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Method for purifying lithium bis(oxalate)borate

A technology of lithium oxalate borate and lithium oxalate borate, which is applied in the chemical industry, can solve the problems of low reaction degree, poor mixing uniformity of raw materials, and unsuitability for large-scale industrial production, and achieve simple purification process, low impurity content, The effect of fast dissolution

Inactive Publication Date: 2012-11-07
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the solid-phase reaction method has the disadvantages of poor mixing uniformity of raw materials, difficult precise control of the reaction process, and low reaction degree. Therefore, the purification method of LiBOB synthesized based on the solid-state reaction method is not suitable for large-scale industrial production.
These purification methods use acetonitrile, acetone, tetrahydrofuran, ethyl acetate and other polar aprotic solvents to purify the LiBOB crude product. Although the impurity content is greatly reduced, the purified product still has about 3% in the electrolyte. insoluble matter
In addition, solvents such as acetonitrile and ethyl acetate used in the purification process are difficult to completely remove, and trace amounts of residual solvents will affect the quality of LiBOB and reduce the high-temperature cycle performance of lithium-ion batteries

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 100 g of LiBOB crude product and pretreated and dried molecular sieves to 800 ml of pretreated anhydrous propylene carbonate, and stir until the solution is balanced. Filter to remove insoluble matter. The filtrate was evaporated and concentrated under vacuum at 100-160°C. The amount of solvent evaporated is about 1 / 3 ~ 4 / 5 of the added amount. Strain while hot. After the filter cake is washed with hot toluene, it is placed in a vacuum drying oven and dried at 80°C for 24 to 48 hours. The obtained white solid substance is 45 g of purified LiBOB.

Embodiment 2

[0028] Add 100 g of LiBOB crude product and pretreated and dried molecular sieve into 800 ml of pretreated anhydrous ethylene carbonate, and stir until the solution is balanced. Filter to remove insoluble matter. The filtrate was evaporated and concentrated under vacuum at 100-160°C. The amount of solvent evaporated is about 1 / 5 of the added amount. The concentrate is placed at -40~10°C for 2~24 hours. After solid-liquid separation, the filtrate was washed with hot toluene, placed in a vacuum drying oven, and dried at 80°C for 24 to 48 hours. The obtained white solid substance is LiBOB 17g after purification.

Embodiment 3

[0030] Add 50 g of LiBOB crude product and pretreated and dried molecular sieves to 400 ml of pretreated anhydrous propylene carbonate, and stir until the solution is balanced. Filter to remove insoluble matter. Put the filtrate in a flask, and add 200 ~ 2000 ml of toluene under constant stirring. A large amount of white crystals precipitated. After standing still for a while, filter, the filter cake is washed with hot toluene, placed in a vacuum drying oven, and dried at 80°C for 24 to 48 hours. The obtained white solid substance is 37 g of purified LiBOB.

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Abstract

The invention provides a method for purifying lithium bis(oxalate)borate, comprising the following steps of: dissolving a lithium bis(oxalate)borate crude product in an aprotic solvent, carrying out molecular sieve drying, filtering, carrying out evaporative concentration, carrying out thickening crystallization or mixed solvent crystallization, and repeating the steps to obtain high-purity lithium bis(oxalate)borate. C13-NMR spectrogram of the purified lithium bis(oxalate)borate is a single peak and its peak appearance location is 158.6 ppm. B11-NMR spectrogram is a single peak and its peak appearance location is 7.37 ppm. The content of metal impurity ions is determined by ICP. Contents of iron, chromium, sodium and nickel are respectively lower than 9 ppm, 1.1 ppm, 5 ppm and 0.4 ppm. The quality of the product accords with requirements of an electrolyte for lithium ion cells, and simultaneously the product is rapidly dissolved in the electrolyte. The purification technology provided by the invention is simple and easy to operate, and is suitable for industrial batch production.

Description

[0001] technical field [0002] The invention belongs to the field of chemical industry and relates to a method for purifying lithium bisoxalate borate (LiBOB) which can be used as electrolyte of lithium ion battery. Background technique [0003] As an important part of lithium-ion batteries, electrolytes are crucial to the performance of lithium-ion batteries. The choice of electrolyte determines the working mechanism of the battery to a large extent, affecting the specific energy, safety, cycle performance, storage performance and cost of the battery. At present, the electrolyte used in commercial lithium-ion batteries is mainly LiFP 6 , which has poor thermal stability, is sensitive to moisture, is easily hydrolyzed, and has low low-temperature conductivity. [0004] In the study of new organic electrolyte lithium salts, new lithium borate salts are various and environmentally friendly, and have attracted more and more attention in recent years. LiBOB is the most likel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/02
Inventor 黄剑莹吴茂祥卢碧强王文国潘荧方桂煌
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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