CN101935300A - Preparation method of high-purity organic chelated chromium nicotinate - Google Patents
Preparation method of high-purity organic chelated chromium nicotinate Download PDFInfo
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- CN101935300A CN101935300A CN2009100629012A CN200910062901A CN101935300A CN 101935300 A CN101935300 A CN 101935300A CN 2009100629012 A CN2009100629012 A CN 2009100629012A CN 200910062901 A CN200910062901 A CN 200910062901A CN 101935300 A CN101935300 A CN 101935300A
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- nicotinic acid
- chromium
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a preparation method of high-purity organic chelated chromium nicotinate, which comprises the following steps of: firstly, adding nicotinic acid into water, stirring the mixture uniformly; slowly adding a cosolvent into solution; when the nicotinic acid is completely dissolved, adding soluble trivalence inorganic chromium salt solution into the solution to perform a catalytic reaction so as to separate a chromium nicotinate crystal out of the mixture; standing the mixture, aging the mixture and then performing centrifugal filtration; and collecting and drying the crystal after the filtration to obtain the high-purity organic chelated chromium nicotinate. The preparation method is performed at normal temperature and normal pressure, a closed device is used, no waste gas, waste liquid or dust is discharged, no pollution and noise are generated by the preparation method, and the preparation method has the advantages of simple preparation process, less equipment investment, easy operation, short batch production cycle and high product purity.
Description
(1) technical field: the present invention relates to a kind of preparation method of fodder additives, specifically is the preparation method of the organic chelated nicotinic acid chromium of high purity that is applied to raise, adds in the feed of poultry breeding industry and culture fishery.
(2) prior art: nicotinic acid chromium be a kind of have improve the animal anti-stress ability, improve lean ratio, improve carcass quality, noresidue, raising animal reproduction performance and improve the novel fodder additive of immunizing power; It is the desirable substitute products that the world and China have prohibited use " clenbuterol hydrochloride "; The relevant in recent years nicotinic acid chromium of China is as the existing more report of the use-testing of fodder additives, the organic chromium of effect and import such as yeast chromium, chromium picolinate are equally matched, but yeast chromium is absorption chromium, chromium combines with zymic and not to be the chemical combination attitude, unstable, and the content of chromium changes with condition, so unstable properties; Chromium picolinate, because pyridine carboxylic acid itself is toxic, so product itself has certain toxicity, and the price height.Past, domestic only had a small amount of nicotinic acid chromium of minority scientific research institution small-scale production, and can be for the nicotinic acid chromium production technique of suitability for industrialized production owing to be subject to the problem of Technology aspect, and through update search, not seeing has definite report.
Existing disclosed production technique is to add organic solvent aborning, can not react at normal temperatures, major cause is because nicotinic acid is water insoluble, must or add organic solvent by heating could dissolve, otherwise be inhomogeneous reaction, and product is again water insoluble and organic solvent, easily causes reaction not exclusively and shortcoming such as product purity is low; Heating or with an organic solvent exists also that technology is cumbersome, equipment is complicated, it is big to drop into, operation is than complexity and security problems.
(3) summary of the invention: it is simple that purpose of the present invention just provides a kind of industrialized producing technology that makes, low equipment investment, and easy handling, batch with short production cycle, product purity height, the preparation method of the organic chelated nicotinic acid chromium of high purity that cost is lower.
The present invention includes following step:
A. nicotinic acid is added in its weight 8-12 water doubly, stirs evenly, slowly add nicotinic acid weight 0.4-0.5 solubility promoter doubly again, stir evenly to nicotinic acid and dissolve fully;
B. in above-mentioned solution, slowly add nicotinic acid weight 0.5-1 solubility trivalent inorganic chromate salt solution doubly, make and separate out the nicotinic acid chromium crystal;
C. leave standstill, ageing centrifuging after 24 hours is collected and is filtered the back crystal, and washing is dried promptly, and mother liquor can be recycled again.
Described solubility promoter is selected a kind of in caustic soda, soda ash or the sodium bicarbonate for use.
Described solubility trivalent inorganic chromate salt is a kind of in chromium trichloride, chromium sulphate or the chromium nitrate.
Nicotinic acid chromium is with solubility inorganic chromium (Cr
3+) salt and nicotinic acid is raw material, under certain conditions, be prepared from through processing steps such as dissolving, catalysis, ageing, crystallization, oven dry; Production technique is simple in order to reach, low equipment investment, easy handling, batch with short production cycle, good product quality, purpose that cost is low, changing the organic solvent in the existing technology into water is solvent, under normal temperature, normal pressure, react, being about to nicotinic acid makes it soluble in water with suitable solubility promoter, this is to realize under the normal temperature and pressure with water being the committed step of reaction system, solubility promoter is selected caustic soda or soda ash or sodium bicarbonate etc. for use, be easy to get, cheaply, nontoxic residue-free; Select solubility trivalent inorganic chromate salt (chromium trichloride for use, chromium sulphate or chromium nitrate etc.) as catalyzer, initiator, reaction is carried out soon, under normal temperature, normal pressure in building-up process, part is slightly excessive, make the whole complexings of inorganic chromium, guarantee the zero release of chromium element, contain the mother liquor of excess ligand and do not discharge after centrifugal, recycle, both reduce the raw material input, reduced cost, accomplished not sewage effluent again, thereby reached the present invention's purpose.
