CN101817759A - Preparation method of L-carnitine nitrate - Google Patents
Preparation method of L-carnitine nitrate Download PDFInfo
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- CN101817759A CN101817759A CN 201010170346 CN201010170346A CN101817759A CN 101817759 A CN101817759 A CN 101817759A CN 201010170346 CN201010170346 CN 201010170346 CN 201010170346 A CN201010170346 A CN 201010170346A CN 101817759 A CN101817759 A CN 101817759A
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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, specifically is the preparation method of the L-carnitine nitrate that a kind of quality is good, yield is high, cost is low.
Background technology
The L-carnitine (L-carnitine) claim L-carnitine again.Another name L-carnitine, 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.The L-carnitine extensively exists as alkali components in muscle, can extract from the meat of pig, calf, horse etc. usually.
Existing document shows, the L-carnitine for the growing of animal, breed, health is extremely important.It has the β-Yang Hua that promotes lipid acid, reduces the content of serum cholesterol and triglyceride level, improves important physiological function such as body tolerance.
The secretory volume of L-carnitine becomes with exercise intensity.When high pressure training, it can guarantee that body avoids the disadvantageous effect of hyperammonemia.Therefore it can add in the drinking-water, drinks for the sportsmen, makes the sportsmen when high pressure training, keeps each metabolic balance in the body, avoids health to come to harm.
The L-carnitine can help fat-reducing, though when using carnitine separately, may be helpless to the minimizing of fat, it can influence the metabolism of fat of body, speed and the loss speed of ratio that its consumption is lost greater than muscle, and make the go on a diet tolerance raising in stage of people.Being particularly suitable for people cooperates and to do aerobic exercise and come fat reducing.Effect is apparent in view.
Along with Developing of Animal Industry, synthetic convenient and safe, growth promoter efficiently is the focus of medicine and trophology research always.In feed, add high-copper, microbiotic, beta-stimulants and injection tethelin etc., have 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.The L-carnitine is because it is easy to use, can play under certain condition and improve sow reproductive performance, improve piglet survival ratio, reduce the thickness of backfat, improve the effect such as quality of meat and egg and come into one's own day by day, and also carry out corresponding research and utilization in medical and food service industry as a kind of novel fodder additives.
Experiment shows that the L-carnitine is a kind of essential nutrients, in the international nutrition academic conference that 1985 hold in Chicago, the L-carnitine is appointed as " multifunctional and nutritional product ".
The L-carnitine has been applied to 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 a food enrichment, can be applicable to aspects such as chewable tablet, drink liquid, capsule, milk powder and milky-drinks.
Because L-carnitine salt becomes the L-carnitine at last through conversions such as oxydase in vivo, is absorbed by health easily.So now the L-carnitine is all made L-carnitine salt and taken, products such as noted above L-carnitine-L-tartrate and L-carnitine hydrochloride are domestic all manufacturer production.The U.S. parties concerned discover that amino acid whose nitrate more helps the amino acid absorption in vivo recently, therefore the L-carnitine are made into the L-carnitine nitrate, with the easier L-carnitine that changes into, are absorbed by health.Dosage can be littler when therefore it used, and oral absorption efficient can be higher.But the producer that does not also have suitability for industrialized production L-carnitine nitrate product at present in the world.
Summary of the invention
The present invention is in order to solve the problem of L-carnitine nitrate large-scale production, and provide a kind of can suitability for industrialized production and yield height, the preparation method of the L-carnitine nitrate that product purity is high.
The technical scheme that the present invention takes is: a kind of preparation method of L-carnitine nitrate: in stirring under 10 ℃～25 ℃ temperature nitric acid is added drop-wise in the L-carnitine, the mol ratio of L-carnitine 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 continuation was stirred and is incubated 15～30 minutes after solution was clarified, the product after the dehydration is air-dry in 50 ℃～70 ℃ stirrings, gets L-carnitine nitrate finished product after 75 ℃ again～85 ℃ dryings.
A kind of preparation method of L-carnitine nitrate: in stirring under 20 ℃ ± 2 ℃ temperature nitric acid is added drop-wise in the L-carnitine, the mol ratio of L-carnitine 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 solution clarification back is stirred and is incubated 20 minutes, the product after the dehydration is air-dry in 60 ℃ ± 5 ℃ stirrings, gets L-carnitine nitrate finished product after 80 ℃ of dryings again.
The condition of decompression dehydration is in the above-mentioned preparation process: 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 L-carnitine and nitric acid to react the reaction conditions gentleness under normal pressure.The present invention adopts the high-quality food grade L-carnitine and the nitric acid of chemical reagent-grade, so the L-carnitine nitrate product impurity of producing is few, quality is good, just reach more than 99% without recrystallization purity, both guaranteed quality, save operation and production time again, 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 L-carnitine of food grade and the nitric acid of chemical reagent-grade to react the reaction conditions gentleness under normal pressure.The mol ratio of L-carnitine and nitric acid is 1: 1, but for the L-carnitine is reacted completely, the add-on of nitric acid is more bigger than L-carnitine.The concentration of nitric acid that the present invention adopts is 65～68%.Because the concentration of nitric acid difference, so add-on has certain variation, but and the ratio of 1 mole of L-carnitine all between 1 to 1.1 mole.
