CN105525093B - A kind of method of simplified Zinc hydrometallurgy process - Google Patents
A kind of method of simplified Zinc hydrometallurgy process Download PDFInfo
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- CN105525093B CN105525093B CN201510985762.6A CN201510985762A CN105525093B CN 105525093 B CN105525093 B CN 105525093B CN 201510985762 A CN201510985762 A CN 201510985762A CN 105525093 B CN105525093 B CN 105525093B
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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
- 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
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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
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/20—Obtaining zinc otherwise than by distilling
- C22B19/26—Refining solutions containing zinc values, e.g. obtained by leaching zinc ores
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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
- 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
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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- 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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Abstract
The present invention discloses a kind of method of simplified Zinc hydrometallurgy process, including Step 1: zinc roasting mine, which is carried out neutral leach, obtains middle immersion liquid and middle phase analysis；Step 2: being added to the middle phase analysis that step 1 obtains containing hot acid leaching is carried out in acid waste liquid, pickle liquor and acid leaching residue are obtained；Step 3: acid leaching residue and ZnS concentrate that step 2 obtains are added to containing carrying out reducing leaching in acid waste liquid, liquid and reducing slag after being restored；Step 4: making neutralizer by zinc roasting mine is added in liquid after reduction that step 3 obtains, obtain neutralizing slag and neutralizer, neutralizes two hot acid of slag return to step and leach；Oxidation Leaching is carried out Step 5: the reducing slag that step 3 obtains is added in the pickle liquor in step 2, obtains Oxidation Leaching liquid and lead silver sulphur slag, Oxidation Leaching liquid returns to step 3 reducing leaching；Step 6: the neutralizer that step 4 is obtained, which is added in zinc roasting mine, carries out the heavy iron of goethite, liquid and goethite slag after heavy iron are obtained.
Description
Technical field
The present invention relates to colored metallurgical industrial field more particularly to a kind of methods of simplified Zinc hydrometallurgy process.
Background technology
Leaching Technology of Zinc Hydrometallurgy has roasted ore routine extract technology, roasted ore hot acid extract technology, zinc sulfide concentrates oxygen
Extract technology is pressed, ratio of the zinc smelting dreg processing cost that roasted ore routine extract technology generates in zinc abstraction cost is gradual
It increases, existing above-mentioned technique has the problems such as long flow path, the rate of recovery are low, Slag treatment is of high cost, there are environmentally friendly hidden danger.
Therefore, the existing technology needs to be improved and developed.
Invention content
In view of above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of sides of simplified Zinc hydrometallurgy process
Method, it is intended to solve the problems such as prior art long flow path, the rate of recovery are low, Slag treatment is of high cost, there are environmentally friendly hidden danger.
Technical scheme is as follows：
A kind of method of simplified Zinc hydrometallurgy process, wherein including：
Step 1: zinc roasting mine, which is carried out neutral leach, obtains middle immersion liquid and middle phase analysis；
Step 2: by the middle phase analysis that step 1 obtains be added to containing in acid waste liquid carry out hot acid leaching, obtain pickle liquor and
Acid leaching residue；
Step 3: being added to the acid leaching residue and ZnS concentrate that step 2 obtains containing reducing leaching is carried out in acid waste liquid, obtain
Liquid and reducing slag after reduction；
Step 4: making neutralizer by zinc roasting mine is added in liquid after reduction that step 3 obtains, obtain neutralizing slag and neutralizer,
Two hot acid of slag return to step is neutralized to leach；
Oxidation Leaching is carried out Step 5: the reducing slag that step 3 obtains is added in the pickle liquor in step 2, is obtained
Oxidation Leaching liquid and lead silver sulphur slag, Oxidation Leaching liquid return to step 3 reducing leaching；
Step 6: the neutralizer that step 4 is obtained is added in zinc roasting mine and carries out goethite and sink iron, obtain after heavy iron liquid and
Goethite slag.
The method of the simplification Zinc hydrometallurgy process, wherein when control neutrality leaches, initial pH is 2.5, and terminal pH is
4.0~4.2。
The method of the simplification Zinc hydrometallurgy process, wherein the residual acid concentration that control hot acid leaches is 70 ~ 80g/L.
The method of the simplification Zinc hydrometallurgy process, wherein the Fe of liquid after control reduction3+< 2g/L.
