CN105925796A - Method for separating and recycling nickel-molybdenum iron from black rock series nickel-molybdenum iron sulfide ores - Google Patents
Method for separating and recycling nickel-molybdenum iron from black rock series nickel-molybdenum iron sulfide ores Download PDFInfo
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- CN105925796A CN105925796A CN201610276361.8A CN201610276361A CN105925796A CN 105925796 A CN105925796 A CN 105925796A CN 201610276361 A CN201610276361 A CN 201610276361A CN 105925796 A CN105925796 A CN 105925796A
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- nickel
- molybdenum
- molybdenum iron
- iron
- black rock
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- KPXNHLPHEBZERE-UHFFFAOYSA-N [Fe]=S.[Mo].[Ni] Chemical compound [Fe]=S.[Mo].[Ni] KPXNHLPHEBZERE-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 30
- VAWNDNOTGRTLLU-UHFFFAOYSA-N iron molybdenum nickel Chemical compound [Fe].[Ni].[Mo] VAWNDNOTGRTLLU-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 239000011435 rock Substances 0.000 title abstract description 6
- 238000004064 recycling Methods 0.000 title abstract 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 47
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 37
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 29
- 239000001301 oxygen Substances 0.000 claims abstract description 29
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 26
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000011733 molybdenum Substances 0.000 claims abstract description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 24
- 239000002893 slag Substances 0.000 claims abstract description 20
- 239000007787 solid Substances 0.000 claims abstract description 19
- 108010038629 Molybdoferredoxin Proteins 0.000 claims abstract description 16
- HBELESVMOSDEOV-UHFFFAOYSA-N [Fe].[Mo] Chemical compound [Fe].[Mo] HBELESVMOSDEOV-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000926 separation method Methods 0.000 claims abstract description 16
- 238000011084 recovery Methods 0.000 claims abstract description 15
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 11
- 239000010703 silicon Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims abstract description 9
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims abstract description 9
- 235000021110 pickles Nutrition 0.000 claims abstract description 8
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 8
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 8
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 23
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 17
- 229910052717 sulfur Inorganic materials 0.000 claims description 17
- 239000011593 sulfur Substances 0.000 claims description 17
- 239000000377 silicon dioxide Substances 0.000 claims description 11
- 238000010298 pulverizing process Methods 0.000 claims description 7
- 238000002386 leaching Methods 0.000 abstract description 17
- 229910052751 metal Inorganic materials 0.000 abstract description 8
- 238000000605 extraction Methods 0.000 abstract description 6
- 229910052742 iron Inorganic materials 0.000 abstract description 6
- 239000002184 metal Substances 0.000 abstract description 6
- 238000005272 metallurgy Methods 0.000 abstract description 2
- 230000001590 oxidative effect Effects 0.000 abstract description 2
- 230000009466 transformation Effects 0.000 abstract 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 18
- 239000011707 mineral Substances 0.000 description 18
- 235000010755 mineral Nutrition 0.000 description 18
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 13
- 238000006243 chemical reaction Methods 0.000 description 11
- DDTIGTPWGISMKL-UHFFFAOYSA-N molybdenum nickel Chemical compound [Ni].[Mo] DDTIGTPWGISMKL-UHFFFAOYSA-N 0.000 description 10
- 238000007254 oxidation reaction Methods 0.000 description 7
- -1 pyrite) Chemical compound 0.000 description 7
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 6
- 229910001447 ferric ion Inorganic materials 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052683 pyrite Inorganic materials 0.000 description 3
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 3
- 239000011028 pyrite Substances 0.000 description 3
- 239000001117 sulphuric acid Substances 0.000 description 3
- 235000011149 sulphuric acid Nutrition 0.000 description 3
- 229910000863 Ferronickel Inorganic materials 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000002734 clay mineral Substances 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 241000206602 Eukaryota Species 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 206010044565 Tremor Diseases 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910001448 ferrous ion Inorganic materials 0.000 description 1
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000010310 metallurgical process Methods 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- MRDDPVFURQTAIS-UHFFFAOYSA-N molybdenum;sulfanylidenenickel Chemical compound [Ni].[Mo]=S MRDDPVFURQTAIS-UHFFFAOYSA-N 0.000 description 1
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 229910052954 pentlandite Inorganic materials 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 description 1
- DNYWZCXLKNTFFI-UHFFFAOYSA-N uranium Chemical compound [U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U] DNYWZCXLKNTFFI-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
-
- 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/008—Wet processes by an alkaline or ammoniacal leaching
-
- 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/04—Working-up slag
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Environmental & Geological Engineering (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to a method for separating and recycling nickel-molybdenum iron from black rock series nickel-molybdenum iron sulfide ores, and belongs to the technical field of metallurgy and chemistry. The method comprises the following steps: crushing and grinding black rock series nickel-molybdenum iron sulfide ores, adding water in a liquid-solid ratio being (2-4):1 mL/g, reacting for 3-5 hours while controlling oxygen pressure to be 0.3-0.5 MPa and controlling a temperature to 170-200 DEG C, thereby obtaining nickel sulfate pickle liquor and molybdenum-iron slag; adding the obtained molybdenum-iron slag into a NaOH solution with concentration being 2-4 mol/L in a liquid-solid ratio being (2-4):1 mL/g, and reacting for 3-5 hours at a temperature of 70-90 DEG C, thereby obtaining a sodium molybdate solution and leaching residues rich in iron and silicon. According to the method, under a high-temperature oxygen pressure condition, water is used as a leaching medium, and extraction and separation of nickel-molybdenum iron are realized by virtue of oxidative transformation on components such as nickel, molybdenum, iron and the like in ores by oxygen; and the technical process is simple, and the metal recovery rate is high.
