CN111270086A - Purification method of cobalt chloride solution - Google Patents
Purification method of cobalt chloride solution Download PDFInfo
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- CN111270086A CN111270086A CN201811472186.5A CN201811472186A CN111270086A CN 111270086 A CN111270086 A CN 111270086A CN 201811472186 A CN201811472186 A CN 201811472186A CN 111270086 A CN111270086 A CN 111270086A
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- mixed solution
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- chloride solution
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
- C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/06—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese
- C25C1/08—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese of nickel or cobalt
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
- C25C7/06—Operating or servicing
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Chemical Kinetics & Catalysis (AREA)
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- Mechanical Engineering (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a purification method of a cobalt chloride solution, which comprises the steps of adding high-purity ferrous chloride into the cobalt chloride solution to obtain a mixed solution, stirring the mixed solution, raising the temperature to 45-50 ℃, adding cobalt oxyhydroxide into the mixed solution to oxidize ferrous ions in the solution to obtain an oxidized mixed solution, adjusting the pH value of the oxidized mixed solution by using liquid alkali to obtain an adjusted mixed solution, and finally filtering and adsorbing to obtain a purified cobalt chloride solution; therefore, the invention can utilize the adsorption effect of the colloid to simultaneously absorb the solid particles and the oil in the cobalt chloride solution, so that the solid particles are less than 30 mg/L, and the oil content is less than 10 mg/L, thereby purifying the cobalt chloride solution, improving the quality of the subsequent process, having simple process and greatly reducing the production cost.
Description
Technical Field
The invention belongs to the technical field of purification of cobalt chloride solution, and particularly relates to a purification method of cobalt chloride solution.
Background
In the electrodeposition process, the cobalt chloride solution is prepared by an extraction process and a mode of dissolving cobalt chloride crystals by chlorination, and the cobalt chloride solution produced by the two modes contains a small amount of solid particle impurities and oil.
The content of solid particle impurities is generally 50-100 mg/L, but the diameter is very small, and is 0.01-0.1 particle, so that the impurities can be brought into a product in the production process, and finally the surface of the cobalt plate is rough and the impurities are high; because the particles are small, the particles can not be removed by adopting a common filtering method, but only ultra-precise filtering can be adopted, but because the particles are small, filtering holes are easy to block when ultra-precise filtering is carried out, and because the filtering filter element is frequently cleaned, the filtering filter element is cleaned every time when the solution is filtered by 50 square, which wastes time and labor. In addition, the ultra-precise filtration has high price, and each set is more than millions.
The content of oil is generally between 20 and 50 mg/L, the process requires that the oil content is below 10 mg/L, otherwise, a cobalt plate can be subjected to 'crusting and delamination' or 'long dark spots' in the electrodeposition process, and the common oil removing method is to use activated carbon for adsorption, but the adsorption capacity of the activated carbon is limited, the adsorption capacity is poorer in an aqueous solution system, each kilogram of activity can only be 10 to 20 oil parts, and the method is equivalent to the method that each kilogram of activated carbon can only be used for treating 0.5 to 1 cobalt chloride solution. In addition, the impurity content of the activated carbon is high, 10-20 times of the purified water for cleaning impurities must be used before each use, and the use is troublesome. And the activated carbon after adsorbing the oil belongs to dangerous solid waste and needs special units for treatment.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a purification method of a cobalt chloride solution.
The embodiment of the invention provides a purification method of a cobalt chloride solution, which is implemented by the following steps:
step 1, adding a cobalt chloride solution into a reaction kettle, and adding high-purity ferrous chloride into the cobalt chloride solution to obtain a mixed solution;
step 2, stirring the mixed solution in the reaction kettle, raising the temperature of the reaction kettle to 45-50 ℃, and adding cobalt oxyhydroxide into the mixed solution to oxidize ferrous ions in the solution to obtain an oxidized mixed solution;
step 3, adjusting the pH value of the oxidized mixed solution by using liquid alkali to make the oxidized mixed solution acidic to obtain an adjusted mixed solution;
and 4, filtering and adsorbing the adjusted mixed solution to obtain a purified cobalt chloride solution.
In the scheme, the mass of the high-purity ferrous chloride added in the step 1 is 10-15 times of the total mass of the particles and the oil in the cobalt chloride solution.
In the scheme, the time for stirring the mixed solution in the reaction kettle in the step 2 is 20-40 min.
In the scheme, the mass of the added cobalt oxyhydroxide in the step 2 is 1.5-2 times of the mass of the added high-purity ferrous chloride.
