CN106399703A - Method for extracting Pb, In and Ag from indium-containing lead silver residues - Google Patents

Method for extracting Pb, In and Ag from indium-containing lead silver residues Download PDF

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Publication number
CN106399703A
CN106399703A CN201610855419.4A CN201610855419A CN106399703A CN 106399703 A CN106399703 A CN 106399703A CN 201610855419 A CN201610855419 A CN 201610855419A CN 106399703 A CN106399703 A CN 106399703A
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lead
indium
leaching
extract
smelting gas
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CN106399703B (en
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曾光祥
李世平
周代江
韦国龙
王志斌
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Guizhou Xing An Environmental Protection Technology Co ltd
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Guizhou Environmental Protection Technology Co Ltd Of Htc
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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
    • C22B7/04—Working-up slag
    • 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
    • C22B11/00—Obtaining noble metals
    • C22B11/04—Obtaining noble metals by wet processes
    • C22B11/042—Recovery of noble metals from waste materials
    • 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
    • C22B13/00—Obtaining lead
    • C22B13/04—Obtaining lead by wet processes
    • C22B13/045—Recovery from waste materials
    • 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
    • C22B58/00—Obtaining gallium or indium
    • 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
    • C25C1/18—Electrolytic production, recovery or refining of metals by electrolysis of solutions of lead
    • 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

Abstract

The invention discloses a method for extracting Pb, In and Ag from indium-containing lead silver residues. The method comprises the following steps of: Pb extracting, In extracting and Ag extracting. The method disclosed by the invention is used for sufficiently recycling resources by recycling valuable metal Pb, In and Ag from the indium-containing lead silver residues, has a very high economic value, and also avoids pollution of the lead silver residues on environment.

