CN113772694A - Preparation method of high-purity sodium hexafluorophosphate - Google Patents
Preparation method of high-purity sodium hexafluorophosphate Download PDFInfo
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- CN113772694A CN113772694A CN202111151265.8A CN202111151265A CN113772694A CN 113772694 A CN113772694 A CN 113772694A CN 202111151265 A CN202111151265 A CN 202111151265A CN 113772694 A CN113772694 A CN 113772694A
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- purity
- sodium hexafluorophosphate
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- -1 sodium hexafluorophosphate Chemical compound 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 235000013024 sodium fluoride Nutrition 0.000 claims abstract description 14
- 239000011775 sodium fluoride Substances 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 13
- 238000005336 cracking Methods 0.000 claims abstract description 12
- 239000012452 mother liquor Substances 0.000 claims abstract description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 10
- 238000002425 crystallisation Methods 0.000 claims abstract description 9
- 230000008025 crystallization Effects 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000001291 vacuum drying Methods 0.000 claims abstract description 7
- 229910013870 LiPF 6 Inorganic materials 0.000 claims abstract description 5
- 229910001290 LiPF6 Inorganic materials 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims abstract description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 5
- 239000011343 solid material Substances 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims abstract description 4
- 238000004064 recycling Methods 0.000 claims abstract description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 3
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 229910001415 sodium ion Inorganic materials 0.000 abstract description 8
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract 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 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 238000009826 distribution Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005243 fluidization Methods 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002001 electrolyte material Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Images
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
-
- 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
-
- 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
- C01P2006/82—Compositional purity water content
Abstract
The application discloses a preparation method of high-purity sodium hexafluorophosphate, which relates to the technical field of sodium ion batteries and comprises the following steps: (1) adding the battery-grade LiPF6 into a cracking kettle under the protection of nitrogen; (2) heating the cracking kettle to a certain temperature and preserving the temperature for a period of time to completely decompose the LiPF 6; (3) adding a proper amount of solvent into a synthesis kettle, adding a certain amount of high-purity sodium fluoride, and stirring and dissolving at a certain temperature; (4) introducing the gas generated in the step (2) into a synthesis kettle, and carrying out fluidized reaction under certain conditions to obtain sodium hexafluorophosphate synthetic liquid; (5) after the reaction is finished, filtering the synthetic liquid to remove insoluble substances to obtain synthetic mother liquid; (6) cooling and crystallizing the synthetic mother liquor, and filtering; (7) and (4) carrying out vacuum drying on the solid material to obtain a finished product of sodium hexafluorophosphate, and recycling the crystallization mother liquor for dissolving sodium fluoride. The obtained product has high purity, high yield, high process safety and simple equipment.
Description
Technical Field
The invention relates to the technical field of sodium ion batteries, in particular to a preparation method of high-purity sodium hexafluorophosphate.
Background
The sodium ion battery is a secondary battery, and realizes the charge and discharge function by means of reversible migration of sodium ions back and forth between a positive electrode and a negative electrode. Compared with lithium hexafluorophosphate which is currently used in large-scale commercial application, sodium hexafluorophosphate has the following advantages: the storage capacity of sodium element on the earth reaches about 3 percent of crust content, and compared with lithium, the storage capacity is only 0.065 percent; from the distribution, the distribution of the sodium element is more uniform compared with the distribution of the lithium element; the sodium battery has higher safety and wider standard voltage range.
The shortage of lithium resources is bound to become an important influence factor for limiting the development of lithium hexafluorophosphate in the future, and the sodium resource required by the sodium ion battery is rich in storage capacity and high in safety performance. Sodium hexafluorophosphate is a hotspot for research of sodium ion batteries as an electrolyte material, and the preparation of high-purity sodium hexafluorophosphate is crucial to the development of sodium ion batteries.
Disclosure of Invention
The invention aims to provide a preparation method of high-purity sodium hexafluorophosphate, which is used for obtaining a high-purity sodium hexafluorophosphate product for a sodium ion battery. The technical scheme is as follows:
the method comprises the following steps: (1) adding the battery-grade LiPF6 into a cracking reaction kettle under the protection of nitrogen; (2) heating the cracking reaction kettle to a certain temperature and preserving the temperature for a period of time to completely decompose the LiPF 6; (3) adding a proper amount of solvent into a synthesis kettle, adding a certain amount of high-purity sodium fluoride, and stirring and dissolving at a certain temperature; (4) introducing the gas generated in the step (2) into a synthesis kettle, and carrying out fluidized reaction under certain conditions to obtain sodium hexafluorophosphate synthetic liquid; (5) after the reaction is finished, filtering the synthetic liquid to remove insoluble substances to obtain synthetic mother liquid; (6) cooling and crystallizing the synthetic mother liquor, and filtering; (7) and (4) carrying out vacuum drying on the solid material to obtain a finished product of sodium hexafluorophosphate, and recycling the crystallization mother liquor for dissolving sodium fluoride.