In the scheme, the mass percent of the liquid caustic soda in the step 3 is 1-2%.
In the scheme, the pH value of the mixed solution oxidized in the step 3 is adjusted to 3.0-3.5.
Compared with the prior art, the invention has the advantages that the ferrous chloride has the function of providing iron ions, the cobalt oxyhydroxide has the function of oxidizing ferrous (divalent) ions into high-valence (trivalent) iron ions, and the ferric ions form ferric hydroxide colloid by adjusting the pH.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a purification method of a cobalt chloride solution, which is implemented by the following steps:
step 1, adding a cobalt chloride solution into a reaction kettle, and adding high-purity ferrous chloride into the cobalt chloride solution, wherein the adding mass of the high-purity ferrous chloride is 10-15 times of the total mass of particles and oil in the cobalt chloride solution, so as to obtain a mixed solution;
the high-purity ferrous chloride is used for analyzing the purity, and the high-purity ferrous chloride is used for providing iron ions.
Step 2, stirring the mixed solution in the reaction kettle for 20-40 min, raising the temperature of the reaction kettle to 45-50 ℃, adding a pre-prepared cobalt oxyhydroxide into the mixed solution to oxidize ferrous ions in the solution, wherein the mass of the added cobalt oxyhydroxide is 1.5-2 times that of the added high-purity ferrous chloride, and obtaining an oxidized mixed solution;
step 3, adjusting the pH value of the oxidized mixed solution to 3.0-3.5 by adopting 1-2% by mass of liquid alkali to obtain an adjusted mixed solution, and adjusting the pH value to generate ferric hydroxide colloid in the adjusted mixed solution;
and 4, adsorbing impurities in the solution by using the ferric hydroxide colloid in the adjusted mixed solution, and filtering to obtain a purified cobalt chloride solution.
The invention can utilize the adsorption effect of the colloid, and simultaneously absorb the solid particles and the oil in the cobalt chloride solution, so that the solid particles are less than 30 mg/L, and the oil content is less than 10 mg/L, thereby purifying the cobalt chloride solution, improving the quality of the subsequent process, having simple process and greatly reducing the production cost.
Example 1
Embodiment 1 of the present invention provides a method for purifying a cobalt chloride solution, which is implemented by the following steps:
step 1, adding a cobalt chloride solution into a reaction kettle, and adding high-purity ferrous chloride into the cobalt chloride solution, wherein the adding mass of the high-purity ferrous chloride is 10 times of the total mass of particles and oil in the cobalt chloride solution, so as to obtain a mixed solution;
step 2, stirring the mixed solution in the reaction kettle for 20min, raising the temperature of the reaction kettle to 45 ℃, adding a pre-prepared cobalt oxyhydroxide into the mixed solution to oxidize ferrous ions in the solution, wherein the mass of the added cobalt oxyhydroxide is 1.5 times of that of the added high-purity ferrous chloride, and obtaining an oxidized mixed solution;
step 3, adjusting the pH value of the oxidized mixed solution to 3.0-3.5 by adopting 1% liquid caustic soda in percentage by mass to obtain an adjusted mixed solution, and adjusting the pH value to generate ferric hydroxide colloid in the adjusted mixed solution;
and 4, adsorbing impurities in the solution by using the ferric hydroxide colloid in the adjusted mixed solution, and filtering to obtain a purified cobalt chloride solution.
Example 2
Embodiment 2 of the present invention provides a method for purifying a cobalt chloride solution, which is implemented by the following steps:
step 1, adding a cobalt chloride solution into a reaction kettle, and adding high-purity ferrous chloride into the cobalt chloride solution, wherein the adding mass of the high-purity ferrous chloride is 12 times of the total mass of particles and oil in the cobalt chloride solution, so as to obtain a mixed solution;
step 2, stirring the mixed solution in the reaction kettle for 30min, raising the temperature of the reaction kettle to 47 ℃, adding a pre-prepared cobalt oxyhydroxide into the mixed solution to oxidize ferrous ions in the solution, wherein the mass of the added cobalt oxyhydroxide is 1.5 times of that of the added high-purity ferrous chloride, and obtaining an oxidized mixed solution;
step 3, adjusting the pH value of the oxidized mixed solution to 3.0-3.5 by adopting 2% liquid caustic soda in percentage by mass to obtain an adjusted mixed solution, and adjusting the pH value to generate ferric hydroxide colloid in the adjusted mixed solution;
and 4, adsorbing impurities in the solution by using the ferric hydroxide colloid in the adjusted mixed solution, and filtering to obtain a purified cobalt chloride solution.
