CN114291805A - Preparation method of potassium hexafluorophosphate - Google Patents
Preparation method of potassium hexafluorophosphate Download PDFInfo
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- CN114291805A CN114291805A CN202110286411.1A CN202110286411A CN114291805A CN 114291805 A CN114291805 A CN 114291805A CN 202110286411 A CN202110286411 A CN 202110286411A CN 114291805 A CN114291805 A CN 114291805A
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- reaction
- potassium
- potassium hexafluorophosphate
- solution
- hexafluorophosphate
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- HZNVUJQVZSTENZ-UHFFFAOYSA-N 2,3-dichloro-5,6-dicyano-1,4-benzoquinone Chemical compound ClC1=C(Cl)C(=O)C(C#N)=C(C#N)C1=O HZNVUJQVZSTENZ-UHFFFAOYSA-N 0.000 title claims abstract 9
- 238000002360 preparation method Methods 0.000 title abstract 4
- 238000006243 chemical reaction Methods 0.000 claims abstract 18
- 238000000034 method Methods 0.000 claims abstract 12
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract 10
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims abstract 10
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 claims abstract 4
- 239000000243 solution Substances 0.000 claims abstract 4
- 239000012266 salt solution Substances 0.000 claims abstract 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical group [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims 3
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims 2
- 239000007795 chemical reaction product Substances 0.000 claims 1
- 238000001035 drying Methods 0.000 claims 1
- 238000001914 filtration Methods 0.000 claims 1
- 229910000027 potassium carbonate Inorganic materials 0.000 claims 1
- 239000007787 solid Substances 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 238000010924 continuous production Methods 0.000 abstract 1
- 208000012839 conversion disease Diseases 0.000 abstract 1
- 239000012535 impurity Substances 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- 239000002699 waste material Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 1
Abstract
The invention provides a preparation method of potassium hexafluorophosphate, which comprises the following steps: carrying out a first reaction on hydrofluoric acid and phosphorus pentoxide to obtain a reaction solution; and carrying out a second reaction on the reaction solution and the potassium salt solution to obtain potassium hexafluorophosphate. Compared with the prior art, the preparation method of potassium hexafluorophosphate provided by the invention uses water generated by reaction as a solvent to realize liquid-liquid reaction for preparing the potassium hexafluorophosphate, and solves the problems of impurity wrapping of products and low reaction conversion rate in the traditional process; meanwhile, a microreactor device is adopted, so that the automation degree is high, the reaction is more sufficient, the time is shorter, the control is more accurate, and the continuous production can be realized. The preparation method of potassium hexafluorophosphate provided by the invention has the advantages of simple process, controllable reaction, good product quality, no three-waste discharge and the like, and is easy to implement and popularize in industrialization.
Description
Technical Field
The invention belongs to the technical field of potassium hexafluorophosphate, and particularly relates to a preparation method of potassium hexafluorophosphate.
Background
Potassium hexafluorophosphate, a white tetragonal crystal, has a melting point of 575 ℃ and a relative density of 2.55, and a solubility of 8.35g/100g of water (25 ℃), is a relatively important inorganic fluoride salt. Potassium hexafluorophosphate can be dissolved in acetonitrile solution, can be used as an organic fluorine substitution agent and used for preparing other hexafluorophosphates and fluorinating agents; potassium hexafluorophosphate is also an important chemical raw material newly developed in the late nineties of the world UV coating industry, and is mainly used as an ultraviolet light initiator (namely an ultraviolet light curing agent) in the coating industry; and also can be used as a catalyst for polymer synthesis. With the continuous progress of science and technology, some large pharmaceutical enterprises abroad in recent years use the protective agent for polypeptide drug synthesis as an important medical intermediate, and the application of the protective agent is more and more extensive.
At present, potassium hexafluorophosphate is prepared by a one-step method or a two-step method by taking phosphorus pentachloride/phosphorus pentafluoride/phosphorus oxychloride and potassium chloride/potassium fluoride as raw materials, and has the process defects of high reaction control difficulty, easy decomposition and sublimation of the phosphorus pentachloride as the raw material, difficult purification of the phosphorus pentafluoride as an intermediate product, low product yield and the like. Therefore, the development of a preparation method of potassium hexafluorophosphate with simple process, safety, controllability, high reaction efficiency and high product purity is urgently needed.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for preparing potassium hexafluorophosphate, which has the advantages of safe and controllable process, high reaction efficiency, high product purity, and easy industrial implementation.
The invention provides a preparation method of potassium hexafluorophosphate, which comprises the following steps:
carrying out a first reaction on hydrofluoric acid and phosphorus pentoxide to obtain a reaction solution;
and carrying out a second reaction on the reaction solution and the potassium salt solution to obtain potassium hexafluorophosphate.
