Fluorinated high-nickel ternary material as well as preparation method and application thereof
A high-nickel ternary material and fluorination technology, applied in chemical instruments and methods, inorganic chemistry, nickel compounds, etc., can solve problems such as increased internal resistance, small performance effects, and loss of nickel source, and achieve complete crystallinity , good rate performance, uniform dispersion effect
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[0040] The invention provides a method for preparing a high-nickel fluoride ternary material, comprising the following steps:
[0041] Vacuum rectification is carried out on the electrolyte solution of the invalid lithium-ion battery, and the residual solution obtained is crystallized with ammonia water to obtain lithium fluoride;
[0042] Lithium fluoride, nickel sulfate, cobalt sulfate, manganese sulfate and water are mixed to obtain a mixed solution;
[0043] Mix the mixed solution and complexing agent, age to obtain a precursor; the chemical formula of the precursor is Ni x co y mn z (OH) 2 nLiF, wherein, x≥0.5, x+y+z=1; n=0.05~0.5;
[0044] The precursor and lithium hydroxide are mixed and then calcined to obtain the high-nickel fluoride ternary material.
[0045] In the present invention, unless otherwise specified, all raw materials are commercially available products well known to those skilled in the art.
[0046] In the invention, vacuum rectification is carrie...
Embodiment 1
[0070] After vacuum distillation of the spent lithium-ion battery electrolyte (vacuum degree of 1KPa, temperature of 115°C), the temperature is controlled at 65°C, and the residual liquid obtained by using ammonia water with a concentration of 1.5mol / L is washed several times to crystallize Lithium fluoride is obtained;
[0071] Lithium fluoride, NiSO 4 ·6H 2 O. CoSO 4 ·7H 2 O, manganese sulfate and water mix, obtain mixed solution, wherein the mol ratio of Ni, Co and Mn is 8:1:1, and the total molar ratio of the mol of Li and Ni, Co and Mn is 0.05:1, described mixed solution The total concentration of solute in medium is 2mol / L;
[0072] At 60°C and a stirring rate of 320r / min, after adding ammonia water with a concentration of 2mol / L to the mixed solution, adjust the pH value to 12 with a NaOH solution with a concentration of 1.5mol / L, and wait for the nickel, cobalt, manganese After being completely deposited on the surface of lithium fluoride, after aging for 11 hours...
Embodiment 2
[0076] After vacuum rectification (vacuum degree: 0.8KPa, temperature: 115°C) of the spent lithium-ion battery electrolyte, the temperature is controlled at 60°C, and the obtained residual liquid is washed with ammonia water with a concentration of 1.5mol / L for several times. Crystallization obtains lithium fluoride;
[0077] Lithium fluoride, NiSO 4 ·6H 2 O. CoSO 4 ·7H 2 O, manganese sulfate and water mix, obtain mixed solution, wherein the mol ratio of Ni, Co and Mn is 8:1:1, and the total molar ratio of the mol of Li and Ni, Co and Mn is 0.1:1, described mixed solution The total concentration of solute in medium is 1.8mol / L;
[0078]At 55°C and a stirring rate of 300r / min, add ammonia water with a concentration of 2mol / L to the mixed solution to keep the concentration of ammonia in the subsequent aging system at 10±0.5g / L, then use a concentration of 1.5mol / L NaOH solution to adjust the pH value to 11.5. After nickel, cobalt and manganese are completely deposited on th...
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