CN115924881A - Method for producing hexafluorophosphate by taking yellow phosphorus as raw material - Google Patents
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- CN115924881A CN115924881A CN202211725358.1A CN202211725358A CN115924881A CN 115924881 A CN115924881 A CN 115924881A CN 202211725358 A CN202211725358 A CN 202211725358A CN 115924881 A CN115924881 A CN 115924881A
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- -1 hexafluorophosphate Chemical compound 0.000 title claims abstract description 48
- OBSZRRSYVTXPNB-UHFFFAOYSA-N tetraphosphorus Chemical compound P12P3P1P32 OBSZRRSYVTXPNB-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- 239000002994 raw material Substances 0.000 title claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 29
- 239000007788 liquid Substances 0.000 claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 22
- 230000008569 process Effects 0.000 claims abstract description 18
- 230000008014 freezing Effects 0.000 claims abstract description 16
- 238000007710 freezing Methods 0.000 claims abstract description 16
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000047 product Substances 0.000 claims abstract description 13
- 150000004673 fluoride salts Chemical class 0.000 claims abstract description 11
- 239000007789 gas Substances 0.000 claims abstract description 11
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims abstract description 9
- 239000012043 crude product Substances 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000000746 purification Methods 0.000 claims abstract description 5
- 239000002904 solvent Substances 0.000 claims description 10
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 9
- 239000003792 electrolyte Substances 0.000 claims description 8
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 7
- 229910052744 lithium Inorganic materials 0.000 claims description 7
- RDOXTESZEPMUJZ-UHFFFAOYSA-N anisole Chemical compound COC1=CC=CC=C1 RDOXTESZEPMUJZ-UHFFFAOYSA-N 0.000 claims description 6
- VAYTZRYEBVHVLE-UHFFFAOYSA-N 1,3-dioxol-2-one Chemical compound O=C1OC=CO1 VAYTZRYEBVHVLE-UHFFFAOYSA-N 0.000 claims description 3
- ZAFNJMIOTHYJRJ-UHFFFAOYSA-N Diisopropyl ether Chemical compound CC(C)OC(C)C ZAFNJMIOTHYJRJ-UHFFFAOYSA-N 0.000 claims description 3
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 claims description 3
- RJUFJBKOKNCXHH-UHFFFAOYSA-N Methyl propionate Chemical compound CCC(=O)OC RJUFJBKOKNCXHH-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
- UZKWTJUDCOPSNM-UHFFFAOYSA-N methoxybenzene Substances CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 claims description 3
- 229940017219 methyl propionate Drugs 0.000 claims description 3
- 229910052698 phosphorus Inorganic materials 0.000 claims description 3
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims 4
- 150000003018 phosphorus compounds Chemical class 0.000 claims 4
- 239000008187 granular material Substances 0.000 claims 2
- 239000000463 material Substances 0.000 abstract description 6
- 239000002253 acid Substances 0.000 abstract description 5
- 230000008878 coupling Effects 0.000 abstract description 3
- 238000010168 coupling process Methods 0.000 abstract description 3
- 238000005859 coupling reaction Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000006467 substitution reaction Methods 0.000 abstract description 3
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 16
- 239000010419 fine particle Substances 0.000 description 8
- OBCUTHMOOONNBS-UHFFFAOYSA-N phosphorus pentafluoride Chemical compound FP(F)(F)(F)F OBCUTHMOOONNBS-UHFFFAOYSA-N 0.000 description 6
- 239000011362 coarse particle Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 4
- 229910013870 LiPF 6 Inorganic materials 0.000 description 4
- 101150058243 Lipf gene Proteins 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 229910013872 LiPF Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 238000004378 air conditioning Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002001 electrolyte material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000005243 fluidization Methods 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- UHZYTMXLRWXGPK-UHFFFAOYSA-N phosphorus pentachloride Chemical compound ClP(Cl)(Cl)(Cl)Cl UHZYTMXLRWXGPK-UHFFFAOYSA-N 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
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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
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Abstract
The invention relates to a method for producing hexafluorophosphate by taking yellow phosphorus as a raw material, belonging to the technical field of hexafluorophosphate production. The invention aims to provide a method for producing hexafluorophosphate by taking yellow phosphorus as a raw material. The method comprises the following steps: a. liquid yellow phosphorus, anhydrous hydrogen fluoride and dry air react to generate PF 5 A crude product; b. PF (particle Filter) 5 Freezing and purifying the crude product, introducing into a reaction kettle containing liquid yellow phosphorus, and igniting to obtain the purified PF 5 A gas; c. PF (particle Filter) 5 Reacting the gas with fluoride salt, extracting the resultant, standing, layering and filtering to obtain liquid hexafluorophosphate. The invention realizes the transverse development of multi-product coupling through material substitution and process innovation, and reduces the resource and energy consumption in the production process. The production process is safe, the danger of reaction is avoided, the purification effect is good, the purity of the obtained hexafluorophosphate is as high as 99.99%, the moisture content is less than 2ppm, and the content of free acid (calculated by HF) is less than 6ppm.
