CN116282084A - Method for preparing sodium hexafluorophosphate in perhalogen organic compound - Google Patents
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- CN116282084A CN116282084A CN202310281508.2A CN202310281508A CN116282084A CN 116282084 A CN116282084 A CN 116282084A CN 202310281508 A CN202310281508 A CN 202310281508A CN 116282084 A CN116282084 A CN 116282084A
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- -1 sodium hexafluorophosphate Chemical compound 0.000 title claims abstract description 46
- 150000002894 organic compounds Chemical class 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 28
- 239000007789 gas Substances 0.000 claims description 22
- 239000007787 solid Substances 0.000 claims description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 13
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 229910052710 silicon Inorganic materials 0.000 claims description 10
- 239000010703 silicon Substances 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 claims description 6
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 5
- 125000004122 cyclic group Chemical group 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000010926 purge Methods 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 125000002015 acyclic group Chemical group 0.000 claims description 4
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 claims description 3
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 3
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 claims description 3
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 claims description 2
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 3
- 239000003792 electrolyte Substances 0.000 abstract description 3
- 230000009972 noncorrosive effect Effects 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 238000000746 purification Methods 0.000 abstract description 2
- 238000005292 vacuum distillation Methods 0.000 abstract description 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 54
- 235000013024 sodium fluoride Nutrition 0.000 description 27
- 239000011775 sodium fluoride Substances 0.000 description 27
- ZQBFAOFFOQMSGJ-UHFFFAOYSA-N hexafluorobenzene Chemical compound FC1=C(F)C(F)=C(F)C(F)=C1F ZQBFAOFFOQMSGJ-UHFFFAOYSA-N 0.000 description 6
- OBCUTHMOOONNBS-UHFFFAOYSA-N phosphorus pentafluoride Chemical compound FP(F)(F)(F)F OBCUTHMOOONNBS-UHFFFAOYSA-N 0.000 description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 3
- 229950011087 perflunafene Drugs 0.000 description 3
- UWEYRJFJVCLAGH-IJWZVTFUSA-N perfluorodecalin Chemical compound FC1(F)C(F)(F)C(F)(F)C(F)(F)[C@@]2(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)[C@@]21F UWEYRJFJVCLAGH-IJWZVTFUSA-N 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 229910001415 sodium ion Inorganic materials 0.000 description 3
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- RWRIWBAIICGTTQ-UHFFFAOYSA-N difluoromethane Chemical compound FCF RWRIWBAIICGTTQ-UHFFFAOYSA-N 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 159000000000 sodium salts Chemical class 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 239000004338 Dichlorodifluoromethane Substances 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- PXBRQCKWGAHEHS-UHFFFAOYSA-N dichlorodifluoromethane Chemical compound FC(F)(Cl)Cl PXBRQCKWGAHEHS-UHFFFAOYSA-N 0.000 description 1
- 235000019404 dichlorodifluoromethane Nutrition 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
Classifications
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0568—Liquid materials characterised by the solutes
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
Abstract
The invention relates to the field of sodium hexafluorophosphate preparation, in particular to a method for preparing sodium hexafluorophosphate in a perhalogen organic compound. The invention is used for NaF and PF 5 Reaction to synthesize NaPF 6 Instead of the liquid medium anhydrous HF used in conventional preparation methods, inert, non-corrosive, non-toxic liquid medium perhalogenated organic compounds are used. Thus, the step of removing HF from the product during purification, such as vacuum distillation, is eliminated, the HF content of sodium hexafluorophosphate is ensured to be less than 10ppm, the quality of sodium hexafluorophosphate applied to electrolyte is improved, and the application effect in batteries is improved.
Description
Technical Field
The invention relates to the field of sodium hexafluorophosphate preparation, in particular to a method for preparing sodium hexafluorophosphate in a perhalogen organic compound.
Background
The energy density of the sodium ion battery is lower than that of the lithium ion battery, but the safety, the working temperature, the cycle period and the economy are obviously better than those of the lithium ion battery. More importantly, precious metals are not needed in the production process of the sodium ion battery, so that the cost of the battery is reduced, and meanwhile, the dependence on scarce resources is greatly reduced. The application of the sodium ion battery is more suitable for the vehicle type with small or miniature electric vehicles and less endurance requirements.
Sodium hexafluorophosphate (NaPF 6) is the most important sodium salt in sodium battery electrolyte, and its preparation method and quality requirements are continuously advancing and increasing. At present, the preparation method of sodium hexafluorophosphate at home and abroad mainly refers to lithium hexafluorophosphate, and the greatest disadvantage of the process is that HF is easy to remain in the product, the HF content in sodium hexafluorophosphate is generally about 50ppm, and the HF content in the product is difficult to be reduced to the level below 10ppm. The residual HF can corrode the battery material, thereby affecting the battery electrical performance. In addition, the process has high requirements on anti-corrosion measures and materials of equipment and production safety measures, and is a cryogenic process, so that the energy consumption is high and the investment is high.
