CN116751121A - Preparation method of high-purity potassium acetate - Google Patents
Preparation method of high-purity potassium acetate Download PDFInfo
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- CN116751121A CN116751121A CN202310360308.6A CN202310360308A CN116751121A CN 116751121 A CN116751121 A CN 116751121A CN 202310360308 A CN202310360308 A CN 202310360308A CN 116751121 A CN116751121 A CN 116751121A
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- potassium acetate
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- diethyl ether
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- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 title claims abstract description 126
- 235000011056 potassium acetate Nutrition 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 90
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 54
- 238000002156 mixing Methods 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 238000005406 washing Methods 0.000 claims abstract description 12
- 239000012047 saturated solution Substances 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 239000012046 mixed solvent Substances 0.000 claims abstract description 10
- 238000004537 pulping Methods 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 239000006228 supernatant Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000005352 clarification Methods 0.000 claims abstract description 6
- 238000005086 pumping Methods 0.000 claims abstract description 6
- 235000019441 ethanol Nutrition 0.000 claims description 15
- 239000007787 solid Substances 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000010009 beating Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims 1
- 229910001415 sodium ion Inorganic materials 0.000 abstract description 16
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 abstract description 13
- 239000000126 substance Substances 0.000 abstract description 6
- 239000000243 solution Substances 0.000 description 17
- 230000000052 comparative effect Effects 0.000 description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 7
- 239000001632 sodium acetate Substances 0.000 description 7
- 235000017281 sodium acetate Nutrition 0.000 description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- 238000000605 extraction Methods 0.000 description 5
- 238000000746 purification Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 229960000583 acetic acid Drugs 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ITRJWOMZKQRYTA-RFZYENFJSA-N Cortisone acetate Chemical compound C1CC2=CC(=O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@@](C(=O)COC(=O)C)(O)[C@@]1(C)CC2=O ITRJWOMZKQRYTA-RFZYENFJSA-N 0.000 description 1
- 241000228143 Penicillium Species 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- LRJOMUJRLNCICJ-JZYPGELDSA-N Prednisolone acetate Chemical compound C1CC2=CC(=O)C=C[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@@](C(=O)COC(=O)C)(O)[C@@]1(C)C[C@@H]2O LRJOMUJRLNCICJ-JZYPGELDSA-N 0.000 description 1
- FPVRUILUEYSIMD-RPRRAYFGSA-N [(8s,9r,10s,11s,13s,14s,16r,17r)-9-fluoro-11-hydroxy-17-(2-hydroxyacetyl)-10,13,16-trimethyl-3-oxo-6,7,8,11,12,14,15,16-octahydrocyclopenta[a]phenanthren-17-yl] acetate Chemical compound C1CC2=CC(=O)C=C[C@]2(C)[C@]2(F)[C@@H]1[C@@H]1C[C@@H](C)[C@@](C(=O)CO)(OC(C)=O)[C@@]1(C)C[C@@H]2O FPVRUILUEYSIMD-RPRRAYFGSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229960002537 betamethasone Drugs 0.000 description 1
- UREBDLICKHMUKA-DVTGEIKXSA-N betamethasone Chemical compound C1CC2=CC(=O)C=C[C@]2(C)[C@]2(F)[C@@H]1[C@@H]1C[C@H](C)[C@@](C(=O)CO)(O)[C@@]1(C)C[C@@H]2O UREBDLICKHMUKA-DVTGEIKXSA-N 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229960003290 cortisone acetate Drugs 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000002274 desiccant Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 229960003657 dexamethasone acetate Drugs 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002934 diuretic Substances 0.000 description 1
- 229940030606 diuretics Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- DQYBDCGIPTYXML-UHFFFAOYSA-N ethoxyethane;hydrate Chemical compound O.CCOCC DQYBDCGIPTYXML-UHFFFAOYSA-N 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 229960001347 fluocinolone acetonide Drugs 0.000 description 1
- FEBLZLNTKCEFIT-VSXGLTOVSA-N fluocinolone acetonide Chemical compound C1([C@@H](F)C2)=CC(=O)C=C[C@]1(C)[C@]1(F)[C@@H]2[C@@H]2C[C@H]3OC(C)(C)O[C@@]3(C(=O)CO)[C@@]2(C)C[C@@H]1O FEBLZLNTKCEFIT-VSXGLTOVSA-N 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000001963 growth medium Substances 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 229960002800 prednisolone acetate Drugs 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 235000019643 salty taste Nutrition 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
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
- C07C51/48—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
-
- 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
-
- 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
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a preparation method of high-purity potassium acetate, which comprises the following steps: (1) Dissolving potassium acetate with the purity of at least 85wt% in water to prepare a potassium acetate saturated solution; (2) Preparing an extractant, wherein the extractant is a mixed solvent of anhydrous diethyl ether and an alcohol solvent, and the volume ratio of the anhydrous diethyl ether to the alcohol solvent is 4-5:1; (3) Pumping the potassium acetate saturated solution and the extractant from two ends of a T-shaped micro-channel continuous flow reactor, mixing in a convection mode, flowing out from an outlet after mixing, entering a clarification device, standing, separating liquid, and obtaining a supernatant; heating and concentrating the supernatant, and pulping; finally, washing with anhydrous diethyl ether to obtain high-purity potassium acetate; the method can improve the purity of the chemical pure potassium acetate to more than 99 weight percent, reduce the sodium ion content to less than 0.02 weight percent, and improve the purity of the analytical pure potassium acetate to more than 99 weight percent and reduce the sodium ion content to less than 0.01 weight percent.