The present invention has following characteristics:
(1) this preparation method carries out under the normal temperature and pressure, has both reduced energy consumption, avoids again supplying with polluting in the Energy processes, and the production unit input is economized, and is easy and simple to handle; (2) will have the organic solvent (ethanol) that uses in the synthesis process now, and all change water solvent into, and reduce and pollute, cost is low; (3) in building-up process, part is slightly excessive, make the whole complexings of inorganic chromium, guarantee that chromium does not have plain zero release, contain the mother liquor of excess ligand and do not discharge after centrifugal, recycle, both reduced the raw material input, reduced cost, accomplish not sewage effluent again; (4) present method is used dead front type equipment, does not have any waste gas, waste liquid or dust and discharges pollution-free and noise; (5) every batch of product yield of producing meets industry standard all more than 92%.
(4) embodiment:
A. 100g nicotinic acid is added in the water of 800ml, stirs evenly, slowly add 50g soda ash to solution nicotinic acid again and dissolve fully, and the color no change;
B. slowly add 50g chromium trichloride solution while stirring and to above-mentioned solution, carry out catalyzed reaction, make and separate out the nicotinic acid chromium crystal;
C. leave standstill, ageing centrifuging after 24 hours is collected and is filtered the back crystal, and 80-105 ℃ was dried by the fire 5 hours down, that is, mother liquor can be recycled again.
Embodiment 2
A. 100g nicotinic acid is added in the water of 1200ml, stirs evenly, slowly add 40g caustic soda to solution nicotinic acid again and dissolve fully, and the color no change;
B. slowly add the 100g chromium sulfate solution while stirring and to above-mentioned solution, carry out catalyzed reaction, make and separate out the nicotinic acid chromium crystal;
C. leave standstill, ageing centrifuging after 24 hours is collected and is filtered the back crystal, and 80-105 ℃ was dried by the fire 5 hours down, that is, mother liquor can be recycled again.
Embodiment 3
A. 100g nicotinic acid is added in the water of 1000ml, stirs evenly, slowly add 45g sodium bicarbonate to solution nicotinic acid again and dissolve fully, and the color no change;
B. slowly add the 80g chromium sulfate solution while stirring and to above-mentioned solution, carry out catalyzed reaction, make and separate out the chromium nitrate crystal;
C. leave standstill, ageing centrifuging after 24 hours is collected and is filtered the back crystal, and 80-105 ℃ was dried by the fire 5 hours down, that is, mother liquor can be recycled again.
Claims (3)
1. the preparation method of the organic chelated nicotinic acid chromium of high purity is characterized in that comprising the steps:
A. nicotinic acid is added in its weight 8-12 water doubly, stirs evenly, slowly add nicotinic acid weight 0.4-0.5 solubility promoter doubly again, stir evenly to nicotinic acid and dissolve fully;
B. in above-mentioned solution, slowly add nicotinic acid weight 0.5-1 solubility trivalent inorganic chromate salt solution doubly, make and separate out the nicotinic acid chromium crystal;
C. leave standstill, ageing centrifuging after 24 hours is collected and is filtered the back crystal, and washing is dried promptly, and mother liquor can be recycled again.
2. the preparation method of the organic chelated nicotinic acid chromium of high purity according to claim 1 is characterized in that: described solubility promoter is selected a kind of in caustic soda, soda ash or the sodium bicarbonate for use.
3. according to the preparation method of the organic chelated nicotinic acid chromium of high purity described in claim 1 or 2, it is characterized in that: described solubility trivalent inorganic chromate salt is a kind of in chromium trichloride, chromium sulphate or the chromium nitrate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100629012A CN101935300A (en) | 2009-06-30 | 2009-06-30 | Preparation method of high-purity organic chelated chromium nicotinate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009100629012A CN101935300A (en) | 2009-06-30 | 2009-06-30 | Preparation method of high-purity organic chelated chromium nicotinate |
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| CN101935300A true CN101935300A (en) | 2011-01-05 |
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| CN2009100629012A Pending CN101935300A (en) | 2009-06-30 | 2009-06-30 | Preparation method of high-purity organic chelated chromium nicotinate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103833826A (en) * | 2013-07-08 | 2014-06-04 | 重庆大学 | Method for preparing niacin-glutathione-trivalent chromium ion chelate |
| CN115053937A (en) * | 2022-06-20 | 2022-09-16 | 浙江惠嘉生物科技股份有限公司 | Preparation method of chromium nicotinate nano dispersion preparation |
-
2009
- 2009-06-30 CN CN2009100629012A patent/CN101935300A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103833826A (en) * | 2013-07-08 | 2014-06-04 | 重庆大学 | Method for preparing niacin-glutathione-trivalent chromium ion chelate |
| CN103833826B (en) * | 2013-07-08 | 2016-02-24 | 重庆大学 | Prepare the method for nicotinic acid-gsh-trivalent chromic ion inner complex |
| CN115053937A (en) * | 2022-06-20 | 2022-09-16 | 浙江惠嘉生物科技股份有限公司 | Preparation method of chromium nicotinate nano dispersion preparation |
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Open date: 20110105 |