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A kind of preparation method of lithium dioxalate borate

A technology of lithium bisoxalate borate and lithium bisoxalate borate, which is applied in the field of preparation of lithium bisoxalate borate, can solve the problems of difficult large-scale production, complex process, and low product purity, and increase the atomic diffusion distance , simple process, precise control of the effect of reaction conditions

Inactive Publication Date: 2012-02-22
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The technical problem to be solved by the present invention is: provide a kind of preparation method of bisoxalate lithium borate, adopt the mixing under the liquid phase condition, react and solid-phase burning, through oxalate compound, lithium salt and boron-containing compound in The synthesis reaction occurs under air conditions, and lithium bisoxalate borate with higher purity and higher yield is obtained, which overcomes the disadvantages of complex process, low product purity and difficulty in large-scale production in the electrolyte process of the prior art

Method used

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  • A kind of preparation method of lithium dioxalate borate
  • A kind of preparation method of lithium dioxalate borate
  • A kind of preparation method of lithium dioxalate borate

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Effect test

Embodiment 1

[0030] In the first step, raw materials are mixed under liquid phase conditions to form raw material slurry

[0031] 28.42 grams of analytically pure solid raw material ammonium oxalate, 13.38 grams of lithium iodide and 6.18 grams of boric acid are added in 240 grams of ethanol aqueous solution, wherein the mol ratio of solid raw material is ammonium oxalate: lithium iodide: boron=2: 1: 1, The aqueous ethanol solution is prepared according to the mass ratio of ethanol: water=1:1, the mass ratio of the solid raw material mixture to the aqueous ethanol solution is 1:5, and is stirred and mixed evenly at 40° C. to form a raw material slurry;

[0032] The second step, liquid phase reaction makes lithium bisoxalate borate slurry

[0033] Place the raw material slurry obtained in the first step in an airtight container, raise the temperature to 120°C under the condition of nitrogen atmosphere and pressure of 0.2MPa, react for 3 hours, then cool down to room temperature to obtain di...

Embodiment 2

[0038] In the first step, raw materials are mixed under liquid phase conditions to form raw material slurry

[0039] 29.84 grams of analytically pure solid raw material ammonium oxalate, 13.38 grams of lithium iodide and 3.48 grams of diboron trioxide are added in 46.7 grams of ethanol aqueous solution, wherein the mol ratio of solid raw material is ammonium oxalate: lithium iodide: boron=2.1:1 : 1, the aqueous ethanol solution is prepared according to the mass ratio of ethanol: water=3: 1, the mass ratio of the solid raw material mixture to the aqueous ethanol solution is 5: 5, and is stirred and mixed evenly at 60° C. to form a raw material slurry;

[0040] The second step, liquid phase reaction makes lithium bisoxalate borate slurry

[0041] Put the raw material slurry obtained in the first step in an airtight container, raise the temperature to 180°C under the condition of argon atmosphere and pressure of 1MPa, react for 1 hour, then cool down to room temperature to obtain b...

Embodiment 3

[0046] In the first step, raw materials are mixed under liquid phase conditions to form raw material slurry

[0047] 29.13 grams of analytically pure solid raw material ammonium oxalate, 13.38 grams of lithium iodide and 3.48 grams of diboron trioxide are added in 138 grams of ethanol aqueous solution, wherein the mol ratio of solid raw material is ammonium oxalate: lithium iodide: boron=2.05: 1 : 1, the aqueous ethanol solution is prepared according to the mass ratio of ethanol: water=2: 1, the mass ratio of the solid raw material mixture and the aqueous ethanol solution is 2: 5, stirred and mixed evenly at 50° C. to form a raw material slurry;

[0048] The second step, liquid phase reaction makes lithium bisoxalate borate slurry

[0049] Put the raw material slurry obtained in the first step in an airtight container, raise the temperature to 150°C under the condition of nitrogen atmosphere and pressure of 0.4MPa, react for 2 hours, then cool down to room temperature, and obt...

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Abstract

A kind of preparation method of lithium bisoxalate borate of the present invention relates to boron compound, and its process step is: the first step, raw material is mixed under the liquid phase condition and forms raw material slurry: analytically pure solid raw material ammonium oxalate, lithium iodide and The boron-containing oxygen compound is added to the aqueous ethanol solution, stirred and mixed evenly to form a raw material slurry; the second step, liquid phase reaction to prepare lithium bisoxalate borate slurry: the raw material slurry obtained in the first step is placed in an airtight container Inside, react to prepare lithium bisoxalate borate slurry; the third step, solid-phase burning to obtain lithium bisoxalate borate finished product: place the lithium bisoxalate borate slurry prepared in the second step in a vacuum oven , dried to powder, then placed in an electric furnace, heated to 200-240°C at a rate of 5-10°C / min, and then kept at this temperature for 1-6 hours to obtain the finished product of lithium bisoxalate borate. The process of the method of the invention is simple, and the obtained lithium bisoxalate borate product has high purity and high yield, and is suitable for large-scale production.

Description

technical field [0001] The technical scheme of the present invention relates to boron compound, specifically a kind of preparation method of bisoxalate lithium borate. Background technique [0002] Lithium bisoxalate borate (abbreviated as LiBOB) is mainly used as an electrolyte salt for lithium-ion batteries, especially for power lithium-ion batteries. [0003] German patent 19829030C1 discloses a method for synthesizing LiBOB using lithium hydroxide (or lithium carbonate), oxalic acid, boric acid (or boron oxide) as raw materials, and water, toluene or tetrahydrofuran as a reaction medium. Its disadvantage is that in the synthesis process of the patented method, if water is used as the reaction medium, the reaction is difficult to control because LiBOB is easy to deliquescence; if an organic solvent is used as the reaction medium, complex operations such as distillation and reflux are involved in the synthesis process, which is not conducive to Mass production. [0004] ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F5/02
Inventor 梁广川乔建辉
Owner HEBEI UNIV OF TECH
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