CN107312934B - A method of abatement solid waste of heavy metal slag Leaching - Google Patents

A method of abatement solid waste of heavy metal slag Leaching Download PDF

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CN107312934B
CN107312934B CN201710375803.9A CN201710375803A CN107312934B CN 107312934 B CN107312934 B CN 107312934B CN 201710375803 A CN201710375803 A CN 201710375803A CN 107312934 B CN107312934 B CN 107312934B
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leaching
solid waste
heavy metal
slag
solid
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CN107312934A (en
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郭秋松
刘志强
李伟
朱薇
张魁芳
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Institute of Resource Utilization and Rare Earth Development of Guangdong Academy of Sciences
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Guangdong Institute of Rare Metals
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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
    • C22B7/006—Wet processes
    • C22B7/007—Wet processes by acid leaching
    • A—HUMAN NECESSITIES
    • A62—LIFE-SAVING; FIRE-FIGHTING
    • A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
    • A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
    • A62D3/10—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by subjecting to electric or wave energy or particle or ionizing radiation
    • A62D3/11—Electrochemical processes, e.g. electrodialysis
    • A62D3/115—Electrolytic degradation or conversion
    • 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
    • A—HUMAN NECESSITIES
    • A62—LIFE-SAVING; FIRE-FIGHTING
    • A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
    • A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
    • A62D2101/40—Inorganic substances
    • A62D2101/43—Inorganic substances containing heavy metals, in the bonded or free state
    • 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)
  • Materials Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Geology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Business, Economics & Management (AREA)
  • Emergency Management (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Toxicology (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Treatment Of Sludge (AREA)

Abstract

A method of the Leaching of abatement solid waste of heavy metal slag, comprise the steps of: solid waste of heavy metal slag is after iron removal by magnetic separation, supplying leaching leaching activator and reduction reinforcing agent are uniformly mixed, leaching preserved material is added, in 1 ~ 3h of leaching leaching in metallic channel under room temperature, flocculant polyacrylamide is added in leaching immersion liquid, electrode is done using metal plate-like or mesh electrode and metallic channel, electricity auxiliary leaches 1 ~ 5h；After the completion of leaching, solid-liquor separation drenches immersion liquid, and filtrate recycles valuable metal, and filter residue is stored up after being washed with hot water.The method of abatement solid waste of heavy metal slag Leaching of the invention, can recycle the valuable metals such as vanadium, copper, cobalt, nickel, zinc, manganese simultaneously, solve harm reduction, the comprehensive utilization of resources problem of solid waste of heavy metal slag.The present invention is suitable for the disinfection attenuation of the ferrous metal wet process solid waste slags such as non-ferrous metals and manganese, chromium such as vanadium, cobalt, copper, zinc, chromium, nickel, and process is generated without new pollution.The method of the present invention simple process and low cost, facilitates heavy industrialization to implement.