The method of the simplification Zinc hydrometallurgy process, wherein the residual acid concentration for controlling Oxidation Leaching is 60 ~ 70g/L.
The method of the simplification Zinc hydrometallurgy process, wherein control neutralize when, initial pH be 1.0, terminal pH be 2.4 ~
2.6。
The method of the simplification Zinc hydrometallurgy process, wherein control goethite sink iron when, initial pH be 3.5 ~ 4.0, eventually
Point pH is 2.5.
Advantageous effect：High temperature high acidic oils section and reducing leaching section are merged into a procedure by the present invention, shorten technique
Flow and reaction time, the Fe generated using flow itself under conditions of not adding other oxidants additionally3+As oxidant,
Oxidation Leaching is carried out to the complete ZnS concentrate of unreacted in reducing leaching slag and sulfur-bearing metallic compound, improves valuable metal leaching
Extracting rate.The present invention solve conventional wet lay leach flow slag rate it is big, pyrogenic attack problem of high cost, at the same solve reinforcing leaching
The problem of going out long flow path.
Description of the drawings
Fig. 1 is a kind of flow chart of the method preferred embodiment of simplified Zinc hydrometallurgy process of the present invention.
Specific implementation mode
The present invention provides a kind of method of simplified Zinc hydrometallurgy process, to make the purpose of the present invention, technical solution and effect
Clearer, clear, the present invention is described in more detail below.It should be appreciated that specific embodiment described herein is only
To explain the present invention, it is not intended to limit the present invention.
A kind of method of simplified Zinc hydrometallurgy process provided by the present invention comprising：
Step 1（Neutrality leaches）, zinc roasting mine be subjected to neutral leach obtain middle immersion liquid and middle phase analysis；
Step 2（Hot acid leaches）, by the middle phase analysis that step 1 obtains be added to containing in acid waste liquid carry out hot acid leaching, obtain
To pickle liquor and acid leaching residue；
Step 3（Reducing leaching）, acid leaching residue and ZnS concentrate that step 2 obtains be added to containing being gone back in acid waste liquid
Original leaches, liquid and reducing slag after being restored；
Step 4（It neutralizes）, zinc roasting mine will be added in liquid after reduction that step 3 obtains make neutralizer, obtain neutralizing slag and
Neutralizer neutralizes two hot acid of slag return to step and leaches；
Step 5（Oxidation Leaching）, the reducing slag that step 3 obtains be added in the pickle liquor in step 2 aoxidize
It leaches, obtains Oxidation Leaching liquid and lead silver sulphur slag, Oxidation Leaching liquid returns to step 3 reducing leaching；
Step 6（Goethite sinks iron）, the neutralizer that obtains step 4 be added in zinc roasting mine and carry out goethite and sink iron, obtain
Liquid and goethite slag after to heavy iron.
The present invention uses processing zinc under the conditions of high temperature low acid to roast mine, the pickle liquor leached using hot acid（Containing Fe3+）
Oxidant is made, the reaction time of whole flow process is shortened, leached mud rate is reduced and slag contains zinc, recovery rate of valuable metals of the present invention
Height, cost recovery are low, and processing procedure environmental protection, environmental pollution are small.
Involved in the present invention to key reaction principle have：
(1)
(2)
(3)
(4)
(5)
(6)
(7)
(8)
The reducing leaching of the present invention（Step 3）In the process, temperature chooses 85 ~ 90 DEG C.It is 1.2 that coefficient, which is added, in ZnS concentrate.
Oxidation Leaching section (step 5) temperature chooses 85 ~ 90 DEG C, and pickle liquor is added, and utilizes the Fe in pickle liquor3+As
Oxidant comes ZnS concentrate superfluous in redox slag and sulfur-bearing metallic compound, contains zinc to reduce lead silver sulphur slag, reduces metal
Loss amount.Find acidity to Oxidation Leaching effect unobvious, preceding liquid Fe in experiment3+Concentration has certain influence to oxidation effectiveness, examination
Test middle guarantee Fe3+Amount is superfluous at least 2 times of the concentrate theoretical amount of reduction.
