CN112225659A - Purification method of chromium propionate - Google Patents
Purification method of chromium propionate Download PDFInfo
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- CN112225659A CN112225659A CN202011224388.5A CN202011224388A CN112225659A CN 112225659 A CN112225659 A CN 112225659A CN 202011224388 A CN202011224388 A CN 202011224388A CN 112225659 A CN112225659 A CN 112225659A
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- chromium propionate
- chromium
- solvent
- propionate
- crystal
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- PYXSPTLIBJZHQW-UHFFFAOYSA-K chromium(3+);propanoate Chemical compound [Cr+3].CCC([O-])=O.CCC([O-])=O.CCC([O-])=O PYXSPTLIBJZHQW-UHFFFAOYSA-K 0.000 title claims abstract description 64
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000000746 purification Methods 0.000 title abstract description 8
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000002904 solvent Substances 0.000 claims abstract description 25
- 239000013078 crystal Substances 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 17
- 235000019441 ethanol Nutrition 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 238000001914 filtration Methods 0.000 claims abstract description 13
- 239000012046 mixed solvent Substances 0.000 claims abstract description 9
- 238000004064 recycling Methods 0.000 claims abstract description 6
- 150000001298 alcohols Chemical class 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 35
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 238000001704 evaporation Methods 0.000 claims description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 238000011084 recovery Methods 0.000 claims description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 abstract description 40
- 235000019260 propionic acid Nutrition 0.000 abstract description 20
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 abstract description 20
- 239000012535 impurity Substances 0.000 abstract description 5
- 238000009826 distribution Methods 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 15
- 239000011651 chromium Substances 0.000 description 14
- 229910052804 chromium Inorganic materials 0.000 description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 239000007787 solid Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- NOESYZHRGYRDHS-UHFFFAOYSA-N insulin Chemical compound N1C(=O)C(NC(=O)C(CCC(N)=O)NC(=O)C(CCC(O)=O)NC(=O)C(C(C)C)NC(=O)C(NC(=O)CN)C(C)CC)CSSCC(C(NC(CO)C(=O)NC(CC(C)C)C(=O)NC(CC=2C=CC(O)=CC=2)C(=O)NC(CCC(N)=O)C(=O)NC(CC(C)C)C(=O)NC(CCC(O)=O)C(=O)NC(CC(N)=O)C(=O)NC(CC=2C=CC(O)=CC=2)C(=O)NC(CSSCC(NC(=O)C(C(C)C)NC(=O)C(CC(C)C)NC(=O)C(CC=2C=CC(O)=CC=2)NC(=O)C(CC(C)C)NC(=O)C(C)NC(=O)C(CCC(O)=O)NC(=O)C(C(C)C)NC(=O)C(CC(C)C)NC(=O)C(CC=2NC=NC=2)NC(=O)C(CO)NC(=O)CNC2=O)C(=O)NCC(=O)NC(CCC(O)=O)C(=O)NC(CCCNC(N)=N)C(=O)NCC(=O)NC(CC=3C=CC=CC=3)C(=O)NC(CC=3C=CC=CC=3)C(=O)NC(CC=3C=CC(O)=CC=3)C(=O)NC(C(C)O)C(=O)N3C(CCC3)C(=O)NC(CCCCN)C(=O)NC(C)C(O)=O)C(=O)NC(CC(N)=O)C(O)=O)=O)NC(=O)C(C(C)CC)NC(=O)C(CO)NC(=O)C(C(C)O)NC(=O)C1CSSCC2NC(=O)C(CC(C)C)NC(=O)C(NC(=O)C(CCC(N)=O)NC(=O)C(CC(N)=O)NC(=O)C(NC(=O)C(N)CC=1C=CC=CC=1)C(C)C)CC1=CN=CN1 NOESYZHRGYRDHS-UHFFFAOYSA-N 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 229940046374 chromium picolinate Drugs 0.000 description 3
- 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 description 3
- 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 3
- 239000012043 crude product Substances 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 102000004877 Insulin Human genes 0.000 description 2
- 108090001061 Insulin Proteins 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 2
- 241000282898 Sus scrofa Species 0.000 description 2
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 229940125396 insulin Drugs 0.000 description 2
- 238000001694 spray drying Methods 0.000 description 2
- 239000011573 trace mineral Substances 0.000 description 2
- 235000013619 trace mineral Nutrition 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 241000699802 Cricetulus griseus Species 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 241000736262 Microbiota Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000003674 animal food additive Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 235000012000 cholesterol Nutrition 0.000 description 1
- 150000001844 chromium Chemical class 0.000 description 1
- 150000001845 chromium compounds Chemical class 0.000 description 1
- 238000009142 chromium supplementation Methods 0.000 description 1
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 230000004153 glucose metabolism Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000002611 ovarian Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- ZQBVUULQVWCGDQ-UHFFFAOYSA-N propan-1-ol;propan-2-ol Chemical compound CCCO.CC(C)O ZQBVUULQVWCGDQ-UHFFFAOYSA-N 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the technical field of chromium propionate production, in particular to a purification method of chromium propionate, which comprises the following steps: s1, adding the crude chromium propionate into a mixed solvent of ethyl acetate and alcohols, and filtering; and S2, stirring, heating, drying, and recycling the solvent to obtain the chromium propionate crystal. The purity of the chromium propionate crystal obtained by the method is more than 99%, the content of impurity propionic acid is less than 0.5%, and the obtained crystal has uniform particle size distribution, good fluidity and low viscosity and is convenient for subsequent feed processing.
