CN115595446A - Method for leaching zinc oxide smoke dust by ultrasonic-enhanced potassium dichromate oxidation - Google Patents
Method for leaching zinc oxide smoke dust by ultrasonic-enhanced potassium dichromate oxidation Download PDFInfo
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- CN115595446A CN115595446A CN202211323094.7A CN202211323094A CN115595446A CN 115595446 A CN115595446 A CN 115595446A CN 202211323094 A CN202211323094 A CN 202211323094A CN 115595446 A CN115595446 A CN 115595446A
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- zinc oxide
- leaching
- smoke dust
- potassium dichromate
- zinc
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 161
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 238000002386 leaching Methods 0.000 title claims abstract description 107
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 78
- 239000000779 smoke Substances 0.000 title claims abstract description 74
- 239000000428 dust Substances 0.000 title claims abstract description 65
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 29
- 230000003647 oxidation Effects 0.000 title claims abstract description 28
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 90
- 229910052732 germanium Inorganic materials 0.000 claims abstract description 61
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims abstract description 61
- 239000011701 zinc Substances 0.000 claims abstract description 53
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 52
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 52
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 230000008569 process Effects 0.000 claims abstract description 10
- 238000005728 strengthening Methods 0.000 claims abstract description 7
- 150000001875 compounds Chemical class 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 17
- 230000001590 oxidative effect Effects 0.000 claims description 13
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims description 9
- 229910052984 zinc sulfide Inorganic materials 0.000 claims description 9
- 239000005083 Zinc sulfide Substances 0.000 claims description 6
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims description 6
- PVADDRMAFCOOPC-UHFFFAOYSA-N germanium monoxide Inorganic materials [Ge]=O PVADDRMAFCOOPC-UHFFFAOYSA-N 0.000 claims description 6
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 4
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 4
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 4
- 229960001763 zinc sulfate Drugs 0.000 claims description 4
- 229940119177 germanium dioxide Drugs 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 2
- 230000002708 enhancing effect Effects 0.000 claims 2
- 239000004480 active ingredient Substances 0.000 claims 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 21
- 229910052742 iron Inorganic materials 0.000 abstract description 9
- 239000002253 acid Substances 0.000 abstract description 8
- 230000008901 benefit Effects 0.000 abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 4
- 239000000084 colloidal system Substances 0.000 abstract description 4
- 238000003723 Smelting Methods 0.000 abstract description 3
- 239000008119 colloidal silica Substances 0.000 abstract description 2
- 230000007547 defect Effects 0.000 abstract description 2
- 238000009854 hydrometallurgy Methods 0.000 abstract description 2
- 239000007787 solid Substances 0.000 description 28
- 239000000706 filtrate Substances 0.000 description 25
- 230000000052 comparative effect Effects 0.000 description 22
- 239000007788 liquid Substances 0.000 description 19
- 230000000694 effects Effects 0.000 description 17
- 238000005406 washing Methods 0.000 description 16
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 12
- 239000000126 substance Substances 0.000 description 11
- 239000000203 mixture Substances 0.000 description 9
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- 238000000926 separation method Methods 0.000 description 8
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- 239000007800 oxidant agent Substances 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 230000003247 decreasing effect Effects 0.000 description 4
- SCCCLDWUZODEKG-UHFFFAOYSA-N germanide Chemical compound [GeH3-] SCCCLDWUZODEKG-UHFFFAOYSA-N 0.000 description 4
- 230000007062 hydrolysis Effects 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 235000010344 sodium nitrate Nutrition 0.000 description 4
- 239000004317 sodium nitrate Substances 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000003517 fume Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011133 lead Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- 239000004071 soot Substances 0.000 description 2
- 229910052950 sphalerite Inorganic materials 0.000 description 2
- WGPCGCOKHWGKJJ-UHFFFAOYSA-N sulfanylidenezinc Chemical compound [Zn]=S WGPCGCOKHWGKJJ-UHFFFAOYSA-N 0.000 description 2
- 238000009210 therapy by ultrasound Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 229910017488 Cu K Inorganic materials 0.000 description 1
- 229910017541 Cu-K Inorganic materials 0.000 description 1
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000001636 atomic emission spectroscopy Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910052949 galena Inorganic materials 0.000 description 1
- MRZMQYCKIIJOSW-UHFFFAOYSA-N germanium zinc Chemical compound [Zn].[Ge] MRZMQYCKIIJOSW-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- -1 iron ions Chemical class 0.000 description 1
