Method for removing impurity element Na and S in precursor cobalt salts of cobaltosic oxide

A technology of cobalt tetroxide and impurity elements, applied in the direction of cobalt oxide/cobalt hydroxide, etc., can solve the problems of increased hydrolysis and dissolution of cobalt salts, increased treatment capacity of cobalt-containing wastewater, and inability to effectively remove them. Chemical properties, inhibition of hydrolysis and dissolution

Inactive Publication Date: 2009-01-07
JIANGSU DONGXIN ENERGY TECH
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  • Summary
  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0004] Since the impurity elements Na and S are mostly Na + and SO 4 2- It exists in a water-soluble form. Therefore, the existing methods can only remove metal elements such as Fe, Cu, Ca, and Mg, but cannot effectively remove sodium and sulfur therein. Although when synthesizing the precursor cobalt salt, the cobalt salt Part of Na and S can be removed during the washing process, but as the amount of washing water increases, the hydrolysis and dissolution of cobalt salts intensify, and the loss of cobalt also increases, thereby increasing the treatment capacity of cobalt-containing wastewater

Method used

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  • Method for removing impurity element Na and S in precursor cobalt salts of cobaltosic oxide

Examples

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Embodiment 1

[0022] a) In a 5L glass container, take industrial-grade cobalt chloride and prepare 2500ml of cobalt chloride solution of 1.8mol / l with deionized water, stir, adjust the pH value to 0.5 with hydrochloric acid, heat to 30°C, add 10 % sodium hypochlorite aqueous solution 5ml, continue stirring for 45 minutes, slowly add 2% dilute ammonia water dropwise to adjust its pH value to 4.5, heat to 90°C, add 3g of industrial grade ammonium fluoride, and keep warm for 60 minutes. After the heat preservation is completed, 2 ml of 23% ammonium sulfide solution is added, and the heat preservation is carried out for 60 minutes. Stop heating and stirring, let it stand for 24 hours, and filter to obtain pure cobalt solution.

[0023] b) Heating the cobalt solution obtained in step a) to 75°C, adding 15% ammonium bicarbonate and 20% ammonia water mixed solution, the amount of ammonium bicarbonate added is 2 times of the total molar amount of cobalt in the solution, ammonia water The amount is...

Embodiment 2

[0030]a) In a 5L glass container, take industrial-grade cobalt sulfate and use deionized water to prepare 2500ml of cobalt sulfate solution of 1.5mol / l, stir, adjust its pH value to 1.5 with 5% dilute sulfuric acid, and heat to 50°C. Add 3ml of 10% industrial hydrogen peroxide, continue to stir for 60 minutes, then heat to 80°C, adjust the pH value to 4.8 with 2% sodium hydroxide, heat to 90°C, and keep warm for 0.5h. After the heat preservation is completed, 3.2 g of industrial grade ammonium fluoride is added, and the heat preservation is carried out for 30 minutes. After the heat preservation is completed, 2 ml of 25% sodium sulfide solution is added, and the heat preservation is carried out for 60 minutes. Stop heating and stirring, let it stand for 6h, and filter to obtain pure cobalt solution.

[0031] b) Heating the cobalt solution obtained in step a) to 90°C, adding 15% aqueous sodium carbonate solution, the amount of sodium carbonate added is 1.3 times the total mola...

Embodiment 3

[0038] a) In a 5L glass container, take industrial-grade cobalt nitrate and prepare 2500ml of cobalt nitrate solution of 1.75mol / l with deionized water, stir, adjust the pH value to 4.5 with hydrochloric acid, heat to 30°C, add 25% 3ml of industrial hydrogen peroxide, continue to stir for 45 minutes, then heat to 80°C, slowly add ammonia water dropwise to adjust the pH value to 4.8, heat to 90°C, and keep warm for 30 minutes. After the heat preservation is completed, 3.2 g of industrial grade ammonium bifluoride is added, and the heat preservation is carried out for 60 minutes. After the heat preservation is completed, 2 ml of 23% ammonium sulfide solution is added, and the heat preservation is carried out for 60 minutes. Stop heating and stirring, let it stand for 12 hours, and filter to obtain pure cobalt solution.

[0039] b) Heating the cobalt solution obtained in step a) to 75°C, adding 15% ammonium oxalate aqueous solution, the addition of ammonium oxalate is 1.2 times ...

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Abstract

The invention relates to a method for removing impurity elements Na and S from the precursor cobalt salt of cobaltosic oxide. The method comprises the steps of adding proper a washing assistant in the process of washing cobalt salt with pure water so as to wash impurity ions Na, SO4<2 minus> contained in the cobalt salt and enable the impurity ions to enter waste washing water, thereby obtaining high purity precursor cobalt salt; calcinating to obtain the high purity cobaltosic oxide. The method has the advantages of simple operation, good impurity removing effect, and less cobalt loss. Both the weight ratio and the content ratio of Na and S to Co in the processed cobalt salt are lower than 1:15000, thereby ensuring the electrochemical activity and building a foundation for promoting the electrochemical properties of lithium cobalt oxide in lithium ion battery anode.

Description

technical field [0001] The invention relates to a method for removing sodium ions and sulfate ions in the preparation process of cobalt trioxide precursor cobalt salt, so as to obtain a pure cobalt salt intermediate, which is used to prepare tricobalt tetroxide as the positive core material of lithium batteries and other electronic materials. technical background [0002] Lithium-ion battery is a new kind of energy, which has many advantages such as high voltage, large capacity, safety and environmental protection, and has been widely accepted and used by people. Cobalt tetroxide is the core positive electrode material of lithium-ion batteries. It is mainly cobalt precursor cobalt salts such as cobalt carbonate or cobalt oxalate made from cobalt solution, and then processed by calcination to produce cobalt tetroxide. If there are more impurity elements in the precursor cobalt salt, especially Na and S, the electrochemical activity of tricobalt tetroxide will be reduced, whic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G51/04
Inventor 戴振华柏瑞芳田一秋丁一东
Owner JIANGSU DONGXIN ENERGY TECH
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