CN109112301A - A method of electrolytic separation iron and zinc in sulfuric acid medium - Google Patents
A method of electrolytic separation iron and zinc in sulfuric acid medium Download PDFInfo
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- CN109112301A CN109112301A CN201811132322.6A CN201811132322A CN109112301A CN 109112301 A CN109112301 A CN 109112301A CN 201811132322 A CN201811132322 A CN 201811132322A CN 109112301 A CN109112301 A CN 109112301A
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- zinc
- iron
- sulfuric acid
- electrolysis
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 220
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 100
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 239000011701 zinc Substances 0.000 title claims abstract description 86
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 81
- 238000000034 method Methods 0.000 title claims abstract description 55
- 238000000926 separation method Methods 0.000 title claims abstract description 32
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 45
- 230000005291 magnetic effect Effects 0.000 claims abstract description 45
- 238000002386 leaching Methods 0.000 claims abstract description 32
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 17
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052751 metal Inorganic materials 0.000 claims abstract description 16
- 239000002184 metal Substances 0.000 claims abstract description 16
- 239000012535 impurity Substances 0.000 claims abstract description 15
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 8
- 229910003481 amorphous carbon Inorganic materials 0.000 claims abstract description 5
- 230000000295 complement effect Effects 0.000 claims abstract description 5
- 239000002070 nanowire Substances 0.000 claims abstract description 5
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 15
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 15
- 229960001763 zinc sulfate Drugs 0.000 claims description 14
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 12
- 229910001447 ferric ion Inorganic materials 0.000 claims description 11
- 238000000746 purification Methods 0.000 claims description 10
- 230000005389 magnetism Effects 0.000 claims description 9
- 239000003792 electrolyte Substances 0.000 claims description 7
- 239000012530 fluid Substances 0.000 claims description 6
- WQSRXNAKUYIVET-UHFFFAOYSA-N sulfuric acid;zinc Chemical compound [Zn].OS(O)(=O)=O WQSRXNAKUYIVET-UHFFFAOYSA-N 0.000 claims description 6
- 239000005083 Zinc sulfide Substances 0.000 claims description 5
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 5
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 claims description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 230000006698 induction Effects 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- HSYFJDYGOJKZCL-UHFFFAOYSA-L zinc;sulfite Chemical group [Zn+2].[O-]S([O-])=O HSYFJDYGOJKZCL-UHFFFAOYSA-L 0.000 claims description 4
- 229910001448 ferrous ion Inorganic materials 0.000 claims description 3
- 230000005415 magnetization Effects 0.000 claims description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 claims description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 2
- 229910000640 Fe alloy Inorganic materials 0.000 claims description 2
- 230000005611 electricity Effects 0.000 claims description 2
- 230000005674 electromagnetic induction Effects 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 2
- FPNCFEPWJLGURZ-UHFFFAOYSA-L iron(2+);sulfite Chemical compound [Fe+2].[O-]S([O-])=O FPNCFEPWJLGURZ-UHFFFAOYSA-L 0.000 claims description 2
- 239000007769 metal material Substances 0.000 claims description 2
- 238000007747 plating Methods 0.000 claims description 2
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 2
- 150000002910 rare earth metals Chemical class 0.000 claims description 2
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical class OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims 1
- 230000001939 inductive effect Effects 0.000 claims 1
- 238000004064 recycling Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 5
- 229910052935 jarosite Inorganic materials 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000005272 metallurgy Methods 0.000 abstract description 2
- 230000001590 oxidative effect Effects 0.000 abstract 1
- 230000003647 oxidation Effects 0.000 description 16
- 238000007254 oxidation reaction Methods 0.000 description 16
- 239000002893 slag Substances 0.000 description 10
- 239000012141 concentrate Substances 0.000 description 8
- 238000009854 hydrometallurgy Methods 0.000 description 7
- AEIXRCIKZIZYPM-UHFFFAOYSA-M hydroxy(oxo)iron Chemical compound [O][Fe]O AEIXRCIKZIZYPM-UHFFFAOYSA-M 0.000 description 7
- 229910052802 copper Inorganic materials 0.000 description 6
- 239000010949 copper Substances 0.000 description 6
- 238000002425 crystallisation Methods 0.000 description 6
- 229910052598 goethite Inorganic materials 0.000 description 6
- 229910052738 indium Inorganic materials 0.000 description 6
- 229910052785 arsenic Inorganic materials 0.000 description 5
