CN116121556A - Nickel cobalt hydroxide intermediate product quality improving method and hydrometallurgical treatment method - Google Patents
Nickel cobalt hydroxide intermediate product quality improving method and hydrometallurgical treatment method Download PDFInfo
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- CN116121556A CN116121556A CN202211661445.5A CN202211661445A CN116121556A CN 116121556 A CN116121556 A CN 116121556A CN 202211661445 A CN202211661445 A CN 202211661445A CN 116121556 A CN116121556 A CN 116121556A
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- 238000000034 method Methods 0.000 title claims abstract description 105
- 239000013067 intermediate product Substances 0.000 title claims abstract description 88
- UUCGKVQSSPTLOY-UHFFFAOYSA-J cobalt(2+);nickel(2+);tetrahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[Co+2].[Ni+2] UUCGKVQSSPTLOY-UHFFFAOYSA-J 0.000 title description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 74
- XTOOSYPCCZOKMC-UHFFFAOYSA-L [OH-].[OH-].[Co].[Ni++] Chemical compound [OH-].[OH-].[Co].[Ni++] XTOOSYPCCZOKMC-UHFFFAOYSA-L 0.000 claims abstract description 63
- 238000002386 leaching Methods 0.000 claims abstract description 48
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 41
- 239000002253 acid Substances 0.000 claims abstract description 33
- 239000012535 impurity Substances 0.000 claims abstract description 31
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 239000000047 product Substances 0.000 claims abstract description 22
- 238000000605 extraction Methods 0.000 claims abstract description 16
- 239000011504 laterite Substances 0.000 claims abstract description 15
- 229910001710 laterite Inorganic materials 0.000 claims abstract description 15
- 239000011777 magnesium Substances 0.000 claims description 51
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 48
- 229910052749 magnesium Inorganic materials 0.000 claims description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 238000001035 drying Methods 0.000 claims description 30
- 238000001556 precipitation Methods 0.000 claims description 21
- 229910017052 cobalt Inorganic materials 0.000 claims description 17
- 239000010941 cobalt Substances 0.000 claims description 17
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 17
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 claims description 16
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 13
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 8
- 230000001376 precipitating effect Effects 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- 239000012065 filter cake Substances 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 238000004090 dissolution Methods 0.000 claims description 5
- 238000009854 hydrometallurgy Methods 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 238000004537 pulping Methods 0.000 claims description 3
- 238000011084 recovery Methods 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims 1
- YTBWYQYUOZHUKJ-UHFFFAOYSA-N oxocobalt;oxonickel Chemical compound [Co]=O.[Ni]=O YTBWYQYUOZHUKJ-UHFFFAOYSA-N 0.000 abstract description 4
- 238000011143 downstream manufacturing Methods 0.000 abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 21
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 18
- 239000000843 powder Substances 0.000 description 11
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 9
- 229910052742 iron Inorganic materials 0.000 description 9
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 8
- 229910052782 aluminium Inorganic materials 0.000 description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 8
- 239000000395 magnesium oxide Substances 0.000 description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 6
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 6
- 238000001704 evaporation Methods 0.000 description 5
- 230000008020 evaporation Effects 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 4
- 235000019341 magnesium sulphate Nutrition 0.000 description 4
- 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 description 4
- 238000001354 calcination Methods 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- 235000019738 Limestone Nutrition 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- 239000004571 lime Substances 0.000 description 2
- 239000006028 limestone Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000005272 metallurgy Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000008267 milk Substances 0.000 description 2
- 210000004080 milk Anatomy 0.000 description 2
- 235000013336 milk Nutrition 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- IPRPPFIAVHPVJH-UHFFFAOYSA-N (4-hydroxyphenyl)acetaldehyde Chemical compound OC1=CC=C(CC=O)C=C1 IPRPPFIAVHPVJH-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229910017709 Ni Co Inorganic materials 0.000 description 1
- 229910003267 Ni-Co Inorganic materials 0.000 description 1
- 229910003262 Ni‐Co Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- TWQMYRYFAWRHJR-UHFFFAOYSA-L [Co].[Ni].[Ni](O)O Chemical compound [Co].[Ni].[Ni](O)O TWQMYRYFAWRHJR-UHFFFAOYSA-L 0.000 description 1