Further, the cracking reaction kettle in the step (1) comprises a heating jacket and an inner cylinder, wherein the inner cylinder is made of 316L materials, and the inner cylinder is sealed with a sealing head.
Further, the certain temperature in the step (2) is 85-190 ℃, and the heat preservation time is 4-12 h.
Further, the solvent in the step (3) is photovoltaic hydrofluoric acid or electronic hydrofluoric acid or crystallization mother liquor, the purity of the sodium fluoride is 99.98% or more, the silicon content is less than or equal to 0.00005%, and the silicon content is calculated by SiO 2.
Further, the amount of the sodium fluoride used in the step (3) is 2.5-5 g/100g of the solvent, the stirring and dissolving temperature is 10-50 ℃, the dissolving pressure is 0-30kpa, and the dissolving time is 1-2 hours.
Further, the certain conditions in the step (4) are that the reaction temperature is 5-55 ℃, the pressure is 0-80kpa, and the reaction time is 4-10 hours.
Further, the cooling speed of the cooling crystallization in the step (6) is 1 ℃/h, the temperature is reduced to minus 30 ℃ and 2 ℃/h, the temperature is reduced to minus 40 ℃, and the temperature is kept for 2-4 h.
Further, the temperature of the vacuum drying in the step (7) is 60-90 ℃, and the vacuum degree is-0.06 to-0.1 Mpa.
Further, the crystallization mother liquor can be repeatedly used for dissolving high-purity sodium fluoride.
The product obtained by the method has high purity, high yield, high process safety and simple equipment.
In conclusion, the technical scheme provided by the invention has the following beneficial effects: the product obtained by the method has high purity, high yield, high process safety and simple equipment.
Drawings
FIG. 1 is an XDR diffraction pattern of sodium hexafluorophosphate prepared by the present invention;
figure 2 is a standard XDR diffraction pattern for sodium hexafluorophosphate.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail below.
Example 1
A preparation method of high-purity sodium hexafluorophosphate specifically comprises the following steps:
(1) adding 200g of battery-grade LiPF6 into a cracking reaction kettle under the protection of nitrogen;
(2) heating the cracking reaction kettle to 85 ℃ and preserving heat for 3.5 hours to decompose LiPF 6;
(3) adding 500g of PV2 a-grade photovoltaic hydrofluoric acid into a synthesis kettle, adding 55g of high-purity sodium fluoride, and stirring and dissolving at 25 ℃ for 2 h;
(4) introducing the gas generated in the step (2) into a synthesis kettle, carrying out fluidization reaction for 8 hours at 10 ℃, and filtering to obtain 706g of sodium hexafluorophosphate synthetic liquid;
(5) cooling the synthetic mother liquor at a cooling rate of 1 ℃/h to-30 ℃ and 2 ℃/h to-40 ℃, preserving heat for 2h, and filtering;
(6) vacuum drying the solid material at 78 ℃ and-0.065 MPa to obtain 185.2g of finished sodium hexafluorophosphate with the yield of 83.6 percent;
(7) product detection: purity 99.992%, moisture content 15ppm, free acid 55 ppm.
Example 2
A preparation method of high-purity sodium hexafluorophosphate specifically comprises the following steps:
(1) adding 400g of battery-grade LiPF6 into a cracking reaction kettle under the protection of nitrogen;
(2) heating the cracking reaction kettle to 185 ℃ and preserving heat for 2 hours to decompose LiPF 6;
(3) adding 1000g of EL-grade electronic hydrofluoric acid into a synthesis kettle, adding 112g of high-purity sodium fluoride, stirring and dissolving at 15 ℃ for 3 h;
(4) introducing the gas generated in the step (2) into a synthesis kettle, carrying out fluidization reaction for 4 hours at 25 ℃, and filtering to obtain 1413g of sodium hexafluorophosphate synthetic liquid;
(5) cooling the synthetic mother liquor at a cooling rate of 1 ℃/h to-30 ℃ and 2 ℃/h to-40 ℃, preserving heat for 4h, and filtering;
(6) vacuum drying the solid material at 88 ℃ and-0.095 MPa to obtain 408.3g of finished sodium hexafluorophosphate product with the yield of 92.3 percent;
product detection: purity 99.995%, moisture content 13ppm, free acid 52 ppm.
Example 3
The sodium hexafluorophosphate prepared by the invention is placed under an XDR diffractometer for analysis, the prepared spectrogram is shown in figure 1, and is compared and analyzed with an X-ray spectrogram (figure 2) of a standard substance (lithium hexafluorophosphate), and by observing the number of diffraction peaks, the peak shape, the angle position and the relative intensity, the sodium hexafluorophosphate can be known as follows: the purity of the sodium hexafluorophosphate prepared by the invention is higher than the standard.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. A preparation method of high-purity sodium hexafluorophosphate comprises the following steps:
(1) adding the battery-grade LiPF6 into a cracking reaction kettle under the protection of nitrogen;
(2) heating the cracking reaction kettle to a certain temperature and preserving the temperature for a period of time to completely decompose the LiPF 6;
(3) adding a proper amount of solvent into a synthesis kettle, adding a certain amount of high-purity sodium fluoride, and stirring and dissolving at a certain temperature;
(4) introducing the gas generated in the step (2) into a synthesis kettle, and carrying out fluidized reaction under certain conditions to obtain sodium hexafluorophosphate synthetic liquid;
(5) after the reaction is finished, filtering the synthetic liquid to remove insoluble substances to obtain synthetic mother liquid;
(6) cooling and crystallizing the synthetic mother liquor, and filtering;
(7) and (4) carrying out vacuum drying on the solid material to obtain a finished product of sodium hexafluorophosphate, and recycling the crystallization mother liquor for dissolving sodium fluoride.
