CN115286013A - Preparation method of hexafluorophosphate - Google Patents
Preparation method of hexafluorophosphate Download PDFInfo
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- CN115286013A CN115286013A CN202211139519.9A CN202211139519A CN115286013A CN 115286013 A CN115286013 A CN 115286013A CN 202211139519 A CN202211139519 A CN 202211139519A CN 115286013 A CN115286013 A CN 115286013A
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- hexafluorophosphate
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- hexafluorophosphoric acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/005—Lithium hexafluorophosphate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D13/00—Compounds of sodium or potassium not provided for elsewhere
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a preparation method of hexafluorophosphate, which comprises the steps of adsorbing an aqueous solution of hexafluorophosphate by using weak base ion exchange resin, washing and drying by using a non-coordinating solvent, and eluting by using a coordinating solvent to obtain an organic solution of hexafluorophosphate. The invention realizes the conversion from the hexafluorophosphate aqueous solution to the organic solution by utilizing the coordination resin, ensures that the subsequent preparation process is safe and controllable, breaks through the fixed thinking that the hexafluorophosphate is prepared by taking the phosphorus pentafluoride as the raw material, avoids the defects of strong corrosivity, poor safety, complex byproducts and the like of the dehydration of fuming sulfuric acid, and is worthy of popularization.
Description
Technical Field
The invention relates to the technical field of chemical synthesis, in particular to a preparation method of hexafluorophosphate.
Background
With the development of new mobile portable power sources, battery technology is also continuously developed, wherein the preparation of hexafluorophosphate is crucial.
In the prior art, phosphorus pentachloride and anhydrous hydrogen fluoride are generally adopted to react to generate phosphorus pentafluoride, and then the phosphorus pentafluoride reacts with corresponding metal fluoride to obtain hexafluorophosphate. Or reacting anhydrous hydrogen fluoride, phosphoric acid or polyphosphoric acid to prepare a hexafluorophosphoric acid aqueous solution, removing moisture by fuming sulfuric acid, and heating to decompose hexafluorophosphoric acid to generate phosphorus pentafluoride, thereby preparing hexafluorophosphate. Or the anhydrous hydrogen fluoride and the hexafluorophosphate are used for preparing the phosphorus pentafluoride by co-heating, and then the phosphorus pentafluoride is converted into other hexafluorophosphates.
However, in the above technical solution, since the difference between the boiling points of hydrogen chloride and phosphorus pentafluoride is too small, it is difficult to obtain a single phosphorus pentafluoride gas by the phosphorus pentachloride method. The hexafluorophosphate co-heating method is poor in economical efficiency and is only suitable for manufacturing of some special salts. The phosphoric acid and polyphosphoric acid method is the only method for preparing phosphorus pentafluoride gas on a large scale at present, but the use of fuming sulfuric acid can cause the generation of fluorosulfonic acid by-products, so that the equipment corrosion is serious and the safety is poor in the production process, and a large amount of fluorine-containing sulfuric acid by-products are generated and need to be processed by a corresponding production line. And a large amount of heat is released in the process of introducing oleum, phosphorus pentafluoride is easy to form various types of phosphorus oxyfluoride compounds in the presence of moisture, and phosphorus pentafluoride gas with high purity can be obtained after multistage deep cooling and gas washing purification are needed.
Disclosure of Invention
The invention provides a preparation method of hexafluorophosphate, which is used for overcoming the defects of strong corrosivity, poor safety, complex byproduct and the like caused by the adoption of fuming sulfuric acid for dehydration in the prior art and realizing safe production.
The invention provides a preparation method of hexafluorophosphate, which comprises the steps of adsorbing an aqueous solution of hexafluorophosphate by using weak base ion exchange resin, washing and drying by using a non-coordinating solvent, and eluting by using a coordinating solvent to obtain an organic solution of hexafluorophosphate.
According to the invention, a resin technology is adopted to treat an aqueous solution of hexafluorophosphoric acid, the coordination groups on the weakly basic ion exchange resin are utilized to fix the hexafluorophosphoric acid on the resin, so that the decomplexation of the hexafluorophosphoric acid and water is realized, the resin after fully adsorbing the hexafluorophosphoric acid is washed and dried by a non-coordinating solvent, the hexafluorophosphoric acid is not eluted or decomposed due to the existence of the coordination groups on the resin, and then the coordination solvent is adopted to elute the hexafluorophosphoric acid from the resin, so that an organic solution of the hexafluorophosphoric acid is obtained. After the hexafluorophosphoric acid organic solution is obtained, the corresponding hexafluorophosphoric acid alkali salt product can be obtained through simple reaction with metal fluoride and post treatment, and the production process is easy to control.