The Chinese patent application publication No. CN 114751431A discloses a preparation method of sodium salt for sodium battery, which comprises the steps of introducing phosphorus pentafluoride gas into a mixture of polyvinyl alcohol modified porous sodium fluoride and hydrogen fluoride liquid, reacting, crystallizing, filtering and drying to obtain sodium hexafluorophosphate. This solution requires the addition of hydrogen fluoride, which is toxic and corrosive and subsequently requires removal.
The Chinese patent with publication number CN 108946769A discloses a preparation method of sodium hexafluorophosphate, wherein phosphorus pentafluoride gas is introduced into a reaction kettle to which sodium fluoride and hydrogen fluoride liquid are added for reaction, so as to obtain sodium hexafluorophosphate solution, and crystallization and drying are realized under the stirring condition, so that sodium hexafluorophosphate is prepared. This solution also requires the addition of hydrogen fluoride, which is toxic and corrosive and subsequently requires removal.
The Chinese patent application publication No. CN 114772614A discloses a low-temperature synthesis method of high-purity sodium hexafluorophosphate, which comprises the steps of dissolving sodium fluoride in organic solvent solution of freon, introducing phosphorus pentafluoride gas into the solution, carrying out low-temperature vacuum reaction, and evaporating freon and the organic solvent to obtain sodium hexafluorophosphate. The freon adopted in the scheme is a mixture of dichlorodifluoromethane and difluoromethane, the use is limited in consideration of the damage to the ozone layer, and the scheme needs to react in the environment of-50 to 10 ℃.
Disclosure of Invention
The invention provides a method for preparing sodium hexafluorophosphate in a perhalogen organic compound, which is simple to operate, safe and environment-friendly, controllable in reaction process, low in cost, high in yield and purity, easy to realize industrial production, and comprises the following specific preparation processes:
a method for preparing sodium hexafluorophosphate in perhalogenated organic compounds, which comprises the following specific steps:
(1) 2.0-8.0g of high-purity NaF solid powder is filled into a clean thick-wall stainless steel reactor, and 10-30mL of perhalogen organic compound is added into the reactor, so that NaF is suspended in the perhalogen organic compound; the perhalogen organic compound is selected from any one or more of acyclic perfluorocarbon, perfluoroolefin or perfluoroolefin ether;
(2) The reactor was then sealed in a glove box and connected to a vacuum line, high pressure indicator and high pressure PF 5 System of gas cylinders, PF 5 Introducing gas into a reactor to make the gas contact with NaF in the perhalogen organic compound, and making the process temperature be 20-80 deg.C, and making reaction so as to obtain the invented NaPF 6 ；
(3) Excess PF is removed from the reactor by cyclic purging followed by vacuum application 5 A gas; transferring the reactor into a nitrogen glove box, opening the reactor in a dry inert environment, and recovering and filtering materials in the reactor;
(4) The filtered residue was dried with nitrogen in a glove box, dried with nitrogen, and unreacted NaF and NaPF formed were recovered as solids 6 Is a mixture of (a) and (b); using NaPF 6 Recovering NaPF from the resulting mixture 6 Filtering to obtain liquid sodium hexafluorophosphate.
The steps are as follows(1) The purity of the medium and high purity NaF solid is 99.98% or above, the silicon content is less than 5ppm, and the silicon content is SiO 2 And (5) counting.
PF in the step (2) 5 The purity is 99.95% or more.
The NaPF of step (4) 6 The good solvent is one or more of ethylene carbonate, propylene carbonate, dimethyl carbonate, diethyl carbonate and methyl ethyl carbonate.
The mass fraction of sodium hexafluorophosphate in the liquid sodium hexafluorophosphate in the step (6) is 30.0-32.0%, the moisture is less than or equal to 20ppm, and the free acid (calculated by HF) is less than or equal to 10ppm.
The acyclic perfluorocarbon in the step (1) is C 6 F 14 Or C 9 F 20 。
The perfluoroolefin in the step (1) is C 3 F 6 Or C 6 F 6 。
The pressure in the step (2) is controlled to be PF 5 The pressure is controlled to be 0.7-1.2Mpa, and the stirring time is 1-5h.
The nitrogen drying temperature in the step (4) is 90-100 ℃.
Compared with the prior art, the invention has the following beneficial effects:
the invention is used for NaF and PF 5 Reaction to synthesize NaPF 6 Instead of the liquid medium anhydrous HF used in conventional preparation methods, inert, non-corrosive, non-toxic liquid medium perhalogenated organic compounds are used. Thus, the step of removing HF from the product during purification, such as vacuum distillation, is eliminated, the HF content of sodium hexafluorophosphate is ensured to be less than 10ppm, the quality of sodium hexafluorophosphate applied to electrolyte is improved, and the application effect in batteries is improved.