Preferably, the hydrofluoric acid is anhydrous hydrofluoric acid.
Preferably, the phosphorus pentoxide is a phosphorus pentoxide solid.
Preferably, the molar ratio of the phosphorus pentoxide to the hydrofluoric acid is 1: (10-14).
Preferably, the temperature of the first reaction is-5 to 5 ℃; the time of the first reaction is 1-2 hours.
Preferably, the potassium salt is selected from potassium hydroxide and/or potassium carbonate.
Preferably, the mass concentration of the potassium salt solution is 20-50%.
Preferably, the temperature of the second reaction is 20-30 ℃.
Preferably, the second reaction is carried out in a microreactor.
Preferably, the second reaction further comprises, after completion of the first reaction:
and filtering, washing and drying the reaction product obtained after the second reaction is finished to obtain potassium hexafluorophosphate.
Compared with the prior art, the preparation method of potassium hexafluorophosphate provided by the invention uses water generated by reaction as a solvent to realize liquid-liquid reaction for preparing the potassium hexafluorophosphate, and solves the problems of impurity wrapping of products and low reaction conversion rate in the traditional process; meanwhile, a microreactor device is adopted, so that the automation degree is high, the reaction is more sufficient, the time is shorter, the control is more accurate, and the continuous production can be realized. The preparation method of potassium hexafluorophosphate provided by the invention has the advantages of simple process, controllable reaction, good product quality, no three-waste discharge and the like, and is easy to implement and popularize in industrialization.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other examples, which may be modified or appreciated by those of ordinary skill in the art based on the examples given herein, are intended to be within the scope of the present invention. It should be understood that the embodiments of the present invention are only for illustrating the technical effects of the present invention, and are not intended to limit the scope of the present invention. In the examples, the methods used were all conventional methods unless otherwise specified.
The invention provides a preparation method of potassium hexafluorophosphate, which comprises the following steps:
carrying out a first reaction on hydrofluoric acid and phosphorus pentoxide to obtain a reaction solution;
and carrying out a second reaction on the reaction solution and the potassium salt solution to obtain potassium hexafluorophosphate.
In the invention, a hexafluorophosphoric acid solution is preferably added for priming in the first reaction process; the method of the first reaction preferably comprises:
mixing a hexafluorophosphoric acid solution and hydrofluoric acid, and then carrying out a first reaction with phosphorus pentoxide to obtain a reaction solution.
In the present invention, the hexafluorophosphoric acid solution used in the first reaction process is preferably an aqueous solution of hexafluorophosphoric acid; the mass concentration of the hexafluorophosphoric acid solution is preferably 70 to 76%, more preferably 71 to 75%, and most preferably 72 to 74%.
In the present invention, the amount of the hexafluorophosphoric acid solution added in the first reaction process is preferably such that the stirring apparatus used in the reaction process is submerged.
In the invention, the temperature of mixing the hexafluorophosphoric acid solution and the hydrofluoric acid is preferably-5 ℃, more preferably-3 ℃, and most preferably-1 ℃.
In the present invention, the hydrofluoric acid is preferably anhydrous hydrofluoric acid.
In the present invention, the phosphorus pentoxide is preferably a phosphorus pentoxide solid.
In the present invention, the phosphorus pentoxide is preferably added in a batch manner, and the rate of addition of the phosphorus pentoxide is preferably controlled so that the temperature of the reaction liquid during the first reaction does not exceed 5 ℃.
In the present invention, the molar ratio of the phosphorus pentoxide to the hydrofluoric acid is preferably 1: (10-14), more preferably 1: (11-13), most preferably 1: 12.
in the invention, the temperature of the first reaction is preferably-5 ℃, more preferably-3 ℃, and most preferably-1 ℃; the time of the first reaction is preferably 1 to 2 hours, and more preferably 1.5 hours.
In the present invention, the potassium salt is preferably a saturated solution of potassium salt; the mass concentration of the potassium salt solution is preferably 20 to 50%, more preferably 30 to 40%, and most preferably 35%.
In the present invention, the potassium salt is preferably selected from potassium hydroxide and/or potassium carbonate.
In the present invention, the method for preparing the potassium salt solution preferably includes:
and mixing the potassium salt and the potassium hexafluorophosphate mother liquor to obtain a potassium salt solution.
In the present invention, the potassium hexafluorophosphate mother liquor is a filtrate obtained by filtering the reaction product obtained after the second reaction is completed.
