CN106868306A - A kind of method of zinc leaching residue valuable metal high efficiente callback - Google Patents
A kind of method of zinc leaching residue valuable metal high efficiente callback Download PDFInfo
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- CN106868306A CN106868306A CN201611207776.6A CN201611207776A CN106868306A CN 106868306 A CN106868306 A CN 106868306A CN 201611207776 A CN201611207776 A CN 201611207776A CN 106868306 A CN106868306 A CN 106868306A
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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
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B7/00—Hydraulic cements
- C04B7/22—Iron ore cements ; Iron rich cements, e.g. Ferrari cements, Kühl cements
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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
- C22B13/00—Obtaining lead
- C22B13/04—Obtaining lead by wet processes
- C22B13/045—Recovery from waste materials
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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
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0084—Treating solutions
- C22B15/0089—Treating solutions by chemical methods
- C22B15/0091—Treating solutions by chemical methods by cementation
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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
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/20—Obtaining zinc otherwise than by distilling
- C22B19/22—Obtaining zinc otherwise than by distilling with leaching with acids
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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
- C22B58/00—Obtaining gallium or indium
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- 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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Abstract
The invention belongs to the zinc abstraction technical field technical field of non-ferrous metal metallurgy industry, more particularly to a kind of method of zinc leaching residue valuable metal high efficiente callback, by presoaking operation, middle sour operation, peracid operation, reduction operation, neutralization step, displacement operation, heavy indium operation, bloodstone iron removal step after being mainly well mixed using high-copper silver-colored zinc phase analysis high and silver enrichment slag；The method is applied to treatment high-copper silver-colored zinc phase analysis high and silver enrichment slag mixed material, the recovery rate of valuable metals such as indium, copper, silver, zinc are high, iron zinc separation process is short, energy-conserving and environment-protective, remarkable in economical benefits, be the synthetical recovery of high-copper silver-colored zinc material high, open the efficient new method of clean environment firendly.
Description
Technical field
The invention belongs to the zinc abstraction technical field technical field of non-ferrous metal metallurgy industry, more particularly to a kind of zinc leaching residue
The method of valuable metal high efficiente callback.
Background technology
More than the 85% of current zinc hydrometallurgy yield Yi Zhan worlds zinc yield, mainly by roasting, leach, it is purification, electrolysis, molten
The operations such as casting composition, wherein leaching residue treating method mainly has two kinds of wet method and pyrogenic process, and pyrogenic process is mainly：Rotary Kiln volatility process and
Blast furnace fuming method, wet method is mainly will be removed iron after zinc and iron leaching using hot acid extract technology, and method for removing iron includes Huang
Krausite method, goethite process, hematite process etc..
Most domestic zinc hydrometallurgy factory uses Rotary Kiln volatility process.But the quantity of slag that the method has leaching is big, energy consumption
High, volatilization kiln exhaust gas are high containing SO2, and tail gas absorbing system is larger, operating cost is higher, and the rate of recovery of dissipated metal is low to ask
Topic；Hot Acid Leaching Jarosite Process, uses, the technical maturity reliability in part smeltery of China, invests relatively low.But
There is siderotil acid slag needs Special slag to store up, and there is environmentally friendly potential problem.Use the iron precipitation by goethite process technique can be with output iron content
Goethite slag higher, advantage is good comprehensive reutilization effect, but the utilization of goethite is still present some problems, pin iron
Though slag amount has been reduced but still needed to pyrogenic attack, the direct yield of zinc metal is relatively low, the valuable metal meeting such as copper-lead during heavy iron
Bring into slag, recovery process is lengthened, cost is raised or rate of recovery reduction is, it is necessary to consider the Utilizing question of high acidic oils slag.
For the problem that above-mentioned zinc abstraction technique is present, a kind of present invention recovery rate of valuable metals of offer is high, clean environment firendly
The method of high-effect treatment high-copper silver-colored zinc phase analysis high and silver enrichment slag mixed material.The technique and existing conventional leaching-volatilization
Kiln handling process is combined, and is capable of achieving the maximizing the benefits of the valuable metals such as copper, silver, indium, moreover it is possible to keep the body of whole Zn system
Product balance and iron balance.
The content of the invention
It is an object of the invention to solve the metal synthetical recovery benefit in zinc abstraction technique in the prior art in leached mud
Low problem, and a kind of method of the zinc leaching residue valuable metal high efficiente callback for providing.