- 229910000358 iron sulfate Inorganic materials 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 1
- 150000002611 lead compounds Chemical class 0.000 description 1
- JQJCSZOEVBFDKO-UHFFFAOYSA-N lead zinc Chemical compound [Zn].[Pb] JQJCSZOEVBFDKO-UHFFFAOYSA-N 0.000 description 1
- XCAUINMIESBTBL-UHFFFAOYSA-N lead(ii) sulfide Chemical compound [Pb]=S XCAUINMIESBTBL-UHFFFAOYSA-N 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 235000018553 tannin Nutrition 0.000 description 1
- 229920001864 tannin Polymers 0.000 description 1
- 239000001648 tannin Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Classifications
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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
- 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
- C22B7/02—Working-up flue dust
-
- 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
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/34—Obtaining zinc oxide
-
- 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
- C22B41/00—Obtaining germanium
-
- 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
- C22B7/007—Wet processes by acid leaching
-
- 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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- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Organic Chemistry (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for ultrasonically strengthening zinc oxide smoke dust leached by potassium dichromate oxidation, and belongs to the technical field of hydrometallurgy and comprehensive resource utilization. The method for ultrasonically strengthening the zinc oxide smoke dust leached by potassium dichromate oxidation comprises the following steps: mixing zinc oxide smoke dust and potassium dichromate, adding a sulfuric acid solution to prepare a reaction solution, and then placing the reaction solution under the conditions of ultrasonic waves and stirring to carry out zinc oxide smoke dust oxidation leaching. The method for leaching zinc and germanium in zinc oxide smoke dust has the advantages of high leaching rate, short leaching time and the like, overcomes the defect that zinc and germanium are adsorbed and precipitated by colloidal silica and iron colloid due to long leaching time of other processes, reduces the acid consumption, can highly enrich lead in the smoke dust and return the lead to smelting and utilization, and has obvious economic benefit.
Description
Technical Field
The invention relates to the technical field of hydrometallurgy and comprehensive utilization of resources, in particular to a method for ultrasonically strengthening zinc oxide smoke dust leached by potassium dichromate oxidation.
Background
Zinc and germanium are widely used in important fields such as battery manufacturing, national defense and military industry and the like. Lead-zinc ore is a main mineral deposit associated with germanium, in the zinc smelting process, the mineral is roasted, leached in neutral, fuming and volatilizing to obtain a byproduct zinc oxide smoke dust, and germanide is hardly dissolved in the process, so that the contents of zinc and germanium in the zinc oxide smoke dust after being enriched are respectively more than 50wt.% and 500g/t. However, with the development of science and technology and the improvement of living standard of people, the demand of zinc and germanium is increasing at home and abroad, so that the quantity of zinc leaching residues is continuously increased, and the resources are increasingly poor. If secondary resources such as zinc leaching residues and the like are not reasonably utilized, the accumulation of byproducts can not only cause environmental pollution, but also cause serious waste of resources, so that the effective leaching of zinc germanium in zinc oxide smoke dust has important significance.
At present, the zinc and the germanium in the germanium-containing zinc oxide smoke dust are treated by two-stage acid leaching in industrial production, and the leaching rate of the zinc and the germanium is usually 90 percent and 80 percent under the process condition. The reason why the leaching rate is low due to the process is as follows: (1) The zinc oxide smoke dust usually contains a large amount of substances which are difficult to dissolve in acid, such as sphalerite, galena and the like, and the substances not only wrap germanium-containing compounds, but also can be mutually substituted with germanium in crystal lattices. (2) Under the condition of low acid, the long-time leaching not only reduces the production efficiency, but also can hydrolyze ferric iron and silicate in the leaching solution, thereby adsorbing and precipitating valuable metals such as zinc, germanium and the like.
Disclosure of Invention
The invention aims to provide a method for ultrasonically strengthening zinc oxide smoke dust leached by potassium dichromate oxidation, which aims to solve the problems in the prior art. The invention takes potassium dichromate as an oxidant and sulfuric acid as a solvent, and aims to provide a method for efficiently and economically leaching zinc and germanium from zinc oxide smoke containing germanium. By adopting the method, the leaching rate of zinc and germanium is obviously improved, the amount of leached residues is reduced, lead compounds are enriched and comprehensively utilized, and the requirements of resource utilization and residue reduction are met.