Specifically, as shown in Figure 1, in step 1, first by electrolysis waste solution（Also can claim to contain acid waste liquid）It is refined with wet method
Zinc mixed liquor in mass ratio 2:The whole acidacidity of liquid after control mixes after 1 ratio mixing（I.e. last acid concentration）For 30-
80g/L（Such as 50g/L）, Fe2+< 0.1g/L, are subsequently placed in storage tank, and liquid after obtained mixing and zinc are roasted mine（Roasting i.e. in figure
Mine）It is added slowly together reactive tank（Have " crystal seed "）, adjust pH values of pulp 2.5 and be passed through oxygen reaction 40min, 40min times
Liquid roasts mine, entire neutrality Leach reaction time 2h with zinc after inside adding the mixing of specified quantity, and temperature is 65-70 DEG C（Such as 68
℃）, terminal pH controls 4.0-4.2（Such as 4.0）, ore pulp progress solid-liquor separation, obtains neutral leachate after reaction（Middle leaching
Liquid）And underflow（Middle phase analysis）, neutral leachate send cleaning procedure to handle, and underflow carries out hot acid leaching.
In step 2, the underflow that step 1 is obtained is by liquid-solid ratio 10-12:1（Such as 11:1）Ratio be added to electrolysis
Waste liquid（I.e. new contains acid waste liquid）In, control beginning acidacidity（Acid concentration when starting）160-180g/L（Such as 170g/L）, instead
It is 85-90 DEG C to answer temperature（Such as 88 DEG C）, reaction time 3h, whole acidacidity（I.e. last acid concentration can also claim residual acid concentration）：
70-80g/L（Such as 75 g/L）, ore pulp progress solid-liquor separation, obtains hot acid leachate after reaction（Pickle liquor）And underflow（Acid
Phase analysis）, hot acid leachate be left in advance Oxidation Leaching section use, underflow carry out reducing leaching.
In step 3, the underflow that step 2 is obtained is by liquid-solid ratio 10:1 ratio is added to electrolysis waste solution（New contains
Acid waste liquid）In, while required ZnS concentrate are added by theoretical calculation, control ZnS concentrate addition coefficient of excess is 1.2（Press matter
For amount than meter, addition is 1.2 times of theoretical amount）, 85-90 DEG C of reaction temperature（85℃）, reaction time 3-4h（Such as 3h）, acid is sour eventually
Degree：50-60g/L（55g/L）, ore pulp progress solid-liquor separation, obtains reducing leaching liquid after reaction（Liquid after reduction）And underflow
（Reducing slag can also claim reducing leaching slag）, reducing leaching liquid be left in advance neutralizing zone use, underflow carry out Oxidation Leaching.
Liquid avoided when neutralization test the generation of alum, liquid Fe after control reduction after consideration reduction3+< 2g/L.
In step 4, reducing leaching liquid and zinc roasting mine that step 3 obtains are added slowly together reactive tank（Have " brilliant
Kind "）In, control pH1.0 reacts 5min, and 10min, terminal pH2.4-2.6 are then reacted under the conditions of pH2.0（Such as 2.5）, then
The reaction was continued（85-90 DEG C of temperature, such as 87 DEG C）, total time 1h is reacted, ore pulp carries out solid-liquor separation after reaction, is neutralized
Liquid and underflow（Neutralize slag）, neutralizer is left in advance hydrolyzes heavy iron section use, and underflow carries out hot acid leaching back to hot acid extracting stage.
In step 5, the underflow that step 3 is obtained is by liquid-solid ratio 10-8:1（Such as 9:1）Ratio be added step 2 production
In the hot acid leachate gone out, 85-90 DEG C of controlling reaction temperature（Such as 86 DEG C）, reaction time 3-4h（Such as 3h）, whole acidacidity：60-
70g/L（65 g/L）, ore pulp progress solid-liquor separation, obtains Oxidation Leaching liquid and underflow after reaction, and Oxidation Leaching liquid returns
It is used to reducing leaching section, lead silver sulphur slag is obtained by filtration in underflow, is sold outside as byproduct.
In step 6, neutralizer and zinc roasting mine that step 4 obtains are added slowly together reactive tank（Have " crystal seed "）
In, control pH3.5-4.0（Such as 3.6）, while it being passed through oxygen reaction 60min, neutralizer and required zinc roasting mine are during which added, is continued
It is passed through liquid Fe after Oxygen control2+< 2.5g/L can stop reacting, terminal pH2.4-2.6（Such as 2.5）, 85-90 DEG C of reaction temperature
（Such as 87 DEG C）, ore pulp progress solid-liquor separation, obtains liquid after heavy iron after reaction（Liquid after hydrolyzing）With goethite slag（Hydrolyze
Slag）, liquid returns to neutral extracting stage and cooks mixed liquor use after heavy iron（That is step 1）, sell outside goethite slag.