The technical solution adopted in the present invention is：
A kind of method of zinc leaching residue valuable metal high efficiente callback, mainly mixes using high-copper silver-colored zinc phase analysis high and silver enrichment slag
By presoaking operation, middle sour operation, peracid operation, reduction operation, neutralization step, displacement operation, heavy indium operation, red iron after uniform
Ore deposit iron removal step：
Step 1）, preimpregnation operation：High-copper silver-colored zinc phase analysis high and silver enrichment slag are mixed in proportion, by mixed material and sulfur acid
Waste electrolyte obtains pre- phase analysis and prepreg solution through preimpregnation, and prepreg solution returns existing Zn system calcining and leaches operation；
Step 2）, middle sour operation：By step 1）In pre- phase analysis and sulfur acid waste electrolyte warp in Ore Leaching obtain middle acid sludge
With middle acid leaching liquor；
Step 3）, peracid operation：By step 2）In the waste electrolyte of middle acid sludge and sulfur acid obtain highly acid slag through high acidic oils
With acid solution high, acid solution high can return to step 2）The bottom liquid of the middle Ore Leaching in, lead smelting gas and washing are obtained after highly acid slag washing
Liquid, wherein, lead smelting gas can be used as the raw material of refining lead；
Step 4）, reduction operation：By step 3）In middle acid leaching liquor through reducing agent reduction obtain reducing slag and reduction after liquid, also
Former slag returns to existing Zn system calcining process dispensing and uses；
Step 5）, neutralization step：By step 4）In reduction after neutralized dose of liquid neutralize obtain gypsum and neutralize after liquid, gypsum can
As cement and the raw material of building materials plasterboard factory；
Step 6）, displacement operation：By step 5）In neutralization after liquid obtain copper ashes and displaced liquid through zinc dust precipitation, copper ashes can do
It is the raw material of copper metallurgy；
Step 7）, heavy indium operation：By step 6）In displaced liquid and step 3）The water lotion warp obtained after middle highly acid slag washing
Liquid after indium enrichment slag and heavy indium is obtained after the heavy indium of heavy indium agent, indium enrichment slag returns the existing smart smart indium of indium operation production；
Step 8）, bloodstone iron removal step：By step 7）In heavy indium after liquid through hematite process except iron obtains bloodstone slag and removes
Liquid after iron, partly except after iron liquid return step 1）Used as the pre- preserved material of preimpregnation, liquid returns existing Zn system calcining leaching after remaining removes iron
Go out the electric zinc of operation production, bloodstone and washing lotion are obtained after the production water washing of bloodstone slag, wherein, bloodstone can be used as cement plant
Raw material, washing lotion can return to step 3）Middle participation highly acid slag washing.
Further, high-copper silver-colored zinc phase analysis high contain zinc 10~25%, iron 15~40%, copper 0.5~3%, indium in preimpregnation operation
0.01~0.05%, silver 0.005~0.06%, silver enrichment slag is containing zinc 20~25%, silver 0.15~1.0%, and both are in following ratio
Mixing is with even：High-copper silver-colored zinc phase analysis high：50~95%, silver enrichment slag：5~50%, described preimpregnation operation, middle sour operation and height
The main component of the waste electrolyte used in sour operation is 40~60g/l of zinc, 150~200g/l of sulfuric acid.
Further, produced in described bloodstone iron removal step except after liquid after iron, liquid can after iron is removed in part therein
Returning replace expense electrolyte to be used as the pre- preserved material of preimpregnation in preimpregnation operation, and bloodstone iron removal step output except in liquid after iron
Containing the g/l of zinc 80~100, the g/l of iron 2~6,30~50 g/l of acid, 90~95 DEG C of temperature, and preimpregnation operation are used except liquid conduct after iron
The reaction condition of pre- preserved material is that initial acidity is 30~50g/l, solvent and solute weight ratio 3~5 in course of reaction:1, reaction time 0.5
~1h.
Further, the reaction condition of described middle sour operation is solvent and solute weight ratio 4~6 in course of reaction:1, reaction temperature
65~75 DEG C of degree, reaction time 6h, acidity is 50~70g/l, and reacted middle acid sludge contains zinc 8~16%, iron 8~15%, copper
0.2~0.4%, silver 0.05~0.5%, reacted middle acid leaching liquor is containing the g/l of zinc 45~70,50~70 g/l containing acid, containing trivalent
The g/l of iron 15~45.
Further, the reaction condition of described peracid operation contains the g/l of zinc 40~60, the g/ of sulfuric acid 150~200 to add
L waste electrolytes, solvent and solute weight ratio 6~8:1,85~95 DEG C of reaction temperature, reaction time 6h, terminal acidity be 110~
130g/l, output contains zinc 2~5%, leaded 10~20%, silver-colored 0.1~1.5% lead silver after reacted highly acid slag is washed through water lotion
Slag and containing the g/l highly acid slag cleaning solutions of zinc 30~50, wherein, lead smelting gas as refining lead raw material, highly acid slag washing lotion enters heavy indium work
Sequence.
Further, the reaction condition of described reduction operation is that middle acid leaching liquor is warming up into 65~85 DEG C, is added also
Former agent, reducing agent used is zinc concentrate, one or more in lead concentrate or low iron vulcanization lead and zinc concentrate, reducing agent addition amount
It is 1.0~1.6 times of Fe3+ theory of reduction amount, 2~6 hours recovery times, 65~85 DEG C of reaction temperature, after reaction end is for reduction
Fe3+ is less than 3g/L, reduction 45~65g/L of concentration sour eventually in liquid, send neutralization step.
Further, the reducing agent used by described reduction operation is low iron vulcanization lead and zinc concentrate.
