Massproduction method of single crystal cobalt-free lithium-rich manganese-based binary material precursor

A technology of cobalt, lithium-rich manganese-based, binary materials, applied in chemical instruments and methods, inorganic chemistry, electrical components, etc., can solve problems such as unfavorable industrialization and complex processes, and achieve the effect of reducing raw material costs and costs.

Pending Publication Date: 2021-01-01
JINGMEN GEM NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The process is complicated, which i

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  • Massproduction method of single crystal cobalt-free lithium-rich manganese-based binary material precursor
  • Massproduction method of single crystal cobalt-free lithium-rich manganese-based binary material precursor
  • Massproduction method of single crystal cobalt-free lithium-rich manganese-based binary material precursor

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Experimental program
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Embodiment 1

[0025] Step 1, nickel sulfate, manganese sulfate are mixed with the aqueous solution A of 2mol / L metal concentration by the ratio of metal molar ratio 20:80, adopt the NaOH solution of 32% as precipitation agent B, the ammoniacal liquor of 17% is as complexing agent C, 20g / L sodium sulfite solution is used as reducing agent D.

[0026] Step 2. Prepare the bottom solution and feed N2 as a protective gas. The pH of the bottom solution is 11.4-11.6, the ammonia concentration is maintained at 3-4g / L, the temperature is controlled at 34-36°C, and the stirring speed is controlled at 400rpm.

[0027] Step 3. Pump solution A, solution B, solution C and solution D into the reactor at the same time at the speed of 300L / h, 80L / h, 20L / h, 30L / h, keep the pH at 11.0-11.2, supernatant liquid ammonia The concentration is 3-4g / L, the temperature is 34-36°C, and the stirring speed is 400rpm.

[0028] Step 4: stop feeding after D50 reaches 3.5um, perform centrifugal washing, drying, screening, ...

Embodiment 2

[0031] Step 1, nickel sulfate, manganese sulfate are mixed with the aqueous solution A of 2mol / L metal concentration by the ratio of metal molar ratio 30:70, adopt the NaOH solution of 32% to be precipitation agent B, the ammoniacal liquor of 17% is as complexing agent C, 20g / L sodium sulfite solution is used as reducing agent D.

[0032] Step 2. Prepare the bottom solution and feed N2 as a protective gas. The pH of the bottom solution is 11.6-11.8, the ammonia concentration is maintained at 4-5g / L, the temperature is controlled at 44-46°C, and the stirring speed is controlled at 350rpm.

[0033] Step 3. Pump solution A, solution B, solution C and solution D into the reactor at the same time at the speed of 450L / h, 120L / h, 40L / h, 45L / h, keep the pH at 11.2-11.4, supernatant liquid ammonia The concentration is 4-5g / L, the temperature is 44-46°C, and the stirring speed is 350rpm.

[0034] Step 4: stop feeding after D50 reaches 3.6um, perform centrifugal washing, drying, sieving...

Embodiment 3

[0036] Step 1, nickel sulfate, manganese sulfate are mixed with the aqueous solution A of 2mol / L metal concentration by the ratio of metal molar ratio 40:60, adopt the NaOH solution of 32% as precipitation agent B, the ammoniacal liquor of 17% is as complexing agent C, 20g / L sodium sulfite solution is used as reducing agent D.

[0037] Step 2. Prepare the bottom solution and feed N2 as a protective gas. The pH of the bottom solution is 11.8-12.0, the ammonia concentration is maintained at 6-8g / L, the temperature is controlled at 49-51°C, and the stirring speed is controlled at 320rpm.

[0038] Step 3. Pump solution A, solution B, solution C and solution D into the reaction kettle at the same time at the speed of 600L / h, 158L / h, 60L / h, 60L / h, keep the pH at 10.8-11.0, supernatant liquid ammonia The concentration is 6-8g / L, the temperature is 49-51°C, and the stirring speed is 320rpm.

[0039] Step 4: stop feeding after D50 reaches 3.8um, perform centrifugal washing, drying, sc...

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Abstract

The invention discloses a mass production method of a single crystal cobalt-free lithium-rich manganese-based binary material precursor. The method comprises: 1, preparing a solution A from a nickel salt and a manganese salt, and adopting a NaOH solution as a precipitating agent B, ammonia water as a complexing agent C and a sodium sulfite solution as a reducing agent D; 2, preparing a base solution, introducing N2, enabling the pH value of the base solution to 11-13 by using ammonia with the concentration of 3-10 g/L, and stirring at a temperature of 30-60 DEG C under a stirring speed of 200-500 rpm; step 3, adding the solution A, a solution B, a solution C and a solution D into a reaction kettle at the same time, and keeping the pH at 10-12, the concentration of supernatant liquid ammonia at 3-10 g/L, the temperature at 30-60 DEG C and the stirring speed at 200-500 rpm; and 4, stopping feeding after D50 reaches the target particle size, and carrying out centrifugal washing, drying, screening, iron removal and packaging to obtain the single-crystal cobalt-free lithium-rich manganese-based binary material precursor.

Description

technical field [0001] The invention belongs to the technical field of chemical material preparation, and in particular relates to a method for mass production of a single crystal cobalt-free lithium-rich manganese-based binary material precursor. Background technique [0002] Lithium-rich manganese-based materials have a high discharge specific capacity, almost twice that of lithium iron phosphate. If matched with silicon-carbon composite materials, the energy density of a battery cell can reach 350Wh / kg. In lithium-rich manganese-based materials, the presence of manganese ore reduces the cost and improves the stability and safety of the material. The future of lithium-rich manganese-based cathode materials can be expected. [0003] Mn(OH) generated due to high pH 2 It is easily oxidized to MnOOH in aqueous solution, so the carbonate co-precipitation process is generally used to prepare the precursor of lithium-rich manganese-based solid solution. However, the carbonate ...

Claims

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Application Information

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IPC IPC(8): C01G45/00H01M4/505H01M4/525
CPCC01G45/00H01M4/505H01M4/525C01P2004/03C01P2006/40Y02E60/10
Inventor 李聪张坤许开华陈康黎俊孙海波范亮姣薛晓斐
Owner JINGMEN GEM NEW MATERIAL
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