Description

A method of abatement solid waste of heavy metal slag Leaching
Technical field
The invention belongs to environmental protection technical fields, are related to a kind of method for cutting down solid waste of heavy metal slag Leaching, especially It is to extract and comprehensively utilize to generate in the non-ferrous metals such as zinc, nickel, cobalt, copper, vanadium and manganese, chrome black non-ferrous metal hydrometallurgy process Residual quantity of heavy metal is high, disinfection harm reduction method of metallurgy acid solid waste slag and neutral solid waste slag that Leaching Heavy Metals are high.
Background technique
Heavy metal ion dissolution is the main reason for solid waste slag generation environment endangers.All kinds of hydrometallurgy solid waste slags are by rainwater Especially acid rain leaching act on, contained by heavy metal can occur dissolution and migration, directly contribute soil environment and water environment Persistent pollution is generated, ecological environment is damaged, seriously threatens human health.China is mineral resources comprehensive utilization and deep processing weight Base is wanted, during the valuable metals metallurgical extraction such as zinc, nickel, cobalt, copper, vanadium, chromium, manganese, output largely remains various heavy Hydrometallurgy solid waste slag, transport transfer and stockpiling landfill process, there are biggish environmental risks.
Vanadium, chromium, nickel, cobalt, manganese, lead, copper, zinc etc. belong to main environment sensitivity heavy metal element, and environmental pollution exists Accumulation property and non-biodegradable are easy to be enriched in food chain, can generate physiological-toxicity to human body, have to ecological environment of human settlements and hold Long property harm.
The Leaching of solid waste slag, using simulation it is lack of standardization landfill, stockpiling or after harmless treatment waste soil When utilization, heavy metal components leach and enter the process of environment from waste residue under the influence of acid precipitation, and in specific field It is leached in conjunction by surface water or underground water, the process of Leaching of Heavy Metals and entrance environment.To protect environment, ensure that human body is strong Health, needs to assess the Leaching of Heavy Metals risk of solid waste slag, and takes the Leaching of aggregate measures abatement solid waste slag.
The heavy metal elements such as vanadium, chromium, nickel, cobalt, manganese, lead, copper, zinc contained by hydrometallurgy solid waste slag, the presence in slag Form is sufficiently complex, and majority belongs to variable valency element, and chemical activity is big.It assists leaching using electrochemistry, passes through anodic oxygen Change and cathodic reduction behavior can promote contained heavy metal element and leach migration, separation and recovery or stable curing.
CN105734298A disclose it is a kind of with shunt co-extraction taking technique valuable gold is recycled from non-ferrous metal solid slag The method of category.The invention includes that one section of pressure leaching and two sections of normal pressure counterflow leaching processes, cadmium manganese cleaning procedure, indium zinc-iron shunt Coextraction process, regeneration of hydrochloric acid process and without MnZn electrodeposition process.This method main target is from non-ferrous metal solid slag The valuable metals such as indium are extracted, technique is more complex, higher cost.
CN201510220900.1 discloses a kind of method that the full immersion of normal temperature and pressure goes out mining and metallurgy solid waste Poisoning element, In toxic element Hg, Cd, Ge, Te, Cr, Ga, Li, In, Sn, Pb, Ni, Tl, As, Sb, Be, F, Co, Bi, Cu and Ag, solid waste At least containing one kind, step includes that leaching agent polyalcohol sulfone class halogen is added to carry out one section of leaching, with sodium chloride plus leaching agent into Two sections of row leachings.The party it is owned by France addition leaching agent conventional leaching method, in solid waste slag including but not limited to heavy metal The synthetical recovery of toxic element does not refer to the method route for reducing Leaching to the sensitive heavy metal element of main environment.
Summary of the invention
The object of the present invention is to provide a kind of method for cutting down solid waste of heavy metal slag Leaching, solid wastes of the present invention Cinder ladle includes the hydrometallurgys solid waste slag such as cobalt, vanadium, zinc, manganese, copper, nickel and chromium, and content of beary metal is high, existence form is complicated.
Method of the invention comprises the steps of: solid waste of heavy metal slag after iron removal by magnetic separation, supplying leaching leaching activator and It restores reinforcing agent to be uniformly mixed, is added and drenches preserved material, in 1 ~ 3h of leaching leaching in metallic channel under room temperature, flocculant is added in leaching immersion liquid and gathers Acrylamide does electrode using metal plate-like or mesh electrode and metallic channel, and electricity auxiliary leaches 1 ~ 5h；After the completion of leaching, liquid is solid Separation leaching immersion liquid, filtrate recycle valuable metal, and filter residue is stored up after being washed with hot water.
The leaching activator be calcium chloride or calcium carbonate, leaching activator additional amount be solid waste slag≤3 ‰.
The reduction reinforcing agent is sodium sulfite, sodium thiosulfate or sodium pyrosulfite, and reduction reinforcing agent additional amount is Solid waste slag≤5 ‰.
The liquid-solid ratio of the sulfuric acid solution that the leaching preserved material is 0.02 ~ 0.5M of concentration, leaching preserved material and solid waste slag is 5 ~ 20: 1(L/ Kg).
It is 10 ~ 80A/m that the electricity auxiliary, which leaches current density,2, tank voltage is 0.7 ~ 3.5V, with metal plate-like or netted electricity Extremely anode, which is powered, leaches 10 ~ 60min, then reversed be powered leaches 1min, and total electricity auxiliary extraction time is 1 ~ 5h.
The metal plate-like or mesh electrode material are stainless steel, titanium or alloy, and metallic channel material is stainless steel or titanium.