Description

A kind of method extracting Pb, In, Ag from lead smelting gas containing indium
Technical field
The present invention relates to the method for wet underwater welding metallic compound and in particular to one kind extract from lead smelting gas containing indium Pb, The method of In, Ag.
Background technology
Extract the valuable metal such as Zn, In, Pb from the material relatively low containing grades such as zinc, indium, lead, silver, generally require first to lead to Cross rotary kiln and carry out reduction-oxidation calcination process, make valuable metal obtain volatilizing and enriching and with the element sepatation such as ferrum, silicon, calcium, have Valency metal Zn, In, Pb overwhelming majority forms oxide and enters bag collection system, then is removed by neutral leaching-purification of leaching liquor Carry out electrolytic separation after miscellaneous and extract zinc, so that the indium in slag is enriched with further by neutral leaching, then carry out sulphuric acid leaching again Go out the In and neutral Zn leaching residual, acid leaching solution is extracted by P204, HCl back extraction separation and Extraction In, acidic leaching residue is Be containing Pb40～55%, In300～600g/t, Ag150～400g/t lead smelting gas.Due to leaching through H2SO4 twice, therefore Lead major part in this lead smelting gas is with PbSO4Form exists, and with the presence of a small amount of with PbS form, and the oxide of In substantially can By H2SO4Leach, but InS can not be by H2SO4Leach, therefore the indium in lead smelting gas is substantially existed with InS form.Why should Also contain higher indium in lead smelting gas, have part indium to be combined with sulfur during being because rotary kiln calcination and generate the InS being easy to volatilize, And reducing roasting process needs to add coal as reducing agent, unavoidably also have certain sulfur in coal, add in raw material and also contain Certain sulfur, therefore, material unavoidably has InS, PbS, ZnS sulfides by rotary kiln reduction roasting and generates, thus Cause the response rate of indium relatively low, the indium content in lead smelting gas is higher.
Indium belongs to rare metal, has very big economic worth and use value, and global indium resource is deficienter, ore deposit Produce amount is few, also disperse very much.And in this lead smelting gas, do not contain only Pb and Ag, also contain substantial amounts of indium, therefore, to this lead smelting gas In indium further fully reclaim extremely be necessary, be also to have very much economic worth.Traditional smelting process of lead smelting gas For pyrometallurgical smelting, use retailoring of blast furnace lead, silver is also reduced to metallic state and enters formation pb-ag alloy in lead bullion, then leads to Cross electrorefining lead separation lead and silver, the method can carry lead well, but the response rate of silver is not high, have partly silver-colored and most of Indium enters in slag and is difficult to reclaim, and causes the waste of rare precious metal resource, and pyrometallurgical smelting of lead is big for environment pollution, energy consumption Height, precious and rare metals recovery rate is low；Secondly, existing great majority produce and process lead smelting gas elder generation separation and Extraction silver using floatation, then with fiery Method extracts lead, and the method is all more satisfactory to the extraction of metallic lead and precious metals silver, but is not suitable for containing rare precious metal indium Lead smelting gas, indium cannot preferably reclaim, and can cause the waste of resource；Also having is exactly to be leached using pressure oxidation, by adding Pressure Oxidation Leaching can make ZnS the and InS sulfides in material oxidized leach so as in Zn and In fully leached back Receive, in leached mud, indium content is naturally relatively low, then pass through other methods smelting lead smelting gas again and reclaim lead and silver, the method is ratio Comparatively ideal recovery method, can make Zn and In disposably fully be extracted, and obtains the higher lead smelting gas of grade, but pressurization There is equipment investment greatly in Oxidation Leaching, equipment, technical staff are had high demands, the defect such as is difficult to carry out, applies for medium-sized and small enterprises. For this present inventor, a kind of method extracting Pb, In, Ag from lead smelting gas containing indium is provided by substantial amounts of experiment and research.
Content of the invention
For solving above-mentioned technical problem, the invention provides a kind of method extracting Pb, In, Ag from lead smelting gas containing indium.
The present invention is achieved by the following technical programs：
A kind of method extracting Pb, In, Ag from lead smelting gas containing indium, the method comprises the following steps：
A, Pb extract：Indium lead smelting gas NH will be contained4F solution is washed, and cleaning mixture returns and recycles, molten using NaOH Liquid carries out alkaline leaching Pb to washed-residue, then leachate is carried out with electrolytic lead processes obtaining lead sponge, lead sponge through briquetting, molten Casting processes and obtains lead pig, and electrolyte returns secondary NaOH alkaline leaching Pb, and secondary leachate returns once to leach and uses；
