Preparation method of lithium manganate precursor for lithium ion battery anode material
A lithium-ion battery and cathode material technology, which is applied in battery electrodes, manganate/permanganate, circuits, etc., to achieve the effects of no three-waste emissions, improved electrochemical cycle performance, and short process flow
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Embodiment 1
[0026] Example 1 : (1) 600g electrolytic MnO 2 , 179.3g LiOH·H 2 O and 480g deionized water are mixed with reactant slurry, add in the autoclave (Li / Mn mol ratio is 0.62, liquid-solid weight ratio H 2 O / MnO 20.8); (2) While stirring, heat up to 180°C, and stir for 3 hours at a constant temperature; (3) Filter the reaction product slurry obtained in step (2), and dry the solid phase product at 110°C for 12 hours, 655.2g of lithium manganate precursor was obtained, and its Li / Mn ratio satisfied the molecular formula Li 1.100 mn 2 o 4 ; The volume of the liquid phase mother liquor is 420 mL, containing Li 1.2mol / L, returning to prepare the next batch of reactant slurry. Gained lithium manganate precursor shows through XRD analysis, has amorphous structure (see attached figure 1 ), and its morphology under the electron microscope is shown in the appendix image 3 . The obtained lithium manganate precursor was heat-treated at 800° C. for 10 hours, ground and pulverized a...
Embodiment 2
[0027] Example 2 : (1) Get 200mL of the mother liquor gained in Example 1 (Li 1.2mol / L), add LiOH·H 2 O 18.8g, then add chemical MnO 2 200g, be mixed with reactant slurry, add in the reactor (Li / Mn molar ratio is 0.3, liquid-solid weight ratio H 2 O / MnO 2 1.0); (2) While stirring, raise the temperature to 200°C, stir and react at a constant temperature for 2.5 hours; (3) Dry the reaction product slurry obtained in step (2) at 120°C for 24 hours to obtain a lithium manganate precursor 213.8 g, whose Li / Mn ratio satisfies the molecular formula Li 0.605 mn 2 o 4 . XRD analysis shows that the lithium manganese oxide precursor has an amorphous structure. The lithium manganate precursor was heat-treated at 750° C. for 12 hours, ground and pulverized after cooling to obtain lithium manganate powder. XRD analysis shows that the phase structure of the powder is mainly spinel lithium manganese oxide, containing a small amount of MnO 2 . The results of chemical analysis show ...
Embodiment 3
[0028] Example 3 : (1) 200g electrolytic MnO 2 , a mixture of 4.6 mol of lithium acetate and lithium hydroxide and 600 g of deionized water to prepare a reaction slurry and add it to the reactor (Li / Mn molar ratio is 2.0, liquid-solid weight ratio H 2 O / MnO 2 3.0); (2) While stirring, the temperature was raised to 110°C, and the stirring was carried out at a constant temperature for 12 hours; (3) After the reaction product slurry obtained in step (2) was filtered to remove the mother liquor, it was dried at 105°C for 12 hours. hours, 225.6g of lithium manganate precursor was obtained, and its Li / Mn ratio satisfied the molecular formula Li 0.971 MnO 2 . The obtained lithium manganate precursor was placed in a high-temperature furnace, heat-treated at a constant temperature of 800° C. for 15 hours, ground and pulverized after cooling. It was proved by XRD detection that the obtained product was lithium manganese oxide with layered structure. Chemical analysis shows that i...
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