Further, the reaction condition of described neutralization step for add nertralizer, nertralizer be white lime and carbide slag,
And white lime and carbide slag are constituted according to following ratio by weight percentage：White lime：60~90%, carbide slag：10~40%, in
It is the 80%~110% of theoretical amount to add weight with agent, neutralizes time 10min, 10~35 DEG C of course of reaction reaction temperature, terminal
Acidity is 5~15g/l.
Further, described displacement operation is that liquid after neutralization is added into displacement operation, adds displacer zinc powder, zinc powder to add
It is 1.5-2.5 times of theoretical amount to enter amount, 60-70 DEG C of reaction temperature, reaction time 2h, and control displaced liquid copper is less than 0.1 g/L
Interior, displaced liquid send heavy indium operation.
Further, the heavy indium agent used by described heavy indium operation is sodium carbonate and manganese carbonate, and reaction condition is to react
60~75 DEG C of journey reaction temperature, the h of reaction time 2~3, terminal acidity is Ph value 3.5-4.5, and sodium carbonate presses with manganese carbonate
Percentage by weight is constituted according to following ratio：Sodium carbonate：30~60%, manganese carbonate：40~70%, it is theory that indium agent of sinking adds weight
The 90%~160% of amount, indium is enriched with liquid after slag and heavy indium obtained by reaction, wherein, indium enrichment slag is more than 0.6% containing indium, send smart indium system
System, liquid send bloodstone iron removal step after heavy indium.
Further, the reaction condition of the bloodstone iron removal step is that liquid after heavy indium is warming up into 150~220 DEG C, plus
Entering oxygen, it is the 110%~200% of theoretical amount that oxygen adds weight, control bloodstone iron removal kettle is pressed in 0.65~
2.8MPa, reacts 3h, except being less than 3g/L containing Fe in liquid after iron, except a liquid part returns to presoak operation after iron, after remaining is except iron
Liquid returns existing Zn system calcining and leaches the electric zinc of operation production, and the bloodstone slag of output carries out multiple countercurrent washing with production water, with
It is washing terminal that the water lotion obtained after washing contains zinc less than 20g/l, and highly acid slag washing is obtained with after washing in the peracid operation
The water lotion for arriving containing zinc less than 50g/l for washing terminal, bloodstone slag after washing output containing zinc 0.5~1.5%, iron content 55~
60% bloodstone, can be used as the raw material in cement plant.
The beneficial effects of the present invention are：
1. from after the flash distillation of iron removal step autoclave except after iron liquid the mixture of slag is directly enriched with high-copper silver-colored zinc phase analysis high and silver
Material mixing, because except after iron liquid temperature degree be up to 90~95 DEG C, be not required to heat up during preimpregnation reaction, that is, save the steam needed for reacting and disappear
Consumption, cools except liquid after iron again, reduces except the construction investment of liquid cooling equipment and production run cost after iron；Preimpregnation purpose master
If the sour molten zinc and water-soluble zinc in the mixed material of zinc leaching residue and silver enrichment slag enter prepreg solution, acid, peracid in reducing subsequently
The leaching burden of operation and the zinc ion content except liquid before iron, and iron in mixed material etc. is stayed in pre- phase analysis, the method is fitted
For processing high-copper silver-colored zinc phase analysis high and silver enrichment slag mixed material, the recovery rate of valuable metals such as indium, copper, silver, zinc is high, iron-zinc
Separation process is short, energy-conserving and environment-protective, remarkable in economical benefits, be the synthetical recovery of high-copper silver-colored zinc material high, open clean environment firendly high
The new method of effect；
2. reducing agent is that low iron vulcanizes lead and zinc concentrate, and the reducing slag lead grade after reduction is enriched with, and zinc enters liquid after reduction, fills
The drawbacks of point solving this kind low iron vulcanization lead and zinc concentrate be difficult, cost recovery is high；
3. countercurrent washing, contains zinc less than 20g/l to determine the washing terminal of washing bloodstone slag according to bloodstone water lotion；And will
This water lotion is applied repeatedly in highly acid slag water-washing process, high to determine washing less than 50g/l containing zinc according to highly acid slag water lotion
The washing terminal of acid sludge, the slag rate that bloodstone and lead smelting gas are optimal after the requirement is washed, minimum slag contains zinc, saves
Industrial water, the cleaning solution enters after heavy indium operation the zinc for both having reclaimed water lotion, and liquid zinc ion is dense after heavy indium is can adjust again
Degree is less than 100g/l, reaches bloodstone except requirement of the iron to solution zinc ion concentration；
4. nertralizer is arranged in pairs or groups and used in proportion using white lime and carbide slag, has both saved cost of supplementary product, and can output high-quality
Product gypsum；
5. indium agent of sinking is arranged in pairs or groups and used in proportion using sodium carbonate with manganese carbonate, and the addition of manganese carbonate is according to manganese ion in Zn system
Content is adjusted, and both ensure that the optimal indium recovery of liquid and indium enrichment slag indium grade after heavy indium, in turn ensure that Zn system manganese
Ion concentration, so as to ensure that the high-quality electrolytic zinc of Zn system output, improves economic benefit.
Brief description of the drawings
A kind of process chart of the method for zinc leaching residue valuable metal high efficiente callback that Fig. 1 is provided for the present invention.