B, In extract：By step a neutral and alkali leached mud H2SO4Solution leaches In, and leachate adopts P204 extraction, HCL molten In is extracted in liquid back extraction, and leaching indium slag is standby；
C, Ag extract：Leaching indium slag thiourea solution in step b is leached Ag, leachate hydrazine hydrate reduction obtains gold Belong to Ag.
NH in described step a4F solution washs the L/S=6-10 of lead smelting gas containing indium, NH4F addition is 10-20g/L, temperature control It is made as 70-80 DEG C, the time is 1-2h.
In described step a, alkaline leaching Pb is carried out to washed-residue using NaOH solution, its alkaline leaching liquid L/S=4- 6, NaOH consumptions are 250-300g/L, and temperature is 85-90 DEG C, and the time is 2-3h, secondary alkaline leaching liquid L/S=6-10, NaOH For 200-250g/L, temperature is 80-90 DEG C, and the time is 3-5h.
In described step a, electrolytic lead is processed is using corrosion resistant plate as electrolytic negative/positive plate, and pole span is 80mm, and tank voltage is 1-1.5V, electric current density is 150-200A/m2, electrolysis temperature be 20-50 DEG C.
Electrolyte in described step a contains Pb10-20g/L.
Described step b neutral and alkali leached mud H2SO4Solution leaches In, its L/S=5-8, H2SO4For 150-100g/L, temperature Spend for 80-90 DEG C, the time is 3-5h.
In described step c, leaching indium slag leaches its L/S=5-8 of Ag with thiourea solution, and PH is 1-1.5, and the concentration of thiourea is 20- 30g/L carbamide is 3-5g/L, and temperature is 50-60 DEG C, and extraction time is 5-8h.
The beneficial effects of the present invention is：The present invention adopts Whote-wet method to extract Pb, In, Ag in lead smelting gas containing indium, containing indium Lead smelting gas first use NH4F solution washs, mainly the H in washing lead smelting gas2SO4, with the consumption of NaOH when reducing alkaline leaching Pb, And in lead smelting gas, also contain 3～10% SiO2, no matter part SiO2 all can be had to be leached shape in acidic leaching or alkaline leaching Become the silicic acid of colloidal, silicic acid can affect the strainability of leaching slurry, and SiO2 also can wrap up valuable metal make its be difficult to by Leach, by adding NH4F makes to exist H in solution+And F+, such that it is able to destroy SiO2, so that the valuable metal of parcel is released, Also leaching slurry strainability, improve production efficiency can be improved, cleaning mixture can also return recycling simultaneously；Through NH4F solution is washed Lead smelting gas containing indium after washing carry out alkaline leaching Pb with NaOH solution, and leachate carries out being electrolysed lead sponge, and lead sponge is through briquetting, molten Casting obtains lead pig, and electrolysis Pb residual liquid returns alkaline leaching and uses；Lead smelting gas containing indium are through alkaline leaching twice, not only separation and Extraction Metallic lead, makes In and Ag staying in slag be enriched with further simultaneously, and the InS composition in slag is anti-with NaOH at high temperature The alkali formula indium compound being soluble in acid should be generated, contain such that it is able to leaching-extracting stripping method separation and Extraction by conventional acid In in indium lead smelting gas；In leached mud leaches Ag with thiourea solution again, and leachate extracts metal Ag with hydrazine hydrate reduction, so, Pb, In, Ag in lead smelting gas containing indium just can get efficiently, fully reclaim, and the present invention will contain indium lead smelting gas and first use NH4F Solution washs, not only can in eccysis slag residual H2SO4, with the consumption of NaOH when reducing next step alkaline leaching Pb additionally it is possible to Destroy SiO2, improve the leaching rate of valuable metal Pb, In, Ag, Si can also be made simultaneously to form the H being easy to filter2SiF6, thus reaching To the strainability improving leaching slurry；Lead smelting gas containing indium after washing first carry out alkaline leaching separation and Extraction Pb, and leached mud is again Carry out acidic leaching separation and Extraction In, because the In in lead smelting gas is substantially InS, be difficult to leach In by acidic leaching, and While carrying out alkaline leaching Pb, InS composition can be reacted with NaOH at high temperature and generate the alkali formula indium compound being soluble in acid, Again extraction indium can be easily separated by acidic leaching；Lead smelting gas containing indium will not be leached thus reaching through During alkaline leaching Pb To the enrichment of In, and acidic leaching In can make Ag stay in slag is enriched with further, and In content can get more than twice Enrichment, Ag content can get the enrichment of more than three times, thus can reduce production cost when extracting In and Ag；The present invention will contain indium Sulphuric acid lead skim passes through to reclaim valuable metal Pb, In, Ag, resource is fully reclaimed, not only has very high economic worth, with When it also avoid the pollution to environment for the lead smelting gas.
Brief description
Fig. 1 is present invention process flow chart
