CN110054559A - A kind of production method of chromium propionate - Google Patents
A kind of production method of chromium propionate Download PDFInfo
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- CN110054559A CN110054559A CN201910299775.6A CN201910299775A CN110054559A CN 110054559 A CN110054559 A CN 110054559A CN 201910299775 A CN201910299775 A CN 201910299775A CN 110054559 A CN110054559 A CN 110054559A
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- chromium
- carbonate
- propionate
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
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- Chemical Treatment Of Metals (AREA)
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Abstract
The invention discloses a kind of production method of chromium propionate, step includes that water and chromium carbonate or/and basic chromic carbonate are added in the reaction kettle with reflux unit, opens ultrasound and involves stirring to pulp, heat temperature raising；Propionic acid is instilled, temperature is controlled；It is completely dissolved subsequent continuation of insurance temperature curing to chromium carbonate or/and basic chromic carbonate, is finally dried to obtain chromium propionate.The technology of the present invention guarantees that propionate is not lost in product chromium propionate using reflux condensate device is installed additional；Promote the dissolution of quickening chromium carbonate or/and basic chromic carbonate using ultrasonic wave, shortens the reaction time；Reaction will not generate hypertoxic Cr VI, and react no coupling product, guarantee that product quality, propionic acid chromium content are greater than 99%, meet all technical requirement.
Description
Technical field
The present invention relates to organic chemical synthesis more particularly to a kind of production technologies of chromium propionate.
Background technique
Chromium is a kind of microelement necessary to animal, animal shown as when lacking chromium cholesterol or blood glucose rise, growth retardation,
Immunity degradation, fertility reduction and lost of life etc..Inorganic chromium is more toxic, to animal and toxic effect per capita.?
In animal husbandry as promoting animal growth all be Organic Chromium, mainly have chromium propionate, nicotinate chromium, chromium picolinate, chromium methionine,
Yeast chromium etc..Organic Chromium is easily absorbed because its is highly-safe, and immune, improvement carcass quality stress, be enhanced by having to alleviate to animal
It the effects of with production performance is improved, is with a wide range of applications on animal husbandry.
One of the regulatory factor of chromium propionate as glucose metabolism is more and more paid attention to, and being listed at present must
The mineral needed add nutrient.Chromium propionate can be improved the production performance of animal, strengthen immunity, improve reproductive performance and improve ketone
Body quality etc. is expected to reduce antibiotics feed addictive dosage, improves the safety of animal product.Meanwhile slow down environment,
The function of the brought breeding performonce fo animals negative effect aspect of the stress factors such as nutrition, physiology also becomes more and more important, and chromium propionate is also
The current broiler chicken industry only one of FDA go through using new microelement, therefore, chromium propionate will be sent out in husbandry sector
Shoot increasingly important role.
Currently, chromium propionate is mainly the following production method: (1) Chinese patent 201810041065.9, Chinese patent
201310194807.9, United States Patent (USP) 86100694, the general principles of these three methods are all made of sexavalence chromic salts chromic anhybride or again
Sodium chromate is reduced into the chromium propionate of trivalent chromium with reducing agent, and this method is maximum to be not thorough the disadvantage is that restoring, and leads to final products
Containing micro hypertoxic Cr VI, Animal nutrition health is influenced, ecological environment is endangered.(2) though Chinese patent 201110345027.0
It so uses and synthesizes chromium hydroxide with chromic salts such as chromium sulfate or chromium chlorides, then the propionic acid synthesized chromium of chromium hydroxide is dissolved with propionic acid,
The chromium hydroxide of this method synthesis jelly, is difficult to separate in the inorganic salts inside chromium hydroxide, and the hydrogen-oxygen of synthesis
Change chromium and be insoluble in propionic acid, cause product content relatively low, and contains undissolved inorganic chromium in product.Meanwhile appealing two kinds of productions
The method of chromium propionate is all made of common reaction kettle, does not install reflux condensate device additional, due to propionic acid heat highly volatile, will lead to
Propionic acid radical content in final products chromium propionate is relatively low, reduces product grade.
Summary of the invention
The main object of the present invention is in view of the above-mentioned deficiencies in the prior art, to provide a kind of producer of chromium propionate
Method can shorten the reaction time, reduce propionate loss, and reaction will not generate hypertoxic Cr VI, no coupling product, guarantee product matter
Amount, propionic acid chromium content are greater than 99%, and product has preferable grade, meets all technical requirement.