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 238000003723 Smelting Methods 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 239000003513 alkali Substances 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 229910052595 hematite Inorganic materials 0.000 description 4
- 239000011019 hematite Substances 0.000 description 4
- 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 4
- 238000006386 neutralization reaction Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 230000002000 scavenging effect Effects 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 229910052787 antimony Inorganic materials 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 229910052793 cadmium Inorganic materials 0.000 description 3
- 239000000428 dust Substances 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 238000009851 ferrous metallurgy Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- KFZAUHNPPZCSCR-UHFFFAOYSA-N iron zinc Chemical compound [Fe].[Zn] KFZAUHNPPZCSCR-UHFFFAOYSA-N 0.000 description 3
- 238000007885 magnetic separation Methods 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 238000004070 electrodeposition Methods 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- 238000005188 flotation Methods 0.000 description 2
- 239000003517 fume Substances 0.000 description 2
- 229910052732 germanium Inorganic materials 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- WJZHMLNIAZSFDO-UHFFFAOYSA-N manganese zinc Chemical compound [Mn].[Zn] WJZHMLNIAZSFDO-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000003472 neutralizing effect Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- 229910052984 zinc sulfide Inorganic materials 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 229910002588 FeOOH Inorganic materials 0.000 description 1
- 101000993059 Homo sapiens Hereditary hemochromatosis protein Proteins 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- GBOGAFPRHXVKNT-UHFFFAOYSA-N [Fe].[In] Chemical compound [Fe].[In] GBOGAFPRHXVKNT-UHFFFAOYSA-N 0.000 description 1
- IXQKTGRUJMZBRU-UHFFFAOYSA-N [S-2].[Zn+2].[Ge+2].[S-2] Chemical compound [S-2].[Zn+2].[Ge+2].[S-2] IXQKTGRUJMZBRU-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 235000011116 calcium hydroxide Nutrition 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910000366 copper(II) sulfate Inorganic materials 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005363 electrowinning Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000002523 gelfiltration Methods 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- NJWNEWQMQCGRDO-UHFFFAOYSA-N indium zinc Chemical compound [Zn].[In] NJWNEWQMQCGRDO-UHFFFAOYSA-N 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000005298 paramagnetic effect Effects 0.000 description 1
- 235000021110 pickles Nutrition 0.000 description 1
- UMPKMCDVBZFQOK-UHFFFAOYSA-N potassium;iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[K+].[Fe+3] UMPKMCDVBZFQOK-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 231100000701 toxic element Toxicity 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- -1 zinc amine Chemical class 0.000 description 1
- 239000011686 zinc sulphate Substances 0.000 description 1
- 235000009529 zinc sulphate Nutrition 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
- 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
- C22B3/20—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
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/16—Electrolytic production, recovery or refining of metals by electrolysis of solutions of zinc, cadmium or mercury
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Geochemistry & Mineralogy (AREA)
- Electrochemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Geology (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Electrolytic Production Of Metals (AREA)
Abstract
The present invention relates to technical field of wet metallurgy, more particularly to the method for a kind of electrolytic separation iron and zinc in sulfuric acid medium, the method of electrolytic separation iron and zinc in sulfuric acid medium, by material after sulfuric acid leaching, reduction ferric iron, removal of impurities, magnetic electrolysis, taking on electric tank cathode mud substance is metal zinc metal sheet, and substance is crystalline iron oxide or amorphous carbon nanowires on the earth of positive pole or in anode region；The magnetic electrolysis is to take diaphragm electrolysis under conditions of complementary field；Separation method of the invention does not use rotary kiln baking to handle and do not use jarosite process or neutralizes oxidizing process or Fe (OH)3Method removes iron, reduces energy consumption and environmental pollution；By sulfuric acid leaching and magnetic electrolysis, separating effect is improved, so that separation product is with high purity, and then is conducive to the recycling of iron, zinc.
Description
Technical field
The present invention relates to technical field of wet metallurgy, and in particular to a kind of side of electrolytic separation iron and zinc in sulfuric acid medium
Method.
