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 PDFInfo
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- 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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- cobalt
- manganese
- nickel
- extraction
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 239000010941 cobalt Substances 0.000 title claims abstract description 36
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 36
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 31
- 239000011572 manganese Substances 0.000 title claims abstract description 28
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000000658 coextraction Methods 0.000 title claims abstract description 15
- 239000012535 impurity Substances 0.000 title claims abstract description 12
- 238000000746 purification Methods 0.000 title claims abstract description 9
- 238000000605 extraction Methods 0.000 claims abstract description 29
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000012074 organic phase Substances 0.000 claims abstract description 19
- 239000002253 acid Substances 0.000 claims abstract description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 5
- 239000008346 aqueous phase Substances 0.000 claims abstract description 5
- 229940044175 cobalt sulfate Drugs 0.000 claims abstract description 5
- 229910000361 cobalt sulfate Inorganic materials 0.000 claims abstract description 5
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims abstract description 5
- 229940099596 manganese sulfate Drugs 0.000 claims abstract description 5
- 235000007079 manganese sulphate Nutrition 0.000 claims abstract description 5
- 239000011702 manganese sulphate Substances 0.000 claims abstract description 5
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims abstract description 5
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims abstract description 5
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims abstract description 5
- 229940053662 nickel sulfate Drugs 0.000 claims abstract description 5
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims abstract description 5
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 5
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 5
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- VNTQORJESGFLAZ-UHFFFAOYSA-H cobalt(2+) manganese(2+) nickel(2+) trisulfate Chemical compound [Mn++].[Co++].[Ni++].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O VNTQORJESGFLAZ-UHFFFAOYSA-H 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims description 5
- 239000007791 liquid phase Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000000243 solution Substances 0.000 description 29
- 238000007127 saponification reaction Methods 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- SEVNKUSLDMZOTL-UHFFFAOYSA-H cobalt(2+);manganese(2+);nickel(2+);hexahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mn+2].[Co+2].[Ni+2] SEVNKUSLDMZOTL-UHFFFAOYSA-H 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
- C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
- C22B3/3846—Phosphoric acid, e.g. (O)P(OH)3
-
- 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
-
- 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
- C22B47/00—Obtaining manganese
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
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
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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011178380.XA CN112322894A (en) | 2020-10-29 | 2020-10-29 | Co-extraction, purification and impurity removal method for nickel, cobalt and manganese |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011178380.XA CN112322894A (en) | 2020-10-29 | 2020-10-29 | Co-extraction, purification and impurity removal method for nickel, cobalt and manganese |
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| CN112322894A true CN112322894A (en) | 2021-02-05 |
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| CN202011178380.XA Pending CN112322894A (en) | 2020-10-29 | 2020-10-29 | Co-extraction, purification and impurity removal method for nickel, cobalt and manganese |
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Cited By (2)
| 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 |
| CN115818732A (en) * | 2022-10-28 | 2023-03-21 | 中南大学 | A method for directly preparing a ternary precursor by co-extracting nickel, cobalt and manganese in the high-pressure leaching solution of laterite nickel ore |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 method for preparing a ternary feed solution by back-extracting a nickel-cobalt-manganese-supported organic phase from a metal nickel acid solution |
| CN109811127A (en) * | 2019-01-31 | 2019-05-28 | 广东省稀有金属研究所 | A method for recovering valuable metals from battery electrode material leaching solution |
-
2020
- 2020-10-29 CN CN202011178380.XA patent/CN112322894A/en active Pending
Patent Citations (4)
| 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 method for preparing a ternary feed solution by back-extracting a nickel-cobalt-manganese-supported organic phase from a metal nickel acid solution |
| CN109811127A (en) * | 2019-01-31 | 2019-05-28 | 广东省稀有金属研究所 | A method for recovering valuable metals from battery electrode material leaching solution |
Cited By (2)
| 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 |
| CN115818732A (en) * | 2022-10-28 | 2023-03-21 | 中南大学 | A method for directly preparing a ternary precursor by co-extracting nickel, cobalt and manganese in the high-pressure leaching solution of laterite nickel ore |
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