Description
Technical Field
The invention relates to the technical field of inorganic salts, in particular to a preparation method of high-purity potassium acetate.
Background
Potassium acetate of the formula CH 3 COOK is white powder, is easy to absorb moisture, has salty taste, low toxicity and combustibility, and is an organic matter. The solution is alkaline to litmus and not alkaline to phenolphthalein. Conventionally used as an analytical reagent to adjust pH; can also be used as a desiccant to produce transparent glass. And also used as a penicillium culture medium in the pharmaceutical industry, potassium acetate is used as a raw material in the production of cortisone acetate, prednisolone acetate, dexamethasone acetate, betamethasone, fluocinolone acetonide and the like. The industry can use them as buffers, diuretics, softeners for textiles and paper, catalysts, etc. The method is used for preparing potassium supplementing pharmaceutical preparations in the pharmaceutical industry, wherein the requirement of medicinal high-purity reagents is higher, and imported reagents are mainly used in China at present.
The conventional production of potassium acetate is carried out by reacting acetic acid with potassium hydroxide or acetic acid with potassium carbonate, purifying system, decolorizing with active carbon, filtering, evaporating and drying to obtain potassium acetate. The method for crystallizing the product by simple reaction is operated in a pipeline, and has high labor cost. CN201510768782.8 discloses a method for preparing potassium acetate by dissolving potassium hydroxide in absolute ethanol under heating condition, adding a proper amount of medicinal glacial acetic acid dropwise, stopping heating after the dropwise addition, sealing, standing overnight at room temperature, separating out flaky crystals, filtering, washing the filtered filter cake with ethanol, drying the flaky crystals in an oven to obtain the finished product of medicinal potassium acetate, wherein at present, the purification and refining of potassium acetate mainly comprises recrystallization, but the impurity content of sodium acetate is mainly doped in the recrystallized potassium acetate, and is not well controlled. The quality standards of the potassium acetate products currently on the market (HG 3-1097-77) are shown in Table 1 below:
TABLE 1 Potassium acetate product quality Standard
Therefore, the impurity ions in the potassium acetate sold at present are mainly sodium ions, wherein the detection and purification raw material contains part of sodium acetate, and how to further remove sodium ions to obtain high-purity potassium acetate, and even medical grade potassium acetate is the technical problem to be solved by the invention.
Disclosure of Invention
In order to solve the technical problems, a preparation method of high-purity potassium acetate is provided. The purity of the chemical pure potassium acetate can be improved to more than 99 weight percent, the sodium ion content is reduced to less than 0.02 weight percent after the purification by the method, the purity of the analysis pure potassium acetate can be improved to more than 99 weight percent, and the sodium ion content is reduced to less than 0.01 weight percent, and the method is suitable for the biotechnology field.
In order to achieve the above purpose, the invention is realized by the following technical scheme:
the preparation method of the high-purity potassium acetate comprises the following steps:
(1) Dissolving potassium acetate with the purity of at least 85wt% in water to prepare a potassium acetate saturated solution;
(2) Preparing an extractant, wherein the extractant is a mixed solvent of anhydrous diethyl ether and an alcohol solvent, and the volume ratio of the anhydrous diethyl ether to the alcohol solvent is 4-5:1;
(3) Pumping the potassium acetate saturated solution and the extractant from two ends of a T-shaped micro-channel continuous flow reactor, mixing in a convection mode, adding mixing kinetic energy through micro-channel convection to enable materials to be fully contacted and mixed, improving extraction contact, flowing out from an outlet after mixing, entering a clarification device, standing, separating liquid, and obtaining a supernatant; heating and concentrating the supernatant, pulping and then obtaining solid; finally, washing the solid by adopting anhydrous diethyl ether, and drying to obtain the high-purity potassium acetate.