Description
Technical Field
The invention relates to a method for producing hexafluorophosphate by taking yellow phosphorus as a raw material, belonging to the technical field of hexafluorophosphate production.
Background
Hexafluorophosphates, including lithium hexafluorophosphate (LiPF) 6 ) And hexafluorophosphorSodium acid (NaPF) 6 ) The electrolyte is a common electrolyte material for preparing lithium ion batteries or sodium ion batteries. LiPF is used to produce all-electric or hybrid-electric vehicles due to increasing turning 6 The demand for (c) has increased dramatically over the last few years. Thus, liPF 6 The price of (c) has risen by more than 500% over the last 3 years.
The existing methods for producing hexafluorophosphate mainly comprise a gas-solid reaction method, a hydrogen fluoride solution method, an organic solution method and an ion exchange method. Among them, the hydrogen fluoride solution method is the most widely used process at home and abroad. The main advantages of the process are that phosphorus pentafluoride and lithium fluoride are easily dissolved in hydrogen fluoride, the whole reaction is easy to carry out and control, and the reaction speed is high.
The invention patent with publication number CN114538406A discloses a preparation method of high-purity lithium hexafluorophosphate, 1) phosphorus pentachloride reacts with anhydrous hydrofluoric acid or hydrogen fluoride gas to prepare phosphorus pentafluoride; 2) Dissolving LiF in an anhydrous HF solvent, introducing the obtained phosphorus pentafluoride into the anhydrous HF solvent, and reacting to obtain an anhydrous HF solution of lithium hexafluorophosphate; 3) Distilling the obtained anhydrous HF solution of lithium hexafluorophosphate to remove hydrofluoric acid, thereby obtaining solid lithium hexafluorophosphate; 4) And (3) recrystallizing the lithium hexafluorophosphate solid by using supercritical carbon dioxide or liquid carbon dioxide as a solvent to obtain the purified lithium hexafluorophosphate. The process adopts HF solution method, the crystallization is not easy to control, and HF remained in the product is used as complex LiPF 6 The HF exists in the product, and the general method is extremely difficult to reduce the HF mass fraction to 1 × 10 -5 Hereinafter, the product purity is greatly affected; residual HF corrodes the cell materials, thereby affecting cell electrical performance. And the process has high requirements on equipment materials, anti-corrosion measures and production safety measures, increases capital investment and has high production cost.
Disclosure of Invention
Aiming at the defects, the technical problem to be solved by the invention is to provide a method for producing hexafluorophosphate by taking yellow phosphorus as a raw material.