Description
Technical Field
The invention relates to the technical field of chromium propionate production, in particular to a purification method of chromium propionate.
Background
Chromium compounds have been used in the printing and tanning industry for a long time and are considered to be toxic and harmful elements, even carcinogens. Curran found until 1954 that the capacity of rat liver to synthesize cholesterol and fatty acids was enhanced by chromium supplementation, suggesting that chromium may be an essential trace element for animals. In 1959, Schwarz and Mertz isolated chromium-containing Glucose Tolerance Factor (GTF), demonstrating that chromium is an element essential for insulin to function during glucose metabolism, and also that chromium is an essential substance for insulin to promote fat synthesis. At present, chromium is considered one of the trace elements essential to humans and animals.
Research proves that the absorption rate of the organic chromium is higher than that of the inorganic chromium, the former is 10-25 percent, and the latter is 1-3 percent or lower. The FDA in the united states of america in 1 month of 1996 first allowed the use of chromium picolinate as a chromium source to be added to a daily ration for swine at an addition level of 200 μ g/kg, and thus most of the current research is focused on chromium picolinate and makes it the major source of chromium products on the market. However, since 1995, Stearns et al first reported that chromium picolinate could cause ovarian cell aberration in Chinese hamster, its safety was of concern and question. Microbiota chromium (TM) is the only organic chromium first approved by the U.S. FDA in 8 months in 2000 that can be used throughout a pig ration and is a feed additive product developed and produced autonomously by the U.S. institutional company. The main component of the feed is chromium propionate, which is a safe and efficient addition form of chromium in the feed and has higher biological value.
At present, the following two methods are mainly used for synthesizing chromium propionate: firstly, hexavalent chromium is used as a chromium source, and is reduced and then reacts with propionic acid to prepare the chromium-containing material (for example, patent CN 86100694A, EP 0897267 and RU 2694234); secondly, the compound is prepared by complexing propionic acid and soluble trivalent chromium salt in an aqueous solution (for example, patent CN 102351680A); for the purification of chromium propionate, in the prior art, ethanol is usually added after drying to fully dissolve the chromium propionate, filtering is performed, the filtrate is concentrated to be thick paste, the thick paste is placed in a vacuum drying oven for drying (such as patent CN 102351680a) or n-propanol is added, heating and stirring are performed until the thick paste is dissolved, filtering is performed, the filtrate is evaporated and concentrated to be paste, and centrifugal spray drying (such as CN 108147961a) is performed.
In order to solve the problems, the applicant unexpectedly finds that the solubility of chromium propionate in ethyl acetate is very low in the process of researching the properties of chromium propionate, and improves the purification process on the basis of the very low solubility, so that the purity of the obtained chromium propionate crystal is over 99 percent, the content of impurity propionic acid is less than 0.5 percent, and the obtained crystal has uniform particle size distribution, good fluidity and low viscosity and is convenient for subsequent feed processing.
Disclosure of Invention
The invention aims to solve the technical problem of providing a purification method of chromium propionate, wherein the purity of the obtained chromium propionate crystal is more than 99 percent, the content of impurity propionic acid is less than 0.5 percent, and the obtained crystal has uniform particle size distribution, good fluidity and low viscosity and is convenient for subsequent feed processing.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for purifying chromium propionate, comprising the steps of:
s1, adding the crude chromium propionate into a mixed solvent of ethyl acetate and alcohols, and filtering;
and S2, stirring, heating, drying, and recycling the solvent to obtain the chromium propionate crystal.
Preferably, the temperature-rising drying solvent recovery in step S2 adopts a staged mode:
s01, stirring for the first time, heating, evaporating and recovering the solvent 1;
and S02, continuously heating to the specified temperature, keeping the temperature constant, drying, and recycling the solvent 2 to obtain the chromium propionate crystal.
Preferably, the mixed solvent in S1 is a mixed solvent of ethyl acetate and an alcohol solvent.
