CN101935300A - Preparation method of high-purity organic chelated chromium nicotinate - Google Patents
Preparation method of high-purity organic chelated chromium nicotinate Download PDFInfo
- Publication number
- 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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- CN
- China
- Prior art keywords
- nicotinic acid
- chromium
- preparation
- organic chelated
- mixture
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- HPCCGRCEBFBZQP-UHFFFAOYSA-N chromium;pyridine-3-carboxylic acid Chemical compound [Cr].OC(=O)C1=CC=CN=C1 HPCCGRCEBFBZQP-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229940038476 chelated chromium Drugs 0.000 title abstract 3
- PVNIIMVLHYAWGP-UHFFFAOYSA-N Niacin Chemical compound OC(=O)C1=CC=CN=C1 PVNIIMVLHYAWGP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 235000001968 nicotinic acid Nutrition 0.000 claims abstract description 19
- 239000011664 nicotinic acid Substances 0.000 claims abstract description 19
- 229960003512 nicotinic acid Drugs 0.000 claims abstract description 19
- 239000013078 crystal Substances 0.000 claims abstract description 12
- 239000000243 solution Substances 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 230000032683 aging Effects 0.000 claims abstract description 7
- 239000012266 salt solution Substances 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 8
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 claims description 8
- 239000012452 mother liquor Substances 0.000 claims description 7
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical class [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 claims description 5
- GRWVQDDAKZFPFI-UHFFFAOYSA-H chromium(III) sulfate Chemical compound [Cr+3].[Cr+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRWVQDDAKZFPFI-UHFFFAOYSA-H 0.000 claims description 5
- 229910021556 Chromium(III) chloride Inorganic materials 0.000 claims description 4
- 229960000359 chromic chloride Drugs 0.000 claims description 4
- QSWDMMVNRMROPK-UHFFFAOYSA-K chromium(3+) trichloride Chemical compound [Cl-].[Cl-].[Cl-].[Cr+3] QSWDMMVNRMROPK-UHFFFAOYSA-K 0.000 claims description 4
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 4
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 4
- 235000017550 sodium carbonate Nutrition 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 2
- 238000006555 catalytic reaction Methods 0.000 abstract description 5
- 239000000428 dust Substances 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract description 2
- 239000002912 waste gas Substances 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract 4
- 238000001914 filtration Methods 0.000 abstract 2
- 238000010923 batch production Methods 0.000 abstract 1
- 150000001844 chromium Chemical class 0.000 abstract 1
- 239000006184 cosolvent Substances 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 11
- 239000011651 chromium Substances 0.000 description 11
- 229910052804 chromium Inorganic materials 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 239000003960 organic solvent Substances 0.000 description 6
- 238000003483 aging Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 2
- 229940046374 chromium picolinate Drugs 0.000 description 2
- GJYSUGXFENSLOO-UHFFFAOYSA-N chromium;pyridine-2-carboxylic acid Chemical compound [Cr].OC(=O)C1=CC=CC=N1.OC(=O)C1=CC=CC=N1.OC(=O)C1=CC=CC=N1 GJYSUGXFENSLOO-UHFFFAOYSA-N 0.000 description 2
- 230000000536 complexating effect Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000003446 ligand Substances 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000002180 anti-stress Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 229960001399 clenbuterol hydrochloride Drugs 0.000 description 1
- OPXKTCUYRHXSBK-UHFFFAOYSA-N clenbuterol hydrochloride Chemical compound Cl.CC(C)(C)NCC(O)C1=CC(Cl)=C(N)C(Cl)=C1 OPXKTCUYRHXSBK-UHFFFAOYSA-N 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000003053 immunization Effects 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- SIOXPEMLGUPBBT-UHFFFAOYSA-N picolinic acid Chemical compound OC(=O)C1=CC=CC=N1 SIOXPEMLGUPBBT-UHFFFAOYSA-N 0.000 description 1
- 244000144977 poultry Species 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 239000003799 water insoluble solvent Substances 0.000 description 1
Landscapes
- Pyridine Compounds (AREA)
- 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 |
Applications Claiming Priority (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 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101935300A true CN101935300A (en) | 2011-01-05 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009100629012A Pending CN101935300A (en) | 2009-06-30 | 2009-06-30 | Preparation method of high-purity organic chelated chromium nicotinate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101935300A (en) |
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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| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20110105 |