CN111455175A - Method for removing calcium and magnesium from nickel-cobalt-manganese solution - Google Patents
Method for removing calcium and magnesium from nickel-cobalt-manganese solution Download PDFInfo
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- CN111455175A CN111455175A CN202010518668.0A CN202010518668A CN111455175A CN 111455175 A CN111455175 A CN 111455175A CN 202010518668 A CN202010518668 A CN 202010518668A CN 111455175 A CN111455175 A CN 111455175A
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- 239000011575 calcium Substances 0.000 title claims abstract description 50
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title claims abstract description 49
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 239000011777 magnesium Substances 0.000 title claims abstract description 46
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 46
- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 36
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-UHFFFAOYSA-N 0.000 title claims abstract description 21
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000012716 precipitator Substances 0.000 claims abstract description 13
- 238000000926 separation method Methods 0.000 claims abstract description 12
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 claims abstract description 9
- DBJLJFTWODWSOF-UHFFFAOYSA-L nickel(ii) fluoride Chemical compound F[Ni]F DBJLJFTWODWSOF-UHFFFAOYSA-L 0.000 claims abstract description 9
- 229910021583 Cobalt(III) fluoride Inorganic materials 0.000 claims abstract description 8
- YCYBZKSMUPTWEE-UHFFFAOYSA-L cobalt(ii) fluoride Chemical compound F[Co]F YCYBZKSMUPTWEE-UHFFFAOYSA-L 0.000 claims abstract description 8
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 8
- 229910021569 Manganese fluoride Inorganic materials 0.000 claims abstract description 7
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 7
- 239000010941 cobalt Substances 0.000 claims abstract description 7
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 7
- CTNMMTCXUUFYAP-UHFFFAOYSA-L difluoromanganese Chemical compound F[Mn]F CTNMMTCXUUFYAP-UHFFFAOYSA-L 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 6
- 239000002893 slag Substances 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims abstract description 3
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 claims description 6
- 229910001424 calcium ion Inorganic materials 0.000 claims description 6
- 229910001425 magnesium ion Inorganic materials 0.000 claims description 6
- 150000002500 ions Chemical class 0.000 claims description 5
- 239000011572 manganese Substances 0.000 claims description 4
- 239000011737 fluorine Substances 0.000 claims description 3
- 229910052731 fluorine Inorganic materials 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 238000000605 extraction Methods 0.000 abstract description 14
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 abstract description 12
- 238000002425 crystallisation Methods 0.000 abstract description 4
- 230000008025 crystallization Effects 0.000 abstract description 4
- 238000009854 hydrometallurgy Methods 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract 1
- 239000007788 liquid Substances 0.000 description 8
- 239000012535 impurity Substances 0.000 description 7
- ZFXVRMSLJDYJCH-UHFFFAOYSA-N calcium magnesium Chemical compound [Mg].[Ca] ZFXVRMSLJDYJCH-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 230000001376 precipitating effect Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 229910001634 calcium fluoride Inorganic materials 0.000 description 3
- 229910000361 cobalt sulfate Inorganic materials 0.000 description 3
- 229940044175 cobalt sulfate Drugs 0.000 description 3
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 description 3
- 229910001635 magnesium fluoride Inorganic materials 0.000 description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 3
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- -1 fluorine ions Chemical class 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- UUCGKVQSSPTLOY-UHFFFAOYSA-J cobalt(2+);nickel(2+);tetrahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[Co+2].[Ni+2] UUCGKVQSSPTLOY-UHFFFAOYSA-J 0.000 description 1
- ASKVAEGIVYSGNY-UHFFFAOYSA-L cobalt(ii) hydroxide Chemical compound [OH-].[OH-].[Co+2] ASKVAEGIVYSGNY-UHFFFAOYSA-L 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910001710 laterite Inorganic materials 0.000 description 1
- 239000011504 laterite Substances 0.000 description 1
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc 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
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical 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
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Geochemistry & Mineralogy (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for removing calcium and magnesium from a nickel-cobalt-manganese solution, belonging to the field of nickel-cobalt hydrometallurgy, which comprises the following operation steps: (1) heating the nickel-cobalt-manganese solution to a certain temperature, adding a certain amount of precipitator, and keeping for a certain time; the precipitator is one or a mixture of more of nickel fluoride, cobalt fluoride and manganese fluoride; (2) carrying out liquid-solid separation on the ore pulp to obtain a solution and calcium and magnesium removing slag; (3) the solution is processed by subsequent processes to obtain nickel products and cobalt products. The invention overcomes the problems of calcium sulfate crystallization and difficult separation caused by P507 extraction and magnesium removal in the traditional P204 extraction and calcium removal method, and is an efficient and green method for removing calcium and magnesium from a nickel-cobalt solution.
Description
Technical Field
The invention belongs to the technical field of nickel-cobalt hydrometallurgy, and relates to a method for removing calcium and magnesium from a nickel-cobalt-manganese solution.