In order to achieve the purpose, the invention provides the following scheme:
one of the technical schemes of the invention is as follows: a method for leaching zinc oxide smoke dust by oxidizing potassium dichromate through ultrasonic strengthening comprises the following steps:
mixing zinc oxide smoke dust and potassium dichromate, adding a sulfuric acid solution to prepare a reaction solution, and then placing the reaction solution under the conditions of ultrasonic waves and stirring to carry out zinc oxide smoke dust oxidation leaching.
The specific reaction is as follows:
ZnS+Fe 3+ ＝Zn 2 ++Fe 2+ +S 0 ；
the main substance in zinc oxide smoke is zinc oxide, which is present in the form of zinc sulfide in addition to zinc oxide, as well as lead and germanium. The sulfide is not dissolved under the condition that only sulfuric acid exists, and meanwhile, according to the representation, germanide in the zinc oxide smoke dust can be enriched (zinc sulfide) in crystal lattices of zinc blende and can be wrapped by the sulfide to prevent germanium from being leached, so that potassium dichromate is introduced as an oxidant to promote the sulfide to be converted into sulfate, and the sulfide is dissolved.
Under the action of ultrasonic wave and sulfuric acid, the insoluble sulfide can be reacted to change the insoluble zinc sulfide into soluble zinc sulfate and expose the germanide coated in the smoke dust. Compared with oxidants such as ozone, hydrogen peroxide and the like, the potassium dichromate does not corrode equipment, and meanwhile, a large amount of additives are not consumed due to decomposition caused by factors such as temperature and the like, so that the production cost is increased, and the potassium dichromate can effectively oxidize insoluble zinc-containing compounds such as zinc blende and the like into soluble substances. Meanwhile, the potassium dichromate used as an oxidant has high oxidation reaction rate, can obviously overcome the problem that a large amount of valuable metals are taken away by hydrolysis-coprecipitation of iron ions and silicate, and ensures that the leaching rates of zinc and germanium respectively exceed 99 percent and 90 percent.
Further, before the reaction solution is prepared, drying and screening the zinc oxide smoke dust to obtain the pretreated zinc oxide smoke dust.
Further, the drying is vacuum drying, and the vacuum degree is 0.005-0.01 MPa; the drying temperature is 60 ℃, and the drying time is 24 hours; the number of the meshes of the adopted screens is 80-200 meshes.
Further, the volume/mass ratio of the sulfuric acid solution to the zinc oxide smoke dust is 6-8 mL/g.
Further, the mass/volume ratio of the potassium dichromate to the sulfuric acid solution is 4.5-33.82 g:1L of the compound.
Further, the concentration of the sulfuric acid solution is 120-200 g/L.
Furthermore, the power of the ultrasonic wave is 90-600W, the frequency is 19.5kHz, and the current is 0.31A; the stirring speed is 50-300 r/min.
Further, the temperature of the oxidation leaching is 40-90 ℃, and the time is 30-180 min.
Further, the main components in the zinc oxide smoke dust comprise a zinc-containing compound and a germanium-containing compound.
Further, the zinc-containing compound includes zinc oxide, zinc sulfide, and zinc sulfate; the germanium-containing compound includes germanium monoxide, germanium dioxide, germanate and sulfide thereof.
The invention discloses the following technical effects:
(1) The method has the advantages of high reaction rate, simple operation and no danger. Under the action of ultrasonic wave, the interior of the solution is violently vibrated, so that the viscosity of a reaction system and the mass transfer resistance between solid and liquid are reduced. In addition, under the action of ultrasonic waves, a large number of micro bubbles are generated in the solution, and along with the growth and the breakage of the bubbles, energy in the bubbles is released, so that micro jet flow and shock wave are generated in a solid-liquid phase, the thickness of a diffusion layer at a solid-liquid interface is weakened, a new reaction interface is generated through continuous denudation, and the reaction is continuously generated. The added potassium dichromate continuously reacts with sulfide and other substances at a new interface, and the crystal lattice substitution and the wrapped germanide are exposed in an acid system, so that the leaching rates of zinc and germanium are respectively improved to more than 99% and 90%, and the slag rate is controlled to be about 30%.
(2) According to the invention, through optimizing each influence parameter, the aim of improving the leaching rate of zinc and germanium is fulfilled, and the aims of comprehensive utilization of resources and harmless treatment are fulfilled.