The present invention is added leaching activator and reduction reinforcing agent is uniformly mixed first by solid waste slag after iron removal by magnetic separation, then Leaching preserved material sulfuric acid solution is added, during drenching preserved material leaching leaching, dilute sulfuric acid can be by remaining diffluent heavy metal compound, gold Belong to salt etc. to leach naturally, the addition of calcium chloride or calcium carbonate can accelerate leached ions migration, and form micro- reaction and leach area.Electrification Learning the redox reaction leached promotes the realizations such as elemental copper, trivalent cobalt, insoluble manganese, the high price vanadium that can not leach naturally to soak in situ Out or stable state solidification, the dissolution leaching rate of the sensitive heavy metal of raising, reduction reinforcing agent can increase reduction, can also after dissolution Play the role of increasing slag body electrical conductivity.During electrochemical leaching, by the way that flocculant polyacrylamide is added and changes electrification Parameter, regulation and conversion oxidation and reduction process are learned, intensity and depth are leached in control redox, easily realization full process automatization Control.The method of abatement solid waste of heavy metal slag Leaching of the invention, can be recycled the valuable metals such as vanadium, copper, cobalt, nickel, zinc, solution It has determined the harm reduction and comprehensive utilization of resources problem of solid waste of heavy metal slag.The present invention is suitable for vanadium, cobalt, copper, zinc, chromium, nickel etc. The disinfection harm reduction of the ferrous metal wet process solid waste slag such as non-ferrous metal and manganese, chromium, process are generated without new pollution.The method of the present invention technique Simply, low in cost, facilitate heavy industrialization to implement.
Specific embodiment
Embodiment 1
To the cobalt hydrometallurgy solid waste slag containing cobalt 0.25%, vanadium 0.12%, nickel 0.02%, copper 0.01%, manganese 0.03% etc., through dry Formula iron removal by magnetic separation, is incorporated 1 ‰ calcium chloride and 2 ‰ sodium pyrosulfites are uniformly mixed, and the bottom that the resistance to acid tank of stainless steel is added is paved；It presses Liquid-solid ratio 10: 1(L/kg) 0.03M dilution heat of sulfuric acid is added, leaching leaching 2h under room temperature；Flocculant polyacrylamide is added in slot, Titanium net, which to be placed, in leaching immersion liquid makees positive electrode, groove body is another pole, in leaching process, current density 30A/m2, tank voltage is 1.2V, the two poles of the earth exchange during electricity auxiliary leaches, and the period is positive energization 50min, and another mistake is leached to energization 1min, total electricity auxiliary Time 3h；After leaching, titanium net electrode is removed, is filtered after stirring；Filtrate recycles the valuable metals such as vanadium, copper, nickel, cobalt, manganese member Element；It is stored up after washing filter residue with hot water, filter residue contains cobalt 0.03%, vanadium 0.02%, nickel 0.01%, copper 0.04%, manganese 0.003%.Cobalt wet process Metallurgical solid waste slag after processing cobalt, vanadium, nickel, copper, manganese Leaching cut rate be respectively 99.2%, 95.5%, 96.1%, 90.8%、98.9%。
Embodiment 2
To the zinc hydrometallurgy solid waste slag containing zinc 0.33%, cobalt 0.05%, vanadium 0.19%, copper 0.08%, manganese 0.17% etc., through dry Formula iron removal by magnetic separation, is incorporated 2 ‰ calcium carbonate and 5 ‰ sodium sulfites are uniformly mixed, and the bottom that the resistance to acid tank of stainless steel is added is paved；By liquid Admittedly than 7: 1(L/kg) leaching leaching 3h under 0.4M dilute sulfuric acid room temperature is added；Flocculant polyacrylamide is added in slot, in leaching immersion liquid It places lead-containing alloy and makees positive electrode, groove body is another pole, in leaching process, current density 60A/m2, tank voltage 3.1V, electricity The two poles of the earth exchange during auxiliary leaches, period are positive energization 30min, and another mistake assists extraction time 2h to energization 1min, total electricity； After leaching, alloy electrode is removed, is filtered after stirring；Filtrate recycles the valuable metals elements such as zinc, vanadium, copper, cobalt, manganese；With heat It is stored up after water washing filter residue, filter residue contains zinc 0.08%, cobalt 0.02%, vanadium 0.03%, nickel 0.01%, copper 0.05%, manganese 0.005%.Zinc is wet Method metallurgy solid waste slag after processing zinc, cobalt, vanadium, copper, manganese Leaching cut rate be respectively 88.1%, 97.4%, 93.5%, 99.3%、99.6%。
Embodiment 3
To containing chromium 0.06%, vanadium 0.09%, lead 0.015%, copper 0.04%, manganese 0.02% chromium hydrometallurgy solid waste slag, through dry type Iron removal by magnetic separation, is incorporated 3 ‰ calcium chloride and 3 ‰ sodium thiosulfate are uniformly mixed, and the bottom that the resistance to acid tank of titanium matter is added is paved；It is solid by liquid Than 10: 1(L/kg) leaching leaching 1h under 0.05M dilute sulfuric acid room temperature is added；Flocculant polyacrylamide is added in slot, in leaching immersion liquid It places ruthenium system multicomponent mixture coating modification titanium plate titanium net and makees positive electrode, groove body is another pole, and in leaching process, current density is 70A/m2, tank voltage 3.2V, the two poles of the earth exchange during electricity auxiliary leaches, and the period is positive energization 40min, and another mistake is to energization 1min, total electricity auxiliary extraction time 1.5h；After leaching, titanium net electrode is removed, is filtered after stirring；Filtrate recycle chromium, vanadium, The valuable metals element such as copper, lead, manganese；It is stored up after washing filter residue with hot water, filter residue contains chromium 0.005%, vanadium 0.01%, lead 0.01%, copper 0.04%, manganese 0.001%.Chromium hydrometallurgy solid waste slag after processing chromium, vanadium, lead, copper, manganese Leaching cut rate be respectively 98.0%、98.9%、55.4%、72.3%、99.5%。

