Method for preparing lithium hexafluorophosphate by using composite solvent

A technology of lithium hexafluorophosphate and composite solvent, which is applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve problems such as failure to realize large-scale industrialization, and achieve the effects of easy reaction, simple production process and good effect.

Inactive Publication Date: 2012-06-13
山东省智能光电新能源研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

From the current point of view, the above-mentioned technologies have more or less problems, and have not achieved large-scale industrialization.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A method for producing lithium hexafluorophosphate material with a composite solvent, the steps are as follows: (1) react with anhydrous orthophosphoric acid, calcium fluoride and sulfur oxide, control the temperature at 70-80°C, react for 2-4 hours, and then raise the temperature of the system To 180 ~ 220 ℃, evaporate PF 5 gas; the reactive formula is:

[0027] 2H 3 PO 4 +5CaF 2 +5SO 3 =2PF 5 + 5CaSO 4 +3H 2 O;

[0028] (2) The evaporated PF 5 After the gas is cooled through a stainless steel tube with a diameter of Ф5-8mm at an ambient temperature of 4-6°C, it is dehydrated through a 4A zeolite molecular sieve to obtain high-purity anhydrous PF 5 Products, in which the zeolite molecular sieves are dried at 400-600°C for 0.5-2 hours, each use of molecular sieves and PF 5 The weight ratio is 1: (10-100);

[0029] (3) Dehydrate diethyl ether and anhydrous acetonitrile with 4A zeolite molecular sieves dried at 500°C, the weight ratio of molecular sieve to diet...

Embodiment 2

[0038] The method for producing lithium hexafluorophosphate material with a composite solvent, the steps are as follows: (1) react with anhydrous orthophosphoric acid, calcium fluoride and sulfur oxide, the temperature is controlled at 80°C, react for 4 hours, then raise the temperature of the system to 180°C, evaporate PF 5 gas; the reactive formula is:

[0039] 2H 3 PO 4 +5CaF 2 +5SO 3 =2PF 5 + 5CaSO 4 +3H 2 O;

[0040] (2) The evaporated PF 5 After the gas is cooled through a stainless steel tube with a diameter of Ф8mm at an ambient temperature of 5°C, it is dehydrated through a 4A zeolite molecular sieve to obtain high-purity anhydrous PF 5 The product, in which the zeolite molecular sieve is dried at 500°C for 1 hour, each time the molecular sieve and PF are used 5 The weight ratio is 1: (10-100);

[0041] (3) Diethyl ether and anhydrous acetonitrile were dehydrated with 4A zeolite molecular sieves dried at 500°C respectively. The weight ratio of molecular sie...

Embodiment 3

[0050] A method for producing lithium hexafluorophosphate material with a composite solvent is as follows: (1) React with 117g of anhydrous orthophosphoric acid, 390g of calcium fluoride and 400g of sulfur oxide in a sealed stainless steel kettle, the temperature is controlled at 80°C, and the reaction is carried out for 4 hours, and then the The temperature of the system is raised to 180°C, and 252gPF is evaporated 5 Gas (2mol); the reaction molecular formula is:

[0051] 2H 3 PO 4 +5CaF 2 +5SO 3 =2PF 5 + 5CaSO 4 +3H 2 O;

[0052] (2) Use high-purity nitrogen as a catalyst to remove the evaporated PF 5 After the gas is cooled through a stainless steel tube with a diameter of Ф5-8mm at an ambient temperature of 4°C, it is dehydrated through 2520 g4A zeolite molecular sieves to obtain high-purity anhydrous PF 5 The product, in which the zeolite molecular sieve is dried at 500°C for 1 hour, each time the molecular sieve and PF are used 5 The weight ratio is 1: (10-100)...

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Abstract

The invention relates to a safe and reliable method for preparing lithium hexafluorophosphate by using a composite solvent. The technical steps of the method are simple. The method comprises steps that: anhydrous phosphoric acid, calcium fluoride and sulfur oxide are subject to a reaction, such that PF5 gas is obtained by evaporation; the evaporated PF5 gas is dehydrated, such that a high-purity anhydrous PF5 product is obtained; diethyl ether and anhydrous methyl cyanide are respectively dehydrated, such that high-purity diethyl ether and anhydrous methyl cyanide are obtained; high-purity lithium fluoride is added to the diethyl ether solution; methyl cyanide is added to the obtained solution; the PF5 gas is slowly delivered into the solution while stirring; when a reaction is finished, high-purity nitrogen is delivered into the solution, such that displacement is carried out until no PF5 gas is remained in a vessel; a dry product Li(CH3CN)4PF6 obtained through distillation is heatedand decomposed, such that LiPF6 is prepared; LiPF6 is dissolved under room temperature, such that a solution with a concentration of 1M is obtained; the solution is filtered by using a precise filterwith a specification of 0.2mum, such that a clarified solution is obtained; the solution is dried, such that a pure LiPF6 product is obtained.

Description

[0001] technical field [0002] The invention relates to a method for manufacturing lithium hexafluorophosphate material, in particular to a method for manufacturing lithium hexafluorophosphate material with a composite solvent. Background technique [0003] Lithium hexafluorophosphate (LiPF 6 ), as a lithium-ion battery electrolyte material, can make lithium-ion batteries have excellent specific energy and energy density, and has received widespread attention since the middle of the last century. It has the following advantages as lithium ion battery electrolyte lithium salt: [0004] 1. Form an appropriate SEI film on the electrode, especially on the carbon negative electrode; [0005] 2. Effective passivation of the positive current collector to prevent its dissolution; [0006] 3. It has a wider electrochemical stability window; [0007] 4. Appropriate solubility and high conductivity in various non-aqueous solvents; [0008] 5. Relatively good environmental friendl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/455H01M10/0568
CPCY02E60/12Y02E60/10
Inventor 宗哲徐涛
Owner 山东省智能光电新能源研究院
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