CN102850241A - Preparation method of guanidine acetic acid nitrate - Google Patents
Preparation method of guanidine acetic acid nitrate Download PDFInfo
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- CN102850241A CN102850241A CN 201110174943 CN201110174943A CN102850241A CN 102850241 A CN102850241 A CN 102850241A CN 201110174943 CN201110174943 CN 201110174943 CN 201110174943 A CN201110174943 A CN 201110174943A CN 102850241 A CN102850241 A CN 102850241A
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- acetic acid
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- acid
- guanidoacetic
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Abstract
A preparation method of guanidine acetic acid nitrate includes stirring guanidine acetic acid and water, dropwise adding nitric acid, with the temperature controlled at 20 DEG C. to 60 DEG C., for 10 minutes, holding temperature, stirring for 20 minutes, and cooling the reaction mixture, to precipitate guanidine acetic acid nitrate white solid. The raw materials used in the preparation method of guanidine acetic acid nitrate of the present invention is guanidine acetic acid of food grade and nitric acid of chemical reagent grade, so that the produced guanidine acetic acid nitrate product has less impurities, good quality, and purity of more than 99% without recrystallization, so as to ensure quality, save process and production time, and improve production efficiency. The invention utilizes the recycled mother liquor to improve yield, with the product yield reaching more than 98%, and reduces the cost. The present invention is low-cost, simple in preparation process and non-polluting, and is free of byproduct and suitable for industrial production.
Description
Technical field
The present invention relates to the preparation method of a seed amino acid nitrate, specifically a kind of preparation method of guanidoacetic acid 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, in order to 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.
Guanidoacetic acid is energy booster, improves the body vigor.Particularly can prolong the time that produces fatigue behind high physical strength, the long-time movable crowd's clothes, improve exercise intensity.Act on the same with creatine but without the side effect of creatine, its dose is also little than creatine.
Because solubleness is more much larger than amino acid in the amidates water, it is transformed into amino acid at last through effects such as oxydase in vivo, compares to take directly that amino acid is easier to be absorbed by health, and the amount of absorption is also large.So amino acid is usually all made amidates and is taken, and generally makes the amino acid salts hydrochlorate more.Recently U.S. parties concerned research discovery, amino acid whose nitrate more is conducive to amino acid absorption in vivo, therefore guanidoacetic acid is made into guanidoacetic acid nitrate, will more easily change into guanidoacetic acid in vivo, is absorbed by health.Dosage can be less when therefore it used, and oral absorption efficient can be higher.
Summary of the invention
The present invention provides a kind of preparation method of guanidoacetic acid nitrate in order to make health more effectively absorb guanidoacetic acid.
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 guanidoacetic acid nitrate of the present invention is as follows: after guanidoacetic acid and water are stirred, drip nitric acid, the control temperature is at 20 ℃～60 ℃, drip after 10 minutes and finish, continued insulated and stirred 20 minutes, the cooling reaction solution is separated out guanidoacetic acid nitrate white solid, after filtration, dry guanidoacetic acid nitrate finished product, the liquid after the filtration continues on for next step production as mother liquor.
The mol ratio of guanidoacetic acid and nitric acid is 1: 1～1.1.The ratio of guanidoacetic acid and water is 1g: 2ml.
Cooling temperature is≤10 ℃.
Advantage and positively effect that the present invention has are: the raw material that the preparation method of guanidoacetic acid nitrate of the present invention adopts is the guanidoacetic acid acid of food grade and the nitric acid of chemical reagent-grade, so the guanidoacetic acid 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 the Recycling Mother Solution Reusability, has improved yield, and the yield of product is reached more than 98%, has reduced cost.Production cost of the present invention is low, and yield is high, and preparation process is simple, and is pollution-free, and no coupling product is fit to large-scale industrial production.
Embodiment
Solubleness among the present invention in the guanidoacetic acid water is less, need add a certain amount of water during reaction, and water is deionized water, to guarantee the quality of product.Below just directly be called water in the narration.The ratio of guanidoacetic acid and water is 1g: 2ml.
The mol ratio of guanidoacetic acid and nitric acid should be 1: 1 among the present invention, but for guanidoacetic acid is reacted completely, nitric acid dosage should be more bigger than guanidoacetic acid.
Liquid after the present invention will filter replaces water to recycle as mother liquor.When it was used for next step production, the crystallization that produces can both be separated out more than 98%, has greatly improved actual recovery, has saved simultaneously valuable water resources.Quality for fear of masterbatch becomes in recycling process greatly, should the product of producing be gone out totally when discharging as far as possible.
