CN112322894A - Co-extraction, purification and impurity removal method for nickel, cobalt and manganese - Google Patents

Co-extraction, purification and impurity removal method for nickel, cobalt and manganese Download PDF

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Publication number
CN112322894A
CN112322894A CN202011178380.XA CN202011178380A CN112322894A CN 112322894 A CN112322894 A CN 112322894A CN 202011178380 A CN202011178380 A CN 202011178380A CN 112322894 A CN112322894 A CN 112322894A
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China
Prior art keywords
cobalt
manganese
nickel
extraction
solution
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CN202011178380.XA
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Chinese (zh)
Inventor
许开华
毕凡
张爱青
李炳忠
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Gem Jiangsu Cobalt Industry Co Ltd
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Gem Jiangsu Cobalt Industry Co Ltd
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Priority to CN202011178380.XA priority Critical patent/CN112322894A/en
Publication of CN112322894A publication Critical patent/CN112322894A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/26Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
    • C22B3/38Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
    • C22B3/384Pentavalent phosphorus oxyacids, esters thereof
    • C22B3/3846Phosphoric acid, e.g. (O)P(OH)3
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00Obtaining nickel or cobalt
    • C22B23/04Obtaining nickel or cobalt by wet processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B47/00Obtaining manganese

Abstract

The invention discloses a nickel-cobalt-manganese three-element co-extraction purification impurity removing method which is characterized in that an initial solution only containing nickel sulfate, cobalt sulfate and manganese sulfate solution is subjected to co-extraction to enable nickel, cobalt and manganese to simultaneously enter an organic phase, raffinate is changed into a sodium sulfate solution without cobalt, nickel, cobalt and manganese, an organic phase loaded with nickel, cobalt and manganese is washed by weak acid and then enters a back extraction section, the back extraction section is subjected to back extraction by using high-concentration sulfuric acid, and nickel, cobalt and manganese in the organic phase simultaneously enter an aqueous phase solution to form a nickel-cobalt-manganese sulfate solution. The method for co-extracting, purifying and removing impurities of nickel, cobalt and manganese provided by the invention reduces the production period, reduces the production cost and increases the benefit.

Description

Co-extraction, purification and impurity removal method for nickel, cobalt and manganese
Technical Field
The invention belongs to the field of chemical purification and impurity removal, and particularly relates to a nickel-cobalt-manganese three-element co-extraction purification and impurity removal method.
Background
Nickel cobalt manganese sulfate has been widely and mature used as a raw material of current ternary precursor materials. The three salt solutions are firstly mixed to form a ternary solution after reaching a certain proportion, and then the ternary solution participates in the synthesis reaction to generate the nickel-cobalt-manganese hydroxide. In the process, the original solution is a pure and single unit solution generated after multiple extraction, impurity removal and enrichment.
The unit sulfate solution is generally subjected to acid dissolution and iron removal and then enters extraction for reaction, the extraction reaction mainly comprises impurity removal and enrichment, and the sulfate solution meeting the ternary synthesis requirement is obtained after the enrichment.
However, the three acid salt solutions are extracted in a full process respectively to obtain qualified solutions. For acid solutions of certain materials (ternary test products and process products), if the whole-flow extraction is carried out, the production period is long, and the cost is high.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for co-extracting, purifying and decontaminating nickel, cobalt and manganese.
The invention is realized by the following technical scheme.
A nickel-cobalt-manganese three-element co-extraction purification impurity removal method comprises the steps of enabling nickel, cobalt and manganese to simultaneously enter an organic phase through co-extraction of an initial solution only containing nickel sulfate, cobalt sulfate and manganese sulfate solution, enabling raffinate to be changed into a sodium sulfate solution without cobalt, nickel, cobalt and manganese, washing the organic phase loaded with nickel, cobalt and manganese through weak acid, then entering a back extraction section, and enabling the back extraction section to perform back extraction through high-concentration sulfuric acid, enabling the nickel, cobalt and manganese in the organic phase to simultaneously enter an aqueous phase solution, and forming a nickel-cobalt-manganese sulfate solution.
The invention utilizes the saponifying extractant P507 to carry out co-extraction on the initial solution, the saponification rate is controlled between 60 percent and 70 percent, and the extraction PH value is 2.0 to 3.0.
The Ni content in the initial solution is 30-50g/l, the Co content is 40-60g/l, and the Mn content is 10-20 g/l.
Preferably, the O/A ratio of the extraction section is controlled to be 0.5:1 to 2: 1.
Preferably, the O/A ratio of the washing section is controlled to be 4:1-8:1, and the liquid phase is sulfuric acid solution with the molar concentration of 1.0-1.5 mol/l.
Preferably, the O/A ratio of the stripping section is controlled to be 3:1-5:1, and the liquid phase is sulfuric acid solution with the molar concentration of 4-6 mol/l.
The invention has the beneficial technical effects that:
the method for co-extracting, purifying and removing impurities of nickel, cobalt and manganese provided by the invention reduces the production period, reduces the production cost and increases the benefit.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
In the following examples, the extractant is saponified P507, and the saponification rate of the extractant is 60-70%.
Example 1
Taking an initial solution only containing nickel sulfate, cobalt sulfate and manganese sulfate solution, wherein the nickel content in the initial solution is 50g/l, the cobalt content is 45g/l, the manganese content is 20g/l, the pH value of the solution is adjusted to be 2.0, nickel, cobalt and manganese simultaneously enter an organic phase through co-extraction, the O/A ratio of an extraction section is controlled to be 2:1, raffinate is changed into a sodium sulfate solution without cobalt, nickel, cobalt and manganese, the organic phase loaded with nickel, cobalt and manganese is washed by a sulfuric acid solution with the molar concentration of 1.25mol/l, the O/A ratio of a washing section is controlled to be 5:1, then the organic phase enters a back-extraction section, the back-extraction section carries out back extraction by using sulfuric acid with the molar concentration of 6.0mol/l, the O/A ratio of the back-extraction section is controlled to be 3:1, and nickel, cobalt and manganese in the organic phase simultaneously enter an aqueous phase to form. The organic phase can enter a saponification section for repeated use after being subjected to back extraction.
Example 2
Taking an initial solution only containing nickel sulfate, cobalt sulfate and manganese sulfate solution, wherein the nickel content in the initial solution is 35g/l, the cobalt content is 60g/l, the manganese content is 15g/l, the pH value of the solution is adjusted to be 3.0, nickel, cobalt and manganese simultaneously enter an organic phase through co-extraction, the O/A ratio of an extraction section is controlled to be 1:1, raffinate is changed into a sodium sulfate solution without cobalt, nickel, cobalt and manganese, the organic phase loaded with nickel, cobalt and manganese is washed by a sulfuric acid solution with the molar concentration of 1.5mol/l, the O/A ratio of a washing section is controlled to be 4:1, then the organic phase enters a back-extraction section, the back-extraction section carries out back extraction by using sulfuric acid with the molar concentration of 4.0mol/l, the O/A ratio of the back-extraction section is controlled to be 5:1, and nickel, cobalt and manganese in the organic phase simultaneously enter an aqueous phase to form. The organic phase can enter a saponification section for repeated use after being subjected to back extraction.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention. It should be noted that other equivalent modifications can be made by those skilled in the art in light of the teachings of the present invention, and all such modifications can be made as are within the scope of the present invention.