2. The method for preparing high-purity sodium hexafluorophosphate according to claim 1, wherein the method comprises the following steps: the cracking reaction kettle in the step (1) comprises a heating jacket and an inner cylinder, wherein the inner cylinder is made of 316L materials, and the inner cylinder is sealed with a sealing head.
3. The method for preparing high-purity sodium hexafluorophosphate according to claim 1, wherein the method comprises the following steps: the certain temperature in the step (2) is 85-190 ℃, and the heat preservation time is 4-12 h.
4. The method for preparing high-purity sodium hexafluorophosphate according to claim 1, wherein the method comprises the following steps: the solvent in the step (3) is photovoltaic hydrofluoric acid or electronic hydrofluoric acid or crystallization mother liquor, the purity of the sodium fluoride is 99.98% or more, the silicon content is less than or equal to 0.00005%, and the silicon content is calculated by SiO 2.
5. The method for preparing high-purity sodium hexafluorophosphate according to claim 1, wherein the method comprises the following steps: the dosage of the sodium fluoride in the step (3) is 2.5-5 g/100g of solvent, the stirring and dissolving temperature is 10-50 ℃, the dissolving pressure is 0-30kpa, and the dissolving time is 1-2 h.
6. The method for preparing high-purity sodium hexafluorophosphate according to claim 1, wherein the method comprises the following steps: the certain conditions in the step (4) are that the reaction temperature is 5-55 ℃, the pressure is 0-80kpa, and the reaction time is 4-10 h.
7. The method for preparing high-purity sodium hexafluorophosphate according to claim 1, wherein the method comprises the following steps: and (4) in the step (6), the cooling speed of the cooling crystallization is 1 ℃/h, the cooling is carried out to-30 ℃, 2 ℃/h, the cooling is carried out to-40 ℃, and the heat preservation is carried out for 2-4 h.
8. The method for preparing high-purity sodium hexafluorophosphate according to claim 1, wherein the method comprises the following steps: in the step (7), the temperature of the vacuum drying is 60-90 ℃, and the vacuum degree is-0.06-0.1 Mpa.
9. The method for preparing high-purity sodium hexafluorophosphate according to claim 1, wherein the method comprises the following steps: the crystallization mother liquor can be repeatedly used for dissolving high-purity sodium fluoride.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115676855A (en) * | 2022-12-30 | 2023-02-03 | 江苏华盛锂电材料股份有限公司 | Preparation method of sodium ion battery electrolyte sodium salt |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1433960A (en) * | 2003-03-08 | 2003-08-06 | 汕头市金光高科有限公司 | Method and equipment for synthesizing hexafluorophosphate |
| US20100322838A1 (en) * | 2007-02-08 | 2010-12-23 | Stella Chemifa Corporation | Method of manufacturing phosphorous pentafluoride and hexafluorophosphate |
| CN106536412A (en) * | 2014-03-31 | 2017-03-22 | 南非核能源股份有限公司 | Production of hexafluorophosphate salt and phosphorous pentafluoride |
| CN113353958A (en) * | 2021-07-29 | 2021-09-07 | 上海绿麟达新材料科技有限公司 | Clean production process of hexafluorophosphate |
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- 2021-09-29 CN CN202111151265.8A patent/CN113772694A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1433960A (en) * | 2003-03-08 | 2003-08-06 | 汕头市金光高科有限公司 | Method and equipment for synthesizing hexafluorophosphate |
| US20100322838A1 (en) * | 2007-02-08 | 2010-12-23 | Stella Chemifa Corporation | Method of manufacturing phosphorous pentafluoride and hexafluorophosphate |
| CN106536412A (en) * | 2014-03-31 | 2017-03-22 | 南非核能源股份有限公司 | Production of hexafluorophosphate salt and phosphorous pentafluoride |
| CN113353958A (en) * | 2021-07-29 | 2021-09-07 | 上海绿麟达新材料科技有限公司 | Clean production process of hexafluorophosphate |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115676855A (en) * | 2022-12-30 | 2023-02-03 | 江苏华盛锂电材料股份有限公司 | Preparation method of sodium ion battery electrolyte sodium salt |
| CN115676855B (en) * | 2022-12-30 | 2023-04-11 | 江苏华盛锂电材料股份有限公司 | Preparation method of sodium ion battery electrolyte sodium salt |
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Application publication date: 20211210 |