Example 3
Embodiment 3 of the present invention provides a method for purifying a cobalt chloride solution, which is implemented by the following steps:
step 1, adding a cobalt chloride solution into a reaction kettle, and adding high-purity ferrous chloride into the cobalt chloride solution, wherein the adding mass of the high-purity ferrous chloride is 12 times of the total mass of particles and oil in the cobalt chloride solution, so as to obtain a mixed solution;
step 2, stirring the mixed solution in the reaction kettle for 30min, raising the temperature of the reaction kettle to 48 ℃, adding a pre-prepared cobalt oxyhydroxide into the mixed solution to oxidize ferrous ions in the solution, wherein the mass of the added cobalt oxyhydroxide is 1.8 times of that of the added high-purity ferrous chloride, and obtaining an oxidized mixed solution;
step 3, adjusting the pH value of the oxidized mixed solution to 3.0-3.5 by adopting 1.5% liquid caustic soda in percentage by mass to obtain an adjusted mixed solution, and adjusting the pH value to generate ferric hydroxide colloid in the adjusted mixed solution;
and 4, adsorbing impurities in the solution by using the ferric hydroxide colloid in the adjusted mixed solution, and filtering to obtain a purified cobalt chloride solution.
Example 4
Embodiment 4 of the present invention provides a method for purifying a cobalt chloride solution, which is implemented by the following steps:
step 1, adding a cobalt chloride solution into a reaction kettle, and adding high-purity ferrous chloride into the cobalt chloride solution, wherein the adding mass of the high-purity ferrous chloride is 15 times of the total mass of particles and oil in the cobalt chloride solution, so as to obtain a mixed solution;
step 2, stirring the mixed solution in the reaction kettle for 40min, raising the temperature of the reaction kettle to 50 ℃, adding a pre-prepared cobalt oxyhydroxide into the mixed solution to oxidize ferrous ions in the solution, wherein the mass of the added cobalt oxyhydroxide is 2 times of that of the added high-purity ferrous chloride, and obtaining an oxidized mixed solution;
step 3, adjusting the pH value of the oxidized mixed solution to 3.0-3.5 by adopting 2% liquid caustic soda in percentage by mass to obtain an adjusted mixed solution, and adjusting the pH value to generate ferric hydroxide colloid in the adjusted mixed solution;
and 4, adsorbing impurities in the solution by using the ferric hydroxide colloid in the adjusted mixed solution, and filtering to obtain a purified cobalt chloride solution.
Example 5
Embodiment 5 of the present invention provides a method for purifying a cobalt chloride solution, which is implemented by the following steps:
step 1, adding a cobalt chloride solution into a reaction kettle, and adding high-purity ferrous chloride into the cobalt chloride solution, wherein the adding mass of the high-purity ferrous chloride is 15 times of the total mass of particles and oil in the cobalt chloride solution, so as to obtain a mixed solution;
step 2, stirring the mixed solution in the reaction kettle for 35min, raising the temperature of the reaction kettle to 48 ℃, adding a pre-prepared cobalt oxyhydroxide into the mixed solution to oxidize ferrous ions in the solution, wherein the mass of the added cobalt oxyhydroxide is 1.5 times of that of the added high-purity ferrous chloride, and obtaining an oxidized mixed solution;
step 3, adjusting the pH value of the oxidized mixed solution to 3.0-3.5 by adopting 1% liquid caustic soda in percentage by mass to obtain an adjusted mixed solution, and adjusting the pH value to generate ferric hydroxide colloid in the adjusted mixed solution;
and 4, adsorbing impurities in the solution by using the ferric hydroxide colloid in the adjusted mixed solution, and filtering to obtain a purified cobalt chloride solution.
Example 6
Embodiment 6 of the present invention provides a method for purifying a cobalt chloride solution, which is implemented by the following steps:
step 1, adding a cobalt chloride solution into a reaction kettle, and adding high-purity ferrous chloride into the cobalt chloride solution, wherein the adding mass of the high-purity ferrous chloride is 10 times of the total mass of particles and oil in the cobalt chloride solution, so as to obtain a mixed solution;
step 2, stirring the mixed solution in the reaction kettle for 35min, raising the temperature of the reaction kettle to 48 ℃, adding a pre-prepared cobalt oxyhydroxide into the mixed solution to oxidize ferrous ions in the solution, wherein the mass of the added cobalt oxyhydroxide is 2 times of that of the added high-purity ferrous chloride, and obtaining an oxidized mixed solution;
step 3, adjusting the pH value of the oxidized mixed solution to 3.0-3.5 by adopting 2% liquid caustic soda in percentage by mass to obtain an adjusted mixed solution, and adjusting the pH value to generate ferric hydroxide colloid in the adjusted mixed solution;
and 4, adsorbing impurities in the solution by using the ferric hydroxide colloid in the adjusted mixed solution, and filtering to obtain a purified cobalt chloride solution.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention.
