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A kind of preparation method of high-purity lithium oxalate

A technology of pure lithium oxalate and lithium oxalate, which is applied in the field of preparation of high-purity lithium oxalate, can solve the problems of not being able to meet the production requirements of lithium difluorooxalate borate, not suitable for large-scale production, and difficult process control, etc., and achieve low content of impurity elements , cheap raw materials, simple process

Active Publication Date: 2019-02-05
HUBEI BAIJIERUI ADVANCED MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Because of this, it is very necessary to produce high-purity lithium oxalate with excellent performance. At present, the traditional method for preparing lithium oxalate is to neutralize lithium carbonate or lithium hydroxide with oxalic acid. The purity of lithium oxalate produced is not high. The process control is not easy, it is not suitable for large-scale production, and cannot meet the demand for the production of lithium difluorooxalate borate

Method used

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  • A kind of preparation method of high-purity lithium oxalate

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Embodiment 1

[0016] A preparation method of high-purity lithium oxalate, the steps are as follows:

[0017] (1) Add 300kg of industrial-grade lithium hydroxide monohydrate into 1500L of pure water, dissolve in a plastic container, stir until the solution is clear, and obtain an industrial-grade lithium hydroxide solution. Weigh 450kg of oxalic acid (mass content ≥ 99.9%) with a molar ratio of 1:2 to the lithium element, stir and dissolve in an enamel container with 450L of pure water at a temperature of 90°C to obtain an oxalic acid solution, and slowly add 90kg of the oxalic acid solution into industrial-grade lithium hydroxide In the solution, stir until the reaction is complete, let it stand for 10 minutes, filter and remove impurities until the solution is clear, and obtain a filtered lithium hydroxide solution.

[0018] (2) Take 162kg from the remaining oxalic acid solution in step (1) and add it to the reactor, stir, then slowly add the filtered lithium hydroxide solution obtained in...

Embodiment 2

[0022] A preparation method of high-purity lithium oxalate, the steps are as follows:

[0023] (1) Add 300kg of industrial-grade lithium hydroxide monohydrate into 1500L of pure water, dissolve in a plastic container, stir until the solution is clear, and obtain an industrial-grade lithium hydroxide solution. Weigh 450kg of oxalic acid (mass content ≥ 99.9%) with a molar ratio of 1:2 to lithium, stir and dissolve in an enamel container with 675L of pure water at a temperature of 95°C to obtain an oxalic acid solution, and slowly add 169kg of oxalic acid solution into industrial grade lithium hydroxide solution, stirred until complete reaction, stood still for 20 min, filtered to remove impurities until the solution was clear, and filtered lithium hydroxide solution was obtained.

[0024] (2) Take 239kg from the remaining oxalic acid solution in step (1) and add it to the reactor, stir, then slowly add the filtered lithium hydroxide solution obtained in step (1), until a small ...

Embodiment 3

[0028] A preparation method of high-purity lithium oxalate, the steps are as follows:

[0029] (1) Add 400kg of industrial-grade lithium hydroxide monohydrate into 2000L of pure water, dissolve in a plastic container, stir until the solution is clear, and obtain an industrial-grade lithium hydroxide solution. Weigh 600kg of oxalic acid (mass content ≥ 99.9%) with a molar ratio of 1:2 to lithium, stir and dissolve in an enamel container with 750L of pure water at a temperature of 100°C to obtain an oxalic acid solution, take 135kg of the oxalic acid solution and slowly add industrial grade lithium hydroxide In the solution, stir until the reaction is complete, let it stand for 30 minutes, filter and remove impurities until the solution is clear, and obtain a filtered lithium hydroxide solution.

[0030] (2) Take 364kg from the remaining oxalic acid solution in step (1) and add it to the reactor, stir, then slowly add the filtered lithium hydroxide solution obtained in step (1),...

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Abstract

The invention belongs to the technical field of preparing methods of electrolyte lithium salt used for a lithium ion battery, and discloses a preparing method for high-purity lithium oxalate. The preparing method includes the steps that 1, an oxalic acid solution is prepared, 10-20% of the oxalic acid solution is added into an industrial grade lithium hydroxide solution, and filtration and impurity removal are carried out until the solution is clear; 20-30% of the remaining oxalic acid solution in the step 1 is added into a reaction kettle, the lithium hydroxide solution filtered in the step 1 is added until a small amount of white precipitate is generated at the bottom, after full reaction, the remaining filtered lithium hydroxide solution and the oxalic acid solution are added into the reaction kettle at the same time and continuously stirred, the temperature is 50-80 DEG C, the pH value is adjusted to 7.0-7.5, and the mixed solution continues to be stirred for 10-30 min; 3, the temperature of the oxalic acid solution in the step 2 is controlled to lower to the normal temperature at the speed of 5-15 DEG C / h, and the oxalic acid solution stands until lithium oxalate sinks to the bottom completely; lithium oxalate is dried. The preparing method is simple in technical process, high in feasibility, safe and environmentally friendly, and product quality is high.

Description

technical field [0001] The invention relates to the technical field of preparation methods of electrolyte lithium salts for lithium ion batteries, in particular to a preparation method of high-purity lithium oxalate. Background technique [0002] In recent years, with the rapid development of the lithium-ion battery industry, the research and development of its electrolyte lithium salt has become increasingly hot, and new lithium salts with new structures and functions have been reported. The most representative and development prospect in the world is lithium difluorooxalate borate (LiODFB). It combines lithium tetrafluoroborate (LiBF 4 ) and lithium bisoxalate borate (LiBOB), the thermal decomposition temperature is as high as 240 ° C, basically no corrosion to electrode materials, good cycle performance, low moisture sensitivity, good high and low temperature performance, rate performance and positive and negative electrode compatibility, etc. Advantages, all aspects of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/41C07C55/07
CPCC07C51/412C07C55/07
Inventor 赵正红李兴徐涛
Owner HUBEI BAIJIERUI ADVANCED MATERIALS
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