Background technique
Currently, China's iron and steel output has reached 5~700,000,000 tons/year, annual output Ferrous Metallurgy dust up to 1,000,000 tons with
On, through magnetic separation of iron ore concentrate, gained tailing containing zinc generally goes back 10% or more iron content after flotation carbon mine, containing zinc 15~30%, leads
To exist in the form of potassium ferrite, experiments have shown that the tailing is easy to by H2SO4It directly leaches, a leaching rate iron and zinc are all up
70% or more.Leachate can reach 70% or more containing Fe, and leachate, up to 10g/L or more, reaches as high as the left side 80g/L containing Zn containing Fe
It is right.Metallic zinc yield in China's is up to 5,000,000 tons/year or more at present, and 90% is obtained by hydrometallurgy.The hydrometallurgy of zinc
Traditional handicraft have neutralize iron removal by oxidation process, the neutralization iron removal by oxidation slag of 10% or more iron content, the slag generally contain zinc 10% with
On, which is returned into rotary kiln disposition, obtain volatilization zinc oxide fumes and main iron content, carbon, silicon kiln slag, the kiln slag strong magnetic of ball milling again
Choosing is only capable of the iron ore concentrate of recycling 50% or so.And zinc oxide fumes are through H2SO4Neutralization iron removal by oxidation must be carried out after leaching,
It can be carried out electrolysis production, the recovery process of iron is long, the rate of recovery is low.
Currently, zinc sulfide concentrates, which directly adopt sulfuric acid, carries out the new trend that high-pressure oxidation leaching has become zinc hydrometallurgy.Its
In iron leaching rate it is also higher, iron content in leachate generally removes iron, but siderotil using jarosite process up to 5g/L or more
Iron content is not high in slag, contains a large amount of SO4 simultaneously2-, cannot act as iron-smelting raw material and production iron chemical products raw material, Zhi Nengzai
Zinc is recycled in reduction roasting in secondary return rotary kiln.In order to make the iron in hyperbaric oxygen leachate become utility, generally using red
Iron ore method is with Fe2O3Crystallization removing, but hematite process needs carry out crystallization removing under 200 DEG C or more, the pressure of 10Mpa or more,
The condition realizes that difficulty is big.
Method in sulfuric acid medium except iron further include in and oxidation goethite process and Fe (OH)3The precipitation method.Goethite process
It needs Fe2+Slowly oxidation removes iron using air, 4 hours time-consuming or more, and gradually neutralizes pH=4 or so, in the form of FeOOH
Precipitating is precipitated in crystallization, and goethite process is easy to filter, and scum amount iron content is higher than jarosite process, but can not wherein be mingled with Fe (OH)3
It generates, and the zinc of adsorption precipitation 10% or so, but the slag must return to rotary kiln processing, otherwise its iron and zinc are all not easily recycled.
Fe(OH)3Precipitation method absorption zinc is more, but Fe (OH)3Gel filtration is difficult.
Above-mentioned zinc hydrometallurgy adds CuSO except iron mostly uses4Make catalyst and carry out separation of iron in goethite form, time-consuming 15 hours with
On.According to adding CuSO4And H2O2It carries out quickly neutralization iron removal by oxidation and then generates Fe (OH)3Probability it is very big, the precipitated iron quantity of slag
Greatly, zinc loss is up to 10% or more, and filtration difficulty, goethite process are only applicable to iron content 1g/L ZnSO4 solution below.
Patent No. CN201010300159.7 discloses slag-free zinc hydrometallurgy of zinc concentrate and mentions indium and produce the side of iron oxide
Method, comprising the following steps: 1, zinc concentrate progress fluosolids roasting, neutral leaching, Weak-acid leaching and purification electrodeposition produce electric zinc；2,
Waste electrolyte after producing electric zinc to low acid leaching residue and electrodeposition carries out high acidic oils, reduction and preneutralization and replaces copper removal；3, right
Liquid carries out neutralizing heavy indium after copper removal；4, after carrying out vulcanization removing heavy metals to liquid after heavy indium, milk of lime is added and neutralizes, obtains deep purifying
Liquid；5, the heavy iron of hydro-thermal method is carried out to deep purifying liquid and obtains ground hematite；6, to the processing of ground hematite removing impurities, soft magnetism oxygen is obtained
Change iron；Using neutralizing heavy indium, hydro-thermal method sink iron, and realization indium-iron and indium-zinc separate and formed ground hematite, handles, reach through removing impurities
It is required to soft magnetism with iron oxide.But effect of this method in terms of iron, zinc separation rate be not significant.