Description
Technical field
The method that the present invention relates to a kind of Black Rock Sequence nickel-molybdenum iron sulphide ore separation and recovery nickel-molybdenum iron, belongs to chemical metallurgy technical field.
Background technology
Carbonaceous series of rocks mineral are a kind of complex multi-metal mineral containing Determination of multiple metal elements; it is created on shake denier to adopt, tremble with fear in the ancient stratum such as open system, Silurian; under the reducing environment of shallow sea, the flammable mineral products of height matter degree are formed by Homonemeae unicellular lower eukaryote; it is characterized in ash-rich; low heat value, outward appearance such as black stone, containing vanadium, molybdenum, nickel, phosphorus, copper, sulfur, ferrum, the Determination of multiple metal elements such as uranium.
China's carbonaceous series of rocks mineral are mainly distributed on west from the western Hunan, through Jiangxi, Anhui two province, east is on the band in West Zhejiang Province, wherein Yuanling-Changde district, Anhua-district of Ningxiang, Linxiang-Chongyang district, Qian Xian-Shexian County district are five areas of rich ore deposits Han vanadium black culm of China, and the black culm of substantial amounts of nickeliferous molybdenum is contained on the ground such as Zhijin County In Guizhou Province, Nayong County, Jinsha County, Tongren City, Zunyi, it is to extract the mineral resources that nickel molybdenum is important.
The material composition complexity of the black carbonaceous series of rocks mineral of nickeliferous molybdenum, it is various that nickel and the occurrence status of molybdenum and tax deposit variation of valence, disperse trickle, in same ore body, it is usually present multiple nickel mineral and molybdenum ore thing, wherein nickel main with the Independent Mineral of nickel, sulfide (such as pyrite), clay mineral relevant, partly with capillose (NiS), two sulfur nickel minerals (NiS2) and polydymite (Ni3S4) form existence, part replaces the Fe in pyrite with pentlandite ((Ni, Fe) S2) form existence, part replaces the Al in silica octahedra " multiple stratum reticulare " and alumina octahedral " list stratum reticulare "3+、Fe3+Deng the silicate entered in clay mineral, aluminosilicate phase, additionally there are the nickel of the organic that part is combined with organo-functional group；Molybdenum is mostly composed and is stored in sulfide, and with pyrite association, predominantly molybdenite (MoS2) and sulfur ferrum molybdenum ore ((Mo, Fe) xSy), separately there is part mainly to replace Al with class matter in-phase version3+、Fe3+Deng entrance mica mineral and silicate phase, other are then present in organic matter with organic form.Owing to the nickel molybdenum in mineral is deposited with the tax of multiple valence state various ways, mutually adulterate association, and disseminated grain size is thinner, argillization state is serious, granularity thickness is the most uneven, and microfine quartz and clay content are higher simultaneously, and the existence of nickel molybdenum presents the features such as complexity, variation, many changes, thus, use technique of preparing to be difficult to valuable mineral separation and concentration.
