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Process for preparing high purity cobalto-cobaltic oxide

A technology of tricobalt tetroxide and a manufacturing method, applied in the directions of cobalt oxide/cobalt hydroxide, etc., can solve the problems of large loss of precious metal cobalt, unsuitable lithium cobalt oxide raw material, unsuitable for industrial production, etc., and achieves simple equipment, low cost, and short production cycle. Effect

Inactive Publication Date: 2005-03-02
曾福兴
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, at this time, there are still a large amount of cobalt ions in the reaction mixture solution that have not entered the precipitation
In the presence of EDTA, the loss of precious metal cobalt is greater
And the calcining time in the embodiment reaches 14~20 hours, is not suitable for industrial production
The cobalt tetroxide produced by this method has a "cobalt content of 73.0-74.0%", wherein the cobalt tetroxide with a mass fraction of 73.55%-74.0% contains more cobaltous oxide, which is not suitable as a raw material for producing lithium cobaltate

Method used

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  • Process for preparing high purity cobalto-cobaltic oxide

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Experimental program
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Embodiment 1

[0022] Embodiment 1. Qualified industrial-grade cobalt sulfate crystals, sodium hydroxide solids, and glucose powder are respectively formulated with deionized water to be CoSO with a cobalt ion concentration of 60g / L 4 Solution, 335g / L NaOH clear solution, 30% glucose solution.

[0023] Add 40LCoSO to a 100L reactor 4 Solution, stir vigorously and heat to above 90°C, add 10.5L of NaOH solution that has been preheated to above 90°C into the reaction kettle, and a precipitation reaction occurs. Continue heating and stirring evenly, inject 30L of deionized water and 1.2L of glucose solution. The precipitate was vacuum filtered and washed 4 to 6 times with deionized water above 70°C, and the filtrate was tested to be neutral and free of SO 4 2- Blot dry. The cobalt ion concentration of the filtrate is less than 0.01g / L. The filter cake is dried at 80°C to 125°C, crushed, and sieved to obtain Co(OH) 2 Powder. Take 1-2kg of powder and put it into a corundum sintering sagger,...

Embodiment 2

[0024] Embodiment 2. with deionized water, qualified industrial grade cobalt nitrate crystal, sodium hydroxide solid, glucose powder are prepared respectively into Co(NO 3 ) 2 Solution, 400g / L NaOH clear solution, 30% glucose solution. The above-mentioned Co(NO 3 ) 2 Solution 250L and NaOH solution 89.5L. to 1m 3 Add 300L of deionized water into the volumetric reaction kettle, under vigorous stirring, adjust the pH value to 13 with NaOH solution, and heat to boiling. Under vigorous stirring, the Co(NO 3 ) 2 The solution and the NaOH solution were simultaneously added into the reaction kettle at a flow rate of 3:1 to cause a precipitation reaction. After the feeding was completed, 10L of glucose solution was injected, the heating was stopped, and the material was discharged immediately. The precipitate is press-filtered and washed with deionized water above 75°C for 4 to 6 times until the filtrate is neutral. The filter cake is dried at 100°C to 120°C, crushed, and siev...

Embodiment 3

[0025] Embodiment 3. in 3000mL large beaker, add 1200mL cobalt ion concentration and be the CoSO of 75g / L 4 solution, heated to 62°C in a water bath. Add 307 mL of NaOH solution with a concentration of 400 g / L preheated to 85 °C to CoSO 4 In solution, the reaction produces Co(OH) 2precipitation. Inject 1200 mL of 65° C. deionized water and 80 mL of 20% sodium dithionite solution. The precipitate is vacuum filtered and washed 5-6 times with deionized water above 65°C until the filtrate is neutral and free of SO 4 2- . The filter cake is dried at 105°C to 120°C, pulverized, and sieved to obtain Co(OH) 2 The powder is put into a corundum sintered sagger, and the thickness of the material layer is 3-5cm. Place in a muffle furnace that can be supplemented with air, bake and calcinate at 250°C to 930°C for 10h. After mild crushing and sieving, the mass fraction of cobalt-containing cobalt obtained from tricobalt tetroxide is 73.05%, and the bulk density is 0.72g / cm 3 , tap ...

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Abstract

The present invention relates to the preparation process of high purity cobalto-cobaltic oxide. Water solution of two-valent cobalt salt and sodium hydroxide solution are reacted in strong stirring and in the conditions of pH 4.5-13.5, 50-100 deg.c and existence of reductant to obtain cobaltous hydroxide precipitate. Where, the weight ratio between cobalt, sodium hydroxide and reductant is 1.00 to 2.0-3.0 to 0.01-0.1. The precipitate is filtered and washed, and the filter cake is dried at 80-125 deg.c, crushed, roasted and calcined at 200-950 deg.c in a calcining furnace for 0.5-14 hr, re-crushed and graded into the high purity cobalto-cobaltic oxide powder.

Description

technical field [0001] The invention relates to a method for producing high-purity tricobalt tetroxide. It provides key raw materials for the production of lithium cobalt oxide, the positive electrode material of lithium-ion secondary batteries, and is also widely used in the manufacturing of catalysts, magnetic materials, electronic materials, etc., and belongs to the field of inorganic chemical industry and power material manufacturing. Background technique [0002] In the modern information society, the rapid development of mobile electronic devices benefits from the excellent electrochemical properties of green lithium-ion secondary batteries: large specific capacity, small size, high working voltage, long cycle life, and small self-discharge. Widely used in mobile phones, mobile computing, aerospace, modern biomedical engineering and other fields. [0003] Lithium cobalt oxide is the most mature production of cathode materials for lithium-ion secondary batteries. The ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G51/04
Inventor 曾福兴
Owner 曾福兴
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