The method for producing hexafluorophosphate by using yellow phosphorus as a raw material comprises the following steps:
a. liquid yellow phosphorus, anhydrous hydrogen fluoride and dry airGas reacts to generate PF 5 A crude product;
b、PF 5 the crude product is purified by freezing and then is introduced into a reaction kettle containing liquid yellow phosphorus for reaction to obtain the purified PF 5 A gas;
c、PF 5 reacting the gas with fluoride salt, controlling the temperature below 15 ℃ in the reaction process, extracting the product by adding a solvent of a lithium battery electrolyte, and filtering by standing and layering to obtain liquid hexafluorophosphate, wherein the fluoride salt is LiF or NaF.
In one embodiment of the invention, in the step b, the freezing temperature for freezing and purifying is-40-15 ℃, and the pressure is less than or equal to 0.5MPa.
In one embodiment of the present invention, in step b, the reaction is carried out at 30 ℃.
In one embodiment of the present invention, in step b, P is formed by the reaction 2 O 3 And c, returning to the step a.
In one embodiment of the present invention, in step c, the fluoride salt is in the form of particles, and the proportion of particles having a particle size of 250 to 380 μm is 25 to 35wt%, and the remainder is particles having a particle size of 100 to 200 μm. In a preferred embodiment of the present invention, the proportion of particles having a particle size of 250 to 380 μm is 30wt%.
In an embodiment of the present invention, in the step c, the solvent of the lithium battery electrolyte is at least one of ethylene glycol dimethyl ether, isopropyl ether, anisole, propylene carbonate, ethyl methyl carbonate, ethylene carbonate, vinylene carbonate and methyl propionate.
In one embodiment of the invention, in the step c, the liquid hexafluorophosphate is concentrated and crystallized and filtered to obtain solid hexafluorophosphate.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention realizes the transverse development of multi-product coupling through material substitution and process innovation, realizes a three-dimensional industrial structure for resource utilization of byproducts and wastes, and reduces the resource and energy consumption in the production process.
2. The production process is safe, and avoidsThe reaction is dangerous, the purification effect is good, and the method can be used for preparing high-purity LiPF 6 Or NaPF 6 。
3. The hexafluorophosphate obtained by the process has the purity of 99.99 percent, the moisture content of less than 2ppm and the free acid (calculated by HF) content of less than 6ppm.
Drawings
FIG. 1 is a process flow diagram of the production of hexafluorophosphate from yellow phosphorus as a raw material in the example of the present invention.
Detailed Description
The invention discloses a method for producing hexafluorophosphate by taking yellow phosphorus as a raw material, which comprises the following steps:
a. liquid yellow phosphorus, anhydrous hydrogen fluoride and dry air react to generate PF 5 A crude product;
b、PF 5 purifying the crude product by freezing, introducing into a reaction kettle containing liquid yellow phosphorus, allowing excessive oxygen to react with yellow phosphorus, and removing oxygen to obtain purified PF 5 A gas;
c、PF 5 reacting the gas with fluoride salt, controlling the temperature below 15 ℃ in the reaction process, extracting the product by adding a solvent of a lithium battery electrolyte, and filtering by standing and layering to obtain liquid hexafluorophosphate, wherein the fluoride salt is LiF or NaF.
The invention starts from reducing the cost, energy requirement and environmental impact of producing hexafluorophosphate, uses yellow phosphorus as a raw material to produce phosphorus pentafluoride, further prepares the hexafluorophosphate, realizes the transverse development of multi-product coupling through material substitution and process innovation, and reduces the resource and energy consumption in the production process. The process has safe production process, avoids the danger of reaction, has good purification effect, and can be used for preparing high-purity hexafluorophosphate.
The moisture content in the drying air of the invention is below 20 wt%.
In one embodiment of the invention, in the step b, the freezing temperature for freezing and purifying is-40-15 ℃, and the pressure is less than or equal to 0.5MPa. By freeze purification, H can be isolated 2 O and HF.
For removing coarse PF 5 The air in the air-conditioning system is,adding liquid yellow phosphorus into a reaction kettle, and reacting to generate P 2 O 3 In one embodiment of the present invention, in step b, the reaction is carried out at 30 ℃.