Specific embodiment
The invention will be further described with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
By 19 tons containing zinc 10%, iron 15%, copper 0.5%, indium 0.01%, silver 0.005% high-copper silver-colored zinc phase analysis high and 1 ton containing zinc 20%,
Silver-colored 0.15% silver medal enrichment slag mixing, sulfur acid 150g/l, the electrolyte that takes containing zinc 40g/l are presoaked as pre- preserved material and mixture,
The solid mass ratio 3 of liquid:1,0.5h is reacted, liquid after 17.6 tons of pre- phase analysis and preimpregnation is obtained, liquid is leached into main system calcining after preimpregnation
Operation；Take the pre- phase analysis that electrolyte adds preimpregnation operation output by sulfur acid 150g/l, containing zinc 40g/l, carry out middle Ore Leaching,
Solvent and solute weight ratio 4:1,65 DEG C of reaction temperature, reaction time 6h, terminal acidity is 50g/l, acid during 9.16 tons are obtained after reaction
Slag, in these acid sludge containing zinc 8%, iron 8%, copper 0.2%, silver 0.05%, reaction obtain the middle g/l of acid solution zinc 45, containing sour 50 g/l,
Containing the g/l of ferric iron 15；Middle acid sludge enters high acidic oils operation, adds and contains the g/l of zinc 40, sour 150 g/l waste electrolytes, liquid stereoplasm
Amount compares 6:1,85 DEG C of reaction temperature, reaction time 6h, terminal acidity is 110g/l, and reacted 5.5 tons of highly acid slags are through washing
4.12 tons of output is heavy containing zinc 2%, leaded 10%, silver-colored 0.1% lead gold and silver slag and the entrance containing the g/l highly acid slags cleaning solution of zinc 30 after liquid washing
Indium operation；The middle acid solution of middle Ore Leaching operation, is warming up to 65 DEG C, adds 4.64 tons of reducing agent zinc concentrate, and reducing agent addition amount is
1 times of Fe3+ theory of reduction amounts, 2 hours recovery times, Fe3+2.8g/L in liquid after reduction, reduction concentration 45g/L sour eventually send
Neutralization step；Liquid enters neutralization step after reduction, first adds weight to account for 10% 0.6 ton of carbide slag, and adding weight, to account for 85% ripe
5.1 tons of lime, it is the 80% of theoretical amount that nertralizer adds weight, neutralizes time 10min, 10 DEG C of reaction temperature, the concentration of whole acid
5g/L；Liquid enters displacement operation after neutralization, adds 300 kilograms of zinc powder, and zinc powder addition is the 150% of theoretical amount, reaction temperature 60
DEG C, reaction time 120min, displaced liquid copper is less than 0.1 g/L；Displaced liquid adds heavy indium agent, first adds weight to account for 30%
0.54 ton of sodium carbonate, adds weight and accounts for 1.26 tons of 70% manganese carbonate, and it is the 90% of theoretical amount to add weight, 60 DEG C of reaction temperature,
Reaction time 2h, between 3.5-4.5, to obtain indium enrichment slag containing indium more than 0.6%, indium enrichment slag send smart indium to terminal acidity pH value
System, liquid send bloodstone iron removal step after heavy indium, and liquid after heavy indium is warming up into 150 DEG C, adds oxygen, and oxygen addition is theory
The 110% of amount, control bloodstone autoclave kettle pressure 0.65MPa, reacts 3h, except being less than 3g/L containing Fe in liquid after iron；Except liquid after iron
A part returns to presoak operation, and liquid returns the electric zinc of existing Zn system calcining leaching operation production, the red iron of output after remaining removes iron
Slag carries out multiple countercurrent washing with production water, with washing after the water lotion that obtains containing zinc less than 20g/l to wash terminal, it is described
, containing zinc less than 50g/l as washing terminal, bloodstone slag is through water for the water lotion that highly acid slag washing is obtained with after washing in peracid operation
6.4 tons of rear output is washed containing zinc 0.5%, the bloodstone of iron content 55%, these bloodstone can be as the raw material in cement plant；The embodiment
It is the embodiment of initial situation, as presoaks the embodiment that operation, middle sour operation and peracid operation all add waste electrolyte.
