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Method for preparing semi-continuous ternary precursor

A semi-continuous, precursor technology, applied in the direction of electrical components, electrochemical generators, battery electrodes, etc., can solve the problems of uneven particle size distribution, complex process, low product activity, etc., and achieve effective narrowing of particle size distribution, shrinking Effect of narrow particle size distribution and increased residence time

Active Publication Date: 2019-12-20
ZHUJI PAWA NEW ENERGY
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Problems solved by technology

The precursor produced by the continuous method has the advantages of good product stability, high product activity, and wide particle size distribution (CN103253717A), but at the same time, there are many fine powders and uneven particle size distribution, resulting in poor consistency of the finished product after sintering.
The precursor produced by the batch method has the advantages of good sphericity, high tap density, and less fine powder (CN104201367A), but there are problems such as low product activity and poor product consistency
The existing patent (CN104201368A) uses a continuous method to produce wide-distributed materials by using a continuous method as a crystal seed, and uses other several kettles as a concentration reactor for intermittent production to solve the problems existing in the continuous and batch production processes. The production process of the production process does not produce small particles, but grows on the original small particles, and maintains a wide particle size distribution while the particles grow densely. However, this method has created new problems, and the process is relatively complicated. In large-scale production In the process, there is a problem that the call of the reactor is difficult to coordinate, which affects the scale production
The patent (CN106025203) tried to solve the above problems by connecting multiple reactors in series, and set different process conditions in different reactors. However, this process can only narrow the product to a certain extent, and due to the cumulative effect of the flow rate, the final reactor The inner overflow flow is very large, which is not conducive to ball formation

Method used

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  • Method for preparing semi-continuous ternary precursor
  • Method for preparing semi-continuous ternary precursor
  • Method for preparing semi-continuous ternary precursor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Ni 0。5 co 0.2 mn 0.3 (OH) 2 : d10=5.1um, d50=10.06um, d90=15.78um, tap density=2.25g / cm 3 , specific surface area = 6.52m 2 / g, which is spherical.

[0031] (1) According to the molar ratio of Ni:Co:Mn 5:2:3, prepare a mixed aqueous solution of nickel-cobalt-manganese soluble salt with a total concentration of 2.0mol / L, and use liquid caustic soda with a concentration of 32% as a precipitant with a concentration of 20%. Aqueous ammonia solution as complexing agent;

[0032] (2) Adjust the stirring speed of the 6500L reactor to 300r / min, and use a precision metering pump to add 2.0mol / L nickel-cobalt-manganese soluble salt solution, 32% liquid caustic soda and 20% ammonia solution into the reactor in parallel , control salt flow to 300L / h, control OH -The molar ratio of / (Ni+Co+Mn)=1.9, the temperature of the reactor is controlled at 60°C, the concentration of ammonia is controlled at 8.5g / L, the speed of the concentrator is controlled at 75r / min, and the effectiv...

Embodiment 2

[0039] Ni 0。5 co 0.2 mn 0.3 (OH) 2 : d10=5.8um, d50=10.16um, d90=14.71um, tap density=2.4g / cm 3 , specific surface area = 6.1m 2 / g, which is spherical.

[0040] (1) According to the molar ratio of Ni:Co:Mn 5:2:3, prepare a mixed aqueous solution of nickel-cobalt-manganese soluble salt with a total concentration of 2.0mol / L, and use liquid caustic soda with a concentration of 32% as a precipitant with a concentration of 20%. Aqueous ammonia solution as complexing agent;

[0041] (2) Adjust the stirring speed of the 6500L reactor to 300r / min, and use a precision metering pump to add 2.0mol / L nickel-cobalt-manganese soluble salt solution, 32% liquid caustic soda and 20% ammonia solution into the reactor in parallel , control salt flow to 300L / h, control OH - The molar ratio of / (Ni+Co+Mn)=1.9, the temperature of the reactor is controlled at 60°C, the concentration of ammonia is controlled at 8.5g / L, the speed of the concentrator is controlled at 75r / min, and the effective...

Embodiment 3

[0048] Ni 0。5 co 0.2 mn 0.3 (OH) 2 : d10=7.54um, d50=10.02um, d90=13.21um, tap density=2.36g / cm 3 , specific surface area = 5.91m 2 / g, which is spherical.

[0049] (1) According to the molar ratio of Ni:Co:Mn 5:2:3, prepare a mixed aqueous solution of nickel-cobalt-manganese soluble salt with a total concentration of 2.0mol / L, and use liquid caustic soda with a concentration of 32% as a precipitant with a concentration of 20%. Aqueous ammonia solution as complexing agent;

[0050] (2) Adjust the stirring speed of the 6500L reactor to 300r / min, and use a precision metering pump to add 2.0mol / L nickel-cobalt-manganese soluble salt solution, 32% liquid caustic soda and 20% ammonia solution into the reactor in parallel , control salt flow to 300L / h, control OH - The molar ratio of / (Ni+Co+Mn)=1.9, the temperature of the reactor is controlled at 60°C, the concentration of ammonia is controlled at 8.5g / L, the speed of the concentrator is controlled at 75r / min, and the effect...

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Abstract

The invention relates to a method for preparing a semi-continuous ternary precursor. The invention provides a method for producing products with different particle size distributions and different degree of sphericity requirements by a single kettle, which solves the problems of uneven particle size distribution, generated fine powders and poor degree of sphericity in the conventional pure continuous process, and the problems of concentrated particle size distribution, dense sphere and low activity in the conventional pure intermittent process. The method uses a complexation control crystallization co-precipitation method, wherein the overflow port of a reaction kettle is connected with an aging tank, the aging tank is connected with a thickener, and the thickener is connected with the feed port of the reaction kettle. The method comprises (a) configuring a certain concentration of metal salt solution, liquid alkali and ammonia water; and adding the solution in the step (a) evenly intothe reaction kettle, wherein the material, after fully filling the reaction kettle, overflows into the aging kettle, the material in the aging kettle is pumped into the thickener by a pneumatic diaphragm, the thickener discharges the clear liquid, and the thick slurry flows back into the reaction kettle, so as to increase the solid content and prolong the residence time to improve the degree of sphericity.

Description

technical field [0001] The invention relates to a preparation method of a semi-continuous ternary precursor. Background technique [0002] With the vigorous development of communication and electronic information technology, electronic equipment has been developed rapidly. The huge demand for consumer electronics such as laptops, tablets, digital cameras, and mobile phones has led to an explosive growth in the demand for energy storage systems. At present, the intelligence, size and weight optimization of these portable electronic devices have also put forward higher requirements for energy storage systems, such as miniaturization, light weight, long cycle life, high safety and high energy density, etc. In general, energy storage systems are mainly classified into primary batteries and secondary batteries. Considering both economic and environmental considerations, secondary batteries are superior to primary batteries and have been widely used in people's daily life. Seco...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/50H01M4/52H01M10/0525
CPCH01M4/364H01M4/502H01M4/523H01M10/0525Y02E60/10
Inventor 王宝良王振宇姚挺
Owner ZHUJI PAWA NEW ENERGY
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