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A method for deep purification and iron removal in cobalt solution

A technology of deep purification and cobalt solution, which is applied in the chemical industry, can solve the problems of increasing production costs, increasing process flow, and preparing high-purity cobalt, and achieves the effect of low cost and good stability

Active Publication Date: 2018-12-07
广州海普电子材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Patent CN103966627A discloses a method suitable for deep removal of iron in cobalt electrolysis or electrowinning solution with an iron concentration lower than 500 mg / L. Phosphate or phosphoric acid is added to the cobalt salt solution to form a stable complex with impurity iron material, and then use the method of electrowinning cobalt to obtain high-purity cobalt with an iron impurity content of less than 0.5ppm. This method introduces sodium and phosphate impurities, and phosphorus-containing wastewater needs to be treated, which increases production costs.
[0005] Patent CN102162031B uses oxidizing trichloroisocyanuric acid as an iron remover, and Fe 2+ Oxidized to water-soluble Fe 3+ , while Co 2+ And the added ammonium oxalate generates cobalt oxalate precipitation, so as to achieve the effect of iron removal, but cobalt oxalate cannot be directly used for electrodeposition to prepare high-purity cobalt, it needs to be further processed, which increases the process flow, and due to trichloroisocyanuric acid and oxalic acid Ammonium will cause ammonia nitrogen wastewater

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  • A method for deep purification and iron removal in cobalt solution
  • A method for deep purification and iron removal in cobalt solution
  • A method for deep purification and iron removal in cobalt solution

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Experimental program
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Effect test

Embodiment 1

[0026] First measure 1000mL CoSO 4 solution (CoSO 4 •7H 2 O crystal powder and ultrapure water), the cobalt ion concentration is 60g / L, and the pH value is adjusted to 2 with concentrated sulfuric acid solution. Then through the ion exchange column equipped with 200ml Monophos resin, the exchange rate of the cobalt solution and the resin is controlled to be 0.2~3.0BV / h, the solution temperature is 50~70°C, the pH value of the solution is 2~3, and the impurity elements after ion exchange adsorption Concentrations are shown in Table 1:

[0027] Table 1 Comparison of iron content before and after purification of cobalt sulfate solution

[0028]

Embodiment 2

[0030] First measure 125L CoSO 4 +CoCl 2 mixed solution (CoSO 4 •7H 2 O crystal powder + CoCl 2 •6H 2 O crystal powder and ultrapure water), the cobalt ion concentration is 100g / L, and the pH value is adjusted to 1 with concentrated sulfuric acid solution. Then through the ion exchange column equipped with 25LMonophos resin, the exchange rate between the cobalt solution and the resin is controlled to be 0.2~3.0BV / h, the solution temperature is 50~70°C, the pH value of the solution is 2~3, and the concentration of impurity elements after ion exchange adsorption As shown in table 2:

[0031] Table 2 Comparison of iron content before and after purification of cobalt sulfate solution

[0032]

Embodiment 3

[0034] First measure 50L CoCl 2 Solution (CoCl 2 •6H 2 O crystal powder and ultrapure water), the cobalt ion concentration is 40g / L, and the pH value is adjusted to 1 with concentrated hydrochloric acid solution. Then through the ion exchange column equipped with 10L Monophos resin, the exchange rate between the cobalt solution and the resin is controlled to be 0.2~3.0BV / h, the solution temperature is 50~70°C, the solution pH is 2~3, and the concentration of impurity elements after ion exchange adsorption as shown in Table 3:

[0035] Table 3 Comparison of iron content before and after purification of cobalt sulfate solution

[0036]

[0037] In order to further verify the deep removal effect of Monophos type resin on impurity iron in cobalt solution, take the CoSO 4 6.0L of the solution is placed in the electrowinning tank, the titanium woven basket is used as the anode, and the cathode is a titanium plate. The electrowinning conditions are as follows: the pH value of ...

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Abstract

The invention relates to a method for deep purification and removal of iron in a cobalt solution. Chelating resin Monophos is adopted, the process comprises the steps that impurity iron in the cobalt solution is deep removed through a dynamic ion-exchange method, then a winning cell is leaded in to conduct electro winning impurity-removing and purifying, and 99.999% high-purity cobalt with the iron content being less than 1 ppm is obtained. The method is suitable for the deep removal of the trace iron in the electro winning cobalt solution. The process is easy to operate, good in stability, low in cost, and environmentally friendly, and resin can be recycled after iron removal treatment.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a method for deeply purifying and removing iron in a cobalt solution. Background technique [0002] High-purity cobalt is an important electronic material. High-purity cobalt with a purity of 3N~4N is widely used in computer storage hard disks, while high-purity cobalt with a purity of 5N and above is mainly used as a key contact material for integrated circuits in the semiconductor industry. [0003] The key to preparing high-purity cobalt lies in the deep purification of impurities in the cobalt solution. Impurity iron in the cobalt solution can lead to inconsistent magnetic properties of electronic components made of high-purity cobalt. At present, the manufacture of high-end integrated circuits generally requires that the impurity Fe content in high-purity cobalt be less than 1ppm. The methods for removing iron in the solution mainly include neutralization method,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B3/42C22B3/20C22B23/00
CPCC22B3/20C22B3/42C22B23/0453Y02P10/20
Inventor 杨斌王广欣陈晓芳赵云超张鹏飞逯峙
Owner 广州海普电子材料科技有限公司