In order to save cost and realize material recycling, in one embodiment of the invention, in step b, P generated by reaction is 2 O 3 Returning to the step a to replace yellow phosphorus as a reaction raw material.
In one embodiment of the present invention, step c is carried out in a fluidized bed reactor or a jacketed kettle reactor. Preferably, in the step c, the fluoride salt is in a granular form, 25 to 35wt% of particles with the grain diameter of 250 to 380 μm are contained, and the balance is particles with the grain diameter of 100 to 200 μm; it is preferable that the ratio of particles having a particle diameter of 250 to 380 μm is 30wt%. The coarse particles can break the fine particles, and the acting force among the fine particles is reduced. Through the configuration of different particles, the agglomeration of fluoride salt particles is effectively reduced, good fluidization is realized, and the generated hexafluorophosphate is prevented from completely coating solid particles, so that the further reaction is prevented, and the yield and the purity are improved.
In the step c, a solvent of the lithium battery electrolyte which can dissolve hexafluorophosphate, which is commonly used in the art, may be used for the extraction, and in one embodiment of the present invention, the solvent of the lithium battery electrolyte in the step c is at least one of ethylene glycol dimethyl ether, isopropyl ether, anisole, propylene carbonate, ethyl methyl carbonate, ethylene carbonate, vinylene carbonate and methyl propionate.
In one embodiment of the invention, in the step c, the liquid hexafluorophosphate is concentrated and crystallized and filtered to obtain solid hexafluorophosphate.
The following examples are provided to further illustrate the embodiments of the present invention and are not intended to limit the invention to the embodiments described.
Example 1
As shown in fig. 1, the lithium hexafluorophosphate is produced by using yellow phosphorus as a raw material by the following method:
(1) Passing dry air through fluidized bed or reaction kettle to remove excessive liquid yellow phosphorus and anhydrous hydrogen fluoridePF formation at 150 ℃ 5 、H 2 O, and the like.
(2) Introducing the crude phosphorus pentafluoride into a freezing bubble tower, wherein the operation temperature is between 40 ℃ below zero and 15 ℃, the operation pressure of the freezing bubble tower is between 0.0 and 0.5MPa, and carrying out freezing separation on H 2 O and HF. For removing coarse PF 5 Adding liquid yellow phosphorus into the reaction kettle, and igniting at 30 ℃ to generate P 2 O 3 And returning to the first fluidized bed or the first reaction kettle.
(3) Purified PF 5 The gas reacts with LiF in a fluidized bed reactor.
30wt% of coarse LiF particles of 250 to 380 μm and the balance of fine particles of 100 to 200 μm are charged into the fluidized bed reactor. The coarse particles can be used for other functions of crushing the fine particles, and the acting force among the fine particles is reduced. The addition of the coarse particles can effectively reduce the agglomeration of LiF particles and realize good reaction.
The temperature is controlled below 15 ℃ during the reaction. Adding ethylene glycol dimethyl ether (DME) into the product to extract, and filtering the mixture through static layering to obtain liquid LiPF 6 Recovering heat generated by yellow phosphorus combustion for concentrating and crystallizing to obtain solid LiPF 6 And (3) returning the product, insoluble LiF, to the fluidized bed reactor in the step 3.
The purity of the purified lithium hexafluorophosphate product obtained by crystallization in this example was 99.99%, the moisture content was less than 2ppm, and the free acid (calculated as HF) content was less than 6ppm.
Example 2
As shown in fig. 1, the following method is adopted to produce sodium hexafluorophosphate by taking yellow phosphorus as a raw material:
(1) PF is generated in a fluidized bed or a reaction kettle by drying air, excessive liquid yellow phosphorus and anhydrous hydrogen fluoride at the temperature of below 150 DEG C 5 、H 2 O, and the like.
(2) Introducing the crude phosphorus pentafluoride into a freezing bubble tower, wherein the operation temperature is-40 ℃ to 15 ℃, the operation pressure of the freezing bubble tower is 0.0-0.5MPa, and H is separated by freezing 2 O and HF. For removing coarse PF 5 Adding liquid yellow phosphorus into the reaction kettle by using medium air, and igniting at 30 ℃ to generate P 2 O 3 Returning to the first fluidised bed orIn a reaction kettle.