- KSHLPUIIJIOBOQ-UHFFFAOYSA-N [O--].[O--].[O--].[O--].[Co++].[Ni++] Chemical compound [O--].[O--].[O--].[O--].[Co++].[Ni++] KSHLPUIIJIOBOQ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- ZGDWHDKHJKZZIQ-UHFFFAOYSA-N cobalt nickel Chemical compound [Co].[Ni].[Ni].[Ni] ZGDWHDKHJKZZIQ-UHFFFAOYSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000001599 direct drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- WRUGWIBCXHJTDG-UHFFFAOYSA-L magnesium sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Mg+2].[O-]S([O-])(=O)=O WRUGWIBCXHJTDG-UHFFFAOYSA-L 0.000 description 1
- 229940061634 magnesium sulfate heptahydrate Drugs 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 238000009868 nickel metallurgy Methods 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Images
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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
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
-
- 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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting 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
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
- C22B23/0423—Halogenated acids or salts thereof
-
- 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
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
- C22B23/043—Sulfurated acids or salts thereof
-
- 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
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
- C22B23/0438—Nitric acids or salts thereof
-
- 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
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
-
- 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
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/065—Nitric acids or salts thereof
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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
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
-
- 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
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/10—Hydrochloric acid, other halogenated acids or salts thereof
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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
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/16—Extraction of metal compounds from ores or concentrates by wet processes by leaching in organic solutions
- C22B3/1608—Leaching with acyclic or carbocyclic agents
- C22B3/1616—Leaching with acyclic or carbocyclic agents of a single type
- C22B3/165—Leaching with acyclic or carbocyclic agents of a single type with organic acids
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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
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Abstract
The invention discloses a quality improvement method for a cobalt nickel hydroxide intermediate product and a hydrometallurgical treatment method for high-pressure leaching of laterite nickel ore. The quality improvement method of the cobalt nickel hydroxide intermediate product is to carry out quality improvement by adopting a process combining high-temperature heat treatment and wet acid leaching treatment. By adopting the method, the quality of the cobalt nickel hydroxide intermediate product can be improved, and the nickel cobalt oxide product with low impurity content and capable of being directly sold is obtained. The product is subjected to high-pressure leaching hydrometallurgical treatment of laterite nickel ore based on the quality improvement, so that the downstream process is simplified, the transportation cost is reduced, the equipment investment is reduced, and the subsequent extraction pressure is reduced.
Description
Technical Field
The invention relates to the technical field of metallurgy, in particular to a quality improvement method for a cobalt nickel hydroxide intermediate product and a hydrometallurgical treatment method for high-pressure leaching of laterite nickel ores containing the same.
Background
At present, the limonite type laterite-nickel ore high-pressure leaching hydrometallurgy is one of the main technological methods of nickel metallurgy. The method comprises the following process flows: leaching-removing iron and aluminum-depositing nickel and cobalt to obtain a large amount of nickel cobalt hydroxide (MHP) intermediate products, wherein impurities of the intermediate products mainly include manganese, magnesium, iron, aluminum and the like; and converting MHP into nickel sulfate solution, namely separating impurities from nickel and cobalt through leaching, impurity removal and extraction, and obtaining a final nickel and cobalt product.
The present inventors have recognized that the above process has the following problems: 1) In the process, the cobalt nickel hydroxide intermediate product is required to be transported, and huge transport cost is generated in the transportation process; 2) The flow of the extraction impurity removal system and the nickel-cobalt separation system is huge, the process is complex, the flow is complex, and some evaporation systems are also required to be built, so that the production investment cost is increased. 3) The reagent to be added during impurity removal can introduce other impurities, and the organic reverse extraction solution is loaded after extraction, so that further neutralization treatment and the like are needed. Therefore, the provision of an efficient treatment method is of great importance in the field of metallurgy.