In the present invention, when the potassium salt solution is a solution obtained by mixing a potassium salt and a potassium hexafluorophosphate mother liquor, the mass concentration of the potassium salt solution refers to the mass content of the potassium salt in the potassium hexafluorophosphate mother liquor.
In the present invention, hexafluorophosphoric acid and potassium ion (HPF) are used in the second reaction process6:K+) The molar ratio of (1-1.05): 1; the hexafluorophosphoric acid is preferably reacted in excess during the second reaction.
In the present invention, the second reaction is preferably carried out in a microreactor, which is preferably selected from a continuous reactor, a static mixer or a tubular reactor.
In the invention, the temperature of the second reaction is preferably normal temperature, more preferably 20-30 ℃, more preferably 22-28 ℃, and most preferably 24-26 ℃.
In the present invention, it is preferable that the second reaction further comprises, after completion of the first reaction:
and filtering, washing and drying the reaction product obtained after the second reaction is finished to obtain potassium hexafluorophosphate.
In the present invention, the method of filtration is preferably selected from suction filtration or pressure filtration.
In the present invention, the method of washing is preferably: rinsing with a small amount of water.
In the present invention, the drying method preferably adopts forced air drying; the drying temperature is preferably 110-130 ℃, more preferably 115-125 ℃, and most preferably 120 ℃; the drying time is preferably 1 to 2 hours, and more preferably 1.5 hours.
Compared with the prior art, the preparation method of potassium hexafluorophosphate provided by the invention uses water generated by reaction as a solvent to realize liquid-liquid reaction for preparing the potassium hexafluorophosphate, and solves the problems of impurity wrapping of products and low reaction conversion rate in the traditional process; meanwhile, a microreactor device is adopted, so that the automation degree is high, the reaction is more sufficient, the time is shorter, the control is more accurate, and the continuous production can be realized. The preparation method of potassium hexafluorophosphate provided by the invention has the advantages of simple process, controllable reaction, good product quality, no three-waste discharge and the like, and is easy to implement and popularize in industrialization.
The raw materials used in the following examples of the present invention are all commercially available products.
Example 1
Priming with a hexafluorophosphoric acid solution, adding 169g of anhydrous hydrofluoric acid, stirring and mixing uniformly, adding 100g of phosphorus pentoxide in batches for reaction, controlling the reaction temperature to be-5 ℃ after the addition is finished, and reacting for 2 hours to obtain 266g of the hexafluorophosphoric acid solution (reaction solution).
Weighing 96g of potassium carbonate, putting the potassium carbonate into potassium hexafluorophosphate mother liquor, stirring to prepare a solution with the mass concentration of 20%, then simultaneously adding the solution and the solution (reaction solution) of the hexafluorophosphoric acid into an open flow reactor at room temperature, uniformly mixing, immediately reacting, filtering, washing and drying the obtained slurry to obtain 242g of potassium hexafluorophosphate; the filtrate is potassium hexafluorophosphate mother liquor which is used for preparing potassium carbonate saturated solution.
The yield of potassium hexafluorophosphate prepared in example 1 of the present invention was calculated as follows:
yield-actual product mass 100%/theoretical product mass
The purity of potassium hexafluorophosphate prepared in example 1 of the present invention was measured according to GB/T19282-2014 "analytical method for lithium hexafluorophosphate product".
The detection result shows that the product yield is 94.6 percent and the purity is 99.16 percent.
Example 2
Priming with a hexafluorophosphoric acid solution, adding 338g of anhydrous hydrofluoric acid, stirring and mixing uniformly, adding 200g of phosphorus pentoxide in batches for reaction, controlling the reaction temperature to be 0 ℃ after the addition is finished, and reacting for 1.5h to obtain 535g of a hexafluorophosphoric acid solution (reaction solution) after the reaction.
Weighing 150g of potassium hydroxide, putting the potassium hydroxide into potassium hexafluorophosphate mother liquor, stirring to prepare a solution with the mass concentration of 50%, then adding the solution and the solution (reaction solution) of the hexafluorophosphoric acid into a static mixer at room temperature, uniformly mixing, immediately reacting, filtering, washing and drying the slurry after reaction to obtain 478.5g of potassium hexafluorophosphate; the filtrate is potassium hexafluorophosphate mother liquor which is used for preparing saturated solution of potassium hydroxide.
The yield and purity of potassium hexafluorophosphate prepared in example 2 of the present invention were measured according to the method of example 1, and the results were 96.9% in product yield and 99.32% in purity.
Example 3
Priming with a hexafluorophosphoric acid solution, adding 254g of anhydrous hydrofluoric acid, stirring and mixing uniformly, adding 150g of phosphorus pentoxide in batches for reaction, controlling the reaction temperature to be 5 ℃ after the addition is finished, and reacting for 1h to obtain 399g of the hexafluorophosphoric acid solution (reaction solution); and returning filter residues for reuse in the synthesis reaction of the hexafluorophosphoric acid.