Preferably, the alcoholic solvent is methanol, ethanol, n-propanol, isopropanol or n-butanol, preferably ethanol.
Preferably, the ratio of ethyl acetate to ethanol is 10:1 to 5:1, preferably 9: 1.
preferably, the temperature of the first temperature rise in the step S01 is 65 to 70 ℃.
Preferably, the temperature of the second temperature rise in the step S02 is 115-120 ℃.
The invention has the beneficial effects that:
1. by improving the solvent, the purity of the chromium propionate crystal is over 99 percent and the content of impurity propionic acid is less than 1 percent after one-time evaporation and drying; 2. according to the invention, ethyl acetate is used as a solvent, the solubility of chromium propionate in ethyl acetate is low, and the chromium propionate is separated out under the premise that the propionic acid can be dissolved during evaporation and separation, so that the propionic acid is prevented from being wrapped in the chromium propionate, and is convenient to further remove, and centrifugal spraying with high use cost is not required; 3. by adding ethanol as an auxiliary solvent, the dissolution of chromium propionate can be promoted, the chromium propionate is dispersed in ethyl acetate, the removal of propionic acid impurities is further promoted, the purity is further improved, the chromium propionate is distilled out by azeotropy with part of ethyl acetate in the evaporation process, and the wrapping of the chromium propionate on propionic acid is further reduced; 4. according to the purification process, the obtained crystals are high in purity, low in viscosity and good in fluidity, industrial production is facilitated, and the problem that the grinding equipment is blocked by the product in the grinding process is solved well.
Drawings
FIG. 1 is a diagram showing experimental results of dissolution of chromium propionate by different solvents according to the present invention;
Detailed Description
In order to facilitate understanding of those skilled in the art, the present invention will be further described with reference to the following examples and drawings, which are not intended to limit the present invention.
Example 1
Preparing a crude product: according to the method disclosed by the patent CN 102351680A, 5L of 40 mass percent chromium sulfate solution is measured, 16L of NaOH solution with the mass concentration of 5% is slowly added, stirring is carried out while adding, filtering is carried out, washing is carried out for 2-3 times by deionized water, drying is carried out to obtain gray green solid, 500g of the product in the last step is taken, added into a reaction kettle, 720mL of propionic acid is added, and stirring and heating are carried out for 1 hour at the temperature of 100 ℃. Filtering, removing insoluble substances, and concentrating to obtain thick paste to obtain crude chromium propionate, wherein the content of chromium propionate is 89% and the content of propionic acid is 6%.
Example 2
50g of the crude chromium propionate obtained in example 1 was added to a mixed solvent of 450mL of ethyl acetate and 50mL of ethanol, and filtered to obtain a clear solution. Stirring and heating, heating to 65-70 ℃ at a heating rate of 10 ℃/h, then keeping constant, distilling for about 2h, recovering the solvent for recycling, separating out a small amount of chromium propionate solid from the chromium propionate solution, heating to 115-120 ℃ at a speed of 60 ℃/h, drying, and recovering the solvent to obtain the chromium propionate crystal.
The purity of the obtained chromium propionate in the crystal is 99.5 percent, the content of the propionic acid is less than 0.3 percent, the granularity of the crystal is uniformly distributed, and the fluidity is good.
Example 3
50g of the crude chromium propionate obtained in example 1 was added to a mixed solvent of 450mL of ethyl acetate and 50mL of ethanol, and filtered to obtain a clear solution. Stirring and heating, heating to 120 ℃ at the heating rate of 60 ℃/h, drying, and recovering the solvent to obtain the chromium propionate crystal.
The purity of the obtained chromium propionate in the crystal is 98.9 percent, the content of the propionic acid is 0.7 percent, the granularity of the crystal is uniformly distributed, and the fluidity is good.
Example 4
Effect of different solvents on chromium propionate preparation:
50g of the crude chromium propionate obtained in the example are added to 500mL of solvent and filtered to give a clear solution. Stirring, heating to 120 ℃ at the speed of 60 ℃/h, drying, and recovering the solvent to obtain the chromium propionate crystal.