Disclosure of Invention
The invention aims to provide a quality improvement method for a cobalt nickel hydroxide intermediate product and a hydrometallurgical treatment method for high-pressure leaching of laterite nickel ores containing the cobalt nickel hydroxide intermediate product. The above object of the present invention is achieved by the following means.
According to one aspect of the invention, the quality improvement method of the cobalt nickel hydroxide intermediate product is characterized in that the cobalt nickel hydroxide intermediate product obtained by precipitating cobalt nickel through a precipitation method in the high-pressure leaching hydrometallurgy process of laterite nickel ore is taken as a raw material, and the water content of the cobalt nickel hydroxide intermediate product is reduced by adopting a process combining high-temperature heat treatment and wet acid leaching treatment, so that magnesium elements serving as impurities are removed, and the quality of the cobalt nickel hydroxide intermediate product is improved.
Optionally, a high temperature heat treatment is adopted first, and then a wet acid leaching treatment is adopted.
Or alternatively, a wet acid leaching treatment is adopted first, and then a high-temperature heat treatment is adopted.
Optionally, the temperature is 300-1000 ℃ and the time is 0.5-6 h during high-temperature heat treatment.
Optionally, during high-temperature heat treatment, the rotary kiln is directly adopted for drying and roasting, or the rotary kiln equipment is adopted for drying and then feeding the dried and roasted.
Optionally, during wet acid leaching treatment, the pH is controlled to be 4-7.5, the temperature is 20-100 ℃, and the time is 0.5-4 h.
Optionally, during wet acid leaching treatment, adding water to slurry, and controlling the liquid-solid ratio (2-8): 1; wherein the acid is one or more selected from hydrochloric acid, sulfuric acid, nitric acid, oxalic acid and carbonic acid.
Optionally, after the wet acid leaching treatment step, the method further comprises: filtering and drying the filter cake, wherein the drying temperature is 100-150 ℃ and the drying time is 2-6 h.
Optionally, the method further comprises: and returning filtrate to a laterite-nickel ore wet method system for nickel-cobalt recovery, wherein the filtrate is a solution containing nickel-cobalt impurities.
Optionally, the water content in the raw materials is 40% -70%, and the magnesium element content is 2% -5%.
Optionally, the final product obtained after upgrading is free of moisture and has a magnesium content of not more than 0.2%.
According to another aspect of the invention, the invention provides a hydrometallurgical treatment method for high pressure leaching of laterite-nickel ores, the method comprising: and (3) carrying out acid dissolution, impurity removal and extraction on the intermediate product after the improvement obtained by the cobalt nickel hydroxide intermediate product quality improvement method to obtain a final nickel cobalt product.
The beneficial effects are that: the invention improves and optimizes the water content and impurity magnesium of the intermediate product by adopting a process combining high-temperature heat treatment and wet acid leaching treatment from the aspect of improving the quality of the intermediate product cobalt nickel hydroxide, reduces the water content of the intermediate product cobalt nickel hydroxide to zero, removes magnesium element in the intermediate product cobalt nickel hydroxide, improves the quality of the intermediate product cobalt nickel hydroxide, and obtains the low-impurity directly-saleable cobalt nickel oxide product.
In addition, by improving the quality of the MHP intermediate product in the high-pressure leaching hydrometallurgical treatment of the laterite nickel ore, the quality of the MHP intermediate product is improved, and the high-pressure leaching hydrometallurgical treatment of the laterite nickel ore is continuously carried out on the product based on the improvement of the quality, so that the downstream process is simplified, the transportation cost is reduced, the equipment investment is reduced, and the subsequent extraction pressure is reduced.
Drawings
FIG. 1 is a schematic flow chart of a method for improving the quality of cobalt nickel hydroxide intermediate products according to the present invention.