Specific embodiment
Below in conjunction with drawings and Examples, technical scheme is further described, but claimed scope is simultaneously It is not limited to described.
Embodiment one
By a collection of containing zinc 11.28%, Pb3.51%, Fe12.47%, Si15.83%, In652g/t, Ag273g/t former Material, obtains cloth bag powder, obtain after sulfuric acid leaching separation and Extraction Zn, In twice contains after rotary kiln reduction-oxidation roasting volatilization Indium lead smelting gas, its chemical composition is：Pb45.04%, In356g/t, Ag279g/t, Zn 2.15%, Fe 1.14%, Si 4.36%, contain indium lead smelting gas with this and carry out alkaline leaching Pb：200g is taken to contain indium lead smelting gas, by liquid-solid ratio L/S=4, leachate (=250g/L, 85 DEG C of temperature, mixing time 2h carry out primary alkali leaching to NaOH；One time leached mud presses L/S=8, leachate again (=250g/L, 85 DEG C of temperature, mixing time 3h carry out 2 leachings to NaOH.One time leachate (1000mL) content is： Pb58.7g/L, Zn2.65g/L, In no content；Secondary leachate (800mL) content is：Pb14.3g/L、Zn1.04g/L；Secondary Leached mud (81.5g) content is：Pb17.32%, In847g/t, Ag652g/t, Zn 1.17%；Leaching rate (slag meter)： Pb84.33%, Zn77.82%；The alkaline leaching rate of filtration is all slow twice.
Embodiment two
Carry out being electrolysed Pb using an alkali immersion (1000mL) in embodiment one, electrolytic condition is：Using corrosion resistant plate as Cathode-anode plate, pole span L=80cm, tank voltage is 1.2V, and electric current density is 150A/m2, 35 DEG C of electrolysis temperature, electrolysis time 8h； Electrolysis lead sponge 43.2g, residual electrolyte contains Pb16.4g/L.
Embodiment three
First carry out NH using lead smelting gas containing indium in embodiment one4F solution washs, and slag presses the condition alkaline leaching of example 1 again Pb, NH4F solution wash conditions are：Liquid-solid ratio L/S=6, NH4F addition is 10g/L, temperature 70 C, mixing time 1h, washing Liquid contains H2SO48.54g/L、Zn1.34g/L、In 9.6mg/L；Secondary alkaline leaching slag (71.4g) content is：Pb12.17%, In914g/t, Ag703g/t, Zn 1.05%；Leaching rate (slag meter)：Pb90.35%；The alkaline leaching rate of filtration is very fast twice.
Example IV
First carry out NH using lead smelting gas containing indium in embodiment one4F solution washs, and adds NH with cleaning mixture in example 34F is extremely 20g/L is washed：Liquid-solid ratio L/S=8,80 DEG C of temperature, mixing time 2h；Cleaning mixture contains H2SO412.05g/L、Zn2.18g/ L、In 13.7mg/L；Washed-residue carries out alkaline leaching Pb：By liquid-solid ratio L/S=6, leachate NaOH (=300g/L, temperature 90 DEG C, mixing time 3h carry out primary alkali leaching；One time leached mud presses L/S=6, leachate NaOH (=200g/L, temperature 80 again DEG C, mixing time 4h carry out secondary leaching.One time leachate (1100mL) content is：Pb62.4g/L, Zn1.92g/L, secondary leaching Going out liquid (600mL) content is：Pb21.6g/L, Zn1.52g/L, secondary leached mud (63.1g) content is：Pb10.64%, In946g/t, Ag732g/t, Zn 0.85%；Leaching rate (slag meter)：Pb 92.54%
Embodiment five
Pressing tank voltage using an alkali immersion in example four is 1.4V, and electric current density is 200A/m2, 45 DEG C of electrolysis temperature, Remaining condition is carried out being electrolysed Pb by embodiment two；Electrolysis lead sponge 46.3g, containing Pb99.21%, residual electrolyte contains Pb14.2g/L.
Embodiment six
Sulfuric acid leaching In is carried out using alkaline leaching slag (50g) secondary in example IV, leaching condition is：Liquid-solid ratio L/S =5, H2SO4150g/L, 85 DEG C of temperature, mixing time 3h, leachate 0.25L, containing In165mg/L, In leaching rate (liquid meter) is 87.3%；Leached mud 35.65g, containing Ag1035g/t, then is 25g/ with thiourea by liquid-solid ratio L/S=8, PH=1.0, thiourea concentration L, carbamide 5g/L, temperature are 55 DEG C of leaching Ag, and extraction time is 6h, and leached mud (31.84g), containing Ag118g/t, silver leaching rate 89.82%.
Embodiment seven
NH is added using cleaning mixture in the example IV of lead smelting gas containing indium in embodiment one4F to 15g/L is washed：Liquid Gu ratio L/S=10,75 DEG C of temperature, mixing time 1.5h；Washed-residue carries out alkaline leaching Pb：By liquid-solid ratio L/S=5, leachate (=300g/L, 85 DEG C of temperature, mixing time 3h carry out primary alkali leaching to NaOH；One time leached mud presses L/S=7, leachate again (=250g/L, 85 DEG C of temperature, mixing time 5h carry out secondary leaching to NaOH；Secondary leached mud (61.7g) content is： Pb8.95%, In941g/t, Ag728g/t, Zn 0.85%；Leaching rate (slag meter)：Pb 93.87%；Leached mud presses liquid-solid ratio L/ S=8, H2SO4200g/L, 90 DEG C of acidic leaching In of temperature, mixing time 4h, In leaching rate (liquid meter) is 92.37%；Leached mud Press liquid-solid ratio L/S=6, PH=1.5 again, thiourea concentration be 30g/L, carbamide 3g/L, temperature be 60 DEG C of leaching Ag, extraction time is 8h, leached mud contains Ag97g/t, silver leaching rate 92.57%.
Embodiment eight
Carry out NH using lead smelting gas containing indium in embodiment one by embodiment seven conditional respectively successively4The washing of F solution, NaOH Leach Pb, H2SO4Leach In, thiourea leaches Ag, Pb, In, Ag leaching rate respectively reaches 93.25%, 94.37%, 90.08%.