The invention breaks through the fixed thinking that the phosphorus pentafluoride is used as the raw material to prepare the hexafluorophosphate, realizes the conversion from the hexafluorophosphate aqueous solution to the organic solution by utilizing the weak alkaline ion exchange resin, and avoids the defects of strong corrosivity, poor safety, complex byproduct and the like of the dehydration of fuming sulfuric acid.
According to the preparation method of the hexafluorophosphate provided by the invention, the molar ratio of the total exchange capacity of the weak base ion exchange resin to the hexafluorophosphoric acid is 0.8-0.95.
The key parameter of the resin is the exchange capacity C in mol/L. The molar ratio of the total exchange capacity of the weak basic ion exchange resin to the hexafluorophosphoric acid is controlled to be 0.8-0.95, namely the volume usage of the resin is insufficient (not reaching 1). If the ratio exceeds 0.8 to 0.95, as in 1.
According to the method for preparing hexafluorophosphate provided by the invention, the weakly basic ion exchange resin is a resin containing weakly basic tertiary amine groups, primary amine groups or secondary amine groups.
Exemplary, non-limiting resin grades and exchange capacities employed in the present invention are Amberlite IRA 67.6 mol/L, amberlite IRA96F 1.3mol/L, amberlite HPR 9700.3 mol/L, D301.4 mol/L.
The group in the weak base ion exchange resin, especially the tertiary amine group, can form a complex structure with hexafluorophosphoric acid to fix the complex structure on a resin matrix. Because of the existence of steric hindrance, the binding force is relatively weak, and the resin can be eluted from the resin matrix through a coordination solvent.
According to the preparation method of the hexafluorophosphate provided by the invention, the non-coordinating solvent is one or more of dichloromethane, dichloroethane and tetrachloroethane.
In the technical scheme of the invention, a non-coordinating solvent with the water content lower than 5ppm is used for washing. Washing with a non-coordinating solvent is carried out for a number of times such that the water content in the solvent after washing is less than 10ppm, preferably 5ppm. This indicates that decomplexing of hexafluorophosphoric acid from water is substantially complete.
According to the preparation method of the hexafluorophosphate provided by the invention, the coordinating solvent is one or more of acetonitrile, diethyl ether, dimethyl carbonate, diethyl carbonate and ethyl methyl carbonate.
According to the method for preparing hexafluorophosphate provided by the invention, the moisture content in the coordinating solvent is less than 5ppm.
According to the preparation method of the hexafluorophosphate provided by the invention, the hexafluorophosphoric acid aqueous solution can be obtained by reacting hydrogen fluoride with one or more of phosphoric acid, polyphosphoric acid and phosphorus pentoxide. The specific method is described in numerous documents and patents, and is a commonly used method for preparing an aqueous hexafluorophosphoric acid solution in the art.
According to the preparation method of the hexafluorophosphate provided by the invention, the preparation method further comprises the following steps: and reacting the hexafluorophosphoric acid organic solution with a metal fluoride, and performing post-treatment to obtain a finished product of hexafluorophosphate.
According to the preparation method of hexafluorophosphate provided by the invention, the metal fluoride is alkali metal fluoride, and the molar ratio of the alkali metal fluoride to the hexafluorophosphoric acid in the organic solution of hexafluorophosphoric acid is 1.01 to 2, preferably 1.02 to 1.05.
According to the preparation method of the hexafluorophosphate provided by the invention, the reaction temperature is 0-60 ℃, and preferably 10-20 ℃.
According to the preparation method of the hexafluorophosphate provided by the invention, the post-treatment comprises filtration, concentration, crystallization and drying.
In some embodiments of the present invention, the method for preparing hexafluorophosphate comprises the steps of:
pumping the hexafluorophosphoric acid solution into a resin adsorption reactor by a metering pump at a rate of 1-50mL/min, preferably 5-15mL/min, and after multiple cycles of adsorption, circularly washing the resin column with dichloroethane with a moisture content of less than 5ppm until the dichloroethane after washing has a moisture content of less than 10ppm, preferably less than 5ppm. And after washing and drying are finished, acetonitrile with the moisture content lower than 5ppm is used as eluent, the resin is circularly washed, and the elution is stopped after the acidity in the acetonitrile eluent is detected to be not increased any more. And filtering the obtained eluent, adding alkali metal fluoride, reacting at 0-60 ℃ and preferably at 10-20 ℃ for 2-24 hours, dissolving most of the alkali metal fluoride in the eluent at a molar ratio of the alkali metal fluoride to the hexafluorophosphoric acid in the organic solution of the hexafluorophosphoric acid of 1.01-2, and filtering to obtain an acetonitrile solution containing hexafluorophosphate, and concentrating, crystallizing and drying to obtain the finished product of the hexafluorophosphate.
