is removed by filtration or centrifugation, and de-ionized water or an ethanol precipitation agent is added into the hydrochloric mixed liquor of the riboflavin which is obtained by the filtration. In the meantime, after supersonic wave action is applied for 10-60 min, regular and spherical riboflavin crystalline solution is obtained; filtering cakes are washed by deionized water by standing and filtration, and finally, after the filtering cakes are dried by hot air, the spherical crystal riboflavin is obtained. The present invention omits traditional crystallizing steps, such as the generation of crystal seeds, grinding, introduction, etc. The periods are shortened; the operation is convenient; the manufactured spherical riboflavin crystallization has the advantage of favorable processing performance; product fluidity is increased; the bulk density of particles is increased, the application of the present invention is convenient, and the product value of the riboflavin is lifted.
Description
Technical field
The present invention relates to a kind of method for preparing spherical crystal lactochrome utilizing solvent supersonic synergetic effect, belong to the technology of preparing of riboflavin.
Background technology
Riboflavin claims vitamins B again
2(VB
2), be a kind of isoalloxazine derivative that contains ribityl.VB
2Very extensive as the base nutrients use, be used for feed and foodstuffs industry in a large number, be only second to vitamin A, D, content can be made feed at 96% product.In food, feed and pharmaceutical industry, also use sometimes as tinting material.The existing chemical synthesis of the production of riboflavin has the biotechnology synthesis method again, but the biological production method is preponderated.At different production methods, the separating and extracting method of riboflavin also has difference.Generally speaking, the separating and extracting method of riboflavin mainly contains: the heavy metallic salt precipitator method, Morehouse method, acid pasting and alkali solution technique.Industrial production mainly adopts back two kinds of methods at present.
Riboflavin is the yellow orange-yellow crystallinity powder that arrives, and multiple different crystalline form is arranged, and show different physical propertiess, typical VB
2Crystalline form be yellow needle-like.Up to now, the VB that sells on production and the market
2Mostly be needle crystal, part is in very thin powder (still being needle crystal).The riboflavin processing characteristics extreme difference of this needle crystal has the feature that is difficult for processing and mobile difference, and bulk density is minimum, and these features make riboflavin be difficult for compressing tablet or hybrid process.For example when processing riboflavin nutrition sheet, because VB
2The flowability difference and destroy the processing characteristics of whole tablet, cause after the film-making mass distribution of riboflavin inhomogeneous.In order to overcome these difficulties, people process after often will making riboflavin form particle with subsidiary again, improve its flowability and compressibility, and granulation process have increased riboflavin production cost and time, have also reduced the purity of riboflavin.
Summary of the invention:
The object of the present invention is to provide a kind of method for preparing spherical crystal lactochrome utilizing solvent supersonic synergetic effect, this method preparation technology is simple, cost is low, the product purity height.
The present invention is realized that by following technical proposals a kind of method for preparing spherical crystal lactochrome utilizing solvent supersonic synergetic effect is characterized in that comprising following process:
(1) mass concentration that the needle crystal riboflavin of mass fraction 1～6 is dissolved in fully mass fraction 10～15 is that the dissolution process temperature is controlled at 0～80 ℃, obtains the riboflavin hydrochloric acid mixed solution in 20%～36% the hydrochloric acid soln main solvent;
(2) under 0～80 ℃ of condition, after filtration or centrifugally remove insoluble solid impurity;
(3) under identical temperature range condition, still by the riboflavin quality, the deionized water or the ethanol precipitation agent of mass fraction 10～200 are added in the riboflavin hydrochloric acid mixed solution of step (2) gained, meanwhile, imposing frequency is that 20～50KHz, power are ultrasonic wave effect 10～60min of 10W～500W, obtains the globose nucleus flavine crystallization solution of rule;
(4) the globose nucleus flavine crystallization solution that obtains is left standstill 30～120min;
(5) filter and use the deionized water wash filter cake, then, filter cake obtains spherical crystal lactochrome utilizing through 40～100 ℃ of warm air dryings 1～14 hour.
Above-mentioned dissolution process temperature is 10～30 ℃; The mass concentration of main solvent hydrochloric acid soln is 22%～30%.
