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Method and device for preparing lithium hexafluorophosphate through dynamic crystallization

A technology of lithium hexafluorophosphate and crystallization, which is applied in the directions of lithium hexafluorophosphate, chemical instruments and methods, lithium compounds, etc., can solve the problems of long crystallization time and uneven growth of crystal particles, and achieves simple structure, improved production efficiency and product quality, and reasonable design. Effect

Active Publication Date: 2016-05-25
DO FLUORIDE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to provide a method for preparing lithium hexafluorophosphate by dynamic crystallization, so as to solve the problems in the prior art that the crystal grains of lithium hexafluorophosphate grow unevenly and the crystallization time is long

Method used

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  • Method and device for preparing lithium hexafluorophosphate through dynamic crystallization
  • Method and device for preparing lithium hexafluorophosphate through dynamic crystallization
  • Method and device for preparing lithium hexafluorophosphate through dynamic crystallization

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Embodiment 1

[0038] The dynamic crystallization of the present embodiment prepares the device of lithium hexafluorophosphate, such as figure 1As shown, it includes a crystallization kettle 1 with a stirring device 11, and the outside of the crystallization kettle is provided with an external circulation pipeline 2 connected to the upper and lower parts of the crystallization kettle respectively, so as to realize the circulating flow of materials inside and outside the crystallization kettle. An ultrasonic probe 13 is provided on the outer circulation pipeline to realize ultrasonic-induced nucleation in the initial stage of crystallization, and a circulation pump is also provided; the upper peripheral panel of the crystallization kettle is provided with a refrigerant pipeline 3 for controlling the cooling rate, and the lower peripheral panel is provided with a heat sink. The medium pipe 4 is used to make a little crystal on the inner wall of the kettle come off, and simultaneously make the s...

Embodiment 2

[0041] The dynamic crystallization of the present embodiment prepares the device of lithium hexafluorophosphate, such as figure 2 As shown, the structure of the crystallization kettle is the same as that in Example 1, and also includes a filter drying integrated machine 8, which is used to simultaneously realize filter drying of the lithium hexafluorophosphate suspension obtained after dynamic crystallization; The liquid port is connected. The all-in-one filtering and drying machine includes a shell, and a filter plate 12 is arranged at the bottom of the inside of the shell, and a stirring device 11 located above the filter plate is arranged inside the shell, and a heat medium pipeline 4 is arranged on the outer plate of the shell. An inert gas inlet 5 and a waste gas outlet 7 are provided at the upper end of the filtering and drying integrated machine 8, a filtrate outlet 9 is provided at the lower end, and a finished product outlet 10 is provided at the side, and its height...

Embodiment 3

[0044] The method for preparing lithium hexafluorophosphate by dynamic crystallization in this embodiment, the process flow is as follows image 3 As shown, the device used is as figure 2 shown, including the following steps:

[0045] 1) Inject the hydrogen fluoride liquid into the reaction kettle that has been added with 1.2 tons of phosphorus pentachloride, wherein the weight ratio of hydrogen fluoride liquid: phosphorus pentachloride is 1:1, and hydrogen fluoride reacts with phosphorus pentachloride at 80°C and 0.18MPa Produce a mixed gas of phosphorus pentafluoride and hydrogen chloride;

[0046] 2) Pass the mixed gas obtained in step 1) into the reaction kettle that has been added with lithium fluoride and hydrogen fluoride liquid, the dosage of lithium fluoride is 0.126 tons, and react at 10°C and 0.1MPa to obtain A total of 7.776 tons of lithium hexafluorophosphate solution, hydrogen chloride gas is regularly discharged and absorbed by water to produce hydrochloric a...

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Abstract

The invention discloses a method and device for preparing lithium hexafluorophosphate through dynamic crystallization. The method includes the following steps of 1, ultrasound induced nucleation, wherein a lithium hexafluorophosphate solution is cooled to minus 10-minus 15 DEG C within 2-3 hours under the action of ultrasonic waves, and a crystallization solution A is obtained; 2, stirring and crystallization, wherein the crystallization solution A is crystallized while being stirred at the cooling rate of 2-3 DEG C / h, and lithium hexafluorophosphate suspension liquid is obtained; filtering and drying are conducted, and the lithium hexafluorophosphate is obtained. According to the method, at the early stage of crystallization, ultrasound induced nucleation is adopted so that the lithium hexafluorophosphate can be subjected to homogeneous nucleation in a supersaturated interface stability zone; gradient cooling crystallization is achieved at a certain cooling rate under the stirring condition along with change of the concentration of the lithium hexafluorophosphate, so that crystal nucleus grows gradually, and a product with even particle size is obtained; the purity of the obtained product reaches 99.99%, the particle size is 40-120 meshes, the whole crystallization process only needs 6-13 hours, wall hanging does not occur easily in the crystallization process, and good economic benefits and social benefits are achieved.

Description

technical field [0001] The invention belongs to the technical field of lithium ion batteries, and in particular relates to a method and a device for preparing lithium hexafluorophosphate by dynamic crystallization. Background technique [0002] Lithium-ion batteries are mainly composed of casing, positive electrode material, negative electrode material, electrolyte and separator. Among them, the electrolyte is the key material of lithium-ion batteries, known as the "blood" of lithium-ion batteries. The main components of the electrolyte are lithium salt electrolytes and organic solvents. Among various types of electrolytes, lithium hexafluorophosphate (LiPF 6 ) is currently the most commonly used electrolyte in lithium-ion batteries, with excellent overall performance. [0003] At present, the most widely used method for industrial production of lithium hexafluorophosphate is the hydrofluoric acid solvent method, that is, phosphorus pentafluoride reacts with lithium fluori...

Claims

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Application Information

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IPC IPC(8): C01D15/00
CPCC01D15/005C01P2006/80
Inventor 侯红军李云峰杨华春薛旭金于贺华郭海涛李霞薛峰峰李磊王建萍
Owner DO FLUORIDE CHEM CO LTD
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