Method for preparing Lithium bis(oxalate)borate

A lithium oxalate borate and lithium bisoxalate borate technology, which is applied in the field of preparing high-purity lithium oxalate borate, can solve the problems of cumbersome steps, affecting product purity, and high cost

Active Publication Date: 2008-04-30
ZHANGJIAGANG HUASHENG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These two methods all have the following problems: in the further drying process, it is easy to cause decomposition and generate lithium hyd...

Method used

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  • Method for preparing Lithium bis(oxalate)borate
  • Method for preparing Lithium bis(oxalate)borate
  • Method for preparing Lithium bis(oxalate)borate

Examples

Experimental program
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Effect test

Embodiment 1

[0095]In a three-necked flask containing 157.3 g (1.334 mol) of methyl oxalate, 30 g (0.4854 mol) of boric acid, and 22 g (0.524 mol) of lithium hydroxide, the temperature was raised to 110° C. under stirring, and the generated methanol was extracted. The temperature is gradually increased to 250°C until there is almost no extraction; the vacuum is turned on to keep the system vacuum at -100Pa, dried for 8-12 hours, and cooled to obtain a solid powder. Use 1000g of acetonitrile as a solvent to feed the reaction product, stir at room temperature for 1 to 2 hours, and filter to obtain a filter cake. After analyzing the components of the filter cake with infrared spectroscopy, it is known that the filter cake is lithium monooxalate borate. Carry out rectification under reduced pressure on the filtrate obtained above, recover 30~60℃ / 2~5kPa distillate 843g, the still material after concentration, filter, obtain filter cake, dry 60℃ / 80Pa, 71g; Through infrared spectrum analysis, γ: ...

Embodiment 2

[0097] In a three-neck flask containing 194.8 g (1.334 mol) of ethyl oxalate, 30 g (0.4854 mol) of boric acid, and 22 g (0.524 mol) of lithium hydroxide, the temperature was raised to 110° C. under stirring, and the generated ethanol was extracted. The temperature is gradually increased to 250°C until there is almost no extraction; the vacuum is turned on to keep the system vacuum at -100Pa, dried for 8-12 hours, and cooled to obtain a solid powder. Use 1000g of acetonitrile as a solvent to feed the reaction product, stir at room temperature for 1 to 2 hours, and filter to obtain a filter cake. After analyzing the components of the filter cake with infrared spectroscopy, it is known that the filter cake is lithium monooxalate borate. Carry out rectification under reduced pressure on the filtrate obtained above, recover 30~60℃ / 2~5kPa distillate 853g, filter the still material after concentration, obtain filter cake, dry 60℃ / 80Pa, 73g; Analyze by infrared spectrum, γ: 1818, 1781...

Embodiment 3

[0099] In a three-necked flask containing 269.5 g (1.334 mol) of butyl oxalate, 17 g (0.2427 mol) of boron oxide, and 22 g (0.524 mol) of lithium hydroxide, the temperature was raised to 110° C. under stirring. The temperature was gradually raised to 250°C, and the produced butanol was extracted until almost no extraction; the vacuum was turned on, and the vacuum of the system was kept at -100Pa, dried for 8-12 hours, and cooled to obtain a solid powder. Use 1000g of acetonitrile as a solvent to feed the reaction product, stir at room temperature for 1 to 2 hours, and filter to obtain a filter cake. After analyzing the components of the filter cake with infrared spectroscopy, it is known that the filter cake is lithium monooxalate borate. Carry out rectification under reduced pressure on the filtrate obtained above, recover 30~60℃ / 2~5kPa distillate 813g, filter the still material after concentration, obtain filter cake, dry 60℃ / 80Pa, 69g; Analyze by infrared spectrum, γ: 1818,...

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Abstract

The invention provides a method for preparing lithium oxalate borate, the method comprising: using alkyl oxalate and a boron-containing compound as raw materials, neutralizing with an alkaline lithium reagent to generate a reaction mixture containing lithium oxalate borate; The lithium reagent is selected from lithium hydroxide or alkaline lithium salts. The preparation method of the invention avoids product decomposition during the drying process, thereby effectively improving product yield and purity.

Description

technical field [0001] The invention relates to a method for preparing lithium oxalate borate, in particular to a method for preparing high-purity lithium oxalate borate. Background technique [0002] Lithium oxalate borate products usually have purity requirements. For example, lithium bisoxalate borate in lithium oxalate borate products is mainly used in the lithium-ion electrolyte of high-power lithium batteries, which can effectively improve its high-temperature cycle performance, especially in the electrolyte of hybrid lithium batteries. The purity of lithium bisoxalate borate has a direct impact on the performance of the electrolyte. [0003] For this reason, it is necessary to obtain a preparation method that is easy to separate and obtain high-purity lithium oxalate borate. [0004] In the existing lithium oxalate borate product, such as the synthesis research of lithium bisoxalate borate, a method that has been reported is to take oxalic acid as a raw material, an...

Claims

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Application Information

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IPC IPC(8): C07F5/02
Inventor 张先林杨志勇刘东汪许诚曹晓东
Owner ZHANGJIAGANG HUASHENG CHEM CO LTD
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