CN114873577A - Preparation method of sodium hexafluorophosphate - Google Patents
Preparation method of sodium hexafluorophosphate Download PDFInfo
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- CN114873577A CN114873577A CN202210565604.5A CN202210565604A CN114873577A CN 114873577 A CN114873577 A CN 114873577A CN 202210565604 A CN202210565604 A CN 202210565604A CN 114873577 A CN114873577 A CN 114873577A
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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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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- 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
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Abstract
The invention discloses a preparation method of sodium hexafluorophosphate, which comprises the following steps: step 1, dissolving phosphorus pentoxide in a certain proportion in a hydrogen fluoride solution to generate a hexafluorophosphoric acid solution; step 2, slowly adding a sodium source with a certain proportion into the hexafluorophosphoric acid solution prepared in the step 1; step 3, heating the solution reacted in the step 2, and removing water and unreacted hydrogen fluoride by using nitrogen gas for blowing; and 4, heating and concentrating the mother liquor obtained in the step 3, dissolving the obtained sodium hexafluorophosphate crude product into a poor solvent for recrystallization, and cooling and drying to obtain the sodium hexafluorophosphate with the purity of more than 99.87 percent. The sodium hexafluorophosphate is synthesized by the method, reactants are hydrogen fluoride solution, phosphorus pentoxide and a high-purity sodium source, no common impurities in industrial production exist, the purity is high, the raw materials are easy to obtain, the reaction is simple, the reaction process is easy to control, the generation of three wastes is less, the obtained product can be applied to sodium ion batteries, and the dependence on lithium ion batteries is relieved.
Description
Technical Field
The invention relates to the technical field of sodium salt of electrolyte for sodium-ion batteries, in particular to a preparation method of sodium hexafluorophosphate.
Background
At present, the demand for ion batteries has increased in recent years due to the ever-increasing demand for electrical energy production and large-scale grid storage. Although lithium ion batteries currently dominate and are mature, because of the greater sodium content than lithium, the sources are wide and distributed worldwideAnd thus is less susceptible to geopolitical price fluctuations and is inexpensive, so that the sodium ion battery has a wider development space. In the periodic table, sodium underlies lithium and therefore the general principles of both batteries are the same, knowledge in the lithium ion battery field helps to accelerate the research and development of sodium ion batteries. During the charging and discharging process, the sodium ion battery system works like a pendulum bob as the sodium ions swing between the two electrodes. During charging, Na + Escapes from the cathode, diffuses through the electrolyte to the anode, and reacts with the anode material. The discharge process is reversed.
NaPF 6 The electrolyte salt has the most application prospect and mainly has the following advantages: (1) the conductive material has higher conductivity, and can enable the battery to have excellent performances such as high energy density, long cycle performance, low self-discharge rate and the like; (2) sodium ion batteries are highly safe and environmentally friendly and are favored for large-scale applications; (3) the storage mechanism of the sodium ion battery is similar to that of a non-aqueous system, the working voltage of the sodium ion battery is far lower than that of an organic solvent electrolyte system and is about 1.23V; (4) has good solubility and higher conductivity in various non-aqueous solvents.
However, NaPF 6 The method has the defects of poor thermal stability, easy deliquescence, more impurities in industrial production, low purity and the like, and can not meet the purity requirement of the sodium ion battery electrolyte, so that the method needs to continuously develop a good sodium ion battery electrolyte with high performance and can avoid the defects.
Chinese patent application publication No. CN113772694A discloses a method for preparing high-purity sodium hexafluorophosphate, in which battery-grade lithium hexafluorophosphate is cracked and dissolved in high-purity hydrogen fluoride, and then sodium fluoride is added to the solution to replace lithium ions. The lithium hexafluorophosphate adopted by the method has higher price, the lithium resource is limited, and the transportation, storage and reaction all need high requirements.
The Chinese patent with application publication number CN108217622A discloses a preparation method of sodium hexafluorophosphate: reacting hexafluorophosphate with a sodium source in a medium to obtain a crude solution of sodium hexafluorophosphate, removing unreacted raw materials contained in the crude solution, and recrystallizing to obtain pure sodium hexafluorophosphate. The method has complex reaction conditions, and impurities are easily introduced in the reaction, so that the purity is reduced.
