阅读说明：本技术 一种对高纯钴电解液中痕量铁去除的方法 (Method for removing trace iron in high-purity cobalt electrolyte ) 是由 赵云超 王广欣 郭明宜 杨斌 李荣坡 唐坤 于 2020-07-02 设计创作，主要内容包括：本发明公开了一种对高纯钴电解液中痕量铁去除的方法,本发明主要采用廉价的DLT-1型螯合树脂来代替国外昂贵的树脂,解决了在制备中高纯钴环节,电解精炼过程中电解液中痕量铁难以去除的问题,该方法操作简单,成本低,稳定性好,绿色环保,且树脂经过酸洗后可循环使用。(The invention discloses a method for removing trace iron in high-purity cobalt electrolyte, which mainly adopts low-cost DLT-1 type chelate resin to replace foreign expensive resin, solves the problem that the trace iron in the electrolyte is difficult to remove in the process of preparing medium-high-purity cobalt and electrolytic refining, and has the advantages of simple operation, low cost, good stability, environmental protection and cyclic use of the resin after acid washing.)

1. A method for removing trace iron in high-purity cobalt electrolyte is characterized by comprising the following steps:

the method comprises the following steps: the electrolyte is prepared from electronic grade cobalt sulfate and UP water, and the concentration of cobalt ions is 50g/L-120 g/L;

step two: deeply purifying and removing iron from the electrolyte obtained in the step one by using DLT-1 cation exchange resin;

step three: performing electrolytic refining on the purified electrolyte obtained in the step two, wherein the electrolytic pole distance is 30-60cm, and the current density is 100-²The electrolysis temperature is 40-80 ℃ and the voltage is 0-12V.

2. The method for removing the trace iron in the high-purity cobalt electrolyte as claimed in claim 1, wherein: the functional group of the cation exchange resin DLT-1 in the second step is a phosphate group (-CH)₂PO(OH)₂)。

3. The method for removing the trace iron in the high-purity cobalt electrolyte as claimed in claim 1, wherein: the anode of the electrolytic refining in the third step is made of a titanium mesh basket, the mesh size is 13.5 x 6mm, and the hook is an integrally bent hook; anode cobalt sheets consumed by electrolysis are arranged in the basket and are commercially available 3N8 electric cobalt; the cathode plate is made of a titanium plate.

Technical Field

The invention relates to the field of preparation of electrolytic refining chip-level high-purity cobalt in the metallurgical industry, in particular to a method for removing trace iron in high-purity cobalt electrolyte.

Background

Cobalt is one of important high-purity metal materials, and is an important material for preparing components such as magnetic recording media, magnetic recording heads, photoelectric devices, magnetic sensors, integrated circuits and the like. Most of the applications are to prepare cobalt into a pure metal target or an alloy target and obtain a functional film meeting the requirements in a film coating mode.

The high-purity cobalt with the purity of 5N or more is mainly used for manufacturing the sputtering target material for the super-large-scale integrated circuit industry. At present, the technology is limited to the technical reason, and the high-purity cobalt of 5N and above needs to be imported in a large quantity, so that the development of the preparation technology of the high-purity cobalt with independent intellectual property rights is particularly important.

The purification stage of cobalt solution mostly adopts solvent extraction, extraction chromatography, membrane separation, ion exchange, electrolysis, etc. to remove metal impurities (such as Fe) in cobalt solution³⁺、Ni²⁺、Cu²⁺、Zn²⁺And the like) removing impurities, and then obtaining the metal cobalt by an electrolytic method.

Patent CN103966627A discloses a method for masking impurity iron ions with phosphoric acid or phosphate to form stable complex, which introduces new impurity ions into the electrolytic cobalt solution, which results in increased phosphorus content of the electrolytic cobalt plate, thus affecting the purity of cobalt, and adding extra process steps for treating phosphorus-containing waste liquid.

Patent CN106636638A discloses a method for purifying a cobalt sulfate solution by dynamic ion exchange with chelating resin Monophos, and then preparing high-purity cobalt with iron content less than 1ppm and 99.999% by electrodeposition, wherein the resin used in the method is expensive, the production cost is greatly increased, and the resin is difficult to buy at home and has long shelf life.

Disclosure of Invention

The invention aims to provide a method for removing trace iron in high-purity cobalt electrolyte, which adopts cheap DLT-1 type chelate resin to replace foreign expensive resin, solves the problem that the trace iron in the electrolyte is difficult to remove in the process of preparing medium-high-purity cobalt and electrolytic refining, and has the advantages of simple operation, low cost, good stability, environmental protection and cyclic use of the resin after acid washing.

In order to achieve the purpose, the invention provides the following technical scheme:

a method for removing trace iron in high-purity cobalt electrolyte is characterized by comprising the following steps:

the method comprises the following steps: the electrolyte is prepared from electronic grade cobalt sulfate and UP water, and the concentration of cobalt ions is 50g/L-120 g/L;

step two: deeply purifying and removing iron from the electrolyte obtained in the step one by using DLT-1 cation exchange resin;

step three: performing electrolytic refining on the purified electrolyte obtained in the step two, wherein the electrolytic pole distance is 30-60cm, and the current density is 100-²The electrolysis temperature is 40-80 ℃ and the voltage is 0-12V;

as a preferred technical scheme of the invention, the functional group of the cation exchange resin DLT-1 in the second step is a phosphate group (-CH)₂PO(OH)₂)。

As a preferred technical scheme of the invention, the anode of the electrolytic refining in the third step is made of a titanium mesh basket, the mesh size is 13.5 x 6mm, and the hook is an integrally bent hook; anode cobalt sheets consumed by electrolysis are arranged in the basket and are commercially available 3N8 electric cobalt; the cathode plate is made of a titanium plate.

Compared with the prior art, the invention has the beneficial effects that: the DLT-1 resin can still achieve over 70 percent of iron removal rate under the condition of high-concentration cobalt ion concentration, has excellent removal effect, is simple to operate, is green and environment-friendly, has low price and is economical and practical.

Drawings

FIG. 1 is a GDMS test report for an electrolytic cobalt plate;

Detailed Description

A method for removing trace iron in high-purity cobalt electrolyte is characterized by comprising the following steps:

the method comprises the following steps: the electrolyte is prepared from electronic grade cobalt sulfate and UP water, and the concentration of cobalt ions is 50g/L-120 g/L;

step two: deeply purifying and removing iron from the electrolyte obtained in the step one by using DLT-1 cation exchange resin;

step three: performing electrolytic refining on the purified electrolyte obtained in the step two, wherein the electrolytic pole distance is 30-60cm, and the current density is 100-²The electrolysis temperature is 40-80 ℃ and the voltage is 0-12V;

as a preferred technical scheme of the invention, the functional group of the cation exchange resin DLT-1 in the second step is a phosphate group (-CH)₂PO(OH)₂)。

As a preferred technical scheme of the invention, the anode of the electrolytic refining in the third step is made of a titanium mesh basket, the mesh size is 13.5 x 6mm, and the hook is an integrally bent hook; anode cobalt sheets consumed by electrolysis are arranged in the basket and are commercially available 3N8 electric cobalt; the cathode plate is made of a titanium plate.