Detailed Description
The following examples further illustrate the technical aspects of the present invention, but are not intended to limit the scope of the present invention.
Example 1
(1) 2g of high-purity NaF solid powder is filled into a clean thick-wall stainless steel reactor, 10mL of perfluorodecalin is added into the reactor, and NaF is suspended in the perfluorodecalin solution;
(2) The reactor was then sealed in a glove box and connected to a vacuum line, high pressure indicator and high pressure PF 5 System of gas cylinders, PF 5 Introducing gas into a reactor, maintaining the pressure at 0.7MPa, enabling the gas to contact NaF in perfluorodecalin, and reacting at the process temperature of 20 ℃ for 1h with stirring to generate NaPF 6 。
(3) Excess PF5 gas was removed from the reactor by cyclic purging followed by application of vacuum. The reactor was then transferred to a nitrogen glove box, opened in a dry inert environment, and the contents of the reactor were recovered and filtered.
(4) The filtered residue was dried in a glove box with nitrogen at 90℃and unreacted NaF and NaPF formed were recovered as a solid 6 Is a mixture of (a) and (b). Use of dimethyl carbonate solvent from NaPF 6 And recovery of NaPF from a mixture of unreacted NaF 6 Filtering to obtain liquid sodium hexafluorophosphate No. 1.
In the step (1), the purity of the high-purity NaF solid is 99.98 percent or more, the silicon content is less than 5ppm, and the silicon content is SiO 2 And (5) counting.
PF in step (2) 5 The purity is 99.95% or more.
Example 2
(1) 4g of a high purity NaF solid powder was charged into a clean thick wall stainless steel reactor, 15mL of hexafluorobenzene was added to the reactor, and NaF was suspended in hexafluorobenzene (C 6 F 6 ) In solution;
(2) The reactor was then sealed in a glove box and connected to a system consisting of vacuum lines, high pressure indicators and high pressure PF5 cylinders, the PF was set 5 Introducing gas into a reactor, keeping the pressure at 1.0MPa, enabling the gas to contact NaF in hexafluorobenzene, stirring for 3h at the process temperature of 50 ℃, and reacting to generate NaPF 6 。
(3) Excess PF is removed from the reactor by cyclic purging followed by vacuum application 5 And (3) gas. The reactor was then transferred to a nitrogen glove box, opened in a dry inert environment and recoveredAnd the material in the reactor was filtered.
(4) The filtered residue was dried in a glove box with nitrogen at a drying temperature of 95℃and unreacted NaF and NaPF formed were recovered as a solid 6 Is a mixture of (a) and (b). Use of diethyl carbonate solvent from NaPF 6 And recovery of NaPF from a mixture of unreacted NaF 6 Filtering to obtain liquid sodium hexafluorophosphate No. 2.
In the step (1), the purity of the high-purity NaF solid is 99.98 percent or more, the silicon content is less than 5ppm, and the silicon content is SiO 2 And (5) counting.
PF in step (2) 5 The purity is 99.95% or more.
Example 3
(1) 8g of a high purity NaF solid powder was charged into a clean thick wall stainless steel reactor, and 20mL of tetrafluoroethylene solvent (C 2 F 4 ) Adding the mixture into a reactor, and suspending NaF in a tetrafluoroethylene solution;
(2) The reactor was then sealed in a glove box and connected to a vacuum line, high pressure indicator and high pressure PF 5 System of gas cylinders, PF 5 Introducing gas into a reactor, keeping the pressure at 1.2MPa, enabling the gas to contact with NaF in tetrafluoroethylene, stirring for 5h at the process temperature of 80 ℃, and reacting to generate NaPF 6 。
(3) Excess PF5 gas was removed from the reactor by cyclic purging followed by application of vacuum. The reactor was then transferred to a nitrogen glove box, opened in a dry inert environment, and the contents of the reactor were recovered and filtered.
(4) The filtered residue was dried in a glove box with nitrogen at a drying temperature of 100 ℃ and unreacted NaF and NaPF formed were recovered as solids 6 Is a mixture of (a) and (b). Use of ethyl methyl carbonate solvent from NaPF 6 And recovery of NaPF from a mixture of unreacted NaF 6 Filtering to obtain liquid sodium hexafluorophosphate No. 3.
In the step (1), the purity of the high-purity NaF solid is 99.98 percent or more, the silicon content is less than 5ppm, and the silicon content is SiO 2 And (5) counting.
PF in step (2) 5 The purity is 99.95% or more.