Claims (6)
1. A method for purifying a cobalt chloride solution, characterized in that it is carried out by the following steps:
step 1, adding a cobalt chloride solution into a reaction kettle, and adding high-purity ferrous chloride into the cobalt chloride solution to obtain a mixed solution;
step 2, stirring the mixed solution in the reaction kettle, raising the temperature of the reaction kettle to 45-50 ℃, and adding cobalt oxyhydroxide into the mixed solution to oxidize ferrous ions in the solution to obtain an oxidized mixed solution;
step 3, adjusting the pH value of the oxidized mixed solution by using liquid alkali to make the oxidized mixed solution acidic to obtain an adjusted mixed solution;
and 4, filtering and adsorbing the adjusted mixed solution to obtain a purified cobalt chloride solution.
2. The method for purifying the cobalt chloride solution according to claim 1, wherein the mass of the high-purity ferrous chloride added in the step 1 is 10-15 times of the total mass of the particulate matters and the oil components in the cobalt chloride solution.
3. The method for purifying a cobalt chloride solution according to claim 2, wherein the time for stirring the mixed solution in the reaction kettle in the step 2 is 20-40 min.
4. The method for purifying a cobalt chloride solution according to claim 3, wherein the mass of the cobalt oxyhydroxide added in the step 2 is 1.5-2 times of the mass of the high-purity ferrous chloride.
5. The method for purifying the cobalt chloride solution according to claim 4, wherein the mass percentage of the liquid caustic soda in the step 3 is 1-2%.
6. The method for purifying a cobalt chloride solution according to claim 5, wherein the pH value of the mixed solution oxidized in the step 3 is adjusted to 3.0-3.5.
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| CN201811472186.5A CN111270086A (en) | 2018-12-04 | 2018-12-04 | Purification method of cobalt chloride solution |
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| CN201811472186.5A CN111270086A (en) | 2018-12-04 | 2018-12-04 | Purification method of cobalt chloride solution |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102930914A (en) * | 2012-11-05 | 2013-02-13 | 桂林电子科技大学 | Processing method of radioactive waste liquid containing uranium |
| US20130280602A1 (en) * | 2011-01-11 | 2013-10-24 | Gs Yuasa International Ltd. | Alkaline secondary battery |
| CN104439280A (en) * | 2014-12-09 | 2015-03-25 | 英德佳纳金属科技有限公司 | Simultaneous preparing method of cobalt hydroxide and cobalt powder |
| CN107460315A (en) * | 2017-08-24 | 2017-12-12 | 中国有色集团刚果矿业有限公司 | A kind of method using copper, cobalt in NF membrane concentrating and separating-neutralization precipitation recovery copper raffinate |
| CN108395034A (en) * | 2018-04-10 | 2018-08-14 | 广东省矿产应用研究所 | Treatment method for removing COD (chemical oxygen demand) in mineral processing wastewater through electrodialysis |
-
2018
- 2018-12-04 CN CN201811472186.5A patent/CN111270086A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130280602A1 (en) * | 2011-01-11 | 2013-10-24 | Gs Yuasa International Ltd. | Alkaline secondary battery |
| CN102930914A (en) * | 2012-11-05 | 2013-02-13 | 桂林电子科技大学 | Processing method of radioactive waste liquid containing uranium |
| CN104439280A (en) * | 2014-12-09 | 2015-03-25 | 英德佳纳金属科技有限公司 | Simultaneous preparing method of cobalt hydroxide and cobalt powder |
| CN107460315A (en) * | 2017-08-24 | 2017-12-12 | 中国有色集团刚果矿业有限公司 | A kind of method using copper, cobalt in NF membrane concentrating and separating-neutralization precipitation recovery copper raffinate |
| CN108395034A (en) * | 2018-04-10 | 2018-08-14 | 广东省矿产应用研究所 | Treatment method for removing COD (chemical oxygen demand) in mineral processing wastewater through electrodialysis |
Non-Patent Citations (1)
| Title |
|---|
| 张桂香等编: "《大学化学实验 无机及分析化学实验分册》", 31 August 2015, 天津大学出版社 * |
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