Further, the alcohol solvent is absolute ethanol and/or absolute methanol; preferably, the alcohol solvent is absolute ethyl alcohol, the absolute ethyl alcohol content is 99.7%, the evaporation residue is less than or equal to 0.001%, and other impurity ions are not additionally introduced.
Further, controlling the flow rates of the potassium acetate saturated solution and the extractant into the microchannel continuous flow reactor so that the volume ratio of the potassium acetate saturated solution to the extractant mixed in the microchannel continuous flow reactor is 2-3:1.
Further, the microchannel continuous flow reactor has a tube diameter of 0.5-1mm and a characteristic dimension of at least 2000 μm; the temperature of mixing in the microchannel continuous flow reactor is 20-50 ℃.
Further, the temperature of the heating concentration is 70-80 ℃; and adding absolute ethyl alcohol to carry out pulping, so that the volume concentration of the material in the absolute ethyl alcohol is 30-35%, pulping for 4-6h, heating and concentrating to obtain solid, and pulping can improve the product purity.
Further, the volume amount of the anhydrous diethyl ether used for washing is 1 to 1.5 times of the total volume amount of the materials; the drying temperature after washing is 70-80 ℃.
Further, the method further comprises the step of recovering the anhydrous diethyl ether and the alcohol solvent through a back extraction process.
The beneficial technical effects are as follows:
according to the invention, a micro-channel continuous flow reactor is adopted to carry out efficient mixing and extraction reaction on a raw material potassium acetate saturated solution and an extracting agent (a mixed solvent of diethyl ether and ethanol) in a convection mode, and as potassium acetate is dissolved in alcohols such as water and ethanol but not dissolved in diethyl ether, and sodium acetate is dissolved in water and diethyl ether but slightly dissolved in ethanol, sodium ion content can be further reduced through efficient mixing and extraction of micro-channels, and high-purity potassium acetate is obtained; the purity of the chemical pure potassium acetate can be improved to more than 99 weight percent, the sodium ion content is reduced to less than 0.02 weight percent after the purification by the method, the purity of the analysis pure potassium acetate can be improved to more than 99 weight percent, and the sodium ion content is reduced to less than 0.01 weight percent, and the method is suitable for the biotechnology field.
Drawings
FIG. 1 is a process flow diagram of a method for preparing high purity potassium acetate according to the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. The following description of at least one exemplary embodiment is merely exemplary in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The numerical values set forth in these examples do not limit the scope of the present invention unless specifically stated otherwise. Techniques, methods known to those of ordinary skill in the relevant art may not be discussed in detail, but should be considered part of the specification where appropriate. In all examples shown and discussed herein, any specific values should be construed as merely illustrative, and not a limitation. Thus, other examples of the exemplary embodiments may have different values.
The experimental methods in the following examples, for which specific conditions are not noted, are generally determined according to national standards; if the national standard is not corresponding, the method is carried out according to the general international standard or the standard requirements set by related enterprises. Unless otherwise indicated, all parts are parts by weight and all percentages are percentages by weight.
Example 1
The preparation method of the high-purity potassium acetate comprises the following steps:
(1) Dissolving potassium acetate (chemical purity) with the purity of 85 weight percent in deionized water to prepare saturated KAc solution;
(2) Preparing an extractant, wherein the extractant is a mixed solvent of anhydrous diethyl ether and absolute ethyl alcohol, and the volume ratio of the anhydrous diethyl ether to the absolute ethyl alcohol is 4.5:1;
(3) Pumping the KAc solution and the extractant from feed pumps at two ends of a T-shaped micro-channel continuous flow reactor, mixing the KAc solution and the extractant in a convection mode, wherein the mixing temperature is 30 ℃, the pipe diameter of the micro-channel continuous flow reactor is 1mm, the characteristic size is 2500 mu m, and the flow rate of the KAc solution and the extractant entering the micro-channel continuous flow reactor is controlled so that the mixing volume ratio of the KAc solution and the extractant in the micro-channel continuous flow reactor is 3:1;
after mixing, flowing out from an outlet and entering a clarification device for standing and separating liquid to obtain a supernatant; heating and concentrating the lower clear liquid at 70 ℃, adding absolute ethyl alcohol to pulp at the same time, so that the volume concentration of the material in the absolute ethyl alcohol is 30%, heating and concentrating after pulping for 5 hours to obtain solid, washing the solid by adopting absolute ethyl ether with the volume of 1 time of the total volume of the material, and drying at a low temperature of 70 ℃ to obtain high-purity KAc.