(3) The method for leaching zinc and germanium in zinc oxide smoke dust has the advantages of high leaching rate, short leaching time and the like, overcomes the defect that zinc and germanium are adsorbed and precipitated by colloidal silica and iron colloid due to long leaching time of other processes, reduces the acid consumption, can highly enrich lead in the smoke dust and return the lead to smelting and utilization, and has obvious economic benefit.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a process flow diagram of example 1 of the present invention;
FIG. 2 is an XRD pattern of zinc oxide soot (raw material) in example 1 of the present invention;
FIG. 3 is an XRD pattern of the residue obtained after the oxidative leaching in example 1 of the present invention;
FIG. 4 is a graph of the effect of leaching time on zinc and germanium leaching rates;
FIG. 5 is a graph showing the effect of leaching time on the leaching rates of lead, iron, silicon and aluminum.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated herein by reference to disclose and describe the methods and materials in connection with which the documents are cited. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The specification and examples are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
The zinc oxide fumes treated in the following examples and comparative examples of the present invention were germanium-containing zinc oxide fumes whose main components were zinc-containing compounds and germanium-containing compounds; the zinc-containing compound is zinc oxide, zinc sulfide, zinc sulfate, etc.; the germanium-containing compound is germanium monoxide, germanium dioxide, germanate and sulfide thereof, the main chemical components are shown in table 1, and the numerical values in table 1 are ICP-OES quantitative analysis numerical values.
TABLE 1 main chemical composition of germanium-containing zinc oxide soot
Ge (g/t) represents the gram of Ge contained in each ton of germanium-containing zinc oxide smoke dust.
The zinc oxide smoke dust adopted in the following examples and comparative examples of the invention is subjected to vacuum drying treatment, wherein the vacuum degree of the vacuum drying treatment is 0.005-0.01 MPa, the drying temperature is 60 ℃, and the drying time is 24h.
In the following examples and comparative examples of the present invention, phase analysis was performed using an X-ray diffractometer (XRD) (D8 ADVANCE) having a Cu-K α as an X-ray source, λ =0.15416nm, a voltage of 40KV or less and a current of 40mA or less.
Example 1
A method for ultrasonically strengthening zinc oxide smoke dust leached by potassium dichromate oxidation comprises the following steps:
(1) The zinc oxide smoke dust is sieved by a 200-mesh sieve, then 40g of the sieved zinc oxide smoke dust (raw material) is weighed, 6.31g of potassium dichromate is weighed, and 280mL of sulfuric acid solution (the concentration is 140 g/L) is weighed.
(2) Mixing zinc oxide smoke dust and potassium dichromate, placing the mixture into a reactor, adding a sulfuric acid solution, uniformly mixing to obtain a reaction solution (the volume/mass ratio of the sulfuric acid solution to the zinc oxide smoke dust in the reaction solution is 7mL, namely, the liquid-solid ratio is 7mL/g, the concentration of potassium dichromate in the reaction solution is 22.54g/L, namely, the mass/volume ratio of potassium dichromate to the sulfuric acid solution is 22.54g/L, namely, 6.31g, 280mL), controlling the ultrasonic power to be 500W, the frequency to be 19.5kHz, the current to be 0.31A and the stirring speed to be 150r/min under the constant temperature condition of 90 ℃, carrying out oxidation leaching, wherein the leaching time is 30min, carrying out solid-liquid separation after completing leaching, and washing a solid by using 25mL of deionized water (serving as a part of a washing solution) to obtain filter residue and a filtrate; drying the filter residue at 60 ℃ for 15h to obtain dry-base filter residue with the mass of 11.81g; removing impurities from the filtrate, performing tannin germanium precipitation, and performing zinc electrodeposition. The specific flow chart is shown in figure 1, the XRD pattern of the zinc oxide smoke dust is shown in figure 2, and the XRD pattern of the filter residue is shown in figure 3.
Comparative example 1
The difference from example 1 is only that no ultrasonic treatment is performed, specifically: mixing zinc oxide smoke dust and potassium dichromate, placing the mixture into a reactor, adding a sulfuric acid solution, controlling the stirring speed to be 150r/min under the constant temperature condition of 90 ℃, carrying out oxidation leaching, wherein the leaching time is 30min, carrying out solid-liquid separation after the leaching is finished, and washing the solid with 25mL of deionized water (a washing solution is used as a part of a filtrate) to obtain filter residue and a filtrate; the residue was dried at 60 ℃ for 15 hours to give a dry residue of 13.61g in mass.