Patent No. CN200510032417.7 discloses iron-zinc and the separation of manganese-zinc and Electrowinning in sulfate
The method of high purity zinc or high-purity zinc powder, the present invention include sulfate liquor reduction, heavy double salt, double salt conversion and ammonia leaching solution purification,
The processes such as electrolysis, preferably solve iron-zinc and manganese-zinc separation problem in sulfate, are preparing MnZn soft magnetism with coprecipitated
While powder, extra zinc is opened a way and recycles, and high purity zinc or high-purity zinc powder is made in this part zinc, its purity >=
99.995%, toxic element cadmium, lead, arsenic, mercury content≤0.0005%, but with alkali soak leaching rate it is undesirable.
In order to overcome the harm of iron in high iron content zinc material, related practitioner has studied alkali leaching method, and zinc is leached as zinc
Sour sodium or zinc amine complex ion enter solution and enter solution, and iron is stayed and separated in slag with zinc, but whether be using NaOH,
NH4Cl or ammonium hydroxide are solvent, and leaching rate is all far below sulfuric acid leaching, and leaches cost and be much higher than sulfuric acid leaching, from alkali immersion liquid
Quality, the cost of middle recycling zinc are below sulfuric acid system, and the iron in leached mud is also required to through ability after rotary kiln processing magnetic separation
Recycling, therefore, limits the popularization of alkali leaching method.
Summary of the invention
The present invention is in order to solve the above technical problems, the present invention provides a kind of in sulfuric acid medium electrolytic separation iron and zinc
Method overcomes high Fe contained zinc material using sulfuric acid smelting by sulfuric acid medium leaching and magnetic electrolytic separation iron and zinc effect
Not the disadvantages of iron when refining, zinc separating effect is not good enough, iron resource waste, smelting cost is higher.
Specifically realized according to following technical scheme:
A method of electrolytic separation iron and zinc in sulfuric acid medium, by material through sulfuric acid leaching, reduction ferric iron, remove
After miscellaneous, magnetic electrolysis, taking on electric tank cathode mud substance is metal zinc metal sheet, and substance is crystallization oxidation on the earth of positive pole or in anode region
Iron or amorphous carbon nanowires；The magnetic electrolysis is to take diaphragm electrolysis under conditions of complementary field.
In the above method, the condition of the magnetic electrolysis: magnetic field strength 10-100A/M, electrolytic current density 500-
700A/ ㎡, electrolytic cell pressure are 3-3.5V, and electrolysis temperature is 25-40 DEG C, electrolysis time 24-48h.
A method of electrolytic separation iron and zinc in sulfuric acid medium specifically comprise the following steps:
S1 sulfuric acid leaching: by iron content, zinc material sulfuric acid leaching, high iron-containing solution of zinc sulfate is obtained；
S2 restores ferric iron: being ferrous iron by the ferric iron back in high iron-containing solution of zinc sulfate, obtains zinc sulfate also
Stoste；
S3 removal of impurities: utilizing zinc powder or sulfide removal zinc sulfate reducing solution, removes GOLD FROM PLATING SOLUTION category impurity, obtains and contains Fe2+
Greater than 10g/L, Zn2+Sulfuric acid zinc purification fluid greater than 80g/L；
The electrolysis of S4 magnetism: sulfuric acid zinc purification fluid being placed in electrolytic cell and carries out magnetic electrolysis, the condition of the magnetic electrolysis
Are as follows: magnetic field strength 10-100A/M, electrolytic current density are 500-700A/ ㎡, and electrolytic cell pressure is 3-3.5V, and electrolysis temperature is
25-40 DEG C, electrolysis time 24-48h, residual electrolyte contains Fe2-5g/L, Zn30-40g/L, H2SO450-100g/L；Through magnetic electricity
Xie Hou obtains metal zinc metal sheet from cathode mud, and crystalline iron oxide or amorphous carbon nanowires sun are obtained on the earth of positive pole or anode region
Pole mud.
In the above method, iron-content 10-40g/L, zinc content 80-100g/L in the iron-containing solution of zinc sulfate of height.
In the above method, the reduction ferric iron is to realize that ferric ion is reduced by the way that sulphite or iron filings is added
Ferrous ion.
In the above method, the sulphite is zinc sulfite or iron sulfite.
In the above method, in removal step, the metal impurities include: Cu, Cd, As, Sb.
In the above method, the sulfide is zinc sulphide or vulcanized sodium or hydrogen sulfide.
In the above method, the electrolytic cell is the diaphragm cell of complementary field, specifically in electrolytic cell longitudinal direction
Two sides are installed by electromagnetic induction coil or permanent magnet.