Advantage that the present invention has and beneficial effect are in particular in:
(1) the present invention adopts the globose nucleus flavine crystallization of solvent supersonic synergetic effect acquisition to have excellent machinability, improves the bulk density of riboflavin finished product flowability and particle greatly, easily handles and good fluidity, makes things convenient for its application, promotes the riboflavin value of the product.
(2) this process is compared with the conventional junction crystal method, has saved steps such as crystal seed generation, grinding, introducing, the shortening cycle, and easy and simple to handle, reduce cost, reduce and pollute, improve the quality of products.
Description of drawings
Spherical nucleus flavine micro-the take pictures figure of Fig. 1 for making with the inventive method.
Embodiment
Below by specific embodiment the present invention is specifically described in detail:
Example one
Get the 800ml mass concentration and be 23.8% hydrochloric acid soln and place large beaker as main solvent, temperature is controlled at 20 ± 1 ℃, constantly under the agitation condition 151.0g purity 96% needle crystal riboflavin is dissolved in the main solvent fully, obtains the riboflavin hydrochloric acid soln.Filter under identical temperature condition, collecting filtrate with beaker is the riboflavin hydrochloric acid soln, and is fixed in the Vltrasonic device tank, and the tank temperature is controlled at 30 ± 1 ℃.After treating that solution temperature is stable, with the speed adding 4400ml precipitation agent deionized water of 400ml/min.Apply frequency when adding precipitation agent and be 40KHz, power and be the ultrasonic wave effect 15 minutes of 128W, leave standstill 50min then, the acquisition size distribution is even, the regular spherulite riboflavin solution of particle diameter 10 μ m～15 μ m, through filtering and use the deionized water wash filter cake, the gained filter cake is through 95 ℃ of warm air dryings 6 hours, obtains purity and be 98% riboflavin crystal 118.3g.
Example two
Get the 400ml mass concentration and be 29.1% hydrochloric acid soln and place large beaker as main solvent, temperature is controlled at 25 ± 1 ℃, constantly under the agitation condition 151.0g purity 96% needle crystal riboflavin is dissolved in the main solvent fully, obtains rib flavine hydrochloric acid soln.Filter under identical temperature condition, it is the riboflavin hydrochloric acid soln that beaker is collected filtrate, and is fixed in the Vltrasonic device tank, and the tank temperature is controlled at 20 ± 1 ℃.After treating that solution temperature is stable, speed with 700ml/min adds 4800ml precipitation agent (deionized water), simultaneously, begin to apply frequency and be 40KHz, power and be the ultrasonic wave effect 10 minutes of 96W, leave standstill 40min then, it is even to obtain size distribution, the regular spherulite riboflavin solution of particle diameter 18 μ m～22 μ m, filter and also to use the deionized water wash filter cake, the gained filter cake is through 80 ℃ of warm air dryings 8 hours, obtains purity and be 98% riboflavin crystal 126.9g.
Example three
Get the 1000ml mass concentration and be 24.0% hydrochloric acid soln and place large beaker as main solvent, temperature is controlled at 25 ± 1 ℃, constantly under the agitation condition 190.0g purity 96% needle crystal riboflavin is dissolved in the main solvent fully, obtains the riboflavin hydrochloric acid soln.Under identical temperature condition, filter, collect filtrate with beaker and be the riboflavin hydrochloric acid soln and be fixed in the Vltrasonic device tank that the tank temperature is controlled at 25 ± 1 ℃.After treating that solution temperature is stable, with the speed adding 5600ml precipitation agent deionized water of 20ml/s.Apply frequency when adding precipitation agent and be 25KHz, power and be the ultrasonic wave effect 25 minutes of 112W, leave standstill 50min then, the acquisition size distribution is even, the regular spherulite riboflavin solution of particle diameter 13 μ m～19 μ m, through filtering and use the deionized water wash filter cake, the gained filter cake is through 95 ℃ of warm air dryings 6 hours, obtains purity and be 98% riboflavin crystal 138.3g.