FIG. 2 is a flow chart of a method for improving quality of cobalt nickel hydroxide intermediate product according to an embodiment of the invention.
FIG. 3 is a flow chart of a method for improving quality of cobalt nickel hydroxide intermediate product according to an embodiment of the invention.
FIG. 4 is a schematic flow chart of a high pressure leaching hydrometallurgical treatment process of laterite-nickel ores in accordance with an embodiment of the invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. The following description of at least one exemplary embodiment is merely exemplary in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Fig. 1 schematically shows a flow chart of a method for improving quality of cobalt nickel hydroxide intermediate products. As shown in fig. 1, the MHP is upgraded by combining the high-temperature heat treatment and the wet acid leaching treatment to obtain the upgraded product.
According to the method, from two aspects of water content and impurity magnesium content, the water content of the cobalt nickel hydroxide intermediate product is reduced to zero by adopting a high-temperature heat treatment process and a wet acid leaching treatment process, the nickel cobalt content is high, magnesium element in the cobalt nickel hydroxide intermediate product is removed, and the quality of the cobalt nickel hydroxide intermediate product is improved. The method has the advantages of no need of changing the existing process and equipment, reduced water content, reduced huge conveying cost, reduced post-treatment physical quantity, greatly reduced impurity magnesium content, reduced subsequent extraction pressure, no need of equipment investment of an evaporation system and the like, and is an efficient process means for improving the MHP quality and expected in refining of the intermediate product of the MHP in the subsequent hydrometallurgical treatment.
According to the high-pressure leaching hydrometallurgical treatment method for the laterite nickel ore, disclosed by the invention, the quality of the nickel cobalt hydroxide intermediate product is improved by the quality improvement method from the quality of the nickel cobalt hydroxide intermediate product, the material object quantity is reduced by roasting, the nickel cobalt content is improved, magnesium is removed, the influence on a downstream process is reduced, and the problems of high cost, large equipment investment, large subsequent extraction pressure and the like in the hydrometallurgical treatment process are solved.
Fig. 2 schematically illustrates a flow of a cobalt nickel hydroxide intermediate product quality improvement method provided in an embodiment of the invention. The quality improvement method for the cobalt nickel hydroxide intermediate product provided in the embodiment is to dry a filter cake of the cobalt nickel hydroxide intermediate product and perform high-temperature heat treatment; and then, carrying out wet selective leaching treatment on the powder obtained after the high-temperature heat treatment, and selectively leaching out Mg element in the powder, wherein other valuable metals are remained in the solid. Specifically, as shown in fig. 2, the method comprises the following steps:
1) Firstly, drying the cobalt nickel hydroxide intermediate product, removing water in MHP, and drying at 100-150 ℃ for 2-6 h to obtain dried massive solid. The flash drying mode can be adopted for drying, and the dried raw materials do not contain moisture.
Wherein, the intermediate product of cobalt nickel hydroxide is a nickel cobalt nickel hydroxide intermediate product MHP obtained by precipitating nickel and cobalt by a precipitation method in the hydrometallurgical process of laterite nickel ore high-pressure leaching, the impurities in the raw materials mainly comprise manganese, magnesium, iron, aluminum and the like, the content of magnesium element is 2% -5%, and the water content is 40% -70%.
2) And (3) carrying out high-temperature heat treatment on the dried massive solid at the temperature of 300-1000 ℃ for 0.5-6 h to obtain solid powder.
The high-temperature heat treatment can be carried out by adopting a rotary kiln, the temperature can be 450 ℃, 550 ℃, 650 ℃, 750 ℃, 850 ℃, 950 ℃ and the like, the time is 0.5-6 h, the hydroxide is decomposed into oxide, and the brown black powder is obtained after roasting. The manganese, magnesium, iron and aluminum in the raw materials exist in the form of hydroxide, and can be effectively decomposed to form oxide under the conditions, and in addition, the inventor also finds that the temperature is too low to be completely decomposed, and the raw materials are easy to agglomerate and can not form loose powder; while too high a temperature increases the energy consumption.