In order to achieve the above-mentioned object of the invention, The technical solution adopted by the invention is as follows:
A kind of production method of chromium propionate, comprising the following steps:
1) water and chromium carbonate or/and basic chromic carbonate are added in reaction kettle, open ultrasound and involve stirring to pulp, heats
Heating；
2) uniform speed slow instills propionic acid, controls 40 DEG C~120 DEG C of temperature；
3) it is completely dissolved subsequent continuation of insurance temperature curing 0.5h~36h to chromium carbonate or/and basic chromic carbonate, is drying to obtain propionic acid
Chromium.
Water is reaction dissolvent in the step 1), and heating temperature is to being not less than 40 DEG C.Chromium carbonate or/and basic chromic carbonate are molten
Not soluble in water in acid or alkali, propionic acid belongs to weak acid, and chromium carbonate or/and basic chromic carbonate are dissolved in propionic acid reaction slowly, solution rate
Slowly, but ultrasonic wave, which is added, can promote solution rate, accelerate reaction rate.
Vigorous reaction can occur very much fastly, can produce a large amount of gas for exothermic heat of reaction, instillation after instillation propionic acid in the step 2)
Bubble and heat.
40 DEG C~120 DEG C of temperature of control is to be higher than 120 DEG C of energy consumption height since lower than 40 DEG C reactions of temperature are slow, reacted
In violent while dangerous.
Reaction kettle in the step 1) is the reaction kettle equipped with reflux condensate device, the power density of the ultrasonic wave
For 1~3W/L.
Condensing to 25 DEG C or less propionates can not be lost completely.
The molar ratio of the chromium and propionic acid in chromium carbonate or/and basic chromic carbonate in the step 2) is 1:6~8.
In laboratory environment, the General reactions scale of construction in 100L or so, at this time propionic acid instill speed control 100L/h~
150L/h。
Curing temperature is 20 DEG C~80 DEG C in the step 3).
Curing is a kind of degree of reaction, increases maturation stage first is that can further promote to react, second is that making extremely
Micro nonreactive chromium carbonate or/and basic chromic carbonate and impurity can be deposited in curing pot bottom, will not influence the product of chromium propionate
Matter.
The molar ratio of water and chromium carbonate in the step 1) or/and the chromium in basic chromic carbonate is not less than 50:1.
Water is the theoretical water that reaction carries out herein, and reducing agent solution can bring a part of water, reaction product into the process
A part of water can be also generated, because being reflux, these water are all inside propionic acid chromium solution, so water and chromium carbonate or/and alkali formula
The molar ratio of chromium in chromium carbonate can maintain reaction to carry out substantially for 50, but the chromium propionate solution concentration prepared is higher,
More water can generally be added convenient for reacting balance progress.
Preferably, the molar ratio of the water in step 1) and chromium carbonate or/and the chromium in basic chromic carbonate is 100:1.
Chromium when technology of the present invention is used for industrial mass production, in water and chromium carbonate or/and basic chromic carbonate
Molar ratio control be 100:1, under this ratio, reacting balance works well, while not will increase facility load, does not need more
The equipment of big carrying capacity, the sexual valence of production are relatively high.
Compared with prior art, the beneficial effects of the present invention are:
The technology of the present invention guarantees that propionate is not lost in product chromium propionate using reflux condensate device is installed additional；Using ultrasound
Wave promotes to accelerate the dissolution of chromium carbonate or/and basic chromic carbonate, shortens the reaction time；Reaction will not generate hypertoxic Cr VI, and
No coupling product is reacted, guarantees that product quality, propionic acid chromium content are greater than 99%, meet all technical requirement.
Specific embodiment
Foregoing invention content of the invention is described in further detail With reference to embodiment.But it should not incite somebody to action
This range for being interpreted as the above-mentioned theme of the present invention is only limitted to following embodiments.The above-mentioned technical idea situation of the present invention is not being departed from
Under, according to ordinary skill knowledge and customary means, various replacements and change are made, the scope of the present invention should all be included in
It is interior.
Embodiment 1
60L water is added in the reaction kettle equipped with reflux condensate device, adds the basic chromic carbonate of chromium content 10.5mol
With chromium carbonate mixture, opens stirring and ultrasonic unit, ultrasonic power density 2W/L is slowly added to 1.5mol propionic acid,
40 DEG C of heating temperature, it is completely dissolved subsequent continuation of insurance temperature curing 15h to basic chromic carbonate and chromium carbonate mixture, temperature 60 C is done
Dry chromium propionate finished product to obtain the final product, finished product content 99.32%.