Embodiment 2
Contain zinc 25%, silver containing zinc 25%, iron 40%, copper 3%, indium 0.05%, the high-copper silver-colored zinc phase analysis high of silver 0.06% and 10 tons by 10 tons
The enrichment slag mixing of 1% silver medal, sulfur acid 200g/l, the electrolyte that takes containing zinc 60g/l are presoaked as pre- preserved material and mixture, and liquid is solid
Mass ratio 5:1,1h is reacted, liquid after 17 tons of pre- phase analysis and preimpregnation is obtained, liquid enters main system calcining leaching operation after preimpregnation；To contain
Sulfuric acid 200g/l, the electrolyte that takes containing zinc 60g/l add the pre- phase analysis for presoaking operation output, carry out middle Ore Leaching, the solid weight of liquid
Than 6:1,75 DEG C of reaction temperature, reaction time 6h, terminal acidity is 70g/l, acid sludge during 8.5 tons are obtained after reaction, in these
Acid sludge containing zinc 16%, iron 15%, copper 0.4%, silver 0. 5%, reaction obtain the middle g/l of acid solution zinc 70, containing sour 70 g/l, containing ferric iron
45 g/l；Middle acid sludge enters high acidic oils operation, adds and contains the g/l of zinc 60, sour 200 g/l waste electrolytes, the solid mass ratio 8 of liquid:1,
95 DEG C of reaction temperature, reaction time 6h, terminal acidity is 130g/l, after reacted 5.2 tons of highly acid slags are washed through water lotion
3.9 tons of output is containing zinc 5%, leaded 20%, silver-colored 1.5% lead gold and silver slag and the heavy indium operation of the entrance containing the g/l highly acid slags cleaning solution of zinc 50；In
The middle acid solution of Ore Leaching operation, is warming up to 85 DEG C, adds 5.24 tons of reducing agent zinc concentrate, and reducing agent addition amount is Fe3+ also principles
1.6 times of stoichiometric, 6 hours recovery times, Fe3+1.6g/L in liquid after reduction, reduction concentration 65g/L sour eventually send neutralization step；
Liquid enters neutralization step after reduction, first adds weight to account for 40% 1.92 tons of carbide slag, adds weight and accounts for 60% white lime 4.48
Ton, it is the 110% of theoretical amount that nertralizer adds weight, neutralizes time 10min, 35 DEG C of reaction temperature, the concentration 15g/L of whole acid；In
Enter displacement operation with rear liquid, add 460 kilograms of zinc powder, zinc powder addition is the 250% of theoretical amount, 70 DEG C of reaction temperature, reaction
Time 120min, displaced liquid copper is less than 0.1 g/L；Displaced liquid adds heavy indium agent, first adds weight to account for 60% sodium carbonate
1.2 tons, add weight and account for 0.8 ton of 40% manganese carbonate, it is the 160% of theoretical amount, 75 DEG C of reaction temperature, reaction time to add weight
3h, between 3.5-4.5, to obtain indium enrichment slag containing indium more than 0.6%, indium enrichment slag send smart indium system to terminal acidity pH value, heavy indium
Liquid send bloodstone iron removal step afterwards, and liquid after heavy indium is warming up into 220 DEG C, adds oxygen, and oxygen addition is the 200% of theoretical amount,
Control bloodstone autoclave kettle pressure 2.8MPa, reacts 3h, except being less than 3g/L containing Fe in liquid after iron；Except a liquid part is returned to after iron
Preimpregnation operation, liquid returns the electric zinc of existing Zn system calcining leaching operation production, the bloodstone slag production of output after remaining removes iron
Water carries out multiple countercurrent washing, with washing after the water lotion that obtains containing zinc less than 20g/l to wash terminal, peracid in peracid operation
Pulp water washes the water lotion obtained with after washing containing zinc less than 50g/l as washing terminal, and 7 tons of output contains zinc to bloodstone slag after washing
1.5%th, the bloodstone of iron content 60%, these bloodstone can be as the raw material in cement plant；The embodiment is the implementation of initial situation
Example, as presoaks the embodiment that operation, middle sour operation and peracid operation all add waste electrolyte.
Embodiment 3
By bloodstone iron removal step output except containing the g/l of zinc 95, the g/l of iron 3.5, sour 42 g/l in liquid after iron, 93.5 DEG C of temperature,
The weight containing zinc 18.5%, iron 22.5%, copper 0.9%, indium 0.032%, silver 0.032% is added to account for 80% 8 tons of zinc leaching residue and containing zinc
23.8%th, the weight of silver 0.42% accounts for 20% silver 2 tons of slag of enrichment, liquid-solid ratio 3:1,1h is reacted, obtain 8.8 tons of pre- phase analysis and preimpregnation
Liquid afterwards, liquid enters main system calcining and leaches operation after preimpregnation, and the acid solution high containing sour 128 g/l of high acidic oils operation adds preimpregnation work
The pre- phase analysis of sequence output, carry out middle Ore Leaching, liquid-solid ratio 4:1,75 DEG C of reaction temperature, reaction time 6h, terminal acidity is
66g/l, acid sludge is containing zinc 8.2%, iron 8.5%, copper 0.23%, silver 0.17% in reacted 4.58 tons；Middle acid sludge enters high acidic oils
Operation, adds and contains the g/l of zinc 55, sour 192 g/l waste electrolytes, liquid-solid ratio 6:1,94 DEG C of reaction temperature, reaction time 6h
, terminal acidity is 128g/l, and reacted 2.75 tons of highly acid slags are washed with the bloodstone water lotion of bloodstone iron removal step output
2.06 tons of output contains zinc 2.2%, leaded 15.8%, silver-colored 0.35% lead gold and silver slag afterwards.48.5 g/l, bis- highly acid slag cleaning solutions containing zinc enter
Enter heavy indium operation, middle Ore Leaching operation containing the g/l of zinc 48.9, containing acid solution in sour 66 g/l, the g/l of ferric iron 19.5, be warming up to
76 DEG C, 2.32 tons of zinc concentrate is added, addition is 1.05 times of Fe3+ theory of reduction amount, 5 hours recovery times, after reduction in liquid
