Preparation method of polyphosphazene urethane single ion solid electrolyte
A technology of solid electrolyte and nitrile urethane, applied in the direction of circuits, electrical components, secondary batteries, etc., can solve the problems of numerous steps, difficulty in changing the ratio and salt concentration, and complicated preparation methods, and achieve high lithium ion migration number, Effect of high electrochemical stability window and high room temperature conductivity
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Embodiment 1
[0029] Step 1, in the there-necked flask of 250ml, the 50ml tetrahydrofuran THF solution containing 9.354g diethylene glycol monomethyl ether (77.85mmol) was added dropwise to 1.779g (74.13 g) dispersed in 50ml THF with a constant pressure dropping funnel. mmol) sodium hydride NaH, magnetic stirring at 40°C under nitrogen protection for 60 minutes until all NaH reaction is complete;
[0030] Step 2: Dissolve 5.00g (0.043mol) of polydichlorophosphazene in 100ml of THF, pour it into a 250ml single-necked flask, add dropwise 2.26g (0.0173mol) of the THF dispersion of lithium taurate, and add 5.5g of TEA as a solution. Acid binding agent, 0.01 g of tetrabutylammonium bromide was added as a catalyst, and then the reaction was stirred and refluxed at room temperature for 12 hours. Then 9.838 g of sodium salt NaO (CH 2 ) 2 O(CH 2 ) 2 OCH 3 , continue to react for 24 hours;
[0031] Step 3, after the reaction is completed, filter, and the filtrate is subjected to rotary evaporat...
Embodiment 2
[0037] Step 1, in the there-necked flask of 250ml, the 50mlTHF solution containing 4..677g diethylene glycol monomethyl ether (38.93mmol) was added dropwise to the 0.889g (37.07g) dispersed in 50mlTHF with a constant pressure dropping funnel. mmol) NaH, magnetic stirring at 40°C under nitrogen protection for 80 minutes until all NaH reaction is complete;
[0038] Step 2: Dissolve 2.500g (0.022mol) of polydichlorophosphazene in 100ml of THF, pour it into a 250ml single-necked flask, add dropwise the THF dispersion of 1.13g (0.008mol) of lithium taurate, and add 2.75g of TEA as a solution. Acid binding agent, 0.01 g of tetrabutylammonium bromide was added as a catalyst, and then the reaction was stirred and refluxed at room temperature for 12 hours. Then 4.919 g of sodium salt NaO (CH 2 ) 2 O(CH 2 ) 2 OCH 3 , continue to react for 24 hours;
[0039] Step 3, after the reaction is completed, filter, and the filtrate is subjected to rotary evaporation to remove THF. The prod...
Embodiment 3
[0045] Step 1, in the there-necked flask of 250ml, the 50mlTHF solution containing 10.289g diethylene glycol monomethyl ether (93.42mmol) was added dropwise to 2.135g (88.96mmol) dispersed in 50mlTHF with a constant pressure dropping funnel Magnetic stirring in NaH at 40°C under nitrogen protection for 60 minutes until all NaH reaction is complete;
[0046] Step 2: Dissolve 6.00g (0.052mol) of polydichlorophosphazene in 100ml of THF, pour it into a 250ml single-necked flask, add dropwise 2.712g (0.0173mol) of the THF dispersion of lithium taurate, add 6.6g of TEA for Acid binding agent, 0.01 g of tetrabutylammonium bromide was added as a catalyst, and then the reaction was stirred and refluxed at room temperature for 12 hours. Then 11.806 g of sodium salt NaO (CH 2 ) 2 O(CH 2 ) 2 OCH 3 , continue to react for 24 hours;
[0047] Step 3, after the reaction is completed, filter, and the filtrate is subjected to rotary evaporation to remove THF. The product was washed three...
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