According to the preparation method of the hexafluorophosphate provided by the invention, the conversion of the hexafluorophosphate aqueous solution into the organic solution is realized by using the weakly basic ion exchange resin, so that the subsequent preparation process is safe and controllable, the fixed thinking of preparing the hexafluorophosphate by using the phosphorus pentafluoride as a raw material is broken, the defects of strong corrosivity, poor safety, complex byproducts and the like in the dehydration of fuming sulfuric acid are avoided, and the preparation method is worthy of popularization.
Detailed Description
To make the objects, technical solutions and advantages of the present invention clearer and more complete, the technical solutions of the present invention will be described below clearly, and it is obvious that the described embodiments are some, not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The embodiment provides a preparation method of lithium hexafluorophosphate, which comprises the following steps:
pumping the hexafluorophosphoric acid aqueous solution after the reaction of hydrogen fluoride and phosphoric acid into a resin adsorption reactor (resin brand and exchange capacity Amberlite I RA671.6mol/L) by a metering pump at a rate of 10mL/min, wherein the molar ratio of the total exchange capacity of the resin (1.6 mol/L. Resin volume (unit L)) to the hexafluorophosphoric acid is 0.85. And after washing and drying are finished, acetonitrile with the moisture content lower than 5ppm is used as eluent, the resin is circularly washed, and the elution is stopped after the acidity in the acetonitrile eluent is detected to be not increased any more. And filtering the obtained eluent, adding lithium fluoride, reacting at 10 ℃ for 24 hours, basically reacting and dissolving the lithium fluoride, filtering to obtain an acetonitrile solution containing lithium hexafluorophosphate, concentrating, crystallizing and drying to obtain the finished product of lithium hexafluorophosphate, wherein the molar ratio of the lithium fluoride to the hexafluorophosphoric acid is 1.02. The yield was 93.4% and the purity was 99.5%.
Example 2
The embodiment provides a preparation method of lithium hexafluorophosphate, which comprises the following steps:
the aqueous hexafluorophosphate solution after the reaction of hydrogen fluoride with polyphosphoric acid was pumped at 15mL/min using a metering pump into a resin adsorption reactor (resin brand and exchange capacity amberlite ira96F 1.3 mol/L) with a molar ratio of total exchange capacity of resin (1.3 mol/L resin volume (unit L)) to hexafluorophosphate of 0.95, and after multiple cycles of adsorption, the resin column was washed with dichloromethane having a moisture content of less than 5ppm until the water content of dichloromethane after washing was less than 10ppm. And after washing and drying are finished, acetonitrile with the moisture content lower than 5ppm is used as eluent, the resin is circularly washed, and the elution is stopped after the acidity in the acetonitrile eluent is detected to be not increased any more. And filtering the obtained eluent, adding lithium fluoride, reacting at 20 ℃ for 12 hours, dissolving the lithium fluoride in a basic reaction, filtering to obtain an acetonitrile solution containing lithium hexafluorophosphate, and concentrating, crystallizing and drying to obtain the finished product of lithium hexafluorophosphate, wherein the molar ratio of the lithium fluoride to the hexafluorophosphoric acid is 1.05.
Example 3
The embodiment provides a preparation method of sodium hexafluorophosphate, which comprises the following steps:
pumping the hexafluorophosphoric acid aqueous solution after the reaction of hydrogen fluoride with polyphosphoric acid into a resin adsorption reactor (resin brand and exchange capacity amberlite hpr 9700.3 mol/L) at a rate of 5mL/min by a metering pump, wherein the molar ratio of the total exchange capacity of the resin (1.3 mol/L resin volume (unit L)) to the hexafluorophosphoric acid is 0.8, and circularly washing the resin column with dichloroethane with a moisture content of less than 5ppm after multiple cycles of adsorption until the water content of the dichloroethane after washing is less than 5ppm. And after the washing and drying are finished, using acetonitrile with the moisture content lower than 5ppm as eluent, circularly washing the resin, and stopping eluting after detecting that the acidity in the acetonitrile eluent is not increased any more. And filtering the obtained eluent, adding sodium fluoride, reacting at 10 ℃ for 24 hours, dissolving the sodium fluoride in a basic reaction, filtering to obtain an acetonitrile solution containing sodium hexafluorophosphate, and concentrating, crystallizing and drying to obtain the finished product of sodium hexafluorophosphate, wherein the molar ratio of the sodium fluoride to the hexafluorophosphoric acid is 1.02. The yield was 88.2% and the purity was 99.1%.