Comparative example 2
The method is the same as the comparative example 1, except that the leaching time is 120min, and filter residue and filtrate are obtained; the residue was dried at 60 ℃ for 15 hours to give a dry residue of 13.93g mass.
Effect example 1
The contents of zinc and germanium in the filtrates of example 1 and comparative examples 1 to 2 were measured, and the leaching rates were calculated, and the results are shown in table 2.
CP-OES quantitative analysis shows that zinc content in zinc oxide smoke is 53.3wt.%, germanium content is 510.10g/t, namely 40g smoke contains 21.32g zinc and 20.4mg germanium.
The leaching rate of zinc is calculated by the following formula:
wherein mu is the leaching rate of zinc, x is the concentration of zinc in the filtrate, v is the volume of the filtrate, w is the content of zinc in the zinc oxide smoke dust, and m is the mass of the added zinc oxide smoke dust.
The leaching rate of germanium is calculated by the following formula:
wherein mu is the leaching rate of germanium, x is the concentration of germanium in the filtrate, v is the volume of the filtrate, w is the content of germanium in the zinc oxide smoke dust, and m is the mass of the added zinc oxide smoke dust.
TABLE 2
As can be seen from Table 2, the leaching rates of zinc and germanium were decreased without the ultrasonic treatment (comparative example 1 and comparative example 2), and the leaching time was prolonged to improve the leaching rate.
Example 2
(1) Sieving zinc oxide smoke dust with 200 mesh sieve, weighing 40g of sieved zinc oxide smoke dust (raw material), 6.31g of potassium dichromate, and 120mL of sulfuric acid solution (concentration is 140 g/L).
(2) Mixing zinc oxide smoke dust and potassium dichromate, placing the mixture into a reactor, adding a sulfuric acid solution, uniformly mixing to obtain a reaction solution (the liquid-solid ratio is 3mL/g, and the concentration of potassium dichromate is 22.54 g/L), controlling the ultrasonic power to be 300W, the frequency to be 19.5kHz, the current to be 0.31A and the stirring speed to be 150r/min under the constant temperature condition of 90 ℃, carrying out oxidation leaching for 30min, carrying out solid-liquid separation after the leaching is finished, washing a solid by 25mL of deionized water (the washing liquid is used as a part of the filtrate), and obtaining filter residue and filtrate; drying the filter residue at 60 ℃ for 15h to obtain dry-based filter residue.
Example 3
The only difference from example 2 is that the amount of sulfuric acid solution used was 160mL (liquid-solid ratio: 4 mL/g).
Example 4
The only difference from example 2 is that the amount of the sulfuric acid solution used was 200mL (liquid-solid ratio: 5 mL/g).
Example 5
The only difference from example 2 is that the amount of the sulfuric acid solution used was 240mL (liquid-solid ratio: 6 mL/g).
Example 6
The only difference from example 2 is that the amount of the sulfuric acid solution used was 280mL (liquid-solid ratio: 7 mL/g).
Example 7
The only difference from example 2 is that the amount of the sulfuric acid solution used was 320mL (liquid-solid ratio: 8 mL/g).
Effect example 2
The contents of zinc and germanium in the filtrates of examples 2 to 7 and the mass of the dry residue were measured, and the leaching rate was calculated (the calculation method was the same as in effect example 1), and the results are shown in table 3.
TABLE 3
As can be seen from Table 3, the leaching rate of germanium is affected by the liquid-solid ratio during leaching, the leaching rate of germanium is higher when the liquid-solid ratio is 7-8 mL/g, and the leaching rate of germanium is lower when the liquid-solid ratio is lower than 3mL/g, mainly because the reaction cannot be completely carried out due to the small amount of added sulfuric acid. When the liquid-solid ratio is less than 7mL/g (the larger the liquid-solid ratio, the lower the viscosity), the reaction system has a higher viscosity, and the diffusion resistance between solid and liquid increases, so that the reaction interface between the metal compound and the sulfuric acid is gradually renewed. When the leaching rate is higher than 7mL/g, the leaching rate of zinc and germanium is not changed greatly. Therefore, the liquid/solid ratio is preferably 7mL/g from the economical viewpoint.