At present, extracting method mainly uses traditional roasting-alkaline leaching, sodium carbonate roasting-water seaoning, the deficiency of this type of method is that calcination is substantially at solid-solid surface generation chemical reaction, and due to nickel molybdenum content low ferrum sulfur content height in the black culm of nickeliferous molybdenum, fundamentally limit the response speed of nickel-molybdenum ore thing and conversion ratio metal recovery rate is low, cost is high, of poor benefits, it is serious that the sulfur dioxide of the generation of roasting simultaneously easily causes environmental pollution.Drawback in order to avoid tradition roasting technique, the technological process that nickel molybdenum is extracted by scientific and technical personnel is improved, develop direct oxygen pressure acid leaching extraction nickel molybdenum technique and the pressure alkali extraction of direct oxygen takes molybdenum, ferronickel slag normal pressure acid leaching extraction nickel technique, but oxygen pressure acid leaching process fails to make full use of the sulfur of mineral, and owing to the conversion of sulfur is suppressed, limit the leaching of nickel molybdenum, and the solution composition complexity obtained needs further purification separation；The nickel molybdenum solution that the ferronickel slag that oxygen pressure alkali soaking technology obtains obtains after normal pressure acidleach is more intractable, there are the problem such as valency metal dispersion, reagent consumption is big, cost is high, nickel molybdenum separation difficulty.
Summary of the invention
The problem existed for above-mentioned prior art and deficiency, the present invention provides the method for a kind of Black Rock Sequence nickel-molybdenum iron sulphide ore separation and recovery nickel-molybdenum iron.The method uses water as leaching medium under the conditions of high temperature oxygen pressure, by oxygen, the oxidation of the compositions such as the nickel in Ore, molybdenum, ferrum is converted, realize the extraction of nickel-molybdenum iron and separate, its technical matters is simple, and metal recovery rate is high, and nickel-molybdenum iron is easily separated, reagent consumption is little, low cost, pollution-free, the present invention is achieved through the following technical solutions.
The method of a kind of Black Rock Sequence nickel-molybdenum iron sulphide ore separation and recovery nickel-molybdenum iron, it specifically comprises the following steps that
(1) first by after Black Rock Sequence nickel-molybdenum iron sulphide ore pulverizing and jevigating, being 2～4:1mL/g to add water according to liquid-solid ratio, to control oxygen pressure be 0.3～0.5MPa, temperature reacts 3～5h under the conditions of being 170～200 DEG C and obtains nickel sulfate pickle liquor and molybdenum iron slag；
(2) molybdenum iron slag step (1) obtained is in the NaOH solution that 2～4:1mL/g addition concentration are 2～4mol/L according to liquid-solid ratio, reacts 3～5h acquisition sodium molybdate solution and the leached muds rich in ferrum silicon under the conditions of temperature is 70～90 DEG C.
In described step (1), Black Rock Sequence nickel-molybdenum iron sulphide ore includes following mass percent component: nickel 1%～6%, molybdenum 4%～9%, ferrum 10～18%, sulfur 20～30% and silica 1 0～17%.
The invention has the beneficial effects as follows:
(1) present invention uses oxygen setting-out soaking technology, make complicated mineral be changed into readily soluble compound during pressure oxidation by traditional handicraft becomes according to the method for the selected high-temperature roasting of mineralogical property and leaching or precipitate is separated from each other, enhance metallurgical process, it is to avoid the smoke pollutions such as sulfur dioxide.
(2) the dipped journey of oxygen setting-out in making full use of Black Rock Sequence nickel-molybdenum iron sulphide ore highly active sulfidal compound be oxidized easily the feature being converted into sulphuric acid, other reagent the most additional, the sulfidal compound in mineral is relied on to aoxidize the sulphuric acid being converted under the conditions of oxygen pressure, the nickel directly converted and dissolve in Black Rock Sequence mineral generates nickel sulfate and enters solution, and dissolution iron rule generates bloodstone slag under the conditions of high temperature oxygen pressure in mineral, utilize the elementary sulfur in leaching process mineral to be converted into sulphuric acid simultaneously, the molybdenum making dissolution is converted into precipitate molybdic acid and enters slag phase, preferably achieve the separation and Extraction of nickel-molybdenum iron.
