Preparation method of lithium bis(oxalato)borate

A technology of bisoxalate lithium borate and lithium salt, which is applied in the field of preparation of bisoxalate lithium borate, can solve the problems of increasing the difficulty of preparation operation control, increasing the difficulty of industrialization, and complicated follow-up purification, so as to achieve easy control of operating process conditions and reduce the difficulty of control , The effect of stable product quality

Inactive Publication Date: 2012-08-08
LANZHOU UNIVERSITY OF TECHNOLOGY
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Problems solved by technology

However, since the synthesis process involves a solid-state reaction between three solid raw materials, the reaction is difficult to complete, and the obtained LiBOB mass percentage is generally only about 95%, which cannot be directly used as an electrolyte for electrochemical devices such as lithium-ion batteries. Complicated follow-up purification must be carried out (see CN 1817888A, CN 100999529), thereby greatly reducing the yield of the product and increasing the difficulty of industrialization
[0010] In addition, the above-mentioned LiBOB preparation process needs to be carried out under vacuum or inert gas protection, which further increases the difficulty of controlling the preparation operation.

Method used

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  • Preparation method of lithium bis(oxalato)borate

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preparation example Construction

[0021] The present invention is the preparation method of bisoxalate lithium borate, and its steps are:

[0022] (1) According to the stoichiometric ratio, first mix lithium salt and oxalic acid evenly, then heat at 40°C-70°C for 1-4h, and finally add boron source to the mixture, and mix all materials thoroughly;

[0023] (2) The mixture is dry-pressed under a pressure of 0.1 MPa to 10 MPa, and reacted by heating to obtain a lithium bisoxalate borate product.

[0024] According to the preparation method of lithium bisoxalate borate described above, the lithium salt used can be LiOH, or Li 2 CO 3 , or lithium alkoxide, the boron source used is H 3 B0 3 , or B 2 o 3 , the purity of the raw material is analytically pure, that is, the mass percentage is about 99.5%, or it is a higher-purity superior grade, or it is spectrally pure, or it is high-purity.

[0025] According to the above-mentioned preparation method of lithium bisoxalate borate, the heating reaction is carried ...

Embodiment 1

[0032] Weigh 7.967g H 2 C 2 o 4 2H 2 O (≥99.5%, mass percentage, the same below), 1.326g LiOH·H 2 O (≥99.5%) mixed evenly, and heated at 60°C for 2h, 1.955g H 3 BO 3 (≥99.5%) mixed evenly. The mixed mixture was pressed into tablets (tablet weight about 1.0g) under a pressure of 2 MPa (gauge pressure), and the pressed tablets were placed in a drying oven, dried in the atmosphere at 120°C for 7 hours, and then Phosphorus pentoxide was added to the drying oven, and the temperature was adjusted to 155° C. to continue drying under normal pressure for 40 hours to obtain 6.081 g of LiBOB product. The product yield is about 99.3%. Measure the oxalate content in the product with potassium permanganate titration, and measure the boron content in the product with mannitol titration, which can reach 90.53%, 5.67% (theoretical values ​​are respectively 90.84%, 5.58%); The water content in the product was determined by non-interference Karl Fischer coulometric titration of base form...

Embodiment 2

[0034] H with a purity of 99.9% to 100.1% 2 C 2 o 4 2H 2 O replaces H in Example 1 2 C 2 o 4 2H 2 O, with H of purity ≥99.95% 3 BO 3 Replace H in Example 1 3 BO 3 , and the rest of the steps are the same as Example 1. The contents of oxalate, boron, and moisture in the obtained LiBOB product remained almost unchanged, while the contents of five metal impurity ions, calcium, magnesium, sodium, potassium, and iron, decreased to 0.00032%, 0.00048%, 0.0014%, 0.00049%, and 0.0010%.

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Abstract

A preparation method of lithium bis(oxalato)borate relates to a preparation method of lithium bis(oxalato)borate for electrolyte of electrochemical equipment such as lithium ion batteries, comprising the following steps of: (1) uniformly mixing lithium salt and oxalate according to stoichiometric ratio, heating at 40-70 DEG C for 1-4h, adding a boron source into a mixture, thoroughly and uniformly mixing various kinds of materials; and (2) carrying out dry-pressing molding on the mixture at the pressure of 0.1MPa-10MPa, followed by heating reaction to obtain the lithium bis(oxalato)borate product.

Description

technical field [0001] The invention relates to a preparation method of lithium bisoxalate borate used as an electrolyte for electrochemical devices such as lithium ion batteries. Background technique [0002] At present, the preparation methods of LiBOB mainly include liquid phase method and general solid phase method: [0003] 1. Liquid phase method: the reaction solvent of liquid phase preparation method can be water (as shown in reaction equation (1), see DE 19829030), also can be anhydrous acetonitrile (as shown in reaction equation (2), see W. Xu, A. J. Shusterman. Electrochem. Solid-State Lett., 2001, 4(1): E1-E4). [0004] [0005] [0006] When using water as the reaction solvent, the resulting LiBOB mass percentage content is lower than 95%, which cannot be directly used as the electrolyte of electrochemical devices such as lithium ion batteries, but must carry out complicated follow-up purification (seeing CN 1817888A, CN100999529), thereby greatly reducing...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/02
Inventor 李世友赵阳雨李步成史新明党斌李贵贤崔孝玲
Owner LANZHOU UNIVERSITY OF TECHNOLOGY
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