Chinese patent application publication No. CN108946769A discloses a method for preparing sodium hexafluorophosphate, which comprises introducing phosphorus pentafluoride gas into a reactor containing lithium fluoride and hydrogen fluoride liquid, and crystallizing and drying while stirring. The phosphorus pentafluoride used in the method has strong corrosivity and strong toxicity, and has higher requirements on transportation and production.
Accordingly, those skilled in the art have made an effort to develop a method for preparing sodium hexafluorophosphate to overcome the above-mentioned problems.
Disclosure of Invention
In view of the above-mentioned defects of the prior art, the technical problem to be solved by the present invention is to provide a new method for preparing sodium hexafluorophosphate, which provides an electrolyte for a sodium ion battery.
In order to realize the purpose, the invention provides a preparation method of sodium hexafluorophosphate, which comprises the following steps:
step 1, dissolving phosphorus pentoxide in a certain proportion in a hydrogen fluoride solution to generate a hexafluorophosphoric acid solution;
step 2, slowly adding a sodium source in a certain proportion into the hexafluorophosphoric acid solution prepared in the step 1;
step 3, heating the solution reacted in the step 2, and removing water and unreacted hydrogen fluoride by using nitrogen gas for blowing;
and 4, heating and concentrating the mother liquor obtained in the step 3, dissolving the obtained sodium hexafluorophosphate crude product into a poor solvent for recrystallization, and cooling and drying to obtain the sodium hexafluorophosphate with the purity of more than 99.87%.
Further, the molar ratio of the phosphorus pentoxide to the hydrogen fluoride in the step 1 is 1: 10-14.
Further, the reaction temperature in the step 1 is-30 ℃ to 30 ℃, and the reaction time is 1 to 6 hours.
Further, the sodium source in the step 2 is one or more of sodium hydroxide, sodium fluoride and metal sodium which are uniformly mixed according to any proportion.
Further, the molar ratio of the sodium source to the hexafluorophosphoric acid in the step 2 is 1-2: 1.
Further, the reaction temperature in the step 2 is-20 ℃ to 30 ℃, and the reaction time is 1 to 6 hours.
Further, the heating temperature in the step 3 is 20-80 ℃, the heating time is 1-5 hours, and preferably, the step 3 further comprises refluxing the gas generated after heating through a condenser to obtain a dilute hydrogen fluoride solution.
Further, the heating temperature in the step 4 is 100-140 ℃, the heating time is 4-8 hours, and preferably, the step 4 further comprises purging with nitrogen so as to remove water vapor and other impurities.
Further, the poor solvent in the step 4 is one or more of dimethyl carbonate, ethyl methyl carbonate, diethyl carbonate, ethylene carbonate, propylene carbonate and ethyl acetate, and is uniformly mixed according to any proportion.
Further, the drying in the step 4 comprises forced air drying and vacuum drying, wherein the forced air drying temperature is 60-80 ℃, and the drying time is 6-8 hours; the vacuum degree of vacuum drying is-0.05 to-0.10 MPa.
Compared with the prior art, the invention has the advantages that:
the sodium hexafluorophosphate is synthesized by the method, reactants are hydrogen fluoride solution, phosphorus pentoxide and a high-purity sodium source, no common impurities in industrial production exist, the purity is high, the raw materials are easy to obtain, the reaction is simple, the reaction process is easy to control, the generation of three wastes is less, the obtained product can be applied to sodium ion batteries, and the dependence on lithium ion batteries is relieved.
The conception, the specific structure, and the technical effects produced by the present invention will be further described below to fully understand the objects, the features, and the effects of the present invention.
Detailed Description
The following describes several preferred embodiments of the present invention to make the technical contents thereof clearer and easier to understand. The present invention may be embodied in many different forms of embodiments and the scope of the invention is not limited to the embodiments set forth herein.