Example four
Get the 500ml mass concentration and be 31.0% hydrochloric acid soln and place large beaker as main solvent, temperature is controlled at 30 ± 1 ℃, constantly under the agitation condition 190.0g purity 96% needle crystal riboflavin is dissolved in the main solvent fully, obtains the riboflavin hydrochloric acid soln.Under identical temperature condition, filter, collect filtrate with beaker and be the riboflavin hydrochloric acid soln and be fixed in the Vltrasonic device tank that the tank temperature is controlled at 25 ± 1 ℃.After treating that solution temperature is stable, with the speed adding 6200ml precipitation agent deionized water of 40ml/s.Apply frequency when adding precipitation agent and be 25KHz, power and be the ultrasonic wave effect 20 minutes of 96W, leave standstill 60min then, the acquisition size distribution is even, the regular spherulite riboflavin solution of particle diameter 20 μ m～26 μ m, through filtering and use the deionized water wash filter cake, the gained filter cake is through 75 ℃ of warm air dryings 10 hours, obtains purity and be 98% riboflavin crystal 143.5g.
Claims (2)
1. method for preparing spherical crystal lactochrome utilizing solvent supersonic synergetic effect is characterized in that comprising following process:
(1) mass concentration that the needle crystal riboflavin of mass fraction 1～6 is dissolved in fully mass fraction 10～15 is that the dissolution process temperature is controlled at 0～80 ℃, obtains the riboflavin hydrochloric acid mixed solution in 20%～36% the hydrochloric acid soln main solvent;
(2) under 0～80 ℃ of condition, after filtration or centrifugally remove insoluble solid impurity;
(3) under identical temperature range condition, still by the riboflavin quality, the deionized water precipitation agent of mass fraction 10～200 is added in the riboflavin hydrochloric acid mixed solution of step (2) gained, meanwhile, imposing frequency is that 20～50KHz, power are ultrasonic wave effect 10～60min of 10W～500W, obtains the globose nucleus flavine crystallization solution of rule;
(4) the globose nucleus flavine crystallization solution that obtains is left standstill 30～120min;
(5) filter and use the deionized water wash filter cake, then, filter cake obtains spherical crystal lactochrome utilizing through 40～100 ℃ of warm air dryings 1～14 hour.
2. by the described method of claim 1, it is characterized in that the dissolution process temperature is 10～30 ℃; The mass concentration of main solvent hydrochloric acid soln is 22%～30%.
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| CNB2005100163160A CN100336814C (en) | 2005-11-23 | 2005-11-23 | Method for preparing spherical crystal lactochrome utilizing solvent supersonic synergetic effect |
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| CNB2005100163160A CN100336814C (en) | 2005-11-23 | 2005-11-23 | Method for preparing spherical crystal lactochrome utilizing solvent supersonic synergetic effect |
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| CN100336814C true CN100336814C (en) | 2007-09-12 |
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| CN102775407B (en) * | 2012-01-20 | 2015-08-05 | 连云港金康医药科技有限公司 | Stable unformed 5-methyltetrahydrofolate salt and preparation method thereof |
| WO2013107236A1 (en) * | 2012-01-20 | 2013-07-25 | 连云港金康和信药业有限公司 | Crystal form of (6s)-5-methyltetrahydrofolate salt and method for preparing same |
| CN104961740B (en) * | 2015-06-02 | 2016-04-27 | 湖北广济药业股份有限公司 | A kind of solid preparation containing riboflavin and preparation method thereof |
| CN113943291B (en) * | 2021-11-30 | 2023-09-08 | 湖北广济药业股份有限公司 | Method for removing residual DNA in riboflavin by nuclease |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2072973U (en) * | 1990-08-17 | 1991-03-13 | 华南理工大学 | Solvent/supersonic wave cooperative coring crystallizer |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2072973U (en) * | 1990-08-17 | 1991-03-13 | 华南理工大学 | Solvent/supersonic wave cooperative coring crystallizer |
Non-Patent Citations (2)
| Title |
|---|
| 超声波对结晶过程的作用及机理 郭志超等，天津化工，第17卷第3期 2003 * |
| 超声频率对HCFC-141b水合物结晶过程的影响研究 刘永红等，哈尔滨工业大学学报，第37卷第5期 2005 * |
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