CN101817759B - Preparation method of L-carnitine nitrate - Google Patents
Preparation method of L-carnitine nitrate Download PDFInfo
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- CN101817759B CN101817759B CN 201010170346 CN201010170346A CN101817759B CN 101817759 B CN101817759 B CN 101817759B CN 201010170346 CN201010170346 CN 201010170346 CN 201010170346 A CN201010170346 A CN 201010170346A CN 101817759 B CN101817759 B CN 101817759B
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Abstract
The invention discloses a preparation method of L-carnitine nitrate, comprising the following steps of: dripping nitric acid into L-carnitine while stirring under the temperature of 10 to 25 DEG C, wherein the mol ratio of the L-carnitine to the nitric acid is 1: 1-1.1; gradually clarifying the solution at the reaction temperature of 40 to 70 DEG C; regulating the pH value of the solution to be 1 to 2 by using the nitric acid; continuously stirring the clarified solution, preserving the temperature for 15 to 30min and then compressing and dehydrating, stirring and air-drying at 50 to 70 DEG C, and drying at 75 to 80 DEG C to obtain an L-carnitine nitrate finished product. In the invention, the L-carnitine and the nitric acid are reacted under the ordinary pressure, and therefore, the reaction conditions are mild. In the preparation method, the food-grade L-arginine and the high-purity nitric acid are adopted as raw materials, therefore, the produced L-carnitine nitrate has good quality and high purity up to more than 99 percent without crystallization; not only the quality is ensured, but also the working procedures are saved. The production efficiency is improved and the yield coefficient is high and is up to more than 98 percent. The preparation method has reasonable and simple process and can be suitable for industrial large production.
Description
Technical field
The present invention relates to the preparation method of a seed amino acid nitrate, the preparation method of the VBT nitrate that specifically a kind of quality is good, yield is high, cost is low.
Background technology
VBT (L-carnitine) claim again L-carnitine.Another name L-BETAIN, DL-carnitine chloride.Chemical name is beta-hydroxy γ-TMA (TriMethylAmine) butyric acid.It is a kind of amino acid that impels fat to be converted into energy.Human body is had no side effect.VBT extensively exists as alkali components in muscle, usually can extract from the meat of pig, calf, horse etc.
Existing document shows, VBT for the growing of animal, breed, health is extremely important.It has the β-oxidation that promotes lipid acid, reduces the content of serum cholesterol and triglyceride level, improves the important physiological function such as body tolerance.
The secretory volume of VBT becomes with exercise intensity.When high pressure training, it can guarantee that body avoids the disadvantageous effect of hyperammonemia.Therefore it can add in drinking-water, drinks for the sportsmen, makes the sportsmen when high pressure training, and each metabolic balance in holder avoids health to come to harm.
VBT can help fat-reducing, although when using carnitine separately, may be helpless to the minimizing of fat, it can affect the metabolism of fat of body, makes its speed of consume losing and the loss speed of ratio greater than muscle, and makes the go on a diet tolerance raising in stage of people.Being particularly suitable for people coordinates and to do aerobic exercise and come fat reducing.Effect is apparent in view.
Along with the development of livestock industry, synthetic convenient and safe, efficient growth promoter is the focus of medicine and Nutritional studies always.Add high-copper, microbiotic, beta-stimulants and injection tethelin etc. in feed, have the shortcomings such as environmental pollution, drug residue, food safety and operation be loaded down with trivial details, be difficult to promote the use of aborning.VBT is because it is easy to use, can play raising sow reproductive performance, raising piglet survival ratio, the reduction thickness of backfat, raising meat and Egg―qualites texts under certain condition and day by day come into one's own as a kind of novel fodder additives, and also having carried out corresponding research and utilization at medicine and food service industry.
Experiment shows that VBT is a kind of essential nutrients, in the international nutrition academic conference that 1985 hold in Chicago, VBT is appointed as " multifunctional and nutritional product ".
VBT has been applied to the fields such as medicine, health care and food at present, and has been defined as legal multipurpose nutritive agent by Switzerland, France, the U.S. and the World Health Organization.China foodstuff additive hygienic standard GB2960-1996 has stipulated that L-carnitine-L-tartrate is food enrichment, can be applicable to the aspects such as chewable tablet, drink, capsule, milk powder and milky-drinks.
Because the VBT salt becomes VBT at last through conversions such as oxydase in vivo, easily absorbed by health.So now VBT is all made the VBT salt and taken, the products such as noted above L-carnitine-L-tartrate and VBT hydrochloride are domestic manufacturer production.The discovery of U.S. parties concerned research recently, amino acid whose nitrate more is conducive to amino acid absorption in vivo, therefore VBT is made into VBT nitrate, will more easily change into VBT, is absorbed by health.When therefore it uses, dosage can be less, and oral absorption efficient can be higher.But the producer that also there is no in the world suitability for industrialized production VBT nitrate product at present.