In the above method, the anode electrolytic cell is made of magnetic induction material, and cathode is made of pure aluminum material.
In the above method, the magnetic induction material is the ferrous alloys material containing rare earth or is coated with manganese dioxide easy magnetization
Metal material.
The method of electrolytic separation iron and zinc provided by the invention in sulfuric acid medium, for handling iron content 10~50%, containing
The Ferrous Metallurgy smoke dust of zinc 25~50%, the neutralization iron removal by oxidation slag of zinc hydrometallurgy, in ferrous acid iron oxide ore when any material,
Use H2SO4It directly leaches, obtains high iron-containing solution of zinc sulfate.
The method of electrolytic separation iron and zinc provided by the invention in sulfuric acid medium, when for handling zinc sulphide germanium concentrate,
The leaching of high pressure sulfuric acid oxidation is carried out, high iron-containing solution of zinc sulfate is obtained.
In the above method, residual electrolyte contains Fe2-5g/L, Zn30-40g/L, H2SO450-100g/L。
The beneficial effects of the present invention are:
Separation method of the invention does not use rotary kiln baking to handle and do not use jarosite process or neutralizes oxidation
Method or Fe (OH)3Method removes iron, reduces energy consumption and environmental pollution；By sulfuric acid leaching and magnetic electrolysis, separating effect is improved,
So that separation product is with high purity, and then be conducive to the recycling of iron, zinc.
The present invention is electrolysed in magnetic field environment so that can magnetic ion or magnetic susceptibility ion will be influenced by magnetic field,
Magnetic deflection occurs, is made in conjunction with anode plate of the strong material of magnetic induction, when electrolytic cell two sides are additional generates magnetic field, anode is by magnetic
Change and then generate magnetic field, thus by Fe2+Deng magnetization and anode region and electrolytic cell two sides are bound by, so that ferrous ion is in sun
It is enriched on polar region or anode；Meanwhile oxygen that solution is released is powered on by Fe in anode2+It is oxidized to Fe3+And generate Fe2O3Or Fe3O4,
The oxide majority is Fe2O3Crystallization, is attached on anode or falls among anode, and Zn2+With diamagnetism, cathode aluminum plate
Do not have magnetism, therefore will not be magnetized, Zn2+Still routinely direction of an electric field powers in cathode and parses zinc, and due to iron
And other paramagnetic fields impurity is influenced by high-intensity magnetic field, can seldom be discharged on cathode, to improve the current efficiency of zinc.
The present invention is first by Fe in leachate3+It is reduced to Fe2+, then with zinc powder or zinc sulphide purification and impurity removal, it is therefore prevented that Fe3+Water
Solution, and then prevent the generation of iron loss and zinc.
The iron oxide crystallization that the present invention is obtained by magnetic electrolysis, improves iron-content, which can be used for iron-smelting raw material
With iron content chemical products raw material, other iron-containing waste residues are not generated.Simultaneously because not adding K required for generating autunezite+
Or Na+Or NH4 +, also it is added without and generates goethite or Fe (OH)3And the neutralizer that must be used, ingredient has not only been saved, has been reduced
Pollution, also reduces electrolysis impact factor, improves electrolysis effectiveness, be conducive to the separation and recycling of zinc and iron.
Specific embodiment
Specific embodiments of the present invention will be described in further detail below, but the invention is not limited to these realities
Mode is applied, it is claimed to still fall within the claims in the present invention for any improvement or replacement on the present embodiment essence spirit
Range.
