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Preparation method of flame-retardant electrolyte by using 2,4,6-trioxo-1,3,5-triazine-triphosphate lithium salt and compound thereof

A lithium triphosphate and electrolyte technology, which is applied in the field of preparation of flame-retardant electrolytes for lithium-ion batteries, can solve the problems of difficulty in meeting the needs of high-performance lithium-ion batteries, few reports of flame-retardant electrolytes, low lithium ion concentration, etc., and achieve high yield , mild conditions and simple preparation process

Active Publication Date: 2020-05-29
SHANDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And low lithium ion concentration, it is difficult to meet the needs of high performance lithium ion batteries
At present, flame retardant electrolytes with high phosphate group and lithium ion content are rarely reported, and 2,4,6-trioxo-1,3,5-triazine-triphosphate lithium salt has not been reported

Method used

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  • Preparation method of flame-retardant electrolyte by using 2,4,6-trioxo-1,3,5-triazine-triphosphate lithium salt and compound thereof
  • Preparation method of flame-retardant electrolyte by using 2,4,6-trioxo-1,3,5-triazine-triphosphate lithium salt and compound thereof
  • Preparation method of flame-retardant electrolyte by using 2,4,6-trioxo-1,3,5-triazine-triphosphate lithium salt and compound thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] [Example 1]: the preparation of TTP:

[0022] Take 60mL of triethyl phosphite (TEP, 0.34mol) into a 200mL three-neck round bottom flask. Under magnetic stirring, divide 14g of trichloroisocyanuric acid (TCCA, 0.06mol) into four batches, slowly add it into triethyl phosphite within 2 hours at room temperature, TCCA dissolves rapidly, and the reaction releases a lot of heat, and releases ethyl chloride alkane gas to obtain a yellow transparent solution. After adding TCCA, raise the temperature to 80-120°C for 8-12 hours, cool to 50°C, evaporate unreacted triethyl phosphite under reduced pressure to obtain 22.9 g of colorless oily liquid, namely 1,3,5-tris Ethylazine-2,4,6-triphosphate (TTP, yield: 78%).

[0023] Adopt same reaction step, the productive rate that carries out reaction with different reactants or under different conditions is as shown in table 1:

[0024] Table 1 The reaction conditions for the preparation of TTP by the reaction of trihaloisocyanuric acid...

Embodiment 2

[0026] [Example 2]: the preparation of TPA:

[0027] Add 23.5g TTP (0.043mol) into 100mL concentrated hydrochloric acid, reflux for 72h under magnetic stirring, cool to 50°C, distill off HCl, ethanol and part of water under reduced pressure, concentrate to 40mL, extract three times with 90mL ethyl acetate, remove untreated Hydrolyzed TTP. The aqueous phase was concentrated to nearly dryness, and dried to constant weight in a vacuum oven at 120°C to obtain 8.9 g of white solid, namely 2,4,6-triketone-1,3,5-triazine-2,4,6 - Triphosphoric acid (TPA, yield: 87%).

[0028] Using the same reaction steps, but extracting with dichloromethane, benzene, toluene or petroleum ether, the yields were 84%, 80%, 82% and 76%, respectively.

[0029] Using the same reaction steps, reflux in concentrated hydrochloric acid for 12h, distill under reduced pressure at 70°C, and extract with ethyl acetate, the yield is 64%.

[0030] The hydrolysis of different ester groups of TTP prepares the produ...

Embodiment 3

[0033] [Example 3] The preparation of 2,4,6-trioxo-1,3,5-triazine-lithium triphosphate, the steps are as follows:

[0034]Take 7.3g of TPA powder (0.02mol) and place it in a beaker, add 20mL of deionized water, stir until completely dissolved, add 60mL of 1mol / L lithium hydroxide solution dropwise to obtain a colorless and clear solution; Reflux for 6 hours, add 20mL of ethanol after cooling, let it stand overnight, a white precipitate is formed, filter with suction, and recrystallize the obtained solid with a liquid of equal volume ratio between deionized water and ethanol, and the obtained pure product is vacuum After drying, 7.5 g of LiTPA white solid was obtained.

[0035] Solubility test: at room temperature, the solubility in an equal volume ratio of ethylene carbonate / dimethyl sulfoxide / N-methylpyrrolidone mixed solvent is 42-87g / L;

[0036] Conductivity test: at room temperature, the conductivity of ethylene carbonate / dimethyl sulfoxide / N-methylpyrrolidone mixed solve...

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Abstract

The invention provides a preparation method of a lithium ion battery flame-retardant electrolyte obtained by compounding high-phosphoric-acid lithium-containing 2,4,6-trioxo-1,3,5-triazine-triphosphate lithium salt, a solvent, an additive and the like. The content of phosphate groups and lithium ions is high, a plurality of lithium ion attachment sites are provided on the premise of realizing a flame-retardant effect, the concentration of lithium ions in the electrolyte is increased, and the use of the flame-retardant additive is reduced. The preparation method is characterized by comprising the following steps: firstly, replacing high-activity chlorine on trichloroisocyanuric acid with phosphite triester to obtain a phosphate compound; hydrolyzing the ester compound to obtain a phosphategroup product; dissolving a lithium salt, the intermediate phosphate and other additives in an organic solvent, and compounding to obtain the novel flame-retardant lithium ion battery electrolyte. Thenovel electrolyte can be used for electrolytes of a lithium ion battery, a lithium oxygen battery and a lithium sulfur battery.

Description

technical field [0001] The invention relates to a preparation method of a flame-retardant electrolyte for a lithium-ion battery, which can not only improve the conductivity of the electrolyte, but also have a good flame-retardant effect, and can be used for lithium-ion batteries, lithium-oxygen batteries or lithium-sulfur battery field. Background technique [0002] As an important part of lithium-ion batteries, electrolyte plays a key role in improving the cycle stability and energy density of lithium-ion batteries. The lithium-ion electrolyte is mostly composed of organic solvents and conductive lithium salts. During use, there may be problems such as thermal shock, overcharge and discharge, which will increase the operating temperature of the battery or the existence of lithium dendrites, resulting in the destruction of its electrolyte membrane. And the internal short circuit of the battery, thermal runaway phenomenon occurs. More than 80% of lithium-ion battery safety ...

Claims

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Application Information

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IPC IPC(8): C07F9/6521H01M10/0525H01M10/0567H01M10/42
CPCC07F9/6521H01M10/0567H01M10/0525H01M10/4235Y02E60/10
Inventor 王素文李忠芳郭辉孙鹏崔伟慧
Owner SHANDONG UNIV OF TECH
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