(3) ferrum during the dipped journey of oxygen setting-out utilizes Black Rock Sequence nickel-molybdenum iron sulphide ore forms Fe in leaching process3+/Fe2+Ion pair, oxidation of divalent iron ion in solution is become ferric ion by dissolved oxygen, and nickel molybdenum sulfidal compound is oxidized to sulfate and least a portion of elementary sulfur etc., Fe by ferric ion further3+/Fe2+The existence of ion pair changes the mechanism of this oxidizing process, make the gas-solid reaction of original oxygen direct oxidation nickel molybdenum sulfidal compound, it is transformed into dioxygen oxidation ferrous ion and generates gas-liquid reaction and the ferric ion liquid-solid reaction to nickel molybdenum sulfidal compound of ferric ion, the oxidation of the transmission and nickel molybdenum sulphide of accelerating oxygen converts
(4) the invention belongs to the high-efficiency cleaning metallurgical technology of a kind of oxidation reaction, its technological process is short, and metal recovery rate is high, and comprehensive resource utilization rate is high, it is not necessary to roasting, smoke-less pollution, reagent consumption is few, and production cost is low.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the invention will be further described.
Embodiment 1
The method of this Black Rock Sequence nickel-molybdenum iron sulphide ore separation and recovery nickel-molybdenum iron, it specifically comprises the following steps that
(1) first by Black Rock Sequence nickel-molybdenum iron sulphide ore (somewhere, Guizhou Black Rock Sequence nickel-molybdenum iron sulphide ore, including following mass percent component: nickel 4.73%, molybdenum 6.89%, ferrum 15.85%, sulfur 25.68% and silica 1 3.5%) pulverizing and jevigating is to after-200 mesh >=90%, it is that 3:1mL/g adds water according to liquid-solid ratio, be passed through industrial oxygen controlling oxygen pressure for 0.5MPa(), temperature be 170～180 DEG C under the conditions of reaction 5h to obtain sulfuric acid concentration be 36g/L nickel sulfate pickle liquor and molybdenum iron slag, the leaching rate of nickel is 97.2%；
(2) molybdenum iron slag step (1) obtained is that 4:1mL/g adds in the NaOH solution that concentration is 2mol/L according to liquid-solid ratio, under the conditions of temperature is 70～80 DEG C, reacts 5h obtains sodium molybdate solution and the leached mud rich in ferrum silicon, molybdenum leaching rate is 94.37%, includes following mass percent component rich in the leached mud of ferrum silicon: nickel 0.45%, molybdenum 0.72%, ferrum 23.17%, silica 1 9.57% and sulfur 1.72%.
Embodiment 2
The method of this Black Rock Sequence nickel-molybdenum iron sulphide ore separation and recovery nickel-molybdenum iron, it specifically comprises the following steps that
(1) first by Black Rock Sequence nickel-molybdenum iron sulphide ore (somewhere, Guizhou Black Rock Sequence nickel-molybdenum iron sulphide ore, including following mass percent component: nickel 4.73%, molybdenum 6.89%, ferrum 15.85%, sulfur 25.68% and silica 1 3.5%) pulverizing and jevigating is to after-200 mesh >=90%, it is that 4:1mL/g adds water according to liquid-solid ratio, be passed through industrial oxygen controlling oxygen pressure for 0.3MPa(), temperature be 180～190 DEG C under the conditions of reaction 3h to obtain sulfuric acid concentration be 27g/L nickel sulfate pickle liquor and molybdenum iron slag, the leaching rate of nickel is 91.73%；
(2) molybdenum iron slag step (1) obtained is that 2:1mL/g adds in the NaOH solution that concentration is 4mol/L according to liquid-solid ratio, under the conditions of temperature is 70～80 DEG C, reacts 4h obtains sodium molybdate solution and the leached mud rich in ferrum silicon, molybdenum leaching rate is 90.16%, includes following mass percent component rich in the leached mud of ferrum silicon: nickel 0.52%, molybdenum 0.81%, ferrum 21.37%, silica 1 8.52% and sulfur 1.91%.
Embodiment 3
The method of this Black Rock Sequence nickel-molybdenum iron sulphide ore separation and recovery nickel-molybdenum iron, it specifically comprises the following steps that
(1) first by Black Rock Sequence nickel-molybdenum iron sulphide ore (somewhere, Guizhou Black Rock Sequence nickel-molybdenum iron sulphide ore, including following mass percent component: nickel 4.73%, molybdenum 6.89%, ferrum 15.85%, sulfur 25.68% and silica 1 3.5%) pulverizing and jevigating is to after-200 mesh >=90%, it is that 2:1mL/g adds water according to liquid-solid ratio, be passed through industrial oxygen controlling oxygen pressure for 0.4MPa(), temperature be 190～200 DEG C under the conditions of reaction 4h to obtain sulfuric acid concentration be 43g/L nickel sulfate pickle liquor and molybdenum iron slag, the leaching rate of nickel is 98.33%；
(2) molybdenum iron slag step (1) obtained is that 3:1mL/g adds in the NaOH solution that concentration is 3mol/L according to liquid-solid ratio, under the conditions of temperature is 80～90 DEG C, reacts 3h obtains sodium molybdate solution and the leached mud rich in ferrum silicon, molybdenum leaching rate is 95.28%, includes following mass percent component rich in the leached mud of ferrum silicon: nickel 0.41%, molybdenum 0.63%, ferrum 24.11%, silicon dioxide 20.79% and sulfur 1.69%.