The following table shows the experimental results:
table 1 quality index of liquid sodium hexafluorophosphate prepared in examples
| Sequence number | Name of the name | Liquid sodium hexafluorophosphate 1# | Liquid sodium hexafluorophosphate 2# | Liquid sodium hexafluorophosphate 3# |
| 1 | Mass percent of sodium hexafluorophosphate,% | 30.2 | 31.6 | 30.8 |
| 2 | Moisture, ppm | ≤10 | ≤10 | ≤10 |
| 3 | Free acid (in HF), ppm | ≤10 | ≤10 | ≤10 |
Examples 4-5 (the following examples are for studying the effect of temperature on the present application)
The following examples are the same as example 1 except for the process temperature of step (2), and the specific process temperatures are as follows:
| process temperature | Mass percent of sodium hexafluorophosphate,% | Moisture, ppm | Free acid (in HF), ppm | |
| Example 4 | 10 | 27.7 | ≤20 | ≤10 |
| Example 5 | 90 | 28.6 | ≤20 | ≤10 |
The above embodiments are only for illustrating the inventive concept of the present invention and not for limiting the protection of the claims of the present invention, and all the insubstantial modifications of the present invention using the concept shall fall within the protection scope of the present invention.
Claims (9)
1. A method for preparing sodium hexafluorophosphate in perhalogenated organic compounds, which is characterized by comprising the following specific steps:
(1) 2.0-8.0g of high-purity NaF solid powder is filled into a reactor, and 10-30mL of perhalogen organic compound is added into the reactor, so that NaF is suspended in the perhalogen organic compound; the perhalogen organic compound is selected from any one or more of acyclic perfluorocarbon, perfluoroolefin or perfluoroolefin ether;
(2) The reactor was then sealed in a glove box and connected to a vacuum line, high pressure indicator and high pressure PF 5 System of gas cylinders, PF 5 Introducing gas into a reactor to make the gas contact with NaF in the perhalogen organic compound, and making the process temperature be 20-80 deg.C, and making reaction so as to obtain the invented NaPF 6 ；
(3) Excess PF is removed from the reactor by cyclic purging followed by vacuum application 5 A gas; transferring the reactor into a nitrogen glove box, opening the reactor in a dry inert environment, and recovering and filtering materials in the reactor;
(4) The filtered residue was dried with nitrogen in a glove box, dried with nitrogen, and unreacted NaF and NaPF formed were recovered as solids 6 Is a mixture of (a) and (b); using NaPF 6 Recovering NaPF from the resulting mixture 6 Filtering to obtain liquid sodium hexafluorophosphate.
2. A process for preparing sodium hexafluorophosphate in a perhalogenated organic compound as claimed in claim 1, wherein: the purity of the high-purity NaF solid in the step (1) is 99.98 percent or more, the silicon content is less than 5ppm, and the silicon content is SiO 2 And (5) counting.
3. A process for preparing sodium hexafluorophosphate in a perhalogenated organic compound as claimed in claim 1, wherein: PF in the step (2) 5 The purity is 99.95% or more。
4. A process for preparing sodium hexafluorophosphate in a perhalogenated organic compound as claimed in claim 1, wherein: the NaPF of step (4) 6 The good solvent is one or more of ethylene carbonate, propylene carbonate, dimethyl carbonate, diethyl carbonate and methyl ethyl carbonate.
5. A process for preparing sodium hexafluorophosphate in a perhalogenated organic compound as claimed in claim 1, wherein: the mass fraction of sodium hexafluorophosphate in the liquid sodium hexafluorophosphate in the step (6) is 30.0-32.0%, the moisture is less than or equal to 20ppm, and the free acid is less than or equal to 10ppm.
6. A process for preparing sodium hexafluorophosphate in a perhalogenated organic compound as claimed in claim 1, wherein: the acyclic perfluorocarbon in the step (1) is C 6 F 14 Or C 9 F 20 。
7. A process for preparing sodium hexafluorophosphate in a perhalogenated organic compound as claimed in claim 1, wherein: the perfluoroolefin in the step (1) is C 3 F 6 Or C 6 F 6 。
8. A process for preparing sodium hexafluorophosphate in a perhalogenated organic compound as claimed in claim 1, wherein: the pressure in the step (2) is controlled to be PF 5 The pressure is controlled to be 0.7-1.2Mpa, and the stirring time is 1-5h.
9. A process for preparing sodium hexafluorophosphate in a perhalogenated organic compound as claimed in claim 1, wherein: the nitrogen drying temperature in the step (4) is 90-100 ℃.
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| CN115285965A (en) * | 2022-08-22 | 2022-11-04 | 衢州市九洲化工有限公司 | Synthetic method of sodium hexafluorophosphate |
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| TW201624809A (en) * | 2014-11-05 | 2016-07-01 | Central Glass Co Ltd | Method for purifying electrolyte solution and method for producing electrolyte solution |
| CN111989295A (en) * | 2018-03-29 | 2020-11-24 | 南非核能Soc有限公司 | Production of lithium hexafluorophosphate |
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