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Purifying process of biethyl diacid lithium borate

A technology of lithium bisoxalate borate and lithium oxalate borate is applied in the field of purification of lithium bisoxalate borate, and can solve the problems of high water content, inability to use lithium ion batteries, low main content and the like

Active Publication Date: 2007-07-18
QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI
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  • Claims
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Problems solved by technology

Therefore, many people currently believe that the product obtained by method 2 is suitable for lithium-ion battery electrolyte lithium salt requirements, while the product obtained by method 1 cannot be applied to lithium-ion batteries because the main content is too low and the water content is too high

Method used

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  • Purifying process of biethyl diacid lithium borate
  • Purifying process of biethyl diacid lithium borate

Examples

Experimental program
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Embodiment 1

[0023] Example 1, 8.10 g of raw materials were added into 100 mL of pretreated fresh anhydrous acetonitrile, and stirred until the dissolution equilibrium was reached. Filter to remove insoluble matter. The filtrate was concentrated by evaporation (it is better to evaporate 1 / 10 of the amount of solvent added). The concentrated solution is stored at -10~-35°C for 2 hours. Solid-liquid separation was carried out by suction filtration. The obtained solid was dried in a vacuum oven for 30 hours (vacuum degree 0.06-0.095Mpa, drying temperature slowly increased from room temperature to 82°C) to obtain a white granular solid substance, which was the purified LiBOB product. The yield and analysis results are shown in Table 1.

[0024] Embodiment 2, using the LiBOB product obtained in Example 1 as a raw material, repeat the steps described in Example 1. The resulting LiBOB product yield and analysis results are shown in Table 1.

[0025] Embodiment 3, using the LiBOB product obta...

Embodiment 4

[0026] Example 4, 6.80 g of raw materials were added into 100 mL of pretreated fresh anhydrous acetone, and stirred until the dissolution equilibrium was reached. Filter to remove insoluble matter. The filtrate was concentrated by evaporation (1 / 20 of the added solvent was distilled off). The concentrated liquid is placed under the freezing condition of -10~-40℃ for 3h. Solid-liquid separation was carried out by suction filtration. The obtained solid was dried in a vacuum oven for 24 hours (the vacuum degree was 0.06-0.095 Mpa, and the drying temperature was slowly increased from room temperature to 57° C.) to obtain a white granular solid substance. The resulting product was purified once more as described above. The resulting LiBOB product yield and analysis results are shown in Table 1.

Embodiment 5

[0027] Example 5, 4.20 g of raw materials were added into 100 mL of pretreated fresh anhydrous tetrahydrofuran, and stirred until the dissolution equilibrium was reached. Filter to remove insoluble matter. The filtrate was concentrated by evaporation (1 / 20 of the added solvent was distilled off). The concentrated liquid is placed under the freezing condition of -10~-40℃ for 3h. Solid-liquid separation was carried out by suction filtration. The obtained solid was dried in a vacuum oven for 24 hours (the vacuum degree was 0.06-0.095 Mpa, and the drying temperature was slowly increased from room temperature to 66° C.) to obtain a white granular solid substance. The resulting product was purified once more as described above. The resulting LiBOB product yield and analysis results are shown in Table 1.

[0028] Table 1 LiBOB product yield and analysis results

[0029]

[0030] Considering the price and toxicity of the selected solvent and combining the implementation...

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Abstract

The process of purifying LiBOB includes the following steps: dissolving LiBOB material with low LiBOB content and high water content in dried and re-distilling treated polar non-protonic solvent to form saturated solution, filtering and evaporating to concentrate; freezing at -10 deg.c to -40 deg.c for 1-5 hr; and vacuum drying to obtain purified LiBOB product. The purified LiBOB product, the infrared spectrum analysis and 13C and 11B nuclear magnetic resonance spectrum show, has total content of Li, B and oxalate ions greater than 99.30 wt%. After twice purifications, the product has water content as low as 0.0014 wt% and the contents of Na, K, Ca, Mg and Fe lower than 0.0020 wt%, 0.0010 wt%, 0.0010 wt%, 0.00040 wt% and 0.00080 wt% separately, and may be used as the lithium salt for lithium ion cell electrolyte.

Description

technical field [0001] The invention belongs to the field of chemical industry, and relates to a method for purifying lithium bisoxalate borate (abbreviated as LiBOB) which can be used as an electrolyte for lithium-ion batteries. Background technique [0002] Lithium salts used in commercialized lithium-ion batteries are mainly LiFP 6 , but its thermal stability is poor, easy to hydrolyze, and low temperature conductivity is low. Therefore, the development of LiFP 6 New lithium salts with better stability, no hydrolysis and wider temperature range have become a research focus in the battery field. The current research on new lithium salts mainly focuses on lithium borate complexes and lithium phosphate complexes. Among them, lithium bisoxalate borate (LiBOB for short) attracts the most attention. [0003] As a new type of electrolyte lithium salt, LiBOB has good thermal and chemical stability, high electrical conductivity and wide electrochemical window. Even in pure PC s...

Claims

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Application Information

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IPC IPC(8): C07F5/04H01M10/40H01M10/0568
CPCY02E60/122Y02E60/10
Inventor 李世友马培华邓小川李法强任齐都
Owner QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI
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