Example 2
The preparation method of the high-purity potassium acetate comprises the following steps:
(1) Dissolving potassium acetate (chemical purity) with the purity of 85 weight percent in deionized water to prepare saturated KAc solution;
(2) Preparing an extractant, wherein the extractant is a mixed solvent of anhydrous diethyl ether and absolute ethyl alcohol, and the volume ratio of the anhydrous diethyl ether to the absolute ethyl alcohol is 4:1;
(3) Pumping the KAc solution and the extractant from two end feed pumps at two ends of a T-shaped micro-channel continuous flow reactor, mixing in a convection mode, wherein the mixing temperature is 23 ℃, the pipe diameter of the micro-channel continuous flow reactor is 1mm, the characteristic size is 2500 mu m, and the flow rate of the KAc solution and the extractant entering the micro-channel continuous flow reactor is controlled so that the mixing volume ratio of the KAc solution and the extractant in the micro-channel continuous flow reactor is 2.5:1;
after mixing, flowing out from an outlet and entering a clarification device for standing and separating liquid to obtain a supernatant; heating and concentrating the lower clear liquid at 75 ℃, adding absolute ethyl alcohol to pulp at the same time, so that the concentration of the total material volume in the absolute ethyl alcohol is 35%, heating and concentrating after pulping for 4 hours to obtain solid, washing the solid by adopting absolute ethyl ether with the total material volume being 1.2 times, and drying at a low temperature of 80 ℃ to obtain high-purity KAc.
Example 3
The preparation method of the high-purity potassium acetate comprises the following steps:
(1) Dissolving potassium acetate (analytically pure) with the purity of 92 weight percent in deionized water to prepare a saturated KAc solution;
(2) Preparing an extractant, wherein the extractant is a mixed solvent of anhydrous diethyl ether and absolute ethyl alcohol, and the volume ratio of the anhydrous diethyl ether to the absolute ethyl alcohol is 5:1;
(3) Pumping the KAc solution and the extractant from feed pumps at two ends of a T-shaped micro-channel continuous flow reactor, mixing the KAc solution and the extractant in a convection mode, wherein the mixing temperature is 50 ℃, the pipe diameter of the micro-channel continuous flow reactor is 1mm, the characteristic size is 2500 mu m, and the flow rate of the KAc solution and the extractant entering the micro-channel continuous flow reactor is controlled so that the mixing volume ratio of the KAc solution and the extractant in the micro-channel continuous flow reactor is 2:1;
after mixing, flowing out from an outlet and entering a clarification device for standing and separating liquid to obtain a supernatant; heating and concentrating the lower clear liquid at 80 ℃, adding absolute ethyl alcohol to pulp at the same time, so that the concentration of the total material volume in the absolute ethyl alcohol is 30%, heating and concentrating after pulping for 6 hours to obtain solid, washing the solid by adopting absolute ethyl ether with the total material volume being 1.5 times, and drying at a low temperature of 75 ℃ to obtain high-purity KAc.
Comparative example 1
The preparation method of the refined KAc of the comparative example is the same as that of example 1, except that the extractant is a mixed solvent of anhydrous diethyl ether and anhydrous ethanol, and the volume ratio of the anhydrous diethyl ether to the anhydrous ethanol is 3:1.
Comparative example 2
The preparation method of the refined KAc of the comparative example is the same as that of the example 1, except that the extractant is a mixed solvent of anhydrous diethyl ether and absolute ethanol, and the volume ratio of the anhydrous diethyl ether to the absolute ethanol is 6:1.
Comparative example 3
The preparation method of refined KAc of this comparative example was the same as in example 1, except that the mixing process was carried out not by using a microchannel continuous flow reactor but by using conventional mechanical stirring at 2000rpm for 6 hours.
Comparative example 4
The preparation method of refined KAc of this comparative example was the same as in example 1, except that anhydrous ethanol was not added to the process of heat concentration for beating, but heat concentration was carried out until a solid was obtained.
