阅读说明：本技术 一种深度净化高纯钴电解液中铁含量的方法 (Method for deeply purifying iron content 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：本发明公开了一种深度净化高纯钴电解液中铁含量的方法,本发明主要采用廉价的D418型螯合树脂来代替国外昂贵的树脂,D418树脂,对于在高浓度的钴离子浓度的情况下,对铁的去除率,依然能达到70％以上,去除效果优异,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 deeply purifying the iron content in high-purity cobalt electrolyte, which mainly adopts cheap D418 type chelate resin to replace expensive resin and D418 resin abroad, can still achieve over 70 percent of iron removal rate under the condition of high-concentration cobalt ion concentration, has excellent removal effect, solves the problem that 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 capability of recycling the resin after acid washing.)

1. A method for deeply purifying the iron content in high-purity cobalt electrolyte is characterized by comprising the following steps: the method comprises the following steps:

the method comprises the following steps: adopting a titanium mesh basket to prepare an electrolytic refining anode, wherein the mesh size of the electrolytic refining anode reaches 13.5 x 6mm, adopting a titanium plate to prepare a cathode plate, and adopting an integrally bent hook to prepare the hook;

step two: preparing an electrolyte from electronic grade cobalt sulfate and UP water, wherein the concentration of cobalt ions in the obtained cobalt solution is 50-120 g/L, the concentration of impurity iron ions is lower than 0.5g/L, and the pH value of the solution is adjusted to 1-3 by using an acid solution or ammonia water;

step three: washing the resin D418 with pure water for 2-3 times, mixing with a cobalt sulfate solution according to the proportion of 1:5, and stirring for adsorption;

step four: introducing the cobalt solution subjected to iron removal by adsorption in the step three into an electrodeposition tank for electrodeposition impurity removal and purification to obtain high-purity cobalt with iron content of less than 1ppm and 99.99%;

2. the method for deeply purifying the iron content in the high-purity cobalt electrolyte according to claim 1, wherein the method comprises the following steps: in the first step, 3N8 electrocobalt is adopted as anode cobalt sheets consumed in the titanium basket net;

3. the method for deeply purifying the iron content in the high-purity cobalt electrolyte according to claim 2, wherein the method comprises the following steps: stirring and adsorbing at room temperature in the third step, wherein the adsorption lasts for 2-3 days;

4. the method for deeply purifying the iron content in the high-purity cobalt electrolyte according to claim 3, wherein the method comprises the following steps: in the step four, the electrolytic refining is carried out, the electrolytic pole distance is 30-60mm, and the current density is 100-²The electrolysis temperature is 40-80 ℃ and the voltage is 0-12V;

5. the method for deeply purifying the iron content in the high-purity cobalt electrolyte as claimed in claim 4, wherein the method comprises the following steps: and step four, detecting the result by adopting a glow discharge mass spectrometer after the electrolytic refining is finished.

Technical Field

The invention relates to the technical field of chemical industry, in particular to a method for deeply purifying the iron content 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

Aiming at the defect problems existing at present, the invention discloses a method for deeply purifying the iron content in high-purity cobalt electrolyte.

The technical scheme of the invention is as follows: a method for deeply purifying the iron content in high-purity cobalt electrolyte comprises the following steps:

the method comprises the following steps: adopting a titanium mesh basket to prepare an electrolytic refining anode, wherein the mesh size of the electrolytic refining anode reaches 13.5 x 6mm, adopting a titanium plate to prepare a cathode plate, and adopting an integrally bent hook to prepare the hook;

step two: preparing electrolyte from electronic grade cobalt sulfate and UP water, wherein the concentration of cobalt ions in the obtained cobalt solution is

50 g/L-120 g/L, the concentration of impurity iron ions is lower than 0.5g/L, and the pH value of the solution is adjusted to 1-3 by acid solution or ammonia water;

step three: washing the resin D418 with pure water for 2-3 times, mixing with a cobalt sulfate solution according to the proportion of 1:5, and stirring for adsorption;

step four: introducing the cobalt solution subjected to iron removal by adsorption in the step three into an electrodeposition tank for electrodeposition impurity removal and purification to obtain high-purity cobalt with iron content of less than 1ppm and 99.99%;

the method comprises the following specific steps:

in the step one, the anode cobalt sheet consumed in the titanium basket net adopts 3N8 electrocobalt

Stirring and adsorbing at room temperature in the third step, wherein the adsorption lasts for 2-3 days;

in the step four, the electrolytic refining is carried out, the electrolytic pole distance is 30-60mm, and the current density is 100-²The electrolysis temperature is 40-80 ℃ and the voltage is 0-12V;

step four, after the electrolytic refining is finished, a glow discharge mass spectrometer is adopted to detect the achievement;

the invention has the beneficial effects that:

the cheap D418 type chelating resin is adopted to replace foreign expensive resin, the problem that trace iron in electrolyte is difficult to remove in the process of electrolytic refining in the process of preparing medium-high purity cobalt is solved, the removal rate of the D418 resin to iron can still reach more than 70% under the condition of high-concentration cobalt ion concentration, the removal effect is excellent, the method is simple to operate, low in cost, good in stability, green and environment-friendly, and the resin can be recycled after acid washing.

Drawings

FIG. 1 shows a GDMS detection report of an electrolytic cobalt plate.

Detailed Description

The present invention is explained in detail by specific experiments below;