CN102850250A - Preparation method of proline nitrate - Google Patents
Preparation method of proline nitrate Download PDFInfo
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- CN102850250A CN102850250A CN 201110174944 CN201110174944A CN102850250A CN 102850250 A CN102850250 A CN 102850250A CN 201110174944 CN201110174944 CN 201110174944 CN 201110174944 A CN201110174944 A CN 201110174944A CN 102850250 A CN102850250 A CN 102850250A
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Abstract
A preparation method of proline nitrate includes dispersing proline with water, dropwise adding nitric acid, with the temperature controlled at 20 DEG C.-60 DEG C., for 30 minutes, holding temperature, stirring for 20 minutes, gradually clarifying the solution, vacuum-removing water at 50 DEG C. to 65 DEG C., cooling the obtained feed solution less than or equal to 10 DEG C. to precipitate solid, filtering and drying to give proline nitrate finished product. The liquid after filtration is used as the mother liquor in the production cycle. The produced proline nitrate product by the present invention has few impurities, good quality, and purity more than 99% without recrystallization. The present invention repeatedly utilizes the mother liquor, to improve the yield, reduce the cost, and save water resource. The invention has no byproduct in the production and almost does not produce waste. The invention is reasonable, simple, environmental-friendly, and suitable for industrial production.
Description
Technical field
The present invention relates to a kind of preparation method of amino acid salts, specifically the preparation method of proline(Pro) nitrate.
Background technology
Amino acid is the base substance that consists of the Animal nutrition desired protein.General people self generate or can obtain to satisfy by food each seed amino acid of somagenic need.But in the situation that special as human infantile period, in the situation that sick, injured or large amount of exercise is taken exercise, for growth needs, recover the balance of various metabolism in the body, strengthening immunity and sportsmen regain one's strength as early as possible, increase muscle strength, just need extra each seed amino acid that replenishes.
The proline(Pro) chemical name is: the pyrrolidone carboxylic acid.A kind of imino-acid of ring-type, proline(Pro) are a kind of non-essential amino acid, and health can be produced proline(Pro) by L-glutamic acid.The people of health diet unlikely lacks proline(Pro) generally speaking.Yet the people who suffers wound (particularly skin injury) such as serious burn, just may need to replenish this seed amino acid.Cartilage or collagen protein cause that the patient of pain also can obtain advantage from the proline(Pro) supplement
Proline(Pro) is that health is produced collagen protein and the required amino acid of cartilage.Its maintenance muscle and joint are flexible, and have the uv light exposure of minimizing and normal aging to cause skin sagging and wrinkling effect.
The effect of proline(Pro) also comprises help human body decomposing protein, is used for creating healthy cell in the body.It is to keeping skin and reticular tissue grow up healthy and sound extremely important (particularly tissue injury position).Proline(Pro) and Methionin all are that production oxyproline and hydroxylysine are needed, and this two seed amino acid makes up collagen protein.Collagen helps the cartilage that heals, and buffering is provided for joint and vertebra.For this reason, the proline(Pro) nutritious supplementary has the treatment osteoarthritis, soft tissue constant tension, and the effect of the disease such as chronic back pain.
Health also needs proline(Pro) to keep muscle tissue.The researchist has been noted that long-distance runner and other are engaged in long-time blue-collar people's proline(Pro) level and can reduce.Therefore, some sportsmen that are engaged in high pressure training may need this supplement to avoid muscle loss.
Because amino acid salts analogy amino acid easily is dissolved in the water, it is transformed into amino acid at last through effects such as oxydase in vivo, compare and take directly that amino acid is easier to be absorbed by health, take so amino acid is all made amidates usually, generally make the amino acid salts hydrochlorate more.Recently U.S. parties concerned research discovery, amino acid whose nitrate more is conducive to Amino Acid Absorption, therefore proline(Pro) is made into proline(Pro) nitrate and takes, and will more easily change into proline(Pro), is absorbed by health.Dosage can be less when it used, and oral absorption efficient can be higher.
Summary of the invention
The present invention provides a kind of preparation method of proline(Pro) nitrate for obtaining the systemic proline(Pro) nitrate of body more preferably.
The present invention is that the technical scheme that the technical problem that exists in the above-mentioned technology of solution is taked is:
The preparation method of a kind of proline(Pro) nitrate of the present invention is as follows: proline(Pro) with water-dispersion after, drip nitric acid, temperature is controlled at 20 ℃～60 ℃, dropwise in 30 minutes, continued insulated and stirred 20 minutes, solution is clarified gradually, vaccum dewatering under 50 ℃～65 ℃ conditions subsequently, feed liquid after dewatering is cooled to≤10 ℃, separate out solid, filter, after the drying proline(Pro) nitrate finished product.The liquid of separating out behind the solid recycles aborning as mother liquor.
The mol ratio of above-mentioned proline(Pro) and nitric acid is 1: 1～1.1.
The ratio of above-mentioned proline(Pro) and water is 1g: 2ml.