The specific embodiment one of step 3：Reducing leaching is carried out under the conditions of 80 DEG C to acid leaching residue and Oxidation Leaching liquid to obtain
Liquid after reducing slag and reduction, wherein in 4 hours reaction time, it is 1.5 that coefficient, which is added, in ZnS concentrate, liquid Fe after reduction3+Concentration
0.53g/L, acidity（H+）For 81.6g/L.
The specific embodiment two of step 3：Reducing leaching is carried out under the conditions of 85 DEG C to acid leaching residue and Oxidation Leaching liquid to obtain
Liquid after reducing slag and reduction, wherein in 3 hours reaction time, it is 1.3 that coefficient, which is added, in ZnS concentrate, liquid Fe after reduction3+Concentration
2.26g/L acidity（H+）For 74.25g/L.
The specific embodiment three of step 3：Reducing leaching is carried out under the conditions of 90 DEG C to acid leaching residue and Oxidation Leaching liquid to obtain
Liquid after reducing slag and reduction, wherein in 2 hours reaction time, it is 1.2 that coefficient, which is added, in ZnS concentrate, liquid Fe after reduction3+Concentration
2.02g/L acidity（H+）For 65.25g/L.
Increase ZnS concentrate and coefficient, liquid Fe after reduction is added3+Much < 2g/L, but the problem is that be added excessive
ZnS, subsequent oxidation extracting stage such as not enough Fe3+Excessive ZnS is aoxidized, there can be lead silver sulphur slag and ask containing zinc is high
Topic, therefore, coefficient is added in ZnS concentrate is advisable for 1.2~1.3.
In the above embodiments, iron reduction rate and recovery time are greatly improved both relative to the prior art.
The present invention uses the metallurgical mode of enhanced leaching, and conventional leached mud rate is reduced to 15% from 50%, is greatly reduced
Slag rate, to reduce pyrogenic process Slag treatment cost.The present invention is innovatively by high temperature high acidic oils and reducing leaching two procedures
A procedure is merged into, in the case where not adding other additives, utilizes the Fe of flow itself generation3+As oxidant, adopt
Fe is restored with zinc concentrate3+It avoids the generation of alum and realizes that the reaction was complete, to improve the leaching of roasting mine, Zinc in Zinc Concentrates, copper, indium
Rate, reduce acidleach, Oxidation Leaching, reducing leaching each process acidity, with improve equipment service life and reduce maintenance cost.
It solves the long flow path of enhanced leaching, occur that alum, slag rate be larger, indium leaching to the inadaptability of high ferro, high silicon raw material, leaching process
The low equal a series of problems of extracting rate.
In conclusion the present invention is for Zinc hydrometallurgy process long flow path in prior art, tedious process, energy consumption is big, equipment
Perishable, valuable metal loses the problems such as big, in such a way that enhanced leaching is metallurgical, substantially reduces the wet-leaching quantity of slag, reduces
Pyrogenic process Slag treatment cost shortens Zinc hydrometallurgy process flow, improves service life of equipment, reduces valuable metal loss.The present invention
Method is easy to operate, and technique is easily controllable, the oxidant generated using flow itself in the case where not adding other additives
Achievable valuable metal maximumlly recycles.
It should be understood that the application of the present invention is not limited to the above for those of ordinary skills can
With improvement or transformation based on the above description, all these modifications and variations should all belong to the guarantor of appended claims of the present invention
Protect range.