Example 1
The preparation method of sodium hexafluorophosphate of the embodiment comprises the following steps:
(1) adding 71g of phosphorus pentoxide into a reaction kettle, slowly adding 120g of anhydrous hydrogen fluoride through an automatic feeding device, fully stirring, controlling the reaction temperature to be-3 ℃ and the reaction time to be 2 hours;
(2) slowly adding 42g of sodium fluoride into the solution in the step (1) through an automatic batch feeder, and reacting for 3 hours at-10 ℃;
(3) heating the solution to 65 ℃ for 4 hours after the reaction, purging by using nitrogen to remove water and unreacted hydrogen fluoride, and connecting the discharged tail gas with a condensing device for recycling;
(4) and (3) heating and concentrating the mother liquor obtained in the step (3) at 120 ℃ for 6 hours, dissolving the obtained sodium hexafluorophosphate crude product in dimethyl carbonate, continuously stirring for 2 hours at 50 ℃, and putting the obtained solid into an oven for drying at 60 ℃ for 6 hours to obtain 167g of sodium hexafluorophosphate with the purity of 99.87%.
Example 2
The preparation method of sodium hexafluorophosphate of the embodiment comprises the following steps:
(1) adding 213g of phosphorus pentoxide into a reaction kettle, slowly adding 300g of anhydrous hydrogen fluoride through an automatic feeding device, fully stirring, controlling the reaction temperature to be-3 ℃ and the reaction time to be 2 hours;
(2) slowly adding 126g of sodium fluoride into the solution in the step (1) through an automatic batch feeder, and reacting for 3 hours at-10 ℃;
(3) heating the solution to 65 ℃ for 4 hours after the reaction, purging by using nitrogen to remove water and unreacted hydrogen fluoride, and connecting the discharged tail gas with a condensing device for recycling;
(4) and (3) heating and concentrating the mother liquor obtained in the step (3) at 120 ℃ for 6 hours, dissolving the obtained sodium hexafluorophosphate crude product in dimethyl carbonate, continuously stirring for 2 hours at 50 ℃, and putting the obtained solid into an oven for drying at 60 ℃ for 6 hours to obtain 503g of sodium hexafluorophosphate with the purity of 99.91%.
Example 3
The preparation method of sodium hexafluorophosphate of the embodiment comprises the following steps:
(1) adding 355g of phosphorus pentoxide into a reaction kettle, slowly adding 550g of anhydrous hydrogen fluoride through an automatic feeding device, fully stirring, controlling the reaction temperature to be-3 ℃ and the reaction time to be 2 hours;
(2) slowly adding 210g of sodium fluoride into the solution in the step (1) through an automatic batch feeder, and reacting for 3 hours at-10 ℃;
(3) heating the solution to 65 ℃ for 4 hours after the reaction, purging by using nitrogen to remove water and unreacted hydrogen fluoride, and connecting the discharged tail gas with a condensing device for recycling;
(4) and (3) heating and concentrating the mother liquor obtained in the step (3) at 120 ℃ for 6 hours, dissolving the obtained sodium hexafluorophosphate crude product in dimethyl carbonate, continuously stirring for 2 hours at 50 ℃, and putting the obtained solid in an oven for drying at 60 ℃ for 6 hours to obtain 838g of sodium hexafluorophosphate with the purity of 99.96 percent.
Example 4
The preparation method of lithium difluoroborate of the embodiment comprises the following steps:
(1) adding 447.3g of phosphorus pentoxide into a reaction kettle, slowly adding 882g of anhydrous hydrogen fluoride through an automatic feeding device, fully stirring, controlling the reaction temperature to be-3 ℃ and the reaction time to be 2 hours;
(2) slowly adding 264.6g of sodium fluoride into the solution in the step (1) through an automatic batch feeder, and reacting for 3 hours at-10 ℃;
(3) heating the solution to 65 ℃ for 4 hours after the reaction, purging by using nitrogen to remove water and unreacted hydrogen fluoride, and connecting the discharged tail gas with a condensing device for recycling;
(4) and (3) heating and concentrating the mother liquor obtained in the step (3) at 120 ℃ for 6 hours, dissolving the obtained sodium hexafluorophosphate crude product in dimethyl carbonate, continuously stirring for 2 hours at 50 ℃, and putting the obtained solid into an oven for drying at 60 ℃ for 6 hours to obtain 1058.4g of sodium hexafluorophosphate with the purity of 99.98%.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.