For further understanding summary of the invention of the present invention, Characteristic, hereby exemplify following examples:
Embodiment 1
Take by weighing guanidoacetic acid 11.7g(0.1 mole) put into reaction flask, add entry 23.4ml, dispersed with stirring is even.Dropping concentration is 65% nitric acid 10g(0.1 mole), temperature is controlled at 25 ℃.Dropwise after 10 minutes, continue to keep temperature to stir 20 minutes, solution is clarified gradually.Then be cooled to 5 ℃, separate out the white solid of guanidoacetic acid nitrate, after filtration, drying, get guanidoacetic acid nitrate finished product.Liquid after the filtration recycles aborning as mother liquor.
Embodiment 2
Take by weighing guanidoacetic acid 11.7g(0.1 mole) put into reaction flask, add mother liquor 23.4ml, dispersed with stirring is even.Dropping concentration is 65% nitric acid 10g(0.1 mole) control temperature at 55 ℃.Dropwise after 10 minutes, continue to keep temperature to stir 20 minutes, solution is clarified gradually.Then be cooled to 10 ℃, separate out the white solid of guanidoacetic acid nitrate.After filtration, drying, get guanidoacetic acid nitrate finished product.Liquid after the filtration recycles aborning as mother liquor.
Embodiment 3
Take by weighing guanidoacetic acid 11.7g(0.1 mole) put into reaction flask, add mother liquor 23.4ml, dispersed with stirring is even.Dropping concentration is 65% nitric acid 10g(0.1 mole) control temperature at 40 ℃.Dropwise after 10 minutes, continue to keep temperature to stir 20 minutes, solution is clarified gradually.Then be cooled to 0 ℃, separate out the white solid of guanidoacetic acid nitrate.After filtration, drying, get guanidoacetic acid nitrate finished product.Liquid after the filtration recycles aborning as mother liquor.
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Claims (3)
1. the preparation method of a guanidoacetic acid nitrate, it is characterized in that the preparation method is as follows: after guanidoacetic acid and water are stirred, drip nitric acid, temperature is controlled at 20 ℃～60 ℃, drips after 10 minutes and finishes, and continues insulated and stirred 20 minutes, the cooling reaction solution, separate out guanidoacetic acid nitrate white solid, after filtration, dry guanidoacetic acid nitrate finished product, the liquid after the filtration recycles aborning as mother liquor.
2. the preparation method of guanidoacetic acid nitrate according to claim 1, the mol ratio that it is characterized in that guanidoacetic acid and nitric acid is 1 1～1.1, the ratio of guanidoacetic acid and water is 1g 2ml.
3. the preparation method of guanidoacetic acid nitrate according to claim 1 is characterized in that cooling temperature is≤10 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110174943 CN102850241A (en) | 2011-06-27 | 2011-06-27 | Preparation method of guanidine acetic acid nitrate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201110174943 CN102850241A (en) | 2011-06-27 | 2011-06-27 | Preparation method of guanidine acetic acid nitrate |
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| CN102850241A true CN102850241A (en) | 2013-01-02 |
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| CN 201110174943 Pending CN102850241A (en) | 2011-06-27 | 2011-06-27 | Preparation method of guanidine acetic acid nitrate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112358421A (en) * | 2020-11-09 | 2021-02-12 | 湖南天成生化科技有限公司 | Preparation method of environment-friendly low-cost creatine nitrate |
| CN114751845A (en) * | 2022-06-13 | 2022-07-15 | 北京君德同创生物技术股份有限公司 | Method for synthesizing soluble glycocyamine complex |
-
2011
- 2011-06-27 CN CN 201110174943 patent/CN102850241A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112358421A (en) * | 2020-11-09 | 2021-02-12 | 湖南天成生化科技有限公司 | Preparation method of environment-friendly low-cost creatine nitrate |
| CN112358421B (en) * | 2020-11-09 | 2022-05-24 | 湖南天成生化科技有限公司 | Preparation method of environment-friendly low-cost creatine nitrate |
| CN114751845A (en) * | 2022-06-13 | 2022-07-15 | 北京君德同创生物技术股份有限公司 | Method for synthesizing soluble glycocyamine complex |
| CN114751845B (en) * | 2022-06-13 | 2022-09-20 | 北京君德同创生物技术股份有限公司 | Method for synthesizing soluble glycocyamine complex |
| WO2023241117A1 (en) * | 2022-06-13 | 2023-12-21 | 北京君德同创生物技术股份有限公司 | Synthesis method for easily-soluble guanidinoacetic acid complex |
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Application publication date: 20130102 |