And (3) detecting the purity and sodium ion content of the KAc product obtained above, and detecting the sodium ion content by ICP-MS.
The results are shown in Table 2.
Table 2 product index of examples and comparative examples
From Table 2, it is clear that the sodium acetate in the saturated potassium acetate solution can be effectively extracted by using the mixed solvent of the extractant of the anhydrous diethyl ether and the anhydrous ethanol in the volume ratio of 4-5:1 compared with the embodiment 1; comparative example 3 employed conventional mechanical agitation without microchannel extraction, with no significant beneficial effect on sodium ion reduction; comparative example 4 was pulped without the addition of absolute ethanol, and the sodium ion content was high compared to example 1. The method can reduce the content of sodium ions in the raw material potassium acetate by at least 60 percent. According to the invention, a saturated potassium acetate solution and an extractant (the volume ratio of the anhydrous ethyl ether to the anhydrous ethanol is 4-5:1) are fully contacted and mixed in a microchannel reactor in a convection manner, so that sodium acetate in the raw materials is fully dissolved in the ethyl ether, potassium acetate is dissolved in the anhydrous ethyl alcohol, the lower clear liquid is obtained by layering, then the anhydrous ethyl alcohol is further added for heating concentration, pulping, and crystallization is carried out after heating concentration to obtain a solid, wherein a small amount of sodium acetate possibly exists in the solid component, then the sodium acetate remained in the anhydrous ethyl ether washing product is further added, and the high-purity potassium acetate is obtained after low-temperature drying. The purification method can improve the purity of the chemical pure potassium acetate to more than 99 weight percent, reduce the sodium ion content to less than 0.02 weight percent, improve the purity of the analytical pure potassium acetate to more than 99 weight percent and reduce the sodium ion content to less than 0.01 weight percent, and is suitable for the technical field of biology.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (6)
1. The preparation method of the high-purity potassium acetate is characterized by comprising the following steps:
(1) Dissolving potassium acetate with the purity of at least 85wt% in water to prepare a potassium acetate saturated solution;
(2) Preparing an extractant, wherein the extractant is a mixed solvent of anhydrous diethyl ether and an alcohol solvent, and the volume ratio of the anhydrous diethyl ether to the alcohol solvent is 4-5:1;
(3) Pumping the potassium acetate saturated solution and the extractant from two ends of a T-shaped micro-channel continuous flow reactor, mixing in a convection mode, flowing out from an outlet after mixing, and allowing the mixture to enter a clarification device for standing and separating liquid to obtain a supernatant; heating and concentrating the supernatant, pulping at the same time, and obtaining a solid; finally, washing the solid by adopting anhydrous diethyl ether, and drying to obtain the high-purity potassium acetate.
2. The method for producing high purity potassium acetate according to claim 1, wherein the alcohol is anhydrous and/or the methanol is anhydrous.
3. The method for preparing high-purity potassium acetate according to claim 1, wherein the flow rates of the potassium acetate saturated solution and the extractant into the microchannel continuous flow reactor are controlled so that the volume ratio of the potassium acetate saturated solution to the extractant mixed in the microchannel continuous flow reactor is 2-3:1.
4. The method for preparing high purity potassium acetate according to claim 1 where the microchannel continuous flow reactor has a tube diameter of 0.5-1mm and a characteristic dimension of at least 2000 μm; the temperature of mixing in the microchannel continuous flow reactor is 20-50 ℃.
5. The method for preparing high purity potassium acetate according to claim 1, wherein the temperature of the heating concentration is 70 to 80 ℃; and adding absolute ethyl alcohol to carry out beating, so that the volume concentration of the material in the absolute ethyl alcohol is 30-35%, and heating and concentrating after beating for 4-6h to obtain a solid.
6. The method for producing high purity potassium acetate according to claim 1, wherein the volume amount of said anhydrous diethyl ether used for said washing is 1 to 1.5 times the total volume amount of the material; the drying temperature after washing is 70-80 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310360308.6A CN116751121A (en) | 2023-04-06 | 2023-04-06 | Preparation method of high-purity potassium acetate |
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| CN116143612A (en) * | 2022-09-09 | 2023-05-23 | 湖南新绿方药业有限公司 | A kind of purification method of pharmaceutical grade potassium sorbate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116143612A (en) * | 2022-09-09 | 2023-05-23 | 湖南新绿方药业有限公司 | A kind of purification method of pharmaceutical grade potassium sorbate |
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