Background
The mixed nickel cobalt hydroxide is a nickel cobalt intermediate product obtained by carrying out high-pressure acid leaching, impurity removal, neutralization and precipitation on the laterite nickel ore, and is an important production raw material for producing products such as battery-grade nickel sulfate, battery-grade cobalt sulfate and the like. The mixed nickel hydroxide and cobalt hydroxide are used to produce battery-grade nickel sulfate and battery-grade cobalt sulfate by a hydrometallurgical process, and the procedures generally comprise sulfuric acid leaching, neutralization and iron and aluminum removal, P204 extraction and impurity removal, P507 nickel, cobalt and magnesium separation and other process steps, such as the method adopted by the companies of Jiangxi river tungsten, Jinchuan and Huayouyi industries.
Conventionally, in the aspect of removing calcium and magnesium from a nickel-cobalt solution, a fluoride precipitation method, a solvent extraction method and the like are mainly used. Fluoride precipitation method using MgF2And CaF2And (3) adding NaF reagent to remove calcium and magnesium ions in the solution, wherein the solubility of the calcium and magnesium ions is very low. The disadvantage of this method is that a large amount of sodium ions is introduced into the solution. The solvent extraction method adopts P204 to extract and remove impurities such as Ca, Mn, Cu, Zn and the like, and P507 to separate nickel, cobalt and magnesium from P204 raffinate to produce battery-grade nickel sulfate and battery-grade cobalt sulfate products, which is also a commonly used method at present. The extraction method for removing calcium and magnesium has the following problems: the P204 is adopted for extraction and calcium removal, a large amount of calcium sulfate crystals block an extraction tank and a pipeline, and the calcium sulfate crystals need to be removed periodically; the P207 is adopted to separate magnesium, a long extraction stage number is needed, and the separation difficulty is also high.
Disclosure of Invention
The invention provides a method for removing calcium and magnesium from a nickel-cobalt-manganese solution, which utilizes a precipitator to remove calcium and magnesium, and the solution after calcium and magnesium removal is sent to the next step for extraction, impurity removal and separation. The new process adopts one or more of nickel fluoride, cobalt fluoride and manganese fluoride as calcium and magnesium precipitating agents, the dosage of the precipitating agents is added according to the theoretical quantity of calcium and magnesium, new impurity ions are not introduced, the influence of calcium sulfate crystallization on P204 extraction can be greatly reduced, the operation quantity of P507 extraction and magnesium separation is reduced, and the method is an efficient and green method for removing calcium and magnesium from a nickel-cobalt solution.
The invention solves the technical problem of providing a method for removing calcium and magnesium from a nickel-cobalt-manganese solution, which adopts one or more of nickel fluoride, cobalt fluoride and manganese fluoride as a calcium-magnesium precipitator, adds the amount of the precipitator according to the theoretical amount of calcium and magnesium, does not introduce new impurity ions, can greatly reduce the influence of calcium sulfate crystallization on P204 extraction, reduces the operation amount of P507 extraction and separation of magnesium, and is an efficient and green method for removing calcium and magnesium from the nickel-cobalt solution.
The technical scheme adopted by the invention is as follows:
a method for removing calcium and magnesium from a nickel-cobalt-manganese solution comprises the following steps:
(1) heating the nickel-cobalt-manganese solution to a certain temperature, adding a precipitator, and keeping for a certain time; the precipitator is one or more of nickel fluoride, cobalt fluoride and manganese fluoride;
(2) carrying out liquid-solid separation on the ore pulp to obtain a solution and calcium and magnesium removing slag;
(3) the solution is processed by subsequent processes to obtain nickel products and cobalt products.
Further, the adding amount of the precipitating agent in the step (1) is that the ratio of the amount of fluorine added into the precipitating agent to the amount of calcium and magnesium ion-containing substances in the nickel-cobalt solution is 2: 1.
Further, the nickel-cobalt-manganese solution in the step (1) is a sulfate or chloride system.
Further, the nickel-cobalt-manganese solution in the step (1) contains one or more ions of nickel, cobalt and manganese.
Further, the certain temperature in the step (1) is 25-95 ℃.
Further, the certain time in the step (1) is 0.5-10 hours.
The invention provides a method for removing calcium and magnesium from a nickel-cobalt-manganese solution, which relates to the following reaction principle:
the nickel fluoride, cobalt fluoride and manganese fluoride are easy to dissolve in water, and the added precipitator can decompose fluorine ions in a solution system. Calcium fluoride and magnesium fluoride are insoluble in water, and fluoride ions in the precipitator and calcium and magnesium ions in the nickel-cobalt-manganese solution are combined to generate precipitates to be removed. The process takes place as follows:
2F-+Ca2+＝CaF2↓
2F-+Mg2+＝MgF2↓
thereby realizing the removal of calcium and magnesium from the nickel-cobalt-manganese solution.