Advantage and positively effect that the present invention has are: the raw material that the present invention adopts is the proline(Pro) of food grade and the nitric acid of chemical reagent-grade, so the proline(Pro) 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.The present invention utilizes Recycling Mother Solution to use, and has improved yield, has reduced cost.Saved valuable water resources.Simultaneously the present invention is no coupling product aborning, produces hardly the three wastes.Preparation method's technique of the present invention is reasonable, simple, environmental protection, is fit to industrialized production.
Embodiment
Solubleness in the invention in the proline(Pro) water is less, need add a certain amount of water during reaction, and water is deionized purified water.Below the narration in just referred to as water.
The mol ratio of proline(Pro) and nitric acid should be 1: 1 among the present invention, but for proline(Pro) is reacted completely, nitric acid dosage should be more bigger than proline(Pro).Scope is between 1～1.1 mole.
Temperature of reaction of the present invention should be controlled at below 60 ℃, and the vaccum dewatering temperature is controlled at below 65 ℃.Otherwise can exert an adverse impact to product.
Liquid after the present invention will filter is recycled as mother liquor.Owing to filtering out the L-Phe nitrate that does not have in addition crystallization in the liquid after the crystallization, when it was used for next step production, the crystallization that produces can both be separated out more than 95%, has greatly improved actual recovery.
For further understanding summary of the invention of the present invention, Characteristic, hereby exemplify following examples:
Embodiment 1
Take by weighing proline(Pro) 23g(0.2 mole) put into reaction flask, after adding entry 46ml and stirring, while stir the nitric acid 20g(0.2 mole that drips 65% concentration), the control temperature is at 55 ℃, dropwised in 20 minutes, continued insulated and stirred 20 minutes, solution is clarified gradually.Be warming up to subsequently 60 ℃
,Vaccum dewatering, the feed liquid after dewatering is cooled to 5 ℃, separates out solid, gets proline(Pro) nitrate finished product after filtration, the drying.Liquid after the filtration recycles aborning as mother liquor.
Embodiment 2
Take by weighing proline(Pro) 23g(0.2 mole) put into reaction flask, after adding mother liquor 46ml stirs, while stir the nitric acid 20g(0.2 mole that drips 65% concentration), the control temperature is 40
℃, dropwised in 10 minutes, continued insulated and stirred 20 minutes, solution is clarified gradually.Be warming up to subsequently 55 ℃, vaccum dewatering, the feed liquid after dewatering is cooled to 10 ℃, separates out solid, gets proline(Pro) nitrate finished product after filtration, the drying.Liquid after the filtration recycles aborning as mother liquor.
Embodiment 3
Take by weighing proline(Pro) 23g(0.2 mole) put into reaction flask, after adding mother liquor 46ml stirs, while stir the nitric acid 20g(0.2 mole that drips 65% concentration), the control temperature is 25
℃, dropwised in 30 minutes, continued insulated and stirred 20 minutes, solution is clarified gradually.Be warming up to subsequently 50 ℃, vaccum dewatering, the feed liquid after dewatering is cooled to 0 ℃, separates out solid, gets proline(Pro) nitrate finished product after filtration, the drying.Liquid after the filtration recycles aborning as mother liquor.
Claims (3)
1. the preparation method of a proline(Pro) nitrate, it is characterized in that the preparation method is as follows: proline(Pro) with water-dispersion after, drip nitric acid, temperature is controlled at 20 ℃-60 ℃, dropwise in 30 minutes, continued insulated and stirred 20 minutes, solution is clarified gradually, subsequently vaccum dewatering under 50 ℃ of-65 ℃ of conditions, feed liquid after dewatering is cooled to≤and 10 ℃, separate out solid, get proline(Pro) nitrate finished product after filtration, the drying, the liquid after the filtration recycles aborning as mother liquor.
2. the preparation method of proline(Pro) nitrate according to claim 1, the mol ratio that it is characterized in that proline(Pro) and nitric acid is 1: 1～1.1.
3. the preparation method of proline(Pro) nitrate according to claim 1, the ratio that it is characterized in that proline(Pro) and water is 1g: 2ml.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110174944 CN102850250A (en) | 2011-06-27 | 2011-06-27 | Preparation method of proline nitrate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201110174944 CN102850250A (en) | 2011-06-27 | 2011-06-27 | Preparation method of proline nitrate |
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| CN102850250A true CN102850250A (en) | 2013-01-02 |
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| CN 201110174944 Pending CN102850250A (en) | 2011-06-27 | 2011-06-27 | Preparation method of proline nitrate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103664705A (en) * | 2013-12-13 | 2014-03-26 | 天津天成制药有限公司 | Citrulline nitrate synthesizing method |
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2011
- 2011-06-27 CN CN 201110174944 patent/CN102850250A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103664705A (en) * | 2013-12-13 | 2014-03-26 | 天津天成制药有限公司 | Citrulline nitrate synthesizing method |
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Application publication date: 20130102 |