Embodiment 1
Certain iron and steel enterprise is to produce Ferrous Metallurgy mixed dust gained after three-level magnetic separation of iron ore concentrate and flotation carbon select carbon mine
Tailing contains Zn 33.4%, iron content 12.8%, and Pb 1.2%, As0.23%, In0.021% carry out the separation of iron zinc according to the following steps
Recycling:
S1 sulfuric acid leaching: by tailing sulfuric acid leaching, liquid-solid ratio 4, H2SO4Concentration 80g/L, 85-90 DEG C of extraction temperature,
Extraction time 2.5h leaches pH=1.5, obtains high iron-containing solution of zinc sulfate, contains total Fe24.5g/L, Zn79.3g/L,
As400mg/L, In42mg/L；
S2 restores ferric iron: using zinc sulfite water reducing agent under the conditions of 40-45 DEG C, carries out Fe3+Reduction, ZnSO3It is added
Amount is ZnSO3/Fe3+=1.2, recovery time 0.5h, reducing solution iron content Fe3+180mg/L；
S3 removal of impurities: reducing solution is handled using zinc powder, obtains scavenging solution 0.01g/L containing Cd, As0.01g/L, Pb0.001g/
L, Sb0.001g/L, Cu, Co, Ni are micro；
The electrolysis of S4 magnetism: sulfuric acid zinc purification fluid being placed in electrolytic cell and carries out magnetic electrolysis, the condition of the magnetic electrolysis
Are as follows: magnetic field strength 20A/m, electrolytic current density are 500A/ ㎡, and electrolytic cell pressure is 3.2V, and electrolysis temperature is 30 DEG C, when electrolysis
Between be 24-48h, electrolyte circulation rate 0.2m3/ h, residual electrolyte 3.5g/L containing Fe, Zn35g/L, H2SO453g/L；24 hours
Stripping metal zinc metal sheet is primary, and cleaning anode is primary within 36 hours；The current efficiency 85.3% of zinc, metal zinc metal sheet contain zinc 99.992%,
Contain Fe 61.8%, the electrolytic efficiency 65.3% of iron after earth of positive pole washing.
Embodiment 2
Certain zinc hydrometallurgy enterprise, which produces, neutralizes iron removal by oxidation goethite slag, chemically examines after washing drying, wherein containing Fe
18.3%, contain Zn10.5%, contains other metal impurities As 0.5%, Sb 1.2%, Ni 0.15%, Co 0.12%.By following
Step carries out iron, zinc separation and recovery:
S1 sulfuric acid leaching: by tailing sulfuric acid leaching, liquid-solid ratio 5, H2SO4Concentration 100g/L, 90 DEG C of extraction temperature, leaching
Time 2h out obtains high iron-containing solution of zinc sulfate, contains total Fe29.3g/L, Zn20.7g/L, iron leaching rate 80%, zinc leaching
Rate 98.5%；
S2 restores ferric iron: with zinc sulfite being reducing agent under the conditions of 45 DEG C, carries out Fe3+Reduction, ZnSO3Additional amount is
ZnSO3/Fe3+=1.2, recovery time 0.5h, reducing solution iron content Fe3+120mg/L, 65g/L containing Zn；
S3 removal of impurities: reducing solution is handled using zinc powder, removes Cu, Ca, As, Sb, Ni, Co, Ge, In, scavenging solution 81.5g/ containing Zn
L, Fe 20.2g/L, other impurities content meet electrolysis and require, scavenging solution pH=5；
The electrolysis of S4 magnetism: sulfuric acid zinc purification fluid being placed in electrolytic cell and carries out magnetic electrolysis, the condition of the magnetic electrolysis
Are as follows: magnetic field strength 50A/m, electrolytic current density are 650A/ ㎡, and electrolytic cell pressure is 3.5V, and electrolysis temperature is 40 DEG C, when electrolysis
Between be 40h, electrolyte circulation rate 0.35m3/ h, to plate MnO2Steel plate is anode, pure aluminum plate be cathode electrolytic cell in carry out magnetic
Property diaphragm electrolysis；The current efficiency of zinc is 82.5%, and Eletrolytic zinc quality is No. 1 zinc of national standard containing Zn 99.99%, anodic oxidation iron
Electrolytic efficiency 78.2%, the earth of positive pole contain Fe 62.5%.
Embodiment 3
Certain zinc sulfide concentrates is obtained through sulfuric acid oxidation acidleach contains Zn118g/L, Fe 5.5g/L, H2SO4The pickle liquor of 50g/L；
With iron reduction Fe3+For Fe2+Afterwards, reducing solution iron content reaches 7.8g/L；It is removed after extracted indium and germanium with zinc powder and vulcanized sodium purification
Cu, Cd, As, As, Bi, Co are removed, scavenging solution presses the magnetic electrolytic condition in embodiment 1 and embodiment 2 respectively and carries out magnetic electrolysis,
The current efficiency of its zinc, anodic oxidation electrolytic iron efficiency and earth of positive pole iron content rate are as shown in table 1:
Table 1
| Zinc current efficiency/% | Anodic oxidation electrolytic iron efficiency/% | Earth of positive pole iron content rate/% | |
| Embodiment 1 | 86.2 | 68.7 | 61.8 |
| Embodiment 2 | 88.5 | 75.3 | 62.3 |
Claims (10)
1. a kind of method of electrolytic separation iron and zinc in sulfuric acid medium, which is characterized in that by material through sulfuric acid leaching, reduction three
After valence iron, removal of impurities, magnetic electrolysis, taking on electric tank cathode mud substance is metal zinc metal sheet, and substance is on the earth of positive pole or in anode region
Crystalline iron oxide or amorphous carbon nanowires；The magnetic electrolysis is to take diaphragm electrolysis under conditions of complementary field.