Claims (2)

1. it is a kind of cut down solid waste of heavy metal slag Leaching method, the solid waste of heavy metal cinder ladle include cobalt, vanadium, zinc, manganese, The cobalt hydrometallurgy solid waste slag of copper, nickel and chromium, zinc hydrometallurgy solid waste slag and chromium hydrometallurgy solid waste slag, it is characterized in that by following Step composition: after iron removal by magnetic separation, supplying leaching leaching activator and reduction reinforcing agent are uniformly mixed solid waste of heavy metal slag, and leaching leaching is added Flocculant polyacrylamide is added in leaching immersion liquid in 1 ~ 3h of leaching leaching in metallic channel under room temperature in agent, using metal plate-like or netted Electrode and metallic channel do electrode, and it is 10 ~ 80A/m that electricity auxiliary, which leaches current density,2, tank voltage is 0.7 ~ 3.5V, and anode, which is powered, to be soaked 10 ~ 60min out, then reversed be powered leach 1min, and electricity auxiliary leaches 1 ~ 5h；After the completion of leaching, solid-liquor separation drenches immersion liquid, and filtrate is returned Valuable metal is received, filter residue is stored up after being washed with hot water；
Leaching leaching activator is calcium chloride or calcium carbonate, leaching leaching activator additional amount be solid waste slag≤3 ‰；
The reduction reinforcing agent is sodium sulfite, sodium thiosulfate or sodium pyrosulfite, and reduction reinforcing agent additional amount is solid waste slag ≤ 5 ‰；
The liquid-solid ratio of the sulfuric acid solution that the leaching preserved material is 0.02 ~ 0.5M of concentration, leaching preserved material and solid waste slag is that 5 ~ 20: 1 unit is L/kg。
2. the method for the Leaching of abatement solid waste of heavy metal slag according to claim 1, it is characterized in that the metal plate Shape or mesh electrode material are stainless steel, titanium or alloy, and metallic channel material is stainless steel or titanium.
CN201710375803.9A 2017-05-25 2017-05-25 A method of abatement solid waste of heavy metal slag Leaching Active CN107312934B (en)

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CN102534231A (en) * 2012-01-09 2012-07-04 湖南邦普循环科技有限公司 Method for extracting nickel and cobalt from nickel-cobalt-containing fluoride residue
CN102765831B (en) * 2012-07-25 2013-10-23 中南大学 Purification method of wastewater containing heavy metal and arsenic
CN103060550B (en) * 2012-12-28 2014-06-25 江苏雄风科技有限公司 Synchronized production method of reducing leaching and oxidizing deironing of cobalt-copper ore
CN103233130B (en) * 2013-05-09 2014-10-29 贵阳中科融实新材料技术有限公司 Chromium slag treatment method
CN103343229A (en) * 2013-06-28 2013-10-09 江西理工大学 Method for comprehensively recovering valuable metals from electroplating waste mud
CN105861822B (en) * 2016-04-06 2017-10-10 广州有色金属研究院 A kind of acids reduction leaching method of cobalt copper mixed oxidization ore deposit

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