Example 5
Dissolution experiments of chromium propionate solids with different solvents
5g of the crude chromium propionate obtained in example 1 was taken, 50mL of organic solvent was added, and the mixture was dissolved by shaking for 30min, wherein the phenomenon of partial dissolution experiment is shown in FIG. 1, and the results are as follows:
| group of | Solvent(s) | In the dissolved state |
| 1 | Water (W) | Completely dissolve |
| 2 | Methanol | Completely dissolve |
| 3 | Ethanol | Completely dissolve |
| 4 | N-propanol | Completely dissolve |
| 5 | Isopropanol (I-propanol) | Completely dissolve |
| 6 | N-butanol | Completely dissolve |
| 7 | Ethyl acetate | Insolubilizing a large amount of solids |
| 8 | Acetone (II) | Insolubilizing a large amount of solids |
Comparative example 1
Preparing a crude product: according to the method disclosed by the patent CN 102351680A, 500mL of 40% chromium sulfate solution is measured, 1600mL of NaOH solution with the mass concentration not higher than 10% is slowly added while stirring, filtering is carried out, deionized water is used for washing for 2-3 times, drying is carried out to obtain a gray-green solid, 50.0g of the product in the last step is taken and added into a reaction kettle, 72mL of propionic acid is added, and stirring and heating are carried out for 1h at the temperature of 100 ℃. Filtering, removing insoluble substances, and concentrating to obtain thick paste to obtain crude chromium propionate, wherein the content of chromium propionate is 89% and the content of propionic acid is 6%.
Adding 50mL of absolute ethyl alcohol into the crude chromium propionate to fully dissolve the crude chromium propionate, filtering, concentrating the filtrate into thick paste, and drying in a vacuum drying oven at 50 ℃ for 8 hours to obtain green solid, wherein the purity of the obtained chromium propionate in the crystal is 97.0%, the content of propionic acid is 2.5%, the crystal is slightly viscous, and the fluidity is general.
Comparative example 2
Preparing a crude product: according to the method disclosed by the patent CN 102351680A, 500mL of 40% chromium sulfate solution is measured, 1600mL of NaOH solution with the mass concentration not higher than 10% is slowly added while stirring, filtering is carried out, deionized water is used for washing for 2-3 times, drying is carried out to obtain a gray-green solid, 50.0g of the product in the last step is taken and added into a reaction kettle, 72mL of propionic acid is added, and stirring and heating are carried out for 1h at the temperature of 100 ℃. Filtering, removing insoluble substances, and concentrating to obtain thick paste to obtain crude chromium propionate, wherein the content of chromium propionate is 89% and the content of propionic acid is 6%.
Adding 50mL of n-propanol into the crude chromium propionate, heating, stirring until the n-propanol is dissolved, filtering, evaporating and concentrating the filtrate to be slurry, and carrying out centrifugal spray drying to obtain the chromium propionate. The purity of the obtained chromium propionate in the crystal is 96.5%, the content of the propionic acid is 2.8%, the crystal is more uniform and slightly viscous, and the fluidity is general.
The results of comparing examples 2 and 3 with comparative examples 1 and 2 clearly show that the experimental results of the examples of the present invention are clearly superior to those of the comparative examples.
Finally, it should be noted that the above-mentioned description is only a preferred embodiment of the present invention, and those skilled in the art can make various similar representations without departing from the spirit and scope of the present invention.
Claims (7)
1. A method for purifying chromium propionate is characterized by comprising the following steps: the method comprises the following steps:
s1, adding the crude chromium propionate into a mixed solvent of ethyl acetate and alcohols, and filtering;
and S2, stirring, heating, drying, and recycling the solvent to obtain the chromium propionate crystal.
2. The method for purifying chromium propionate as claimed in claim 1, wherein: in the step S2, the temperature-raising drying solvent recovery adopts a segmented mode:
s01, stirring for the first time, heating, evaporating and recovering the solvent 1;
and S02, continuously heating to the specified temperature, keeping the temperature constant, drying, and recycling the solvent 2 to obtain the chromium propionate crystal.
3. The method for purifying chromium propionate as claimed in claim 1, wherein: the mixed solvent in the S1 is a mixed solvent of ethyl acetate and an alcohol solvent.
4. The method of claim 3, wherein the purifying step comprises: the alcohol solvent is methanol, ethanol, n-propanol, isopropanol or n-butanol, preferably ethanol.
5. The method of claim 3, wherein the purifying step comprises: the ratio of ethyl acetate to ethanol is 10:1-5:1, preferably 9: 1.
6. the method for purifying chromium propionate as claimed in claim 2, wherein: the temperature of the first temperature rise in the step S01 is 65 to 70 ℃.
7. The method for purifying chromium propionate as claimed in claim 2, wherein: the temperature of the second temperature rise in the step S02 is 115-120 ℃.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4528175A (en) * | 1982-11-18 | 1985-07-09 | Allied Corporation | Production of chromium (III) compounds |
| CN102351680A (en) * | 2011-11-04 | 2012-02-15 | 广西大学 | Synthesis technique of chromium propionate |
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2020
- 2020-11-05 CN CN202011224388.5A patent/CN112225659B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4528175A (en) * | 1982-11-18 | 1985-07-09 | Allied Corporation | Production of chromium (III) compounds |
| CN102351680A (en) * | 2011-11-04 | 2012-02-15 | 广西大学 | Synthesis technique of chromium propionate |
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