The invention has the following advantages: one or more of nickel fluoride, cobalt fluoride and manganese fluoride are used as a calcium-magnesium precipitator, the amount of the precipitator is added according to the theoretical amount of calcium and magnesium, no new impurity ions are introduced, the influence of calcium sulfate crystallization on P204 extraction can be greatly reduced, and the operation amount of P507 extraction separation of magnesium is reduced. The method has the advantages of simple process, strong operability and easy industrial implementation.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
Detailed Description
Example 1
The iron-removed liquid of the nickel-cobalt-manganese solution in a certain plant comprises the following components:
| element(s) | Al | Fe | Ca | Co | Cr | Cu | Mg | Mn | Ni | Zn |
| component/(g/L) | 0.06 | 0.004 | 0.56 | 9.09 | 0.025 | 0.24 | 1.56 | 3.54 | 95.7 | 1.73 |
Heating the solution 500m L to 30 deg.C, adding 3.78g nickel fluoride according to theoretical amount of calcium and magnesium, removing calcium and magnesium for 6h, separating liquid from solid to obtain calcium and magnesium residue and calcium and magnesium-removed liquid, wherein the calcium and magnesium-removed liquid contains calcium 0.01 g/L and magnesium 0.02 g/L.
Example 2
The nickel-cobalt-manganese solution of a certain factory contains 0.54 g/L of calcium and 2.34 g/L of magnesium, the solution 500m L is heated to 70 ℃, 5.31g of nickel fluoride is added according to the theoretical calculation of calcium and magnesium, the time for removing calcium and magnesium is 5 hours, the liquid-solid separation is carried out to obtain calcium-magnesium slag and the liquid after removing calcium and magnesium, the liquid after removing calcium and magnesium contains 0.008 g/L of calcium and 0.016 g/L of magnesium.
Example 3
The nickel-cobalt-manganese solution of a certain factory contains 0.57 g/L of calcium and 2.03 g/L of magnesium, the solution 500m L is heated to 90 ℃, 4.74g of cobalt fluoride is added according to the theoretical amount of calcium and magnesium, the time for removing calcium and magnesium is 3 hours, liquid-solid separation is carried out to obtain calcium-magnesium slag and a liquid after removing calcium and magnesium, the liquid after removing calcium and magnesium contains 0.012 g/L of calcium and 0.018 g/L of magnesium.
Claims (6)
1. The method for removing calcium and magnesium from the nickel-cobalt-manganese solution is characterized by comprising the following operation steps:
(1) heating the nickel-cobalt-manganese solution to a certain temperature, adding a precipitator, and keeping for a certain time; the precipitator is one or more of nickel fluoride, cobalt fluoride and manganese fluoride;
(2) carrying out liquid-solid separation on the ore pulp to obtain a solution and calcium and magnesium removing slag;
(3) the solution is processed by subsequent processes to obtain nickel products and cobalt products.
2. The method of claim 1, wherein the amount of the precipitant added in step (1) is such that the ratio of the amount of fluorine added to the precipitant to the amount of calcium and magnesium ions contained in the nickel cobalt solution is 2: 1.
3. The method of claim 1, wherein the nickel cobalt manganese solution in step (1) is a sulfate or chloride system.
4. The method of claim 1, wherein the nickel-cobalt-manganese solution in step (1) contains one or more ions of nickel, cobalt, and manganese.
5. The method according to claim 1, wherein the certain temperature in step (1) is 25 to 95 ℃.
6. The method according to claim 1, wherein the certain time in the step (1) is 0.5 to 10 hours.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010518668.0A CN111455175A (en) | 2020-06-09 | 2020-06-09 | Method for removing calcium and magnesium from nickel-cobalt-manganese solution |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010518668.0A CN111455175A (en) | 2020-06-09 | 2020-06-09 | Method for removing calcium and magnesium from nickel-cobalt-manganese solution |
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| CN202010518668.0A Pending CN111455175A (en) | 2020-06-09 | 2020-06-09 | Method for removing calcium and magnesium from nickel-cobalt-manganese solution |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112095013A (en) * | 2020-09-27 | 2020-12-18 | 贵州中伟资源循环产业发展有限公司 | Method for removing calcium and magnesium ions in nickel-cobalt-manganese solution and method for recycling nickel-cobalt-manganese ternary waste |
| CN113249593A (en) * | 2021-07-06 | 2021-08-13 | 金驰能源材料有限公司 | Two-stage process for removing calcium and magnesium from solutions containing nickel, cobalt, manganese and lithium |
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| CN112095013A (en) * | 2020-09-27 | 2020-12-18 | 贵州中伟资源循环产业发展有限公司 | Method for removing calcium and magnesium ions in nickel-cobalt-manganese solution and method for recycling nickel-cobalt-manganese ternary waste |
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| CN113249593A (en) * | 2021-07-06 | 2021-08-13 | 金驰能源材料有限公司 | Two-stage process for removing calcium and magnesium from solutions containing nickel, cobalt, manganese and lithium |
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Application publication date: 20200728 |