Example 8
(1) Sieving zinc oxide smoke dust with a 200-mesh sieve, then weighing 40g of the sieved zinc oxide smoke dust (raw material), weighing 6.31g of potassium dichromate, and weighing 280mL of sulfuric acid solution (with the concentration of 120 g/L).
(2) Mixing zinc oxide smoke dust and potassium dichromate, placing the mixture into a reactor, adding a sulfuric acid solution, uniformly mixing to obtain a reaction solution (the liquid-solid ratio is 7mL/g, the concentration of potassium dichromate is 22.54 g/L), controlling the ultrasonic power to be 300W, the frequency to be 19.5kHz, the current to be 0.31A and the stirring speed to be 150r/min under the constant temperature condition of 80 ℃, carrying out oxidation leaching for 30min, carrying out solid-liquid separation after leaching, washing solids with 25mL of deionized water (washing liquid is part of filtrate), and obtaining filter residue and filtrate; drying the filter residue at 60 ℃ for 15h to obtain dry-based filter residue.
Example 9
The only difference from example 8 is that the concentration of the sulfuric acid solution was 140g/L.
Example 10
The only difference from example 8 is that the concentration of the sulfuric acid solution was 160g/L.
Example 11
The only difference from example 8 is that the concentration of the sulfuric acid solution was 180g/L.
Example 12
The only difference from example 8 is that the concentration of the sulfuric acid solution was 200g/L.
Comparative example 3
The only difference from example 11 is that potassium dichromate is replaced by an equal mass of iron sulfate.
Fe in ferric sulfate 3+ Has the function of oxidation.
Comparative example 4
The only difference from example 11 is that potassium dichromate is replaced by sodium nitrate of equal mass.
Sodium nitrate in sodium nitrate is oxidizing and has an oxidizing effect.
Comparative example 5
The only difference from example 11 is that potassium dichromate was replaced with sodium nitrate of equal mass and the time for oxidative leaching was adjusted to 60min.
Effect example 3
The contents of zinc and germanium in the filtrates and the qualities of the dry residue were measured in examples 8 to 12 and comparative examples 3 to 5, and the leaching rate was calculated (the calculation method was the same as in effect example 1), and the results are shown in table 4.
TABLE 4
As can be seen from table 4, the reason why the leaching rate is rather decreased by extending the leaching time in comparative example 4 as compared with comparative example 5 is that: the reaction time is prolonged, so that some substances (such as silicate, aluminum-containing compound, iron-containing compound and the like) in the oxidizing smoke gradually react into the solution, and the pH value of the system is increased. In the reaction process, the hydrolysis of silicate and other substances is a dynamic process, and when the pH is more than 2 or less than 2, the silicate is hydrolyzed, so that at the beginning of the leaching reaction, the hydrolysis of silicate occurs as the silicate is dissolved in the sulfuric acid solution, so the leaching rate (rising or falling) of zinc and germanium depends on the adsorption amount of colloid formed by the silicate and the dissolution amount of zinc and germanium, whichever is larger or smaller. That is, at the beginning of the leaching reaction, only a small amount of silicate is hydrolyzed, and at this time, the adsorption amount of silica gel is small, and the dissolution amount of zinc and germanium is large, so that the leaching rate of zinc and germanium tends to increase. When zinc and germanium are leached in a large amount, residual zinc and germanium can be gradually dissolved only at a slow speed, more silicate is dissolved in sulfuric acid at the moment, more silica gel is generated, the adsorption capacity is larger, namely, the adsorption capacity is larger than the dissolution capacity of zinc and germanium, and the leaching rate of zinc and germanium is caused to show a descending trend.
Example 13
(1) The zinc oxide smoke dust is sieved by a 200-mesh sieve, then 40g of the sieved zinc oxide smoke dust (raw material) is weighed, 1.26g of potassium dichromate is weighed, and 280mL of sulfuric acid solution (with the concentration of 120 g/L) is weighed.
(2) Mixing zinc oxide smoke dust and potassium dichromate, placing the mixture into a reactor, adding a sulfuric acid solution, uniformly mixing to obtain a reaction solution (the liquid-solid ratio is 7mL/g, and the concentration of potassium dichromate is 4.5 g/L), controlling the ultrasonic power to be 300W, the frequency to be 19.5kHz, the current to be 0.31A and the stirring speed to be 150r/min under the constant temperature condition of 80 ℃, carrying out oxidation leaching for 30min, carrying out solid-liquid separation after the leaching is finished, washing the solid with 25mL of deionized water (the washing liquid is used as a part of the filtrate), and obtaining filter residue and filtrate; drying the filter residue at 60 ℃ for 15h to obtain dry-based filter residue.
