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Preparation method of electrolyte double-oxalate based lithium borate for lithium ion battery

A technology of lithium oxalate borate and lithium hydrogen oxalate, applied in chemical instruments and methods, compounds containing elements of group 3/13 of the periodic table, organic chemistry, etc., can solve unstable product quality, difficult to control temperature accurately, reaction Complex process and other problems, to achieve the effect of less impurities, sufficient reaction and high degree of reaction

Inactive Publication Date: 2013-04-10
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

This method is difficult to accurately control the temperature and the product quality is not stable
[0009] In patent 200910068837.9, the raw materials are mixed into a slurry in an ethanol aqueous solution under liquid phase conditions, and then reacted in a sealed tank, and then the product is obtained by a solid-phase burning method. The reaction process of this method is complicated

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 4000g of oxalic acid, 600g of lithium hydroxide, 980g of boric acid, and 2500ml of water into the reaction kettle, and raise the temperature to 80°C while stirring, and gradually increase the temperature to 120°C. Xylene was added and produced water was withdrawn until substantially none was produced. Turn on the vacuum and dry at 150° C. for 12 to 24 hours to obtain solid powder lithium bisoxalate borate. Repeatedly dissolving and purifying with acetonitrile for 3 times, the C-NMR spectrum of the product obtained was a single peak with a peak position of 158.6 ppm, and the B-NMR spectrum was a single peak with a peak position of 7.37 ppm.

Embodiment 2

[0025] Add 3980g of oxalic acid, 660g of lithium hydroxide, 930g of boric acid, and 2300ml of water into the reaction kettle, and raise the temperature to 80°C under stirring, and gradually rise to 120°C. Toluene was added, and the produced water was withdrawn until substantially none was produced. Turn on the vacuum and dry at 150° C. for 12 to 24 hours to obtain solid powder lithium bisoxalate borate. Repeatedly dissolving and purifying with acetonitrile for 3 times, the C-NMR spectrum of the product obtained was a single peak with a peak position of 158.6 ppm, and the B-NMR spectrum was a single peak with a peak position of 7.37 ppm.

Embodiment 3

[0027] Add 3500g of oxalic acid, 520g of lithium hydroxide, 870g of boric acid, and 2000ml of water into the reaction kettle, and raise the temperature to 80°C under stirring, and gradually rise to 120°C. Methyl carbonate was added, and produced water was withdrawn until essentially none was produced. Turn on the vacuum and dry at 150° C. for 12 to 24 hours to obtain solid powder lithium bisoxalate borate. Repeatedly dissolving and purifying with ethyl acetate 3 times, the C-NMR spectrum of the obtained product is a single peak, the peak position is 158.6ppm, and the B-NMR spectrum is a single peak, the peak position is 7.37ppm.

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Abstract

The invention provides a preparation method of electrolyte double-oxalate based lithium borate for lithium ion battery and relates to a preparation method of battery level double-oxalate based lithium borate (LiBOB), which is applicable for the field of lithium ion battery and the like. A liquid phase synthesis method is used. The preparation method comprises the following steps of adding reaction raw materials consisting of a lithium compound, a boron compound, an oxalate compound and a solvent into a reaction kettle according to a ratio, heating and reacting under normal pressure, adding a water-carrying agent during the reaction process, and separating out water, thereby obtaining the product. The preparation method is simple in technology and full in reaction; and the double-oxalate based lithium borate product prepared by the preparation method is high in yield and high in purity, thus the preparation method is suitable for large-scale industrial production.

Description

technical field [0001] The invention provides a method for preparing lithium bisoxalate borate (LiBOB). The invention relates to the field of chemical synthesis, in particular to a preparation method of bisoxalyl lithium borate. The lithium bisoxalate borate prepared by the invention is used as the electrolyte of the lithium ion battery. Background technique [0002] Electrolyte is an important part of lithium-ion battery electrolyte. 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. Therefore, the optimization and innovation of the electrolyte system is indispensable for the development of lithium-ion batteries. Currently, the electrolyte salt used in commercial Li-ion batteries is LiPF 6 , is very sensitive to trace water, and the HF generated by reacting with water is easy to corrode the positive electrode material and curre...

Claims

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Application Information

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IPC IPC(8): C07F5/02
Inventor 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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