In this embodiment, the free water in MHP can be removed by drying before the high-temperature heat treatment, and the free water can be removed rapidly under the above conditions, and the free water can be removed completely after about 4 hours, which increases the energy consumption. Of course, the method is not limited thereto, and a rotary kiln may be used for direct drying and calcination.
After the treatment, the MHP product with the water content of 40-70% is dehydrated and converted into an oxide with unchanged metal content and less physical quantity, so that the valuable metal content of the intermediate product is further enriched, and a large amount of freight in the intermediate link is saved; the above treatment step may also decompose basic sulphates of the individual metals entrained in the hydroxide into sulphates.
3) Selectively dissolving out magnesium element from solid powder obtained by high-temperature heat treatment by adopting an acid leaching treatment method, pulping by adding water, and controlling the liquid-solid ratio (2-8) to be 1; for example, the pH can be controlled to be 4-7.5 in a range of 2:1, 4:1, 6:1, etc., the temperature can be controlled to be 20-100 ℃, for example, the temperature can be 40 ℃, 60 ℃,80 ℃ and the like, the time is 0.5-4 h, and the intermediate product after lifting is obtained after filtration and drying. Wherein, the acid can be one or more of hydrochloric acid, sulfuric acid, nitric acid, oxalic acid, carbonic acid and the like.
Some of the soluble salts originally entrained in MHP are directly dissolved by water, such as magnesium sulfate, during the wet treatment process described above. Because the metal precipitation sequence is Fe-Al-Ni-Co-Mn-Mg, the acid washing can wash away some magnesium, the magnesium oxide is dissolved out by controlling the pH value in the non-dissolving zone of Ni-Co, and the pH value is adjusted to 4.5 by adding acid or carbon dioxide is introduced.
4) And filtering and drying after acid leaching treatment to obtain a low-impurity nickel cobalt oxide powder product. The product can be sold after being packaged, and the subsequent treatment cost is reduced.
In addition, the treated nickel-cobalt impurity solution can be returned to a laterite nickel ore wet system for nickel-cobalt recovery, for example, the solution after iron and aluminum removal is mixed to remove first-stage nickel-cobalt precipitation, and then the solution after iron and aluminum removal is returned to remove second-stage nickel-cobalt precipitation.
Fig. 3 schematically illustrates a flow of a second cobalt nickel hydroxide intermediate product quality improvement method provided in an embodiment of the invention. The method for improving the quality of the cobalt nickel hydroxide intermediate product provided by the embodiment is different from the previous embodiment in that the acid leaching treatment is carried out at the forefront, namely, the steps of removing Mg in MHP ore pulp, filtering, high-temperature treatment and the like are carried out, so that the quality of the cobalt nickel hydroxide intermediate product is improved. Specifically, as shown in fig. 2, the method comprises the following steps:
1) And selectively dissolving out magnesium element in the cobalt nickel hydroxide intermediate product by adopting an acid leaching treatment method, and filtering to obtain a filter cake. The specific acid leaching treatment conditions were the same as in the previous example.
2) And (3) drying the filter cake at 100-150 ℃ for 2-6 h, and removing water in the filter cake by drying.
3) And (3) carrying out high-temperature heat treatment on the solid obtained after drying at the temperature of 300-1000 ℃ for 0.5-4 h to obtain a lifted intermediate product.
The quality of the cobalt nickel hydroxide intermediate product is improved by adopting a combined process of high-temperature heat treatment and wet acid leaching treatment based on the cobalt nickel hydroxide intermediate product obtained by precipitating nickel and cobalt by a precipitation method in the hydrometallurgical process of laterite-nickel ore high-pressure leaching.
Two combinations are schematically shown in fig. 2 and 3, one for removal of magnesium after calcination and one for removal of magnesium after calcination. Based on the self water content of MHP, the method can preferably adopt a wet method for removing magnesium, and then adopting a drying and then adopting a fire method for treatment; compared with the method of drying and fire treatment before wet treatment and drying and lifting, the method can further reduce energy consumption under the condition of basically the same process effect.