Summary of the invention
The present invention is in order to solve the problem of VBT nitrate large-scale production, and provide a kind of can suitability for industrialized production and yield high, the preparation method of the VBT nitrate that product purity is high.
The technical scheme that the present invention takes is: a kind of preparation method of VBT nitrate: in stirring at 10 ℃～25 ℃ temperature with nitric acid dropping in VBT, the mol ratio of VBT and nitric acid is 1: 1～1.1.Temperature of reaction is at 40 ℃～70 ℃, and molten clarification gradually is 1～2 with nitric acid regulator solution pH; Decompression dehydration after after solution is clarified, continuation is stirred and is incubated 15～30 minutes, the product after dehydration is air-dry in 50 ℃～70 ℃ stirrings, then gets VBT nitrate finished product after 75 ℃～85 ℃ dryings.
A kind of preparation method of VBT nitrate: in stirring at 20 ℃ ± 2 ℃ temperature with nitric acid dropping in VBT, the mol ratio of VBT and nitric acid is 1: 1; 60 ℃ ± 5 ℃ of temperature of reaction, solution is clarified gradually, is 2 with nitric acid regulator solution pH; Decompression dehydration after after the solution clarification, stirring is incubated 20 minutes, the product after dehydration is air-dry in 60 ℃ ± 5 ℃ stirrings, then gets VBT nitrate finished product after 80 ℃ of dryings.
In above-mentioned preparation process, the condition of decompression dehydration is: temperature is 50 ℃～65 ℃, and vacuum tightness is more than 500 mmhg.
Advantage and positively effect that the present invention has are: the present invention adopts VBT and nitric acid to react under normal pressure, and reaction conditions is gentle.The present invention adopts high-quality food grade VBT and the nitric acid of chemical reagent-grade, so the VBT nitrate product impurity of producing is few, quality is good, just reach more than 99% without recrystallization purity, both guaranteed quality, save again operation and production time, improved production efficiency, reduced cost.Preparation were established of the present invention rationally, simply is fit to industrialized production, and yield reaches more than 98%.
Embodiment
The present invention adopts the VBT of food grade and the nitric acid of chemical reagent-grade to react under normal pressure, and reaction conditions is gentle.The mol ratio of VBT and nitric acid is 1: 1, but for VBT is reacted completely, the add-on of nitric acid is more bigger than VBT.The concentration of nitric acid that the present invention adopts is 65～68%.Because concentration of nitric acid is different, so add-on has certain variation, but and the ratio of 1 mole of VBT all between 1 to 1.1 mole.
The solubleness of VBT of the present invention in water is large, and the water in nitric acid just can be entirely molten with VBT, therefore need not add water.But the reaction of VBT and nitric acid is thermopositive reaction, and is violent for fear of reaction, heat up too fast, and the untimely decomposition that causes of dispelling the heat, when beginning to react, temperature must be low, between 10 ℃ to 25 ℃.Generally maintain 20 ℃ ± 2 ℃, and control the speed that nitric acid adds, take the method that drips.Due to the low temperature effect speed of response, therefore drip at nitric acid and finish the rear temperature of reaction that improves.General temperature is preferably in 60 ℃ ± 5 ℃ below 70 ℃.But also can control low temperature when just beginning to drip nitric acid, control subsequently rate of addition and temperature, utilize the temperature of the heat reacting by heating solution of reaction generation, fast reaction speed.Temperature of reaction can not surpass 70 ℃, otherwise VBT can be damaged, and affects the yield of final product.Along with temperature raises, speed of response is accelerated, and solution is more and more clarified, and stirs all the time in this process, makes reactant distribution even, and reaction is accelerated.Reaction finishes when solution is clarified fully.Also need continue to stir insulation 15～30 minutes this moment.
It is acid that product VBT nitrate of the present invention is, and pH should be 2.Generally finish before measurement pH in reaction, if acidity less than 2, drips nitric acid, controlling pH value of solution with nitric acid is 2.Because when producing, the mol ratio of nitric acid is slightly larger than VBT, so if pH allows, can not affect quality product between 2 and 1.
In the present invention, the solubleness of VBT nitrate in reaction soln is large, is all crystallisate and the water of VBT nitrate in container after reaction finishes, and can't separate, and therefore adopts the decompression method dehydration.Decompression method is industry common technology.The vacuum tightness of decompression dehydration is more than 500 mmhg, and temperature is 50 ℃～65 ℃.Because product after dehydration is thick, can't further remove moisture with the drying method, so that the reactant after dewatering carries out is air-dry, air-dry method is also industry common technology, stir incessantly in 50 ℃～70 ℃ scopes when air-dry, to accelerate air flowing, take away moisture.
The method not restriction of the present invention to drying, the method for every suitable VBT nitrate drying can be used, as methods such as moisture eliminator, spray method dryings.Dry temperature is 75 ℃～85 ℃, and temperature is too low, and product can conglomeration.Temperature surpasses 85 ℃, and VBT nitrate can decompose, and quality is affected.The present embodiment adopts 80 ℃ of dryings.