Claims (7)

1. a kind of from lead smelting gas containing indium extract Pb, In, Ag method, including it is characterised in that：
A, Pb extract：Indium lead smelting gas NH will be contained4F solution is washed, and cleaning mixture returns and recycles, using NaOH solution pair Washed-residue carries out alkaline leaching Pb, then leachate is carried out electrolytic lead process obtain lead sponge, lead sponge at briquetting, founding Reason obtains lead pig, and electrolyte returns secondary NaOH alkaline leaching Pb, and secondary leachate returns once to leach and uses；
B, In extract：By step a neutral and alkali leached mud H2SO4Solution leaches In, and leachate adopts P204 extraction, HCL solution anti- Extract and take In, leaching indium slag is standby；
C, Ag extract：Leaching indium slag thiourea solution in step b is leached Ag, leachate hydrazine hydrate reduction obtains metal Ag.
2. according to claim 1 from lead smelting gas containing indium extract Pb, In, Ag method it is characterised in that：Described step NH in a4F solution washs the L/S=6-10 of lead smelting gas containing indium, NH4F addition is 10-20g/L, and temperature control is 70-80 DEG C, the time For 1-2h.
3. according to claim 1 from lead smelting gas containing indium extract Pb, In, Ag method it is characterised in that：Described step In a, alkaline leaching Pb is carried out to washed-residue using NaOH solution, its alkaline leaching liquid L/S=4-6, NaOH consumption is 250- 300g/L, temperature is 85-90 DEG C, and the time is 2-3h, and secondary alkaline leaching liquid L/S=6-10, NaOH are 200-250g/L, temperature For 80-90 DEG C, the time is 3-5h.
4. according to claim 1 from lead smelting gas containing indium extract Pb, In, Ag method it is characterised in that：Described step In a, electrolytic lead is processed is using corrosion resistant plate as electrolytic negative/positive plate, and pole span is 80mm, and tank voltage is 1-1.5V, electric current density For 150-200A/m2, electrolysis temperature be 20-50 DEG C.
5. according to claim 1 from lead smelting gas containing indium extract Pb, In, Ag method it is characterised in that：Described step Electrolyte in a contains Pb10-20g/L.
6. according to claim 1 from lead smelting gas containing indium extract Pb, In, Ag method it is characterised in that：Described step B neutral and alkali leached mud H2SO4Solution leaches In, its L/S=5-8, H2SO4For 150-100g/L, temperature is 80-90 DEG C, the time For 3-5h.
7. according to claim 1 from lead smelting gas containing indium extract Pb, In, Ag method it is characterised in that：Described step In c, leaching indium slag leaches its L/S=5-8 of Ag with thiourea solution, and PH is 1-1.5, and the concentration of thiourea is 3-5g/ for 20-30g/L carbamide L, temperature is 50-60 DEG C, and extraction time is 5-8h.
CN201610855419.4A 2016-09-27 2016-09-27 A kind of method that Pb, In, Ag are extracted from lead smelting gas containing indium Expired - Fee Related CN106399703B (en)

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CN109136575A (en) * 2018-08-31 2019-01-04 唐山鹤兴废料综合利用科技有限公司 A kind of process of the more metallic dusts of wet-treating
CN109735716A (en) * 2019-03-11 2019-05-10 北京科技大学 A method of extracting lead from containing lead solution
CN112921357A (en) * 2021-01-01 2021-06-08 冯建成 Technology for preparing lead by electrolytic zinc preparation of nonmagnetic stainless steel anode

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CN104611568A (en) * 2014-11-18 2015-05-13 贵州宏达环保科技有限公司 Method for extraction of metal lead, silver, zinc, indium and germanium from lead sulfate slag

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CN109136575A (en) * 2018-08-31 2019-01-04 唐山鹤兴废料综合利用科技有限公司 A kind of process of the more metallic dusts of wet-treating
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CN109735716A (en) * 2019-03-11 2019-05-10 北京科技大学 A method of extracting lead from containing lead solution
CN112921357A (en) * 2021-01-01 2021-06-08 冯建成 Technology for preparing lead by electrolytic zinc preparation of nonmagnetic stainless steel anode

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