Claims (2)
1. a kind of method of simplified Zinc hydrometallurgy process, which is characterized in that including：
Step 1: zinc roasting mine, which is carried out neutral leach, obtains neutral leachate and neutral phase analysis；
Step 2: being added to the neutral phase analysis that step 1 obtains containing hot acid leaching is carried out in acid waste liquid, pickle liquor and acid are obtained
Phase analysis；
Step 3: being added to the acid leaching residue and ZnS concentrate that step 2 obtains containing reducing leaching is carried out in acid waste liquid, restored
Liquid and reducing slag afterwards；
Step 4: making neutralizer by zinc roasting mine is added in liquid after reduction that step 3 obtains, obtains neutralizing slag and neutralizer, neutralize
Two hot acid of slag return to step leaches；
Oxidation Leaching is carried out Step 5: the reducing slag that step 3 obtains is added in the pickle liquor in step 2, is aoxidized
Leachate and lead silver sulphur slag, Oxidation Leaching liquid return to step 3 reducing leaching；
Step 6: the neutralizer that step 4 is obtained, which is added in zinc roasting mine, carries out the heavy iron of goethite, liquid and needle iron after heavy iron are obtained
Slag;
The Fe of liquid after control reduction3+< 2g/L；
It is 1.2~1.3 that coefficient, which is added, in ZnS concentrate；
In step 1, acid waste liquid and zinc hydrometallurgy mixed liquor in mass ratio 2 will be contained first:Mixing is controlled after 1 ratio mixing
The whole acidacidity of liquid is 30-80g/L, Fe afterwards2+< 0.1g/L, are subsequently placed in storage tank, and liquid after obtained mixing and zinc are roasted mine
It is added slowly together the reactive tank of crystal seed, pH values of pulp 2.5 is adjusted and is passed through oxygen and react 40min, 40min is added in the time
Liquid roasts mine, entire neutrality Leach reaction time 2h with zinc after the mixing of specified quantity, and temperature is 65-70 DEG C, terminal pH controls
4.0-4.2, ore pulp progress solid-liquor separation, obtains neutral leachate and neutral phase analysis after reaction, and neutral leachate send purification
Process processing, neutral phase analysis carry out hot acid leaching；
In step 2, the neutral phase analysis that step 1 is obtained is by liquid-solid ratio 10-12:1 ratio is added to containing in acid waste liquid, is controlled
Beginning acidacidity 160-180g/L processed, reaction temperature are 85-90 DEG C, reaction time 3h, whole acidacidity 70-80g/L, after reaction
Ore pulp carries out solid-liquor separation, obtains pickle liquor and acid leaching residue, and pickle liquor is left to the use of Oxidation Leaching section in advance, and acid leaching residue is restored
It leaches；
In step 3, the acid leaching residue that step 2 is obtained is by liquid-solid ratio 10:1 ratio be added to it is new containing in acid waste liquid, together
When by theoretical calculation be added needed for ZnS concentrate, control ZnS concentrate addition coefficient of excess is 1.2,85-90 DEG C of reaction temperature, instead
3-4h between seasonable, whole acidacidity：50-60g/L, after reaction ore pulp carry out solid-liquor separation, liquid and reducing slag after being restored,
Liquid is left to neutralizing zone use in advance after reduction, and reducing slag carries out Oxidation Leaching；
In step 4, liquid after reduction that step 3 obtains and zinc roasting mine are added slowly together in the reactive tank of crystal seed,
It controls pH1.0 and reacts 5min, 10min is then reacted under the conditions of pH2.0, terminal pH2.4-2.6 then proceedes to react, temperature
It is 85-90 DEG C, reacts total time 1h, ore pulp carries out solid-liquor separation after reaction, obtains neutralizer and neutralizes slag, neutralizer is pre-
It is left to the heavy iron section of hydrolysis to use, neutralizes slag and carry out hot acid leaching back to hot acid extracting stage；
In step 5, the reducing slag that step 3 is obtained is by liquid-solid ratio 10-8:The pickle liquor of step 2 output is added in 1 ratio
In, 85-90 DEG C of controlling reaction temperature, reaction time 3-4h, whole acidacidity：60-70g/L, ore pulp progress liquid is solid after reaction
Separation obtains Oxidation Leaching liquid and lead silver sulphur slag, and Oxidation Leaching liquid is used back to reducing leaching section, and lead silver sulphur slag is obtained by filtration
Lead silver sulphur slag；
In step 6, neutralizer and zinc roasting mine that step 4 obtains are added slowly together in the reactive tank of crystal seed, controlled
PH3.5-4.0 processed, while it being passed through oxygen reaction 60min, neutralizer and required zinc roasting mine are during which added, continues to be passed through Oxygen control
Liquid Fe afterwards2+< 2.5g/L stop reaction, and terminal pH2.4-2.6,85-90 DEG C of reaction temperature, ore pulp progress liquid is solid after reaction
Separation obtains liquid and goethite slag after heavy iron, and liquid cooks mixed liquor use back to neutral extracting stage after heavy iron.
2. the method for simplified Zinc hydrometallurgy process according to claim 1, which is characterized in that control goethite sink iron when,
Initial pH is 3.5 ~ 4.0, and terminal pH is 2.5.
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