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Preparation method of sodium hexafluorophosphate

A technology of sodium hexafluorophosphate and hexafluorophosphoric acid, which is applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of high toxicity, achieve the effects of less three wastes, ease dependence, and easy control of the reaction process

Pending Publication Date: 2022-08-09
JIANGSU XINTAI MATERIALS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Phosphorus pentafluoride used in this method is highly corrosive and highly toxic, and puts forward higher requirements for transportation and production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The preparation method of the sodium hexafluorophosphate of the present embodiment comprises the following steps:

[0030] (1) in the reaction kettle, add 71g of phosphorus pentoxide, slowly add anhydrous hydrogen fluoride 120g by automatic feeding device, fully stir, control the reaction temperature to be -3 ℃, and the reaction times is 2 hours;

[0031] (2) slowly add 42g sodium fluoride to the solution of step (1) by automatic feeder, react 3 hours at -10 ℃;

[0032] (3) After the reaction, the solution was heated to 65°C for 4 hours, and the water and unreacted hydrogen fluoride were removed by nitrogen purging, and the exhaust gas discharged at the same time was connected to the condensing device for recycling;

[0033] (4) The mother liquor obtained in step (3) was heated and concentrated at 120°C for 6 hours, the obtained crude product of sodium hexafluorophosphate was dissolved in dimethyl carbonate, and the obtained solid was continuously stirred at 50°C for 2 ...

Embodiment 2

[0035] The preparation method of the sodium hexafluorophosphate of the present embodiment comprises the following steps:

[0036] (1) in the reaction kettle, add 213g of phosphorus pentoxide, slowly add anhydrous hydrogen fluoride 300g by automatic feeding device, fully stir, control the reaction temperature to be -3 ℃, and the reaction times is 2 hours;

[0037] (2) slowly add 126g sodium fluoride to the solution of step (1) by automatic feeder, react 3 hours at -10 ℃;

[0038] (3) After the reaction, the solution was heated to 65°C for 4 hours, and the water and unreacted hydrogen fluoride were removed by nitrogen purging, and the exhaust gas discharged at the same time was connected to the condensing device for recycling;

[0039] (4) The mother liquor obtained in step (3) was heated and concentrated at 120°C for 6 hours, the obtained crude product of sodium hexafluorophosphate was dissolved in dimethyl carbonate, and the obtained solid was continuously stirred at 50°C for ...

Embodiment 3

[0041] The preparation method of the sodium hexafluorophosphate of the present embodiment comprises the following steps:

[0042] (1) in the reaction kettle, add 355g of phosphorus pentoxide, slowly add anhydrous hydrogen fluoride 550g by automatic feeding device, fully stir, control the reaction temperature to be-3 ℃, and the reaction times is 2 hours;

[0043] (2) slowly add 210g of sodium fluoride to the solution of step (1) by automatic feeder, react at -10 ℃ for 3 hours;

[0044] (3) After the reaction, the solution was heated to 65°C for 4 hours, and the water and unreacted hydrogen fluoride were removed by nitrogen purging, and the exhaust gas discharged at the same time was connected to the condensing device for recycling;

[0045] (4) The mother liquor obtained in step (3) was heated and concentrated at 120°C for 6 hours, the obtained crude product of sodium hexafluorophosphate was dissolved in dimethyl carbonate, and the obtained solid was continuously stirred at 50°...

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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 in a certain proportion into the hexafluorophosphoric acid solution prepared in the step 1; step 3, heating the solution after the reaction in the step 2, and removing water and unreacted hydrogen fluoride by nitrogen stripping; 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 sodium hexafluorophosphate with the purity of 99.87% or above. According to the method, sodium hexafluorophosphate is synthesized, reactants are a hydrogen fluoride solution, phosphorus pentoxide and a high-purity sodium source, common impurities in industrial production do not exist, the purity is high, raw materials are easy to obtain, the reaction is simple, the reaction process is easy to control, few three wastes are generated, the obtained product can be applied to a sodium ion battery, and dependence on a lithium ion battery is relieved.

Description

Technical field [0001] The invention relates to the technical field of electrolyte sodium salt for sodium ion batteries, and in particular to a preparation method of sodium hexafluorophosphate. Background technique [0002] Currently, demand for ion batteries has surged in recent years due to growing demand for electrical energy production and large-scale grid storage. Although lithium-ion batteries currently dominate and are well established, sodium-ion batteries have Wider development space. Sodium is located below lithium in the periodic table, so the general principles of the two batteries are the same, and knowledge in the field of lithium-ion batteries can help accelerate research and development of sodium-ion batteries. Sodium-ion battery systems work like a pendulum as sodium ions swing between two electrodes during charge and discharge. During the charging process, Na + Escapes from the cathode, diffuses through the electrolyte to the anode, and reacts with the ...

Claims

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Application Information

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IPC IPC(8): C01B25/455
CPCC01D13/00C01P2006/80Y02E60/10
Inventor 王向东叶志松黄琴李越
Owner JIANGSU XINTAI MATERIALS TECH CO LTD
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