2. as described in claim 1 in sulfuric acid medium electrolytic separation iron and zinc method, which is characterized in that the magnetic electricity
The condition of solution: magnetic field strength 10-100A/M, electrolytic current density are 500-700A/ ㎡, and electrolytic cell pressure is 3-3.5V, electrolysis
Temperature is 25-40 DEG C, electrolysis time 24-48h.
3. as described in claim 1 in sulfuric acid medium electrolytic separation iron and zinc method, which is characterized in that specifically include as
Lower step:
S1 sulfuric acid leaching: by iron content, zinc material sulfuric acid leaching, high iron-containing solution of zinc sulfate is obtained；
S2 restores ferric iron: being ferrous iron by the ferric iron back in high iron-containing solution of zinc sulfate, obtains zinc sulfate reducing solution；
S3 removal of impurities: utilizing zinc powder or sulfide removal zinc sulfate reducing solution, removes GOLD FROM PLATING SOLUTION category impurity, obtains and contains Fe2+It is greater than
10g/L, Zn2+Sulfuric acid zinc purification fluid greater than 80g/L；
The electrolysis of S4 magnetism: sulfuric acid zinc purification fluid being placed in electrolytic cell and carries out magnetic electrolysis, the condition of the magnetic electrolysis are as follows: magnetic
Field intensity is 10-100A/M, and electrolytic current density is 500-700A/ ㎡, and electrolytic cell pressure is 3-3.5V, electrolysis temperature 25-40
DEG C, electrolysis time 24-48h, residual electrolyte contains Fe2-5g/L, Zn30-40g/L, H2SO450-100g/L；After magnetism electrolysis,
Metal zinc metal sheet is obtained from cathode mud, and crystalline iron oxide or the amorphous carbon nanowires earth of positive pole are obtained on the earth of positive pole or anode region.
4. as described in claim 1 in sulfuric acid medium electrolytic separation iron and zinc method, which is characterized in that the high iron content
Solution of zinc sulfate in iron-content 10-40g/L, zinc content 80-100g/L.
5. as described in claim 1 in sulfuric acid medium electrolytic separation iron and zinc method, which is characterized in that it is described reduction three
Valence iron is to realize that ferric ion is reduced into ferrous ion by the way that sulphite or iron filings is added.
6. as described in claim 1 in sulfuric acid medium electrolytic separation iron and zinc method, which is characterized in that the sulfurous acid
Salt is zinc sulfite or iron sulfite.
7. as described in claim 1 in sulfuric acid medium electrolytic separation iron and zinc method, which is characterized in that the sulfide
For zinc sulphide or vulcanized sodium or hydrogen sulfide.
8. as described in claim 1 in sulfuric acid medium electrolytic separation iron and zinc method, which is characterized in that the electrolytic cell
For the diaphragm cell of complementary field, electromagnetic induction coil or permanent magnet specifically are installed in the two sides of electrolytic cell longitudinal direction.
9. as described in claim 1 in sulfuric acid medium electrolytic separation iron and zinc method, which is characterized in that the electrolytic cell
Anode is made of magnetic induction material, and cathode is made of pure aluminum material.
10. as described in claim 1 in sulfuric acid medium electrolytic separation iron and zinc method, which is characterized in that the magnetic
Inductive material is ferrous alloys material containing rare earth or the metal material for being coated with manganese dioxide easy magnetization.
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| CN113816433A (en) * | 2021-10-15 | 2021-12-21 | 兰州理工大学 | Method for preparing porous ferric oxide with adjustable pore size by using iron-containing solid waste acid leaching solution |
| CN115747832A (en) * | 2022-11-01 | 2023-03-07 | 昆明理工大学 | Method for one-step purification and manganese removal and co-production of low-iron zinc from manganese-containing zinc sulfate solution in zinc hydrometallurgy |
| CN119221042A (en) * | 2024-11-29 | 2024-12-31 | 扬州新达再生资源科技有限公司 | A device and method for purifying zinc powder from zinc-containing slag |
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