Fig. 4 schematically illustrates a laterite-nickel ore high pressure leaching hydrometallurgical treatment process provided in an embodiment of the invention, comprising:
1) And (3) carrying out high-pressure leaching treatment on the laterite nickel ore to remove iron and aluminum, and precipitating nickel and cobalt by adopting a precipitation method to obtain a cobalt nickel hydroxide intermediate product. Wherein, HPAL is leached under high pressure, for example, sulfuric acid is added into an autoclave at 250 ℃, valuable elements in laterite nickel ore are leached, meanwhile, impurities are leached, and limestone is generally adopted to remove iron and aluminum, and nickel cobalt is precipitated to form an MHP intermediate product. The precipitation method comprises one of an active magnesium oxide or magnesium hydroxide precipitation method, a sodium hydroxide precipitation method, and a calcium oxide or calcium hydroxide precipitation method.
The water content of the cobalt nickel hydroxide intermediate product obtained by the step ranges from 40% to 70%, the content of magnesium element is 2% to 5%, and compared with other impurities, the magnesium content of the cobalt nickel hydroxide intermediate product obtained by adopting a magnesium oxide precipitation method is higher, the magnesium content of the cobalt nickel hydroxide intermediate product is generally 3% to 5%, the magnesium content of the cobalt nickel hydroxide intermediate product obtained by adopting a sodium hydroxide and lime milk precipitation method is lower, the magnesium content of the cobalt nickel hydroxide intermediate product is generally 2% to 3%, the magnesium content of the high-content impurity magnesium can cause higher subsequent extraction pressure, and the magnesium sulfate evaporation system is also required to be built for post-treatment, so that the equipment investment is high.
2) The quality of the cobalt nickel hydroxide intermediate product is improved by adopting the quality improvement method of the cobalt nickel hydroxide intermediate product, so that an improved intermediate product is obtained. The intermediate product after lifting does not contain moisture, the content of impurity magnesium is reduced, and the magnesium can be effectively removed to be not higher than 0.2%.
3) And (3) carrying out acid dissolution, impurity removal and extraction on the lifted intermediate product to obtain a nickel-cobalt product. Wherein, the acid dissolution, impurity removal and extraction are all conventional methods. In the step, the intermediate product based on the removal of magnesium after lifting is used, the material quantity of post treatment is reduced, the content of magnesium impurity is greatly reduced, the extraction pressure is reduced, the steps of extracting magnesium, back extracting magnesium to form magnesium sulfate solution and producing magnesium sulfate heptahydrate by evaporation and crystallization are omitted, the process is simplified, and the investment cost is reduced.
The technical scheme in the invention is further described below with reference to specific embodiments:
example 1
The MHP product (nickel 39%, cobalt 3.5%, magnesium 3%, water content 65%) was precipitated with sodium hydroxide. Firstly, drying, wherein the drying temperature is controlled to be 120 ℃, and the drying time is 4 hours; and carrying out high-temperature heat treatment on the dried massive solid, wherein the treatment temperature is 900 ℃, and the treatment time is 2 hours. Secondly, treating the brown-black powder obtained by high-temperature heat treatment by adopting a sulfuric acid leaching stirring mode, controlling the pH value to be 6, controlling the time to be 2 hours, and controlling the temperature to be 40 ℃ at room temperature. And filtering and drying after the treatment is finished, and obtaining a lifted product. The product was determined to contain no moisture, 55% nickel, 5.3% cobalt, and 0.05% magnesium.