Weighing 111.5g of potassium hydroxide, putting the potassium hydroxide into potassium hexafluorophosphate mother liquor, stirring to prepare a solution with the mass concentration of 40%, then adding the solution and a hexafluorophosphoric acid solution (reaction solution) into a static mixer at room temperature at the same time, uniformly mixing, immediately reacting, filtering, washing and drying slurry after reaction to obtain 348g of potassium hexafluorophosphate; the filtrate is potassium hexafluorophosphate mother liquor which is used for preparing saturated solution of potassium hydroxide.
The yield and purity of potassium hexafluorophosphate prepared in example 3 of the present invention were measured according to the method of example 1, and the results were found to be 95% yield and 99.21% purity.
Compared with the prior art, the preparation method of potassium hexafluorophosphate provided by the invention uses water generated by reaction as a solvent to realize liquid-liquid reaction for preparing the potassium hexafluorophosphate, and solves the problems of impurity wrapping of products and low reaction conversion rate in the traditional process; meanwhile, a microreactor device is adopted, so that the automation degree is high, the reaction is more sufficient, the time is shorter, the control is more accurate, and the continuous production can be realized. The preparation method of potassium hexafluorophosphate provided by the invention has the advantages of simple process, controllable reaction, good product quality, no three-waste discharge and the like, and is easy to implement and popularize in industrialization.
While only the preferred embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.
Claims (10)
1. A method for preparing potassium hexafluorophosphate, comprising:
carrying out a first reaction on hydrofluoric acid and phosphorus pentoxide to obtain a reaction solution;
and carrying out a second reaction on the reaction solution and the potassium salt solution to obtain potassium hexafluorophosphate.
2. The method of claim 1, wherein the hydrofluoric acid is anhydrous hydrofluoric acid.
3. The method of claim 1, wherein the phosphorus pentoxide is a phosphorus pentoxide solid.
4. The method of claim 1, wherein the phosphorus pentoxide and hydrofluoric acid are present in a molar ratio of 1: (10-14).
5. The method according to claim 1, wherein the temperature of the first reaction is-5 to 5 ℃; the time of the first reaction is 1-2 hours.
6. The process according to claim 1, characterized in that the potassium salt is selected from potassium hydroxide and/or potassium carbonate.
7. The method according to claim 1, wherein the potassium salt solution has a mass concentration of 20 to 50%.
8. The method according to claim 1, wherein the temperature of the second reaction is 20 to 30 ℃.
9. The method of claim 1, wherein the second reaction is conducted in a microreactor.
10. The method of claim 1, further comprising, after completion of the second reaction:
and filtering, washing and drying the reaction product obtained after the second reaction is finished to obtain potassium hexafluorophosphate.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110286411.1A CN114291805A (en) | 2021-03-17 | 2021-03-17 | Preparation method of potassium hexafluorophosphate |
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| CN202110286411.1A CN114291805A (en) | 2021-03-17 | 2021-03-17 | Preparation method of potassium hexafluorophosphate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115535994A (en) * | 2022-10-18 | 2022-12-30 | 河南省氟基新材料科技有限公司 | Preparation method of lithium difluorophosphate |
| CN116375056A (en) * | 2023-03-31 | 2023-07-04 | 江苏泰际材料科技有限公司 | Potassium hexafluorophosphate and method for preparing potassium hexafluorophosphate |
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| US20170015563A1 (en) * | 2014-03-31 | 2017-01-19 | The South African Nuclear Energy Corporation Limited | Production of a hexafluorophosphate salt and of phosphorous pentafluoride |
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2021
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| US20010041158A1 (en) * | 1999-08-17 | 2001-11-15 | W. Novis Smith | Preparation of phosphorus pentafluoride |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115535994A (en) * | 2022-10-18 | 2022-12-30 | 河南省氟基新材料科技有限公司 | Preparation method of lithium difluorophosphate |
| CN115535994B (en) * | 2022-10-18 | 2024-05-17 | 河南省氟基新材料科技有限公司 | Preparation method of lithium difluorophosphate |
| CN116375056A (en) * | 2023-03-31 | 2023-07-04 | 江苏泰际材料科技有限公司 | Potassium hexafluorophosphate and method for preparing potassium hexafluorophosphate |
| CN116375056B (en) * | 2023-03-31 | 2024-10-25 | 江苏泰际材料科技有限公司 | Potassium hexafluorophosphate and method for preparing potassium hexafluorophosphate |
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