Embodiment 2
12.6L water is added in the reaction kettle equipped with reflux condensate device, adds the chromium carbonate of chromium content 7mol, opens
Stirring and ultrasonic unit, ultrasonic power density 1W/L, are slowly added to 1.1mol propionic acid, and 100 DEG C of heating temperature, to carbonic acid
Chromium is completely dissolved subsequent continuation of insurance temperature curing 10h, and temperature 70 C is spray-dried up to chromium propionate finished product, finished product content 99.58%.
In this embodiment, 12.6L water is added, chromium is 7mol in chromium carbonate, and the molar ratio of water and chromium is 100:1.
Embodiment 3
50L water is added in the reaction kettle equipped with reflux condensate device, adds the basic chromic carbonate of chromium content 7.2mol,
Stirring and ultrasonic unit, ultrasonic power density 2.5W/L are opened, is slowly added to 1.2mol propionic acid, 105 DEG C of heating temperature,
It is completely dissolved subsequent continuation of insurance temperature curing 20h to basic chromic carbonate, temperature 45 C is spray-dried up to chromium propionate finished product, and finished product contains
Amount 99.19%.
Embodiment 4
17.1L water is added in the reaction kettle equipped with reflux condensate device, adds the chromium carbonate of chromium content 9.5mol, opens
Opening stirring and ultrasonic unit, ultrasonic power density 1.2W/L is slowly added to 1.3mol propionic acid, and 120 DEG C of heating temperature, to
Chromium carbonate is completely dissolved subsequent continuation of insurance temperature curing 36h, 20 DEG C of temperature, is spray-dried up to chromium propionate finished product, finished product content
99.72%.
In this embodiment, 17.1L water is added, chromium is 9.5mol in chromium carbonate, and the molar ratio of water and chromium is 100:1.
Embodiment 5
100L water is added in the reaction kettle equipped with reflux condensate device, adds the basic chromic carbonate of chromium content 8mol,
Stirring and ultrasonic unit, ultrasonic power density 3W/L are opened, is slowly added to 1mol propionic acid, 115 DEG C of heating temperature, to alkali
Formula chromium carbonate is completely dissolved subsequent continuation of insurance temperature curing 15h, 65 DEG C of temperature, is spray-dried up to chromium propionate finished product, finished product content
99.41%.
Embodiment 6
50L water is added in the reaction kettle equipped with reflux condensate device, adds the basic chromic carbonate of chromium content 7.5mol
With chromium carbonate mixture, opens stirring and ultrasonic unit, ultrasonic power density 2.6W/L is slowly added to 1mol propionic acid,
60 DEG C of heating temperature, it is completely dissolved subsequent continuation of insurance temperature curing 0.5h to basic chromic carbonate and chromium carbonate mixture, 80 DEG C of temperature, is done
Dry chromium propionate finished product to obtain the final product, finished product content 99.40%.
Embodiment 7
5.85L water is added in the reaction kettle equipped with reflux condensate device, adds the chromium carbonate of chromium content 6.5mol, opens
Opening stirring and ultrasonic unit, ultrasonic power density 1.5W/L is slowly added to 1mol propionic acid, and 95 DEG C of heating temperature, to carbon
Sour chromium is completely dissolved subsequent continuation of insurance temperature curing 5h, 75 DEG C of temperature, is spray-dried up to chromium propionate finished product, finished product content 99.23%.
In this embodiment, 5.85L water is added, chromium is 6.5mol in chromium carbonate, and the molar ratio of water and chromium is 50:1.
Embodiment 8
162L water is added in the reaction kettle equipped with reflux condensate device, adds the basic chromic carbonate of chromium content 90mol
With chromium carbonate mixture, opens stirring and ultrasonic unit, ultrasonic power density 1W/L are slowly added to 15mol propionic acid, add
55 DEG C of hot temperature is completely dissolved subsequent continuation of insurance temperature curing 32h to basic chromic carbonate and chromium carbonate mixture, 30 DEG C of temperature, dry
Up to chromium propionate finished product, finished product content 99.20%.
In this embodiment, 162L water is added, chromium is 90mol in basic chromic carbonate and chromium carbonate mixture, and water and chromium rub
You are than being 100:1.
Embodiment 9
64.8L water is added in the reaction kettle equipped with reflux condensate device, adds the basic carbonate of chromium content 72mol
Chromium opens stirring and ultrasonic unit, ultrasonic power density 2W/L, is slowly added to 10mol propionic acid, and 40 DEG C of heating temperature,
It is completely dissolved subsequent continuation of insurance temperature curing 1h to basic chromic carbonate, 80 DEG C of temperature, is spray-dried up to chromium propionate finished product, finished product content
99.02%.