The solubleness of L-carnitine of the present invention in water is big, and the water in the nitric acid just can be molten entirely with the L-carnitine, therefore need not add water.But the reaction of L-carnitine and nitric acid is thermopositive reaction, and violent for fear of reaction, it is too fast to heat up, the untimely decomposition that causes of dispelling the heat, and temperature must be low when beginning to react, between 10 ℃ to 25 ℃.Generally maintain 20 ℃ ± 2 ℃, and the speed of control nitric acid adding, the method that drips taked.Because therefore the low temperature effect speed of response is dripped at nitric acid and is finished back raising temperature of reaction.General temperature is preferably in 60 ℃ ± 5 ℃ below 70 ℃.But also can when just beginning to drip nitric acid, control low temperature, control rate of addition and temperature subsequently, utilize the temperature of the heat reacting by heating solution of reaction generation, fast reaction speed.Temperature of reaction can not surpass 70 ℃, otherwise the L-carnitine can be damaged, and influences 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 L-carnitine nitrate of the present invention is, and pH should be 2.Generally finishing before measurement pH in reaction, if acidity less than 2, drips nitric acid, is 2 with nitric acid control pH value of solution.Because the mol ratio of nitric acid is slightly larger than the L-carnitine when producing, so if pH allows, can not influence quality product between 2 and 1.
The solubleness of L-carnitine nitrate in reaction soln is big among the present invention, and it all is the crystallisate and the water of L-carnitine nitrate that reaction finishes in the container of back, can't separate, and therefore adopts the decompression method dehydration.Decompression method is an industry common technology.The vacuum tightness of decompression dehydration is more than 500 mmhg, and temperature is 50 ℃～65 ℃.Because dehydration back product is thick, can't further remove moisture with the drying method, so that the reactant after will dewatering carries out is air-dry, air-dry method also is an industry common technology, in 50 ℃～70 ℃ scopes, stir incessantly when air-dry,, take away moisture to accelerate air flowing.
The present invention to the exsiccant method without limits, every suitable L-carnitine nitrate exsiccant method can be used, as methods such as moisture eliminator, spray method dryings.The exsiccant temperature is 75 ℃～85 ℃, and temperature is low excessively, and product can conglomeration.Temperature surpasses 85 ℃, and the L-carnitine nitrate can decompose, and quality is affected.Present embodiment adopts 80 ℃ of dryings.
For further understanding summary of the invention of the present invention, characteristics and effect, enumerate following examples now, be described in detail as follows:
Embodiment 1
Under 20 ℃ ± 2 ℃ temperature, while stirring 94 kilograms in 68% nitric acid is added drop-wise in 162 kilograms of L-carnitines, drips complete postheating 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.Insulation 20 minutes is continued to stir in solution clarification back.Keep 60 ℃ ± 5 ℃ temperature decompression dehydrations then, vacuum tightness remains on more than 500 mmhg.The reactant that dehydration obtains is air-dry in 55 ℃ ± 5 ℃ stirrings, again in 80 ℃ of oven dry, promptly get L-carnitine nitrate finished product.
Embodiment 2
Stir down 20 ℃ ± 2 ℃ temperature 94 kilogram of 68% nitric acid is added drop-wise in 162 kilograms of L-carnitines, control nitric acid rate of addition and heat-up rate drip to finish and have reached 50 ℃, do not heat outside not needing.Along with temperature rising solution is clarified gradually.Finishing before measurement pH value in reaction, is 2 with nitric acid regulator solution pH.Insulation 25 minutes is continued to stir in solution clarification back.Keep 50 ℃ ± 5 ℃ temperature decompression dehydrations then, vacuum tightness remains on more than 500 mmhg.The reactant that dehydration is obtained stirs air-dry in 65 ℃ ± 5 ℃ scopes, continues at 80 ℃ of oven dry, L-carnitine nitrate finished product.
Claims (3)
1. the preparation method of a L-carnitine nitrate is characterized in that: in stirring under 10 ℃～25 ℃ temperature nitric acid is added drop-wise in the L-carnitine, the mol ratio of L-carnitine 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 continuation was stirred and is incubated 15～30 minutes after solution was clarified, the product after the dehydration is air-dry in 50 ℃～70 ℃ stirrings, gets L-carnitine nitrate finished product after 75 ℃ again～85 ℃ dryings.
2. the preparation method of L-carnitine nitrate according to claim 1 is characterized in that: in stirring under 20 ℃ ± 2 ℃ temperature nitric acid is added drop-wise in the L-carnitine, the mol ratio of L-carnitine 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 continuation was stirred and is incubated 20 minutes after solution was clarified, and the product after the dehydration is air-dry in 60 ℃ ± 5 ℃ stirrings, gets L-carnitine nitrate finished product after 80 ℃ of dryings again.
3. the preparation method of L-carnitine nitrate according to claim 1 and 2 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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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
2010
- 2010-05-12 CN CN 201010170346 patent/CN101817759B/en not_active Expired - Fee Related
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 |
|---|
| 《中国优秀博硕士论文全文数据库（硕士）工程科技Ⅰ辑》 20020615 漆淑华 左旋肉碱盐酸盐的合成 B016-158 1-3 , * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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