(3) Purified PF 5 The gas is reacted with NaF in a fluidized bed reactor.
In the fluidized bed reactor, 30wt% of coarse NaF particles of 250 to 380 μm are added, and the balance is fine particles of 100 to 200 μm. The coarse particles can be used for other functions of crushing the fine particles, and the acting force among the fine particles is reduced. The addition of the coarse particles can effectively reduce the agglomeration of NaF particles and realize good reaction.
The temperature is controlled below 15 ℃ during the reaction. The resultant is extracted by adding glycol dimethyl ether (DME), and liquid NaPF is obtained by static layered filtration 6 Recovering heat generated by yellow phosphorus combustion, and concentrating and crystallizing to obtain solid NaPF 6 The product, insoluble NaF, was returned to the fluidized bed reactor.
The purified sodium hexafluorophosphate obtained by crystallization in this example has a purity of 99.99%, a moisture content of less than 2ppm, and a free acid (calculated as HF) content of less than 6ppm.
Claims (7)
1. The method for producing the hexafluorophosphate by taking the yellow phosphorus as the raw material is characterized by comprising the following steps of:
a. liquid yellow phosphorus, anhydrous hydrogen fluoride and dry air react to generate PF 5 A crude product;
b、PF 5 the crude product is purified by freezing and then is introduced into a reaction kettle containing liquid yellow phosphorus for reaction to obtain the purified PF 5 A gas;
c、PF 5 reacting the gas with fluoride salt, controlling the temperature below 15 ℃ in the reaction process, extracting the product by adding a solvent of a lithium battery electrolyte, and filtering by standing and layering to obtain liquid hexafluorophosphate, wherein the fluoride salt is LiF or NaF.
2. The process for producing hexafluorophosphate of claim 1, wherein said step of adding said phosphorous compound to said aqueous solution comprises: in the step b, the freezing temperature of freezing purification is-40 to 15 ℃, and the pressure is less than or equal to 0.5MPa.
3. The process for producing hexafluorophosphate of claim 1, wherein said step of adding said phosphorous compound to said aqueous solution comprises: in step b, the reaction is carried out at 30 ℃.
4. The process for producing hexafluorophosphate of claim 1, wherein said step of adding said phosphorous compound to said aqueous solution comprises: in step b, P formed by the reaction 2 O 3 And c, returning to the step a.
5. The process for producing hexafluorophosphate as claimed in claim 1, wherein said process comprises the steps of: in the step c, the fluoride salt is granular, 25 to 35 weight percent of granules with the grain diameter of 250 to 380 mu m are contained, and the balance is granules with the grain diameter of 100 to 200 mu m; it is preferable that the proportion of particles having a particle diameter of 250 to 380 μm is 30% by weight.
6. The process for producing hexafluorophosphate of claim 1, wherein said step of adding said phosphorous compound to said aqueous solution comprises: in the step c, the solvent of the lithium battery electrolyte is at least one of ethylene glycol dimethyl ether, isopropyl ether, anisole, propylene carbonate, methyl ethyl carbonate, ethylene carbonate, vinylene carbonate and methyl propionate.
7. The process for producing hexafluorophosphate as claimed in claim 1, wherein said process comprises the steps of: and c, concentrating and crystallizing the liquid hexafluorophosphate, and filtering to obtain the solid hexafluorophosphate.
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| WANG, H: "Hollow fiber supported ionic liquid membrane microextraction for preconcentration of kanamycin sulfate with electrochemiluminescence detection", JOURNAL OF ELECTROANALYTICAL CHEMISTRY, 1 December 2014 (2014-12-01) * |
| 缪光武: "五氟化磷的制备及纯化技术研究进展", 低温与特气, 28 October 2020 (2020-10-28) * |
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