Example 4
The embodiment provides a preparation method of lithium hexafluorophosphate, which comprises the following steps:
the hexafluorophosphate aqueous solution after the reaction of hydrogen fluoride and phosphorus pentoxide was pumped at a rate of 10mL/min into a resin adsorption reactor (resin brand and exchange capacity d3011.4 mol/L) using a metering pump, wherein the molar ratio of the total exchange capacity of the resin (1.4 mol/L resin volume (unit L)) to the hexafluorophosphate was 0.9. After the washing and drying are finished, the dimethyl carbonate with the moisture content lower than 5ppm is used as eluent, the resin is circularly washed, and the elution is stopped after the acidity in the dimethyl carbonate eluent is detected not to be increased any more. And filtering the obtained eluent, adding lithium fluoride, reacting at 10 ℃ for 24 hours, dissolving the lithium fluoride in a basic reaction, filtering to obtain a dimethyl carbonate solution containing lithium hexafluorophosphate, concentrating, crystallizing and drying to obtain the finished product of lithium hexafluorophosphate, wherein the molar ratio of the lithium fluoride to the hexafluorophosphoric acid is 1.02. The yield is 90.2 percent and the purity is 99 percent.
Example 5
The embodiment provides a preparation method of lithium hexafluorophosphate, which comprises the following steps:
pumping the hexafluorophosphoric acid aqueous solution after the reaction of hydrogen fluoride and phosphoric acid into a resin adsorption reactor (resin brand and exchange capacity Amberlite I RA671.6mol/L) by a metering pump at a rate of 10mL/min, wherein the molar ratio of the total exchange capacity of the resin (1.6 mol/L. Resin volume (unit L)) to the hexafluorophosphoric acid is 1.05. And after the washing and drying are finished, using acetonitrile with the moisture content lower than 5ppm as eluent, circularly washing the resin, and stopping eluting after detecting that the acidity in the acetonitrile eluent is not increased any more. And filtering the obtained eluent, adding lithium fluoride, reacting at 10 ℃ for 24 hours, basically reacting and dissolving the lithium fluoride, filtering to obtain an acetonitrile solution containing lithium hexafluorophosphate, concentrating, crystallizing and drying to obtain the finished product of lithium hexafluorophosphate, wherein the molar ratio of the lithium fluoride to the hexafluorophosphoric acid is 1.02. The yield was reduced to 70% and the purity was relatively stable, comparable to that of example 1.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, and not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A preparation method of hexafluorophosphate is characterized by comprising the steps of adsorbing an aqueous solution of hexafluorophosphate by using weak base ion exchange resin, washing and drying by using a non-coordinating solvent, and eluting by using a coordinating solvent to obtain an organic solution of hexafluorophosphate.
2. The method for producing hexafluorophosphate according to claim 1, wherein the molar ratio of the total exchange capacity of said weakly basic ion exchange resin to hexafluorophosphoric acid is 0.8 to 0.95.
3. The method for producing a hexafluorophosphate salt according to claim 1 or 2, wherein said weakly basic ion exchange resin is a resin comprising a weakly basic tertiary amine group, a weakly basic primary amine group or a weakly basic secondary amine group.
4. The method according to claim 1 or 2, wherein the non-coordinating solvent is one or more of dichloromethane, dichloroethane, and tetrachloroethane.
5. The method of claim 1 or 2, wherein the coordinating solvent is one or more of acetonitrile, diethyl ether, dimethyl carbonate, diethyl carbonate, and ethyl methyl carbonate.
6. The method according to claim 3 or 4, wherein the moisture content in each of the non-coordinating solvent and the coordinating solvent is less than 5ppm.
7. The method for the production of hexafluorophosphate of any one of claims 1 to 6, further comprising: and reacting the hexafluorophosphoric acid organic solution with a metal fluoride, and performing post-treatment to obtain a finished product of hexafluorophosphate.
8. The method according to claim 7, wherein the metal fluoride is an alkali metal fluoride, and the molar ratio of the alkali metal fluoride to the hexafluorophosphoric acid in the organic solution of hexafluorophosphoric acid is 1.01 to 2, preferably 1.02 to 1.05.
9. The process for the preparation of hexafluorophosphate of claim 7, wherein said reaction temperature is 0-60 ℃, preferably 10-20 ℃.
10. The method for the preparation of hexafluorophosphate of claim 7, wherein said post-treatment comprises filtration, concentration, crystallization and drying.
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