Preparation method of large-granularity cobaltosic oxide

A technology of tricobalt tetroxide and large particle size, which is applied in the direction of cobalt oxide/cobalt hydroxide, etc., can solve the problems of unfavorable industrial production and cumbersome process, and achieve the effect of avoiding excessive impurity content and simple requirements for calcination equipment

Inactive Publication Date: 2018-09-04
LANZHOU JINCHUAN NEW MATERIAL SCI & TECH
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Problems solved by technology

This patent requires multiple cycles of crystallization in the cobalt carbonate synthesis stage, the process is cumbersome, and it is not conducive to industrial production
Chinese invention patent CN201210401514.9 discloses "a method and device for preparing spherical cobalt tetroxide with large particle size". Predetermined production particle size, then the suspension in the discharge port is passed back into the reaction device to continue the reaction until the particle size of cobalt tetroxide at the discharge port of the reaction device is not less than the predetermined production particle size, the suspension is passed into the Spherical cobalt tetroxide is obtained by filtering in a filter press. The precipitant used in this patent is hydroxide, which is different from this patent application, and the suspension needs to be re-introduced into the reaction device repeatedly to continue the reaction. The process is cumbersome

Method used

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  • Preparation method of large-granularity cobaltosic oxide
  • Preparation method of large-granularity cobaltosic oxide
  • Preparation method of large-granularity cobaltosic oxide

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Experimental program
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Embodiment 1

[0039] Prepare 1mol / L cobalt chloride solution as A solution, 1mol / L sodium carbonate solution as B solution, add 5 mL of hydrazine hydrate solution with a mass content of 30% for every liter of 5mol / L ammonia solution as C solution, 5mol / L The hydrogen peroxide solution is used as the D solution, and the 2mol / L sodium hydroxide solution is used as the E solution.

[0040] Synthesis reaction: at the beginning of the synthesis reaction, A solution, B solution, and C solution were added to the reaction kettle in parallel, and the cobalt carbonate synthesis reaction was carried out under strong stirring. During the reaction, the ammonia concentration of the reaction solution was strictly controlled to be 5g / L; The temperature of the system is 70°C, the flow rate of solution A is 100L / h for 0~1h, 200L / h for 1~2h, 300L / h for 2~3h, 400L / h for 3~4h, and 400L / h for 4h to synthesis The flow rate of the end time period is 500L / h, the flow rate of solution B is 1.02 times of the correspo...

Embodiment 2

[0047]Prepare 1.5mol / L cobalt sulfate solution as A solution, 1.5mol / L sodium carbonate solution as B solution, add 15mL hydrazine hydrate solution with a mass content of 30% for every liter of 8mol / L ammonia solution as C solution, 6mol / L The hydrogen peroxide solution is used as the D solution, and the 4mol / L sodium hydroxide solution is used as the E solution.

[0048] Synthesis reaction: at the beginning of the synthesis reaction, A solution, B solution, and C solution were added to the reactor in parallel, and the cobalt carbonate synthesis reaction was carried out under strong stirring. During the reaction, the ammonia concentration of the reaction solution was strictly controlled to be 8g / L; The temperature of the system is 65°C, the flow rate of solution A is 100L / h for 0~1h, 200L / h for 1~2h, 300L / h for 2~3h, 400L / h for 3~4h, and 400L / h for 4h to synthesis The flow rate of the end time period is 500L / h, the flow rate of solution B is 1.05 times of the corresponding flo...

Embodiment 3

[0055] Prepare 2mol / L cobalt nitrate solution as A solution, 2mol / L sodium carbonate solution as B solution, add 20mL hydrazine hydrate solution with a mass content of 30% for every liter of 10mol / L ammonia solution as C solution, and 8mol / L hydrogen peroxide Solution as D solution, 6mol / L sodium hydroxide solution as E solution.

[0056] Synthesis reaction: at the beginning of the synthesis reaction, A solution, B solution, and C solution were added to the reaction kettle in parallel, and the cobalt carbonate synthesis reaction was carried out under strong stirring. During the reaction, the ammonia concentration of the reaction solution was strictly controlled to be 6g / L; The temperature of the system is 75°C, the flow rate of solution A is 100L / h for 0~1h, 200L / h for 1~2h, 300L / h for 2~3h, 400L / h for 3~4h, and 400L / h for 4h to synthesis The flow rate of the end time period is 500L / h, the flow rate of solution B is 1.1 times of the corresponding flow rate of each flow rate zo...

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Abstract

The invention discloses a preparation method of large-granularity cobaltosic oxide. The preparation method is characterized by synthesizing cobalt carbonate of which the granularity is 20 to 30 mu m in a wet process in a shortest time through the ways of reducing nucleation number during a synthesis initial stage by taking a cobalt solution in certain concentration as a cobalt source, a sodium carbonate solution as a precipitator, an ammonia solution as a complexing agent and hydrazine hydrate as a reducing agent; oxidizing a synthetic product into hydroxyl cobalt oxide under a certain pH (Potential of Hydrogen) value condition after completing the synthesis by utilizing a hydrogen peroxide solution in certain concentration, then washing and drying a mixture, and calcining under a certaincondition, thus obtaining a large-granularity cobaltosic oxide product. By utilizing the technology, the spherical or spherical-like large-granularity cobaltosic oxide product of which the laser granularity is 15 to 25 mu m, the tap density is greater than 2.0 g / cm<3> and the specific surface area is 1.0 to 3.0 m<2> / g can be prepared within a short time.

Description

technical field [0001] The invention belongs to the technical field of lithium ion batteries, and in particular relates to a preparation method of large-grained cobalt trioxide used for preparing lithium cobalt oxide, a cathode material of lithium ion batteries. Background technique [0002] Lithium-ion batteries made of lithium cobalt oxide as the positive electrode material have the characteristics of light weight, large capacity, high specific energy, high working voltage, stable discharge, suitable for high-current discharge, good cycle performance, and long life. They are mainly used in 3C digital fields . [0003] Lithium cobalt oxide is developing in the direction of high voltage, high compaction, and high cycle performance, and the requirements for the raw material cobalt trioxide are getting higher and higher. co 3 o 4 It is a functional material with special structure and properties, Co 3 o 4 The market is already facing the status quo of gradual shrinkage, an...

Claims

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Application Information

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IPC IPC(8): C01G51/04
CPCC01G51/04C01P2004/32C01P2004/61C01P2006/11C01P2006/12
Inventor 陈文福陈晓闯王红忠刘世红吴来红郭培庆赵亮周春元
Owner LANZHOU JINCHUAN NEW MATERIAL SCI & TECH
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