Fe3+ 2.8g/L, reduction concentration 62g/L sour eventually send neutralization step, and liquid enters neutralization step after reduction, first adds weight to account for
0.45 ton of 15% carbide slag, adds weight and accounts for 2.55 tons of 85% white lime, and it is the 99% of theoretical amount to add weight, neutralizes the time
10min, 32 DEG C of temperature, the concentration 11g/L of whole acid；Liquid enters displacement operation after neutralization, adds 150 kilograms of zinc powder, zinc powder to add
It is the 155% of theoretical amount to measure, 65 DEG C of reaction temperature, reaction time 120min, the g/L of displaced liquid copper 0.02, and displaced liquid is added
Heavy indium agent, first adds weight to account for 50% 0.45 ton of sodium carbonate, adds weight and accounts for 0.45 ton of 50% manganese carbonate, and it is reason to add weight
The 106% of stoichiometric, 72 DEG C of reaction temperature, reaction time 3h, indium enrichment slag contains indium 0.85%, except liquid is that liquid enters after heavy indium before iron
Bloodstone iron removal step, is warming up to 185 DEG C, adds oxygen, and oxygen addition is the 160% of theoretical amount, bloodstone autoclave kettle
Pressure 1.35MPa, reacts 3h, and except 2.8g/L containing Fe in liquid after iron, except a liquid part returns to presoak operation after iron, remaining is except iron
Liquid returns existing Zn system calcining and leaches the electric zinc of operation production afterwards, and the bloodstone slag of output carries out multiple countercurrent washing with production water,
The water lotion obtained after with washing containing zinc less than 20g/l as washing terminal, wash to be obtained after washing in peracid operation by highly acid slag
Water lotion containing zinc be washing terminal less than 50g/l, bloodstone slag after washing 3.2 tons of output containing zinc 0.78%, iron content 59%
Bloodstone, the embodiment be presoak use in operation output in iron removal step except after iron liquid as pre- preserved material, middle sour operation use
The situation of the embodiment of high acidic oils liquid, i.e. waste liquid recycling.
Embodiment 4
By bloodstone iron removal step output except containing the g/l of zinc 82, the g/l of iron 2.5, sour 35 g/l in liquid after iron, 91 DEG C of temperature, plus
Enter the weight containing zinc 19.5%, iron 20.8%, copper 1.2%, indium 0.025%, silver 0.025% and account for 50% 5 tons of zinc leaching residue and containing zinc
22.5%th, the weight of silver 0.28% accounts for 50% silver 5 tons of slag of enrichment, liquid-solid ratio 5:1,0.5h is reacted, obtain 8.5 tons of pre- phase analysis and pre-
Liquid after leaching, liquid enters main system calcining leaching operation after preimpregnation, and the acid solution high containing sour 108.5 g/l of high acidic oils operation is added in advance
The pre- phase analysis of operation output are soaked, middle Ore Leaching, liquid-solid ratio 6 is carried out:1,68 DEG C of reaction temperature, reaction time 6h, terminal acidity
It is 56.5g/l, acid sludge is containing zinc 12.5%, iron 12.6%, copper 0.25%, silver 0.22% in reacted 4.25 tons；Middle acid sludge enters high
Ore Leaching operation, adds and contains the g/l of zinc 45, sour 185 g/l waste electrolytes, liquid-solid ratio 8:1,91 DEG C of reaction temperature, reaction
Time 6h, terminal acidity is water of bloodstone of 111.5g/l, reacted highly acid slag and bloodstone iron removal step output
Output contains zinc 4.9%, leaded 12.8%, silver-colored 1.95 tons of 0.91% lead gold and silver slag after wash liquid.Containing zinc highly acid slag of 35.6 g/l
Cleaning solution enters heavy indium operation, middle Ore Leaching operation containing the g/l of zinc 48, containing acid in sour 56.5 g/l, the g/l of ferric iron 28.6
Liquid, is warming up to 75 DEG C, adds 2.62 tons of zinc concentrate, and addition is 1.2 times of Fe3+ theory of reduction amount, 4 hours recovery times, reduction
Fe3+1.6g/L in liquid, reduces concentration 53.2g/L sour eventually and send neutralization step afterwards, and liquid enters neutralization step after reduction, first adds
Weight accounts for 30% 0.96 ton of carbide slag, adds weight and accounts for 2.24 tons of 70% white lime, and it is the 102% of theoretical amount to add weight, in
With time 10min, 32 DEG C of temperature, the concentration 9.5g/L of whole acid；Liquid enters displacement operation after neutralization, adds 230 kilograms of zinc powder, zinc
Powder addition is the 180% of theoretical amount, 68 DEG C of reaction temperature, reaction time 120min, the g/L of displaced liquid copper 0.06；After displacement
Liquid adds heavy indium agent, first adds weight to account for 30% 0.3 ton of sodium carbonate, adds weight and accounts for 0.7 ton of 70% manganese carbonate, adds weight
Be the 108% of theoretical amount, 68 DEG C of reaction temperature, reaction time 2.5h, indium enrichment slag indium containing I 0.72%, except before iron liquid into red iron
Ore deposit iron removal step, is warming up to 170 DEG C, adds oxygen, and oxygen addition is the 120% of theoretical amount, bloodstone autoclave kettle pressure
1.05MPa, reacts 3h, except 2.2g/L containing Fe in liquid after iron, except a liquid part returns to presoak operation after iron, after remaining removes iron
Liquid returns existing Zn system calcining and leaches the electric zinc of operation production, and the bloodstone slag of output carries out multiple countercurrent washing with production water, with
The water lotion obtained after washing is washing terminal less than 20g/l containing zinc, and highly acid slag is washed to be obtained after washing in peracid operation
Water lotion is washing terminal less than 50g/l containing zinc, and 3.5 tons of output contains zinc 0.8%, the red iron of iron content 56% to bloodstone slag after washing
Ore deposit, the embodiment be presoak use in operation output in iron removal step except after iron liquid as pre- preserved material, middle sour operation peracid
The situation of the embodiment of leachate, i.e. waste liquid recycling.
