Preparation method of high-purity lithium bis(oxalato)borate
A lithium bis-oxalate borate and high-purity technology is applied in the field of preparation of high-purity lithium bis-oxalate borate, and can solve the problems of difficulty in obtaining raw materials for synthesis routes, difficulty in industrial production, and low synthesis efficiency.
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Embodiment 1
[0039] A preparation method of high-purity lithium bisoxalate borate comprises the following specific steps:
[0040] S1 ball milling: uniformly mix anhydrous oxalate and boron in a molar ratio of 2:1, put them into a ball mill and mill for 0.5h, then dissolve the mixed powder into ultrapure water at a mass ratio of 1:20 to obtain solution A;
[0041] S2 Dissolving: Lithium powder is dissolved in ethylene carbonate according to the mass ratio of 1:10 to obtain solution B;
[0042] S3 cycle heating; put the A liquid and B obtained in steps S1 and S2 into the tubular reactor according to the mass ratio of 1:2 for heating reaction, the reaction temperature is 60 ° C; micro-negative pressure reaction, the pressure is -0.001Mpa; The moisture generated under negative pressure forms an azeotrope with diethyl carbonate at high temperature and is discharged out of the system under negative pressure; diethyl carbonate and water are separated in the static tank, and diethyl carbonate is ...
Embodiment 2
[0050] A preparation method of high-purity lithium bisoxalate borate comprises the following specific steps:
[0051] S1 ball milling: uniformly mix anhydrous oxalate and boron in a molar ratio of 3.5:1, put them into a ball mill for 1 hour, and then dissolve the mixed powder into ultrapure water at a mass ratio of 1:30 to obtain solution A;
[0052] S2 dissolution: Lithium powder is dissolved in ethylene carbonate according to the mass ratio of 1:15 to obtain solution B;
[0053] S3 cycle heating; put the A liquid and B obtained in steps S1 and S2 into the tubular reactor according to the mass ratio of 1:3 for heating reaction, the reaction temperature is 68 ° C; micro-negative pressure reaction, the pressure is -0.001Mpa; The moisture generated under negative pressure forms an azeotrope with diethyl carbonate at high temperature and is discharged out of the system under negative pressure; diethyl carbonate and water are separated in the static tank, and diethyl carbonate is ...
Embodiment 3
[0061] A preparation method of high-purity lithium bisoxalate borate comprises the following specific steps:
[0062] S1 ball milling: uniformly mix anhydrous oxalate and boron in a molar ratio of 5:1, put them into a ball mill and mill for 1.5 hours, then dissolve the mixed powder into ultrapure water at a mass ratio of 1:50 to obtain solution A;
[0063] S2 Dissolving: Lithium powder is dissolved in ethylene carbonate according to the mass ratio of 1:20 to obtain solution B;
[0064] S3 cycle heating; put the A liquid and B obtained in steps S1 and S2 into the tubular reactor according to the mass ratio of 1:5 for heating reaction, the reaction temperature is 75 °C; slight negative pressure reaction, the pressure is -0.001Mpa; The moisture generated under negative pressure forms an azeotrope with diethyl carbonate at high temperature and is discharged out of the system under negative pressure; diethyl carbonate and water are separated in the static tank, and diethyl carbonat...
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