Example 2
Firstly, roasting a laterite-nickel ore hydrometallurgical MHP product (the dry basis magnesium content is 2.1%) containing 65% of water at 800 ℃ for 2 hours to obtain brown black powder after roasting. Secondly, pulping the brown-black powder by adopting water, controlling the liquid-solid ratio at 2:1, controlling the temperature at 60 ℃ for 2 hours, adjusting the pH value to 5.0 by adopting sulfuric acid, filtering, washing and drying to obtain a low-impurity nickel cobalt oxide powder product which can be directly sold. The leaching rates of nickel and cobalt are respectively 0.12 percent and 0.56 percent, and the leaching rate of magnesium is more than 90 percent. The detection proves that the magnesium content in the final nickel cobalt oxide product is only 0.13 percent.
Example 3
The MHP product (nickel 39%, cobalt 3.5%, magnesium 3%, water content 65%) was precipitated with sodium hydroxide. Firstly, treating by adopting a mode of stirring by carbonic acid leaching, introducing carbon dioxide, controlling the pH value to be 4, controlling the time to be 2 hours, and controlling the temperature to be 40 ℃ at room temperature. Secondly, drying the filter cake, wherein the drying temperature is controlled at 120 ℃ and the drying time is 4 hours; and (3) carrying out high-temperature treatment on the dried massive solid, wherein the treatment temperature is 900 ℃, and the treatment time is 2 hours. The solid obtained is the final product. The product contains no moisture, 51% of nickel, 4.9% of cobalt and 0.2% of magnesium according to measurement.
Example 4
Firstly, carrying out high-pressure leaching treatment on laterite nickel ore, neutralizing with limestone at 250 ℃ to remove iron and aluminum, and precipitating nickel and cobalt by adopting a sodium hydroxide precipitation method to obtain a nickel cobalt hydroxide intermediate product MHP. The water content of the product is 63% and the magnesium content is 2.5% according to the measurement.
Secondly, drying and high-temperature heat treatment is firstly carried out on the cobalt nickel hydroxide intermediate product MHP, wherein the cobalt nickel hydroxide intermediate product MHP is dried for 3 hours at 150 ℃ and baked for 3 hours at 800 ℃; and then acid leaching treatment is adopted, carbon dioxide is introduced, pH=5 is controlled, the temperature is normal, the time is 4 hours, quality is improved, and an intermediate product with 0.15 percent of magnesium is obtained after the improvement.
And finally, carrying out acid dissolution on the lifted intermediate product by adopting sulfuric acid, adopting p204 to remove impurities (remove impurities such as manganese, copper, zinc and the like), separating nickel and cobalt by using a p507 extractant, and extracting cobalt to obtain a final nickel and cobalt product. Compared with the method without improving the quality, the extraction pressure is small.
The following advantages are also provided in some embodiments of the present invention over the prior art:
(1) The intermediate product of nickel cobalt hydroxide obtained by precipitating nickel cobalt in the prior art has high water content, generally 40% -70%, wherein the magnesium oxide precipitation method is relatively low, but also reaches 45%, and due to the high water content, the MHP is transported to a refinery from a production place, which is equivalent to more than half of water transported, and huge transportation cost is consumed. According to the method, the water content of the cobalt nickel hydroxide intermediate product is reduced from the water content, so that the transportation cost of MHP is reduced.
(2) The nickel content obtained by precipitating nickel and cobalt by adopting a magnesium oxide precipitation method is only about 35%, and the nickel content can reach about 40% by adopting a sodium hydroxide precipitation method, so that the physical quantity is larger, and the subsequent treatment is inconvenient. According to the method, from the perspective of physical quantity, the physical quantity is reduced by improving the content of valuable elements on the dry basis of the cobalt nickel hydroxide intermediate product, and the follow-up treatment process is more convenient to carry out after improvement.
(3) The MHP magnesium content obtained by different precipitation methods is different, the magnesium content obtained by the magnesium oxide precipitation method is generally 3% -5%, and the magnesium content obtained by the sodium hydroxide and lime milk precipitation method is generally 2% -3%. According to the method, the content of impurities in the cobalt nickel hydroxide intermediate product, particularly the content of magnesium in the cobalt nickel hydroxide intermediate product is reduced, so that the subsequent extraction pressure is reduced, the equipment investment cost is reduced, and the problem of high investment cost caused by a magnesium sulfate evaporation system which is required to be built in the prior art is avoided.