Claims (10)
1. a kind of method of zinc leaching residue valuable metal high efficiente callback, it is characterised in that：Mainly using high-copper silver-colored zinc phase analysis high
By presoaking operation, middle sour operation, peracid operation, reduction operation, neutralization step, displacement work after well mixed with silver enrichment slag
Sequence, heavy indium operation, bloodstone iron removal step：
Step 1）, preimpregnation operation：High-copper silver-colored zinc phase analysis high and silver enrichment slag are mixed in proportion, by mixed material and sulfur acid
Waste electrolyte obtains pre- phase analysis and prepreg solution through preimpregnation, and prepreg solution returns existing Zn system calcining and leaches operation；
Step 2）, middle sour operation：By step 1）In pre- phase analysis and sulfur acid waste electrolyte warp in Ore Leaching obtain middle acid sludge
With middle acid leaching liquor；
Step 3）, peracid operation：By step 2）In the waste electrolyte of middle acid sludge and sulfur acid obtain highly acid slag through high acidic oils
With acid solution high, acid solution high can return to step 2）The bottom liquid of the middle Ore Leaching in, lead smelting gas and washing are obtained after highly acid slag washing
Liquid, wherein, lead smelting gas can be used as the raw material of refining lead；
Step 4）, reduction operation：By step 3）In middle acid leaching liquor through reducing agent reduction obtain reducing slag and reduction after liquid, also
Former slag returns to existing Zn system calcining process dispensing and uses；
Step 5）, neutralization step：By step 4）In reduction after neutralized dose of liquid neutralize obtain gypsum and neutralize after liquid, gypsum can
As cement and the raw material of building materials plasterboard factory；
Step 6）, displacement operation：By step 5）In neutralization after liquid obtain copper ashes and displaced liquid through zinc dust precipitation, copper ashes can do
It is the raw material of copper metallurgy；
Step 7）, heavy indium operation：By step 6）In displaced liquid and step 3）The water lotion warp obtained after middle highly acid slag washing
Liquid after indium enrichment slag and heavy indium is obtained after the heavy indium of heavy indium agent, indium enrichment slag returns the existing smart smart indium of indium operation production；
Step 8）, bloodstone iron removal step：By step 7）In heavy indium after liquid through hematite process except iron obtains bloodstone slag and removes
Liquid after iron, partly except after iron liquid return step 1）Used as the pre- preserved material of preimpregnation, liquid returns existing Zn system calcining leaching after remaining removes iron
Go out the electric zinc of operation production, bloodstone and washing lotion are obtained after the production water washing of bloodstone slag, wherein, bloodstone can be used as cement plant
Raw material, washing lotion can return to step 3）Middle participation highly acid slag washing.
2. the method for a kind of zinc leaching residue valuable metal high efficiente callback according to claim 1, it is characterised in that：Preimpregnation operation
Middle high-copper silver-colored zinc phase analysis high contain zinc 10~25%, iron 15~40%, copper 0.5~3%, indium 0.01~0.05%, silver 0.005~0.06%,
Silver is enriched with slag containing zinc 20~25%, silver 0.15~1.0%, and both match somebody with somebody even in the mixing of following ratio：High-copper silver-colored zinc phase analysis high：50~
95%, silver enrichment slag：5~50%；The waste electrolyte used in described preimpregnation operation, middle sour operation and peracid operation it is main
Composition is 40~60g/l of zinc, 150~200g/l of sulfuric acid.
3. the method for a kind of zinc leaching residue valuable metal high efficiente callback according to claim 1, it is characterised in that：Described is red
Produced in iron ore iron removal step except after liquid after iron, part therein except after iron liquid can return preimpregnation operation in replace expense electrolyte to make
For the pre- preserved material of preimpregnation is used, and bloodstone iron removal step output except containing the g/l of zinc 80~100, the g/ of iron 2~6 in liquid after iron
L, 30~50 g/l of acid, 90~95 DEG C of temperature, and preimpregnation operation are used except liquid is initial acid as the reaction condition of pre- preserved material after iron
It is 30~50g/l to spend, solvent and solute weight ratio 3~5 in course of reaction:1,0.5~1h of reaction time.