Embodiment 4
The method of this Black Rock Sequence nickel-molybdenum iron sulphide ore separation and recovery nickel-molybdenum iron, it specifically comprises the following steps that
(1) first by Black Rock Sequence nickel-molybdenum iron sulphide ore (somewhere, Guizhou Black Rock Sequence nickel-molybdenum iron sulphide ore, including following mass percent component: nickel 1%, molybdenum 4%, ferrum 18%, sulfur 30% and silica 1 0%) pulverizing and jevigating is to after-200 mesh >=90%, be that 2:1mL/g adds water according to liquid-solid ratio, be passed through industrial oxygen controlling oxygen pressure for 0.4MPa(), temperature be 190～200 DEG C under the conditions of reaction 4h to obtain sulfuric acid concentration be nickel sulfate pickle liquor and molybdenum iron slag；
(2) molybdenum iron slag step (1) obtained is that 3:1mL/g adds in the NaOH solution that concentration is 3mol/L according to liquid-solid ratio, reacts 3h and obtain sodium molybdate solution and the leached mud rich in ferrum silicon under the conditions of temperature is 80～90 DEG C.
Embodiment 5
The method of this Black Rock Sequence nickel-molybdenum iron sulphide ore separation and recovery nickel-molybdenum iron, it specifically comprises the following steps that
(1) first by Black Rock Sequence nickel-molybdenum iron sulphide ore (somewhere, Guizhou Black Rock Sequence nickel-molybdenum iron sulphide ore, including following mass percent component: nickel 6%, molybdenum 9%, ferrum 10%, sulfur 20% and silica 1 7%) pulverizing and jevigating is to after-200 mesh >=90%, be that 2:1mL/g adds water according to liquid-solid ratio, be passed through industrial oxygen controlling oxygen pressure for 0.4MPa(), temperature be 190～200 DEG C under the conditions of reaction 4h to obtain sulfuric acid concentration be nickel sulfate pickle liquor and molybdenum iron slag；
(2) molybdenum iron slag step (1) obtained is that 3:1mL/g adds in the NaOH solution that concentration is 3mol/L according to liquid-solid ratio, reacts 3h and obtain sodium molybdate solution and the leached mud rich in ferrum silicon under the conditions of temperature is 80～90 DEG C.
Above the detailed description of the invention of the present invention is explained in detail, but the present invention is not limited to above-mentioned embodiment, in the ken that those of ordinary skill in the art are possessed, it is also possible to various changes can be made on the premise of without departing from present inventive concept.
Claims (2)
1. the method for a Black Rock Sequence nickel-molybdenum iron sulphide ore separation and recovery nickel-molybdenum iron, it is characterised in that specifically comprise the following steps that
(1) first by after Black Rock Sequence nickel-molybdenum iron sulphide ore pulverizing and jevigating, being 2～4:1mL/g to add water according to liquid-solid ratio, to control oxygen pressure be 0.3～0.5MPa, temperature reacts 3～5h under the conditions of being 170～200 DEG C and obtains nickel sulfate pickle liquor and molybdenum iron slag；
(2) molybdenum iron slag step (1) obtained is in the NaOH solution that 2～4:1mL/g addition concentration are 2～4mol/L according to liquid-solid ratio, reacts 3～5h acquisition sodium molybdate solution and the leached muds rich in ferrum silicon under the conditions of temperature is 70～90 DEG C.
The method of Black Rock Sequence nickel-molybdenum iron sulphide ore the most according to claim 1 separation and recovery nickel-molybdenum iron, it is characterised in that: in described step (1), Black Rock Sequence nickel-molybdenum iron sulphide ore includes following mass percent component: nickel 1%～6%, molybdenum 4%～9%, ferrum 10～18%, sulfur 20～30% and silica 1 0～17%.
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