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Co-production method for lithium oxalyldifluoroborate and lithium tetrafluoroborate

A technology of lithium oxalate difluoroborate and lithium tetrafluoroborate is applied in chemical instruments and methods, boron halide compounds, compounds containing elements of Group 3/13 of the periodic table, etc. The problem of unevenness and high product yield can achieve the effect of low production cost, high product purity and high product yield.

Inactive Publication Date: 2013-10-30
LANZHOU UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It uses Li 2 C 2 o 4 or LiF and BF 3 Reaction, but the requirements for reaction equipment and raw materials are high, and the reaction is not uniform
It is also possible to use LiF and (C 2 h 5 ) 2 O·BF 3 Obtained by direct reaction, the yield of the product obtained by this method is high but the purification is difficult

Method used

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  • Co-production method for lithium oxalyldifluoroborate and lithium tetrafluoroborate
  • Co-production method for lithium oxalyldifluoroborate and lithium tetrafluoroborate
  • Co-production method for lithium oxalyldifluoroborate and lithium tetrafluoroborate

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Experimental program
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Effect test

Embodiment 1

[0014] The coproduction method of lithium oxalate difluoroborate and lithium tetrafluoroborate, the steps are:

[0015] (1) Add 10g of lithium oxalate and 25mL of anhydrous diethyl ether dried at 120°C for 4 hours into a dry reactor equipped with a stirrer and stir evenly, then add 24.6mL of BF 3 ·O(C 2 h 5 ) 2 (BF 3 The concentration is 45%~47%) solution, heat reflux and stir, to ensure that the raw materials are fully mixed. React at 80°C for 6h, filter and separate the solid-liquid mixture after the reaction, and then dry the separated solid at 50°C to 170°C under normal pressure for 6h, add a desiccant to the drying oven, and continue drying for 6h, Get LiODFB and LiBF 4 mixture of crude products.

[0016] (2) The crude product mixture was dissolved in 25 mL of diethyl carbonate in a reactor with a stirrer, and stirred and refluxed at 110° C. for 3 h. After the solution was filtered, it was evaporated at 110°C, and after reaching a saturated solution, it was crystal...

Embodiment 2

[0021] The coproduction method of lithium oxalate difluoroborate and lithium tetrafluoroborate, the steps are:

[0022] (1) will BF 3 Gas passes through H 2 o 2 0.1%~0.2%,H 2 O 2%~10% and H 2 SO 4 90% to 98% of the absorption liquid is washed and passed into the buffer bottle. Weigh 9g Li 2 C 2 o 4 Add 30mL of pretreated fresh anhydrous acetonitrile to the 100mL three-neck flask containing the magnetron, and slowly pass the purified BF from the buffer bottle into it under stirring conditions. 3 , heated up to 80°C, condensed and refluxed for 14h, and filtered with suction. The filtrate was concentrated until anhydrous acetonitrile was distilled off, the heating was stopped, the remaining liquid was concentrated, cooled and crystallized, the obtained solid was suction filtered and dried at 150°C and a vacuum of 0.08 MPa for 24 hours to obtain a white solid, which was detected as LiODFB and LiBF 4 Mixture of crude products.

[0023] (2) The mixture of crude products w...

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Abstract

The invention discloses a co-production method for lithium oxalyldifluoroborate and lithium tetrafluoroborate. The co-production method comprises the following steps of: (1) uniformly mixing compounds containing lithium salts and BF3 in an aprotic nonpolar solvent or a solvent with a low aprotic polarity in a molar ratio of (1: 1: 3)-(1: 1.25: 3.75) of lithium to boron to fluorine; (2) refluxing for 1-48 hours at a temperature of 30-100 DEG C, then performing solid-liquid separation, and drying the obtained solid substance to obtain crude products LiODFB and LiBF4; and (3) performing purification and separation on the obtained crude products for one time, or performing purification for many times.

Description

technical field [0001] The present invention relates to lithium oxalate difluoroborate (LiODFB) and lithium tetrafluoroborate (LiBF 4 ) Coproduction preparation. Background technique [0002] LiODFB, as a new type of electrolyte lithium salt, has both LiBF 4 The advantages of LiBOB and LiBOB, such as the ability to form a stable and low-resistance SEI film with propylene carbonate (PC) on the surface of carbon-based electrodes, have almost no dissolution and erosion on manganese and iron-based positive electrode materials, and the electrolyte The high and low temperature performance, cycle performance, and abuse performance of the assembled battery are excellent, making it the most promising new type of lithium salt. [0003] Since LiODFB was first reported, many people have continuously improved its preparation method, initially using LiBF 4 、CH(CF 3 ) 2 OLi, H 2 C 2 o 4 for the raw material as well as Tsujioka et al. using H 2 C 2 o 4 、LiBF 4 and AlCl 3 LiODFB...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/02C01B35/06
Inventor 崔孝玲赵伟徐晓莉史新明赵阳雨李步成张宏明李永立毛丽萍李贵贤李世友
Owner LANZHOU UNIVERSITY OF TECHNOLOGY
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