Example 14
(1) The zinc oxide smoke dust is sieved by a 200-mesh sieve, then 40g of the sieved zinc oxide smoke dust (raw material) is weighed, 9.47g of potassium dichromate is weighed, and 280mL of sulfuric acid solution (with the concentration of 120 g/L) is weighed.
(2) Mixing zinc oxide smoke dust and potassium dichromate, placing the mixture into a reactor, adding a sulfuric acid solution, uniformly mixing to obtain a reaction solution (the liquid-solid ratio is 7mL/g, the concentration of potassium dichromate is 33.82 g/L), controlling the ultrasonic power to be 200W, the frequency to be 19.5kHz, the current to be 0.31A and the stirring speed to be 150r/min under the constant temperature condition of 90 ℃, carrying out oxidation leaching for 30min, carrying out solid-liquid separation after leaching, washing solids with 25mL of deionized water (washing liquid is part of filtrate), and obtaining filter residue and filtrate; drying the filter residue at 60 ℃ for 15h to obtain dry-based filter residue.
Example 15
(1) The zinc oxide smoke dust is sieved by a 200-mesh sieve, then 40g of the sieved zinc oxide smoke dust (raw material) is weighed, 6.31g of potassium dichromate is weighed, and 280mL of sulfuric acid solution (the concentration is 140 g/L) is weighed.
(2) Mixing zinc oxide smoke dust and potassium dichromate, placing the mixture into a reactor, adding a sulfuric acid solution, uniformly mixing to obtain a reaction solution (the liquid-solid ratio is 7mL/g, the concentration of potassium dichromate is 22.54 g/L), controlling the ultrasonic power to be 500W, the frequency to be 19.5kHz, the current to be 0.31A and the stirring speed to be 150r/min under the constant temperature condition of 90 ℃, carrying out oxidation leaching for 180min, carrying out solid-liquid separation after leaching, washing solids with 25mL of deionized water (washing liquid is part of filtrate), and obtaining filter residue and filtrate; drying the filter residue at 60 ℃ for 15h to obtain dry-based filter residue.
Example 16
(1) The zinc oxide smoke dust is sieved by a 200-mesh sieve, then 40g of the sieved zinc oxide smoke dust (raw material) is weighed, 6.31g of potassium dichromate is weighed, and 280mL of sulfuric acid solution (the concentration is 140 g/L) is weighed.
(2) Mixing zinc oxide smoke dust and potassium dichromate, placing the mixture into a reactor, adding a sulfuric acid solution, uniformly mixing to obtain a reaction solution (the liquid-solid ratio is 7mL/g, the concentration of potassium dichromate is 22.54 g/L), controlling the ultrasonic power to be 300W, the frequency to be 19.5kHz, the current to be 0.31A and the stirring speed to be 150r/min under the constant temperature condition of 60 ℃, carrying out oxidation leaching for 30min, carrying out solid-liquid separation after leaching, washing solids with 25mL of deionized water (washing liquid is part of filtrate), and obtaining filter residue and filtrate; drying the filter residue at 60 ℃ for 15h to obtain dry-based filter residue.
Effect example 4
The contents of zinc and germanium in the filtrates and the mass of the dry residue in examples 13 to 16 were measured, and the leaching rate was calculated (the calculation method was the same as in effect example 1), and the results are shown in table 5.
TABLE 5
Example 13 has a low initial acid sulfuric acid concentration, a low reaction temperature and a low oxidant concentration compared to comparative example 2, so example 13 is far less effective than comparative example 2.
Example 14 has a lower sulfuric acid concentration than comparative example 2, the acid concentration has a decisive effect on the leaching rate during leaching, and the effect of ultrasound is less than that of sulfuric acid.
Example 15 compared to comparative example 2, the reaction time was longer and it was found from our study that the leaching rate was increased by 2-5% with and without the addition of ultrasound. However, longer leaching time, so that silicate and Fe are leached 3+ The colloid generated by hydrolysis absorbs a lot of zinc and germanium and dissolves them, and the negative effect of the absorption is much larger than the positive effect of the ultrasonic wave, so the leaching rate of example 15 is much lower than that of comparative example 2.
