All-solid-state metal lithium battery and preparation method thereof
An all-solid-state, metal lithium technology, applied in the manufacture of electrolyte batteries, batteries, secondary batteries, etc., can solve problems such as hidden safety hazards and flammability of polymers
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Embodiment 1
[0039] A flame retardant additive, comprising the steps of:
[0040] Step S11: Add o-xylene into the flask, then feed 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide with nitrogen gas at a temperature of 90°C and a speed of 400r / min Stir at low temperature for 20 minutes, then slowly add diethylene succinic acid into the flask, and after the addition is complete, reflux at 140°C for 7 hours. After the reaction, the reaction solution is cooled to room temperature, and the intermediate 1 is obtained by suction filtration;
[0041] Step S12: Add the intermediate 1 prepared in step S1 into a flask filled with deionized water, stir for 20 min at a rotation speed of 400 r / min, then add thionyl chloride to it, heat up to 60° C. for reflux reaction for 9 h, and the reaction ends Afterwards, the temperature was raised to 80° C. to remove unreacted thionyl chloride, and the solvent was removed by rotary evaporation to obtain intermediate 2;
[0042] Step S13: Add dichloromethane and...
Embodiment 2
[0045] A flame retardant additive, comprising the steps of:
[0046] Step S11: Add o-xylene in the flask, then feed 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide into nitrogen gas at a temperature of 90°C and a speed of 500r / min Stir at low temperature for 25 minutes, then slowly add diethylene succinic acid into the flask, and reflux at 145°C for 7.5 hours after the addition is complete. After the reaction, the reaction solution is cooled to room temperature, and the intermediate 1 is obtained by suction filtration;
[0047] Step S12: Add the intermediate 1 prepared in step S1 into a flask filled with deionized water, stir for 20 min at a rotation speed of 400 r / min, then add thionyl chloride therein, raise the temperature to 65° C. for 9.5 h under reflux, and react After the end, the temperature was raised to 82.5°C again to remove the unreacted thionyl chloride, and the solvent was removed by rotary evaporation to obtain intermediate 2;
[0048] Step S13: Add dichloro...
Embodiment 3
[0051] A flame retardant additive, comprising the steps of:
[0052] Step S11: Add o-xylene in the flask, then feed 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide with nitrogen gas at a temperature of 90°C and a speed of 600r / min Stir at low temperature for 30 minutes, then slowly add diethylene succinic acid into the flask, and reflux at 150°C for 8 hours after the addition is complete. After the reaction, the reaction solution is cooled to room temperature, and the intermediate 1 is obtained by suction filtration;
[0053] Step S12: Add the intermediate 1 prepared in step S1 into a flask filled with deionized water, stir for 20 min at a rotation speed of 400 r / min, then add thionyl chloride to it, heat up to 70°C and reflux for 10 h, and the reaction ends Afterwards, the temperature was raised to 85° C. to remove unreacted thionyl chloride, and the solvent was removed by rotary evaporation to obtain intermediate 2;
[0054] Step S13: Add dichloromethane and triethylamin...
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