Preparation method of flame-retardant electrolyte for lithium ion battery

A lithium-ion battery and electrolyte technology, which is applied in the field of preparation of lithium battery flame-retardant electrolytes, can solve the problems of complex synthesis process, high equipment and operation requirements, and high difficulty of lithium hexafluorophosphate, and achieve good thermal stability, temperature resistance, and conditions mild effect

Active Publication Date: 2020-05-22
SHANDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the synthesis process of lithium hexafluorophosphate is complex, involving high and low temperature treatment, anhydrous and oxygen-free operation, strong corrosion protection and other production links, which is difficult, and it is easy to hydrolyze, requiring high equipment and operation

Method used

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  • Preparation method of flame-retardant electrolyte for lithium ion battery
  • Preparation method of flame-retardant electrolyte for lithium ion battery
  • Preparation method of flame-retardant electrolyte for lithium ion battery

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] [Example 1]: Preparation of TTDP. Take 60mL of triethyl phosphite (TEP, 0.34mol) into a 200mL three-neck round bottom flask. Under magnetic stirring, 11.1g of cyanuric chloride (TCT, 0.06mol) was divided into three batches, and slowly added to triethyl phosphite within 1 hour at room temperature, TCT gradually dissolved, the reaction released a lot of heat, and released ethyl chloride alkane gas to obtain a yellow transparent solution. After adding TCT, raise the temperature to 100-105°C for 8 hours, cool to 50°C, slowly add 35mL of petroleum ether (boiling range 60-90°C), continue to stir and cool to room temperature, and stir overnight, a large amount of colorless crystals are precipitated. Suction filtration, wash 3 times with 20mL petroleum ether, remove unreacted TEP and TCT, obtain colorless crystal 22.9g, namely 1,3,5-triazine-2,4,6-triphosphate ethyl ester (TTDP, produced rate: 78%).

[0022] Adopt same reaction step, the productive rate that carries out reac...

Embodiment 2

[0025] [Example 2]: Preparation of TPT. Add 19.6g TTDP (0.04mol) into 130mL concentrated hydrochloric acid, reflux for 36h under magnetic stirring, cool to 50°C, distill off HCl under reduced pressure, concentrate to 40mL, extract three times with 90mL ethyl acetate to remove unhydrolyzed TTDP. The aqueous phase was concentrated to nearly dryness, and dried in a vacuum oven at 120° C. for 12 hours to obtain 12.3 g of a white solid, namely 1,3,5-triazine-2,4,6-triphosphoric acid (TPT, yield: 96% ).

[0026] Using the same reaction steps, but extracting with dichloromethane, benzene, toluene or petroleum ether, the yields were 94%, 89%, 91% and 85%, respectively.

[0027] 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 84%.

[0028] The hydrolysis of different ester groups of TTDP prepares the productive rate of TPT as shown in Table 2:

[0029] The hydrolysis...

Embodiment 3

[0031] [Example 3]: Preparation of LiTPT. Take 9.63g TPT (0.03mol) and add it into 20mL deionized water, stir at room temperature for 30min to fully dissolve it. Get 6.65g lithium carbonate (0.09mol) and dissolve in 30mL 0.1mol L -1 dilute hydrochloric acid. The hydrochloric acid solution was added dropwise to the TPT aqueous solution, stirred at room temperature for 12 h, the solvent was concentrated, and vacuum-dried to constant weight to obtain LiTPT solid with a yield of 95%.

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Abstract

The invention relates to a preparation method of a flame-retardant electrolyte for a lithium ion battery. The electrolyte is a novel flame-retardant electrolyte which is compounded by taking melaminering-containing lithium triphosphonate with a novel structure as a main component. The preparation method comprises the following steps: reacting 2, 4, 6-trichloro-1, 3, 5-triazine (cyanuric chloride,TCT) with phosphite ester, performing hydrolyzing to introduce three phosphate groups, and reacting the ternary phosphonic acid with lithium hydroxide, lithium oxide or lithium carbonate to obtain the novel cyanuric ring-containing lithium triphosphonate. A lithium salt, an intermediate phosphate and other additives are dissolved in an organic solvent for compounding to obtain the novel flame-retardant lithium ion battery electrolyte. The novel 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 the preparation of a flame-retardant electrolyte for a lithium battery. The electrolyte has high electrical conductivity, and its flame retardant function plays an important role in improving the safety performance of lithium-ion batteries. Can be used in lithium-ion batteries, lithium-oxygen batteries, lithium-sulfur batteries. [0002] technical background [0003] Lithium secondary batteries have the advantages of high working voltage, high specific energy, high specific power, small self-discharge and no memory effect, etc., and have become a hot spot in the research and development of secondary batteries and have been widely used. The electrolyte of conventional lithium-ion batteries is an organic liquid, which has hidden dangers such as flammability, explosion, and liquid leakage. Therefore, the development of solid-state lithium batteries has become a current research hotspot. At present, solid-state electrolytes mainly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/0566H01M10/0567H01M10/0568H01M10/0569H01M10/42H01M10/0525
CPCH01M10/0566H01M10/0567H01M10/0568H01M10/0569H01M10/4235H01M10/0525H01M2300/0025Y02E60/10
Inventor 王素文李忠芳孙鹏王传刚崔伟慧
Owner SHANDONG UNIV OF TECH
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