Claims (10)
1. The preparation method of sodium hexafluorophosphate is characterized by comprising the following steps of:
step 1, dissolving phosphorus pentoxide in a certain proportion in a hydrogen fluoride solution to generate a hexafluorophosphoric acid solution;
step 2, slowly adding a sodium source in a certain proportion into the hexafluorophosphoric acid solution prepared in the step 1;
step 3, heating the solution reacted in the step 2, and removing water and unreacted hydrogen fluoride by using nitrogen gas for blowing;
and 4, heating and concentrating the mother liquor obtained in the step 3, dissolving the obtained sodium hexafluorophosphate crude product into a poor solvent for recrystallization, and cooling and drying to obtain the sodium hexafluorophosphate with the purity of more than 99.87%.
2. The method for preparing sodium hexafluorophosphate according to claim 1, wherein the molar ratio of phosphorus pentoxide to hydrogen fluoride in step 1 is 1: 10 to 14.
3. The method for preparing sodium hexafluorophosphate of claim 1, wherein the reaction temperature in step 1 is-30 ℃ to 30 ℃ and the reaction time is 1 to 6 hours.
4. The method for preparing sodium hexafluorophosphate of claim 1, wherein the sodium source in step 2 is one or more of sodium hydroxide, sodium fluoride and metallic sodium which are uniformly mixed in any proportion.
5. The method for preparing sodium hexafluorophosphate according to claim 1, wherein the molar ratio of the sodium source to the hexafluorophosphoric acid in step 2 is 1-2: 1.
6. The method for preparing sodium hexafluorophosphate of claim 1, wherein the reaction temperature in step 2 is-20 ℃ to 30 ℃ and the reaction time is 1 to 6 hours.
7. The method for preparing sodium hexafluorophosphate of claim 1, wherein the heating temperature in step 3 is 20 ℃ to 80 ℃ and the heating time is 1 to 5 hours, preferably, step 3 further comprises refluxing the gas generated after heating through a condenser to obtain a dilute hydrogen fluoride solution.
8. The method for preparing sodium hexafluorophosphate according to claim 1, wherein the heating temperature in step 4 is 100 ℃ to 140 ℃ and the heating time is 4 to 8 hours, preferably, step 4 further comprises purging with nitrogen gas to remove water vapor and other impurities.
9. The method for preparing sodium hexafluorophosphate of claim 1, wherein said poor solvent in step 4 is one or more selected from dimethyl carbonate, ethyl methyl carbonate, diethyl carbonate, ethylene carbonate, propylene carbonate, and ethyl acetate, and is mixed uniformly in any proportion.
10. The method for preparing sodium hexafluorophosphate according to claim 1, wherein the drying in step 4 comprises forced air drying and vacuum drying, wherein the temperature of forced air drying is 60-80 ℃, and the drying time is 6-8 hours; the vacuum degree of vacuum drying is-0.05 to-0.10 MPa.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115385365A (en) * | 2022-10-26 | 2022-11-25 | 如鲲(江苏)新材料科技有限公司 | Preparation method of hexafluorophosphate solution, product and application thereof |
| CN115924880A (en) * | 2022-12-09 | 2023-04-07 | 湖北九宁化学科技有限公司 | Method for preparing sodium hexafluorophosphate by water phase method and application thereof |
| CN116924437A (en) * | 2023-09-19 | 2023-10-24 | 深圳新宙邦科技股份有限公司 | Sodium salt preparation method and sodium ion battery |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115385365A (en) * | 2022-10-26 | 2022-11-25 | 如鲲(江苏)新材料科技有限公司 | Preparation method of hexafluorophosphate solution, product and application thereof |
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| CN115924880A (en) * | 2022-12-09 | 2023-04-07 | 湖北九宁化学科技有限公司 | Method for preparing sodium hexafluorophosphate by water phase method and application thereof |
| CN115924880B (en) * | 2022-12-09 | 2023-07-04 | 湖北九宁化学科技有限公司 | Method for preparing sodium hexafluorophosphate by aqueous phase method and application thereof |
| CN116924437A (en) * | 2023-09-19 | 2023-10-24 | 深圳新宙邦科技股份有限公司 | Sodium salt preparation method and sodium ion battery |
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