Synthesis Technology and Synthesis Device of Lithium Difluorophosphate

A technology of lithium difluorophosphate and synthesis process, which is applied in the direction of phosphorus compounds, inorganic chemistry, chemical instruments and methods, etc., can solve the problems of low boiling point and high cost of fluorine-containing silane, and achieve high product quality, low production cost and excellent reaction conditions mild effect

Active Publication Date: 2022-07-01
湖北迈可凯科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent (CN201510639734.9) alcoholylates metaphosphoric acid, then fluorides it with hydrogen fluoride to obtain monofluorophosphoric acid, reacts monofluorophosphoric acid with phosphorus oxyfluoride gas to prepare difluorophosphoric acid, and then reacts with lithium chloride. The whole preparation process has no Water generation, LiPO avoided 2 f 2 Hydrolysis issues, but using chloride salts as lithium source may introduce chloride ion impurities
Another Chinese patent (CN200780031231.7) uses lithium hexafluorophosphate and organosiloxane containing Si-O-Si structure to prepare an electrolyte containing difluorophosphate. The fluorine-containing silane obtained after the reaction has a low boiling point, is easy to remove, and is extremely selective. High, the data shows that no other impurities are introduced, but because lithium hexafluorophosphate is used as the raw material, the cost is relatively high

Method used

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  • Synthesis Technology and Synthesis Device of Lithium Difluorophosphate
  • Synthesis Technology and Synthesis Device of Lithium Difluorophosphate

Examples

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Effect test

Embodiment 1

[0035] Lithium difluorophosphate synthesis devices such as figure 1 As shown, it includes: a reaction unit, a filtration unit, an evaporative crystallization unit, a drying unit, and a recovery unit.

[0036] In this embodiment, the reaction unit is used for the reaction of phosphorus oxygen compound, lithium fluoride and phosphorus pentafluoride; specifically, the reaction unit is composed of A reaction kettle 1 and B reaction kettle 2. Reactor 1 and Reactor B of Reactor 2 are alternately used as the main reactor for the reaction.

[0037] When the A reactor 1 is used as the main reactor, the B reactor 2 is used as the auxiliary reactor, and anhydrous hydrogen fluoride, phosphorus oxide and lithium fluoride are added in the A reactor 1, and anhydrous hydrogen fluoride, phosphorus oxide and lithium fluoride are also added in the B reactor 2. Oxygen compound and lithium fluoride, and then to A reactor 1 Phosphorus pentafluoride gas is introduced into it, and the reaction ends...

Embodiment 2

[0044] The synthesis device of lithium difluorophosphate is different from Embodiment 1 in that the reaction unit of this embodiment only includes one reaction kettle.

Embodiment 3

[0046] The synthesis technique of lithium difluorophosphate adopts the synthesis device in Example 1, and its synthesis technique is such as figure 2 shown, including the following steps:

[0047] (1) A reactor 1 and B reactor 2 are replaced three times with high-purity nitrogen, then to A reactor 1, B reactor 2, respectively, add hydrogen fluoride 1000mL, start agitator;

[0048] (2) under nitrogen protection, add 65g lithium fluoride and 295g phosphorus pentoxide in A reactor 1 three times, and add 65g lithium fluoride and 295g phosphorus pentoxide in B reactor 2 three times, control The temperature of A reactor 1 and B reactor 2 is -8±2°C, and the pressure of nitrogen is 0.1-0.5MPa;

[0049] (3) after stirring for 1h, feed phosphorus pentafluoride gas into the A reactor 1, control the reaction temperature to be 2±2°C, and after the reaction for 8h, obtain the reaction product, and no longer absorb phosphorus pentafluoride in the A reactor 1 gas, then the reaction ends, a...

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Abstract

The invention provides a synthesis process and a synthesis device of lithium difluorophosphate, belonging to the technical field of lithium difluorophosphate synthesis. , the reaction generates lithium difluorophosphate; specifically, under the protection of inert gas, phosphorus oxide compound and lithium fluoride are first added to anhydrous hydrogen fluoride medium, and then phosphorus pentafluoride is introduced to react. The present invention uses phosphorus oxide compound, lithium fluoride and phosphorus pentafluoride as raw materials, and in anhydrous hydrogen fluoride medium, synthesizes lithium difluorophosphate in one step, the technological process is short, and the production cost is low. Compared with using lithium hexafluorophosphate as raw material, the present invention The production cost is lower by more than 50%; the process of the invention does not generate water, does not contain chloride ions, and has high product quality.

Description

technical field [0001] The invention belongs to the technical field of synthesis of lithium difluorophosphate, in particular to a synthesis process of lithium difluorophosphate. In addition, the invention also relates to a synthesis device of lithium difluorophosphate. Background technique [0002] In recent years, lithium difluorophosphate (LiPO 2 F 2 ) as a functional additive with excellent performance, it is widely used in the electrolyte of lithium-ion secondary batteries to improve the chemical stability of lithium hexafluorophosphate (LiPF6), the most commonly used lithium salt in commercial lithium-ion batteries. Extremely sensitive shortcomings. LiPO 2 F 2 A low-impedance interface film can be formed on the surface of the positive and negative electrodes of a lithium-ion battery to suppress side reactions between the electrode and the electrolyte, thereby improving the cycle life of the battery. [0003] With LiPO 2 F 2 It is widely used, and its preparation ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/455
CPCC01B25/455C01P2006/80
Inventor 陈建生梁斌王天桃
Owner 湖北迈可凯科技有限公司
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