In this embodiment, 64.8L water is added, chromium is 72mol in basic chromic carbonate, and the molar ratio of water and chromic acid chromium is 50:
1。
Embodiment 10
21.6L water is added in the reaction kettle equipped with reflux condensate device, adds the basic chromic carbonate of chromium content 12mol
With chromium carbonate mixture, opens stirring and ultrasonic unit, ultrasonic power density 2.5W/L are slowly added to 1.5mol third
Acid, is completely dissolved subsequent continuation of insurance temperature curing 36h to basic chromic carbonate and chromium carbonate mixture by 80 DEG C of heating temperature, and 30 DEG C of temperature,
It is drying to obtain chromium propionate finished product, finished product content 99.78%.
In this embodiment, 21.6L water is added, chromium is 12mol in basic chromic carbonate and chromium carbonate mixture, and water and chromium rub
You are than being 100:1.
In summary: the technology of the present invention guarantees that propionate is not lost in product chromium propionate using reflux condensate device is installed additional；
Promote the dissolution of quickening chromium carbonate or/and basic chromic carbonate using ultrasonic wave, shortens the reaction time；Reaction will not generate severe toxicity six
Valence chromium, and no coupling product is reacted, guarantee that product quality, propionic acid chromium content are greater than 99%, meet all technical requirement.
Claims (6)
1. a kind of production method of chromium propionate, it is characterised in that the following steps are included:
1) water and chromium carbonate or/and basic chromic carbonate are added in reaction kettle, open ultrasound and involve stirring to pulp, heating rises
Temperature；
2) uniform speed slow instills propionic acid, controls 40 DEG C~120 DEG C of temperature；
3) it is completely dissolved subsequent continuation of insurance temperature curing 0.5h~36h to chromium carbonate or/and basic chromic carbonate, is drying to obtain chromium propionate.
2. the production method of chromium propionate according to claim 1, it is characterised in that: the reaction kettle in the step 1) is dress
There is the reaction kettle of reflux condensate device, the power density of the ultrasonic wave is 1~3W/L.
3. the production method of chromium propionate according to claim 1, it is characterised in that: chromium carbonate in the step 2) or/
Molar ratio with chromium and propionic acid in basic chromic carbonate is 1:6~8.
4. the production method of chromium propionate according to claim 1, it is characterised in that: curing temperature is 20 in the step 3)
DEG C~80 DEG C.
5. according to the production method of the described in any item chromium propionates of claim 2~4, it is characterised in that: in the step 1)
The molar ratio of water and chromium carbonate or/and the chromium in basic chromic carbonate is not less than 50:1.
6. the production method of chromium propionate according to claim 5, it is characterised in that: water in step 1) and chromium carbonate or/
Molar ratio with the chromium in basic chromic carbonate is 100:1.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112209821A (en) * | 2020-11-05 | 2021-01-12 | 建明(中国)科技有限公司 | Preparation method of chromium propionate |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351680A (en) * | 2011-11-04 | 2012-02-15 | 广西大学 | Synthesis technique of chromium propionate |
| CN103288622A (en) * | 2013-05-21 | 2013-09-11 | 天津市化学试剂研究所 | Preparation method of chromium propionate |
| US20170066707A1 (en) * | 2015-09-04 | 2017-03-09 | Nutech Biosciences, Inc. | Process for Forming Chromium Propionate as an Agricultural Feed Additive |
| CN107814697A (en) * | 2016-09-14 | 2018-03-20 | 天津市化学试剂研究所有限公司 | A kind of preparation method of n Propanoic acid chromium |
-
2019
- 2019-04-15 CN CN201910299775.6A patent/CN110054559A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351680A (en) * | 2011-11-04 | 2012-02-15 | 广西大学 | Synthesis technique of chromium propionate |
| CN103288622A (en) * | 2013-05-21 | 2013-09-11 | 天津市化学试剂研究所 | Preparation method of chromium propionate |
| US20170066707A1 (en) * | 2015-09-04 | 2017-03-09 | Nutech Biosciences, Inc. | Process for Forming Chromium Propionate as an Agricultural Feed Additive |
| CN107814697A (en) * | 2016-09-14 | 2018-03-20 | 天津市化学试剂研究所有限公司 | A kind of preparation method of n Propanoic acid chromium |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112209821A (en) * | 2020-11-05 | 2021-01-12 | 建明(中国)科技有限公司 | Preparation method of chromium propionate |
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