The description of the present invention has been presented for purposes of illustration and description, and is not intended to be exhaustive or limited to the invention in the form disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, and to enable others of ordinary skill in the art to understand the invention for various embodiments with various modifications as are suited to the particular use contemplated.
Claims (12)
1. The quality improvement method is characterized in that the quality improvement method takes a cobalt nickel hydroxide intermediate product obtained by precipitating nickel and cobalt by a precipitation method in the high-pressure leaching hydrometallurgy process of laterite nickel ore as a raw material, and reduces the water content of the cobalt nickel hydroxide intermediate product and removes magnesium element impurities by adopting a combined process of high-temperature heat treatment and wet acid leaching treatment, so as to improve the quality of the cobalt nickel hydroxide intermediate product.
2. The method for improving the quality of the cobalt nickel hydroxide intermediate product according to claim 1, wherein the high-temperature heat treatment is adopted first, and then the wet acid leaching treatment is adopted.
3. The method for improving the quality of the cobalt nickel hydroxide intermediate product according to claim 1, wherein wet acid leaching treatment is adopted first, and then high-temperature heat treatment is adopted.
4. The method for improving the quality of the cobalt nickel hydroxide intermediate product according to claim 1, wherein the temperature is 300-1000 ℃ and the time is 0.5-6 h during the high-temperature heat treatment.
5. The method for improving the quality of the cobalt nickel hydroxide intermediate product according to claim 2, wherein the cobalt nickel hydroxide intermediate product is directly dried and roasted by a rotary kiln or is roasted by a rotary kiln device after being dried.
6. The method for improving the quality of the cobalt nickel hydroxide intermediate product according to claim 1, wherein the pH is controlled to be 4-7.5, the temperature is 20-100 ℃ and the time is 0.5-4 h during the wet acid leaching treatment.
7. The method for improving the quality of the cobalt nickel hydroxide intermediate product according to claim 1, which is characterized in that when wet acid leaching treatment is carried out, water is added for pulping, and the liquid-solid ratio (2-8) is controlled to be 1; wherein the acid is one or more selected from hydrochloric acid, sulfuric acid, nitric acid, oxalic acid and carbonic acid.
8. The method for improving the quality of the cobalt nickel hydroxide intermediate product according to claim 2, further comprising, after the wet acid leaching treatment step: filtering and drying the filter cake, wherein the drying temperature is 100-150 ℃ and the drying time is 2-6 h.
9. The method for improving the quality of a cobalt nickel hydroxide intermediate product according to claim 8, further comprising: and returning filtrate to a laterite-nickel ore wet method system for nickel-cobalt recovery, wherein the filtrate is a solution containing nickel-cobalt impurities.
10. The method for improving the quality of the cobalt nickel hydroxide intermediate product according to claim 1, wherein the water content of the raw materials is 40-70%, and the content of magnesium element is 2-5%.
11. The method for improving the quality of cobalt nickel hydroxide intermediate product according to claim 1, wherein the final product obtained after the quality improvement contains no moisture and no magnesium content of more than 0.2%.
12. The hydrometallurgical treatment method for high-pressure leaching of laterite nickel ore is characterized by comprising the following steps:
the improved intermediate product obtained by the quality improvement method of cobalt nickel hydroxide intermediate product according to any one of claims 1-11 is subjected to acid dissolution, impurity removal and extraction to obtain the final nickel cobalt product.
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| PCT/CN2023/140944 WO2024131932A1 (en) | 2022-12-23 | 2023-12-22 | Method for improving quality of intermediate product of mixed nickel-cobalt hydroxide precipitate, and hydrometallurgical treatment method |
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| WO2024131932A1 (en) * | 2022-12-23 | 2024-06-27 | 中国恩菲工程技术有限公司 | Method for improving quality of intermediate product of mixed nickel-cobalt hydroxide precipitate, and hydrometallurgical treatment method |
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