For further understanding summary of the invention of the present invention, Characteristic, hereby enumerate following examples, be described in detail as follows:
Embodiment 1
While stirring 94 kilograms, 68% nitric acid is added drop-wise to 162 kilograms of VBTs at 20 ℃ ± 2 ℃ temperature in, drips Bi Suihou and be heated to 60 ℃ ± 5 ℃, along with temperature rising solution is clarified gradually.Finishing before measurement pH value in reaction, is 2 with nitric acid regulator solution pH.Continue to stir insulation 20 minutes after the solution clarification.Then keep 60 ℃ ± 5 ℃ temperature decompression dehydrations, vacuum keep is more than 500 mmhg.The reactant that dehydration obtains is air-dry in 55 ℃ ± 5 ℃ stirrings, then in 80 ℃ of oven dry, namely get VBT nitrate finished product.
Embodiment 2
Under 20 ℃ ± 2 ℃ temperature stir with 94 kilogram of 68% nitric acid dropping to 162 kilogram VBT in, control nitric acid dropping speed and heat-up rate, drip to finish and reached 50 ℃, do not need not heat outward.Along with temperature rising solution is clarified gradually.Finishing before measurement pH value in reaction, is 2 with nitric acid regulator solution pH.Continue to stir insulation 25 minutes after the solution clarification.Then keep 50 ℃ ± 5 ℃ temperature decompression dehydrations, vacuum keep is more than 500 mmhg.The reactant that dehydration is obtained stirs air-dry in 65 ℃ ± 5 ℃ scopes, continues at 80 ℃ of oven dry, gets VBT nitrate finished product.
Claims (3)
1. the preparation method of a VBT nitrate is characterized in that: in stirring at 10 ℃～25 ℃ temperature with nitric acid dropping in VBT, the mol ratio of VBT and nitric acid is 1: 1～1.1; Temperature of reaction is at 40 ℃～70 ℃, and solution is clarified gradually, is 1～2 with nitric acid regulator solution pH; Decompression dehydration after after solution is clarified, continuation is stirred and is incubated 15～30 minutes, the product after dehydration is air-dry in 50 ℃～70 ℃ stirrings, then gets VBT nitrate finished product after 75 ℃～85 ℃ dryings.
2. the preparation method of VBT nitrate according to claim 1 is characterized in that: in stirring at 20 ℃ ± 2 ℃ temperature with nitric acid dropping in VBT, the mol ratio of VBT and nitric acid is 1: 1; Temperature of reaction is 60 ℃ ± 5 ℃, and solution is clarified gradually, is 2 with nitric acid regulator solution pH, decompression dehydration after after solution is clarified, continuation is stirred and is incubated 20 minutes, and the product after dehydration is air-dry in 60 ℃ ± 5 ℃ stirrings, then gets VBT nitrate finished product after 80 ℃ of dryings.
3. the preparation method of VBT nitrate according to claim 1 and 2, it is characterized in that: the condition of above-mentioned decompression dehydration is: temperature is 50 ℃～65 ℃, and vacuum tightness is more than 500 mmhg.
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| CN 201010170346 CN101817759B (en) | 2010-05-12 | 2010-05-12 | Preparation method of L-carnitine nitrate |
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| CN 201010170346 CN101817759B (en) | 2010-05-12 | 2010-05-12 | Preparation method of L-carnitine nitrate |
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| CN101817759B true CN101817759B (en) | 2013-06-05 |
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| CN 201010170346 Expired - Fee Related CN101817759B (en) | 2010-05-12 | 2010-05-12 | Preparation method of L-carnitine nitrate |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102392061A (en) * | 2011-09-29 | 2012-03-28 | 重庆邮电大学 | Chemical-enzyme method for preparing D-basic amino acid hydrochloride |
| CN103664667A (en) * | 2013-12-16 | 2014-03-26 | 天津天成制药有限公司 | Preparation method for acetyl-L-carnitine nitrate |
| CN112079738A (en) * | 2020-09-18 | 2020-12-15 | 内蒙古精晶生物科技有限公司 | Preparation method of L-carnitine catecholate |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0150688A1 (en) * | 1983-12-28 | 1985-08-07 | Sigma-Tau Industrie Farmaceutiche Riunite S.p.A. | Salts of L-carnitine and alkanoyl L-carnitines and process for preparing same |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0150688A1 (en) * | 1983-12-28 | 1985-08-07 | Sigma-Tau Industrie Farmaceutiche Riunite S.p.A. | Salts of L-carnitine and alkanoyl L-carnitines and process for preparing same |
Non-Patent Citations (1)
| Title |
|---|
| 漆淑华.左旋肉碱盐酸盐的合成.《中国优秀博硕士论文全文数据库（硕士）工程科技Ⅰ辑》.2002,B016-158. * |
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