4. the method for a kind of zinc leaching residue valuable metal high efficiente callback according to claim 1, it is characterised in that：In described
The reaction condition of sour operation is solvent and solute weight ratio 4~6 in course of reaction:1,65~75 DEG C of reaction temperature, reaction time 6h,
Acidity is 50~70g/l, and reacted middle acid sludge contains zinc 8~16%, iron 8~15%, copper 0.2~0.4%, silver 0.05~0.5%, instead
Middle acid leaching liquor after answering is containing the g/l of zinc 45~70,50~70 g/l containing acid, containing the g/l of ferric iron 15~45.
5. the method for a kind of zinc leaching residue valuable metal high efficiente callback according to claim 1, it is characterised in that：Described height
The reaction condition of sour operation contains the g/l of zinc 40~60, the g/l waste electrolytes of sulfuric acid 150~200, solvent and solute weight ratio 6~8 to add:
1,85~95 DEG C of reaction temperature, reaction time 6h, terminal acidity is 110~130g/l, and reacted highly acid slag is through water lotion
Output is containing zinc 2~5%, leaded 10~20%, silver-colored 0.1~1.5% lead smelting gas and containing the washing of the g/l highly acid slags of zinc 30~50 after washing
Liquid, wherein, used as the raw material for refining lead, highly acid slag washing lotion enters heavy indium operation to lead smelting gas.
6. the method for a kind of zinc leaching residue valuable metal high efficiente callback according to claim 1, it is characterised in that：Described goes back
The reaction condition of former operation is that middle acid leaching liquor is warming up into 65~85 DEG C, adds reducing agent, reducing agent used is zinc concentrate,
Lead concentrate or low iron vulcanization lead and zinc concentrate in one or more, reducing agent addition amount be Fe3+ theory of reduction amount 1.0~1.6
Times, 2~6 hours recovery times, 65~85 DEG C of reaction temperature, reaction end is that Fe3+ is less than 3g/L in liquid after reducing, and reduction is eventually
45~the 65g/L of concentration of acid, send neutralization step.
7. the method for a kind of zinc leaching residue valuable metal high efficiente callback according to claim 1, it is characterised in that：In described
With the reaction condition of operation to add nertralizer, nertralizer is white lime and carbide slag, and white lime and carbide slag by weight hundred
Divide than being constituted according to following ratio：White lime：60~90%, carbide slag：10~40%, it is theoretical amount that nertralizer adds weight
80%~110%, time 10min, 10~35 DEG C of course of reaction reaction temperature are neutralized, terminal acidity is 5~15g/l.
8. the method for a kind of zinc leaching residue valuable metal high efficiente callback according to claim 1, it is characterised in that：Described puts
It is that liquid after neutralization is added into displacement operation to change operation, adds displacer zinc powder, and zinc powder addition is 1.5-2.5 times of theoretical amount,
60-70 DEG C of reaction temperature, reaction time 2h, less than in 0.1 g/L, displaced liquid send heavy indium operation to control displaced liquid copper.
9. the method for zinc leaching residue valuable metal high efficiente callback according to claim 1, it is characterised in that：Described heavy indium work
Heavy indium agent used by sequence is sodium carbonate and manganese carbonate, and reaction condition is 60~75 DEG C of course of reaction reaction temperature, reaction time 2
~3 h, terminal acidity is Ph value 3.5-4.5, and sodium carbonate and manganese carbonate are by weight percentage according to following ratio composition：Carbon
Sour sodium：30~60%, manganese carbonate：40~70%, it is the 90%~160% of theoretical amount that indium agent of sinking adds weight, and indium is rich obtained by reaction
Liquid after collection slag and heavy indium, wherein, indium enrichment slag is more than 0.6% containing indium, send smart indium system, and liquid send bloodstone iron removal step after heavy indium.
10. the method for zinc leaching residue valuable metal high efficiente callback according to claim 1, it is characterised in that：The bloodstone
The reaction condition of iron removal step is that liquid after heavy indium is warming up into 150~220 DEG C, adds oxygen, and it is theoretical amount that oxygen adds weight
110%~200%, control bloodstone iron removal kettle is pressed in 0.65~2.8MPa, reacts 3h, except being less than containing Fe in liquid after iron
3g/L, except a liquid part returns to presoak operation after iron, remaining except after iron liquid return existing Zn system calcining and leach operation production electricity
Zinc, the bloodstone slag of output carries out multiple countercurrent washing with production water, is less than 20g/l containing zinc with the water lotion obtained after washing
Washing terminal, the water lotion that highly acid slag washing is obtained with after washing in the peracid operation is less than 50g/l as washing terminal containing zinc,
Output contains zinc 0.5~1.5%, the bloodstone of iron content 55~60% to bloodstone slag after washing, can be used as the raw material in cement plant.
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| CN109112301A (en) * | 2018-09-27 | 2019-01-01 | 贵州宏达环保科技有限公司 | A method of electrolytic separation iron and zinc in sulfuric acid medium |
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