In example 16, compared with comparative example 2, the reaction temperature is lower, the low temperature reduces the movement rate of each substance in the reaction system, the mass transfer rate is slower, the collision probability among molecules is smaller, and the reaction rate is reduced, so the leaching rate of example 16 is slightly lower than that of comparative example 2.
Effect example 5
The experimental parameters of 30min leaching time were the same as example 1, only the leaching time was changed, and the other parameters were the same as example 1, so that a leaching (zinc and germanium) effect graph with the change of the leaching time was obtained, and the results are shown in fig. 4.
FIG. 4 is a graph of the effect of leaching time on zinc and germanium leaching rates;
the experimental parameters for 30min of leaching time were the same as example 1, only the leaching time was changed, and the other parameters were the same as example 1, and a leaching (lead, iron, silicon and aluminum) effect graph according to the leaching time was obtained, and the results are shown in fig. 5.
According to the influence of the reaction time on the leaching rates of zinc and germanium (fig. 4), it can be found that the leaching rate of zinc shows a plateau trend at first and shows a decreasing trend after 60min, and the leaching rate of germanium shows a decreasing trend as a whole, along with the extension of the reaction time. Analysis of the reaction diagram (fig. 5) of iron and silicon in combination with the reaction time is mainly because some substances (such as silicate) in the zinc oxide smoke slowly react due to long-time leaching, so that the pH in the liquid rises to reach the pH at which silicon and iron (particularly silicon) are hydrolyzed, the iron content in the solution starts to decrease at 60min, and the silicon content in the solution decreases at 90min, which are both caused by hydrolysis.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (10)
1. The method for ultrasonically strengthening zinc oxide smoke dust in the oxidation leaching of potassium dichromate is characterized by comprising the following steps of:
mixing zinc oxide smoke dust and potassium dichromate, adding a sulfuric acid solution to prepare a reaction solution, and then placing the reaction solution under the conditions of ultrasonic waves and stirring to carry out zinc oxide smoke dust oxidation leaching.
2. The method for ultrasonic-enhanced potassium dichromate oxidation leaching of zinc oxide smoke dust according to claim 1, wherein the method further comprises drying and screening the zinc oxide smoke dust before preparing the reaction solution to obtain pretreated zinc oxide smoke dust.
3. The method for enhancing the zinc oxide smoke dust through potassium dichromate oxidation leaching by ultrasonic waves as claimed in claim 2, wherein the drying is vacuum drying, and the vacuum degree is 0.005-0.01 MPa; the drying temperature is 60 ℃, and the drying time is 24 hours; the number of the meshes of the adopted screens is 80-200 meshes.
4. The ultrasonic-enhanced potassium dichromate oxidative leaching zinc oxide fume method according to claim 1, characterized in that the volume/mass ratio of the sulfuric acid solution and the zinc oxide fume is 6-8 mL/g.
5. The ultrasonic-enhanced potassium dichromate oxidation leaching zinc oxide smoke method according to claim 1, characterized in that the mass/volume ratio of potassium dichromate to sulfuric acid solution is 4.5-33.82 g:1L of the total amount of the active ingredients.
6. The ultrasonic-enhanced potassium dichromate oxidation leaching zinc oxide smoke method according to claim 1, characterized in that the concentration of the sulfuric acid solution is 120-200 g/L.
7. The method for enhancing the zinc oxide smoke leaching by potassium dichromate oxidation through ultrasonic waves according to claim 1, wherein the power of the ultrasonic waves is 90-600W, the frequency is 19.5kHz, and the current is 0.31A; the stirring speed is 50-300 r/min.
8. The ultrasonic-enhanced potassium dichromate oxidation leaching zinc oxide smoke dust method according to claim 1, characterized in that the temperature of the oxidation leaching is 40-90 ℃ and the time is 30-180 min.
9. The ultrasonic enhanced potassium dichromate oxidative leaching zinc oxide fume process of claim 1, wherein the main components in the zinc oxide fume include zinc-containing compounds and germanium-containing compounds.
10. The ultrasonic enhanced potassium dichromate oxidative leach zinc oxide fume process of claim 9, wherein the zinc-containing compounds include zinc oxide, zinc sulfide, and zinc sulfate; the germanium-containing compound includes germanium monoxide, germanium dioxide, germanate and its sulfide.
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