Flame-retardant solid-liquid mixed solid electrolyte, preparation method and lithium battery containing flame-retardant solid-liquid mixed solid electrolyte
A solid-state electrolyte and solid-liquid mixing technology, applied in the field of electrolytes, can solve the problems of flammability of electrolytes, deterioration of electrode-electrolyte interface, reduction of mechanical strength of electrolytes, etc. effect of reaction
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preparation example 1
[0074] The synthesis of preparation example 1 phosphorus-containing organic compound 1#
[0075] In a four-neck flask equipped with a stirrer, a thermometer, a constant pressure dropping funnel, and a condenser, add 54g (0.4mol) of pentaerythritol and 50ml of solvent toluene, heat up to 50°C, add phosphorus trichloride dropwise, and then heat up to reflux. During this process, a slight negative pressure should be maintained in the system. After the reflux, the unreacted phosphorus trichloride, solvent and hydrogen chloride were distilled off under reduced pressure to obtain a yellow transparent viscous liquid, which was cooled to room temperature and solidified to obtain the intermediate product (I). The yield was 95%. Selection of material ratio The molar ratio of phosphorus trichloride to pentaerythritol is 2.5:1.
[0076] Add 60mL of solvent to the intermediate product (I) in the first step, raise the temperature to about 50°C and wait for it to completely dissolve, then ...
preparation example 2
[0079] The synthesis of preparation example 2 phosphorus-containing organic compound 2#
[0080] 2,2-Bis(bromomethyl)-1,3-bis[(2-bromopropyl-2-chloropropyl)phosphate]propane
[0081] In a four-necked beaker equipped with a stirrer, a thermometer, a dropping funnel, and a condenser, add 34g (0.25mol) of pentaerythritol and solvent toluene. Add 1 / 2 amount of phosphorus trichloride dropwise, while slowly raising the temperature to 50°C, and react for 2 hours. Then warm to reflux. At the same time, add another 1 / 2 amount of phosphorus trichloride dropwise. During this process, a certain low vacuum is maintained from time to time. After reflux reaction for 3 hours, filter while it is hot, and evaporate unreacted phosphorus trichloride, solvent and hydrogen chloride under reduced pressure to obtain a yellow transparent viscous liquid, which is recorded as intermediate (I). The crude yield is 98%, and no purification is necessary. The molar ratio of phosphorus chloride to pentaer...
Embodiment 1
[0086] Take lithium bistrifluoromethanesulfonylimide at a molar concentration of 1 mol / L and dissolve it in a mixed solution of triethyl phosphate and vinylene carbonate (volume ratio: 1.5:1), and stir to completely dissolve it under dry conditions , and then, add azobisisobutyronitrile (0.1%, molar ratio to vinylene carbonate) into the mixed solution, stir and dissolve to obtain a transparent and uniform solution, namely the precursor solution. The precursor solution is polymerized at 45 degrees Celsius to obtain a flame-retardant solid-liquid mixed solid electrolyte. Put the battery filled with the precursor solution at 45 degrees Celsius to initiate the polymerization of the precursor electrolyte, and then a battery using a flame-retardant solid-liquid mixed solid electrolyte can be obtained.
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