Claims (6)

1. A nickel-cobalt-manganese three-element co-extraction purification impurity-removing method is characterized in that an initial solution only containing nickel sulfate, cobalt sulfate and manganese sulfate solution is subjected to co-extraction to enable nickel, cobalt and manganese to simultaneously enter an organic phase, raffinate is changed into a sodium sulfate solution without cobalt, nickel, cobalt and manganese, the organic phase loaded with nickel, cobalt and manganese is washed by weak acid and then enters a back-extraction section, and the back-extraction section performs back extraction by using high-concentration sulfuric acid to enable nickel, cobalt and manganese in the organic phase to simultaneously enter an aqueous phase solution to form a nickel-cobalt-manganese sulfate solution.
2. The method for co-extracting, purifying and decontaminating nickel, cobalt and manganese as claimed in claim 1, wherein the co-extraction process employs P507 as an extractant, and the extraction pH is 2.0-3.0.
3. The method of claim 1, wherein the initial solution contains Ni in an amount of 30-50g/l, Co in an amount of 40-60g/l, and Mn in an amount of 10-20 g/l.
4. The method for co-extracting, purifying and decontaminating nickel, cobalt and manganese as claimed in claim 1, wherein the O/A ratio of the extraction section is controlled to be 0.5:1-2: 1.
5. The method for co-extraction, purification and impurity removal of nickel, cobalt and manganese as claimed in claim 1, wherein the O/A ratio of the washing section is controlled to be 4:1-8:1, and the liquid phase is sulfuric acid solution with a molar concentration of 1.0-1.5 mol/l.
6. The method for co-extraction, purification and impurity removal of nickel, cobalt and manganese as claimed in claim 1, wherein the O/A ratio of the stripping section is controlled to be 3:1-5:1, and the liquid phase is sulfuric acid solution with molar concentration of 4-6 mol/l.
CN202011178380.XA 2020-10-29 2020-10-29 Co-extraction, purification and impurity removal method for nickel, cobalt and manganese Pending CN112322894A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114134324A (en) * 2021-10-29 2022-03-04 荆门市格林美新材料有限公司 Method for extracting and purifying nickel-cobalt-manganese ternary solution

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106319228A (en) * 2016-08-26 2017-01-11 荆门市格林美新材料有限公司 Method for recycling nickel, cobalt and manganese synchronously from waste residues containing nickel, cobalt and manganese
CN108281637A (en) * 2018-01-29 2018-07-13 蒋央芳 A kind of preparation method of nickle cobalt lithium manganate
CN109706328A (en) * 2019-01-31 2019-05-03 金驰能源材料有限公司 A kind of method of metallic nickel acid dissoluting liquid back extraction load nickel cobalt manganese organic phase preparation ternary feed liquid
CN109811127A (en) * 2019-01-31 2019-05-28 广东省稀有金属研究所 A method of recycling valuable metal from battery electrode material leachate

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106319228A (en) * 2016-08-26 2017-01-11 荆门市格林美新材料有限公司 Method for recycling nickel, cobalt and manganese synchronously from waste residues containing nickel, cobalt and manganese
CN108281637A (en) * 2018-01-29 2018-07-13 蒋央芳 A kind of preparation method of nickle cobalt lithium manganate
CN109706328A (en) * 2019-01-31 2019-05-03 金驰能源材料有限公司 A kind of method of metallic nickel acid dissoluting liquid back extraction load nickel cobalt manganese organic phase preparation ternary feed liquid
CN109811127A (en) * 2019-01-31 2019-05-28 广东省稀有金属研究所 A method of recycling valuable metal from battery electrode material leachate

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114134324A (en) * 2021-10-29 2022-03-04 荆门市格林美新材料有限公司 Method for extracting and purifying nickel-cobalt-manganese ternary solution

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