CN105779771A - Method for recycling valuable metal in zinc smelting sludge - Google Patents
Method for recycling valuable metal in zinc smelting sludge Download PDFInfo
- Publication number
- CN105779771A CN105779771A CN201610172381.0A CN201610172381A CN105779771A CN 105779771 A CN105779771 A CN 105779771A CN 201610172381 A CN201610172381 A CN 201610172381A CN 105779771 A CN105779771 A CN 105779771A
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- CN
- China
- Prior art keywords
- mud
- valuable metal
- sludge
- zinc abstraction
- zinc
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Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid 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
- C22B19/30—Obtaining zinc or zinc oxide from metallic residues or scraps
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a method for recycling valuable metal in zinc smelting sludge. The method comprises the steps that sludge of a zinc smelting system and tap water are mixed and then put into an ultrasonic device to be subjected to ultrasonic vibration, and sludge clinker is obtained; the sludge clinker and a dilute acid solution are mixed and then put into a pressurization reaction kettle, the reaction temperature and the reaction time are controlled, valuable metal ions are dissolved out, and clean sludge is obtained; the clean sludge is put into a plate filter pressing device, a filter aid is added, the clean sludge is filtered and dried after cleaning, and sludge powder with the water content lower than 5% is obtained; and reaction liquid obtained after filtering returns to the zinc smelting system to be purified and electrolyzed, and zinc metal is obtained through recycling. The sludge powder obtained through the method can be used for producing cement products or glass ceramics which are high in performance, contained heavy metal ions can all return to a zinc electrolysis system, and harmless, minimal and resourceful utilization of dangerous waste zinc smelting sludge can be thoroughly achieved. The method is simple, feasible, high in environmental protection benefit and production efficiency, less in equipment investment and low in energy consumption.
Description
Technical field
The invention belongs to metallurgical technology changing rejected material to useful resource, innoxious process for treating field, be specifically related to a kind of reclaim the method for valuable metal in zinc abstraction mud.
Background technology
The solid waste and the use waste material kind that produce in plumbous zinc industry selecting and purchasing smelting process are many, in " National Hazard refuse register " (version in 2008), 20 kinds of lead-zinc smelting refuses of clear stipulaties are hazardous waste, and the wastewater treatment mud produced in Lead-Zinc Sintering Process is hazardous waste (refuse code: 331-022-48).In lead, Making Acid in Zhuzhou Smelter process, adopt pickling spray process to gas cleaning.This operation produces substantial amounts of waste acid, and waste acid usually contains sulphuric acid, sulfurous acid, lead, zinc, hydrargyrum, arsenic, fluorine etc..Major part enterprise adopts the method such as lime method, Calx iron salt method two sections that this waste acid is processed at present, it may be achieved the qualified discharge of waste water.In said method processing procedure, substantial amounts of gypsum tailings and wastewater treatment mud can be produced.These wastewater treatment mud contain moisture 25% ~ 55%, and the Zn content in mud is 5% ~ 15% simultaneously.
Along with the increase year by year of China's lead-zinc smelting yield, produce substantial amounts of lead-zinc smelting mud, if do not dealt carefully with, not only waste resource, but also contaminated environment.For this, develop a kind of method reclaiming valuable metal in zinc abstraction mud tool and be of great significance.
Summary of the invention
It is an object of the invention to provide and a kind of reclaim the method for valuable metal in zinc abstraction mud.
The object of the present invention is achieved like this, comprises the steps to realize:
(1) put in ultrasonic equipment after zinc abstraction system sludge being mixed with tap water, carry out supersonic oscillations, obtain mud grog；
(2) after the mud grog after oscillation treatment being mixed with dilute acid soln, put in compressive reaction still, control reaction temperature and response time, dissolution valuable metal ions, obtain clean mud；
(3) cleaning mud is put in plate filtering equipment, add filter aid, scrubbed rear filtration drying, obtain the moisture content mud powder lower than 5%；
(4) reactant liquor after filtering returns in zinc abstraction system, carries out purifying, electrolysis, reclaims and obtains metallic zinc.
The mud powder that the present invention obtains can be used for producing high performance cement products or devitrified glass, can thoroughly realize innoxious, the minimizing of hazardous waste zinc abstraction mud, recycling, and contained heavy metal ion all can return zinc electrolysis system.The method is simple, it is thus achieved that product can be applied in actual production, environmental benefit is high, and production efficiency is high, and equipment investment is few, and energy consumption is low.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described, but never in any form the present invention is any limitation as, and based on present invention teach that any conversion made, each falls within scope.
The present invention comprises the steps:
(1) put in ultrasonic equipment after zinc abstraction system sludge being mixed with tap water, carry out supersonic oscillations, obtain mud grog；
(2) after the mud grog after oscillation treatment being mixed with dilute acid soln, put in compressive reaction still, control reaction temperature, response time and reaction pressure, dissolution valuable metal ions, obtain clean mud；
(3) cleaning mud is put in plate filtering equipment, add filter aid, scrubbed rear filtration drying, obtain the moisture content mud powder lower than 5%；
(4) reactant liquor after filtering returns in zinc abstraction system, carries out purifying, electrolysis, reclaims and obtains metallic zinc.
Described zinc abstraction system sludge moisture is 25% ~ 55%, and the Zn content in mud is 5% ~ 15%.
The supersonic oscillations frequency of described step (1) is 15 ~ 80kHz, and the supersonic oscillations time is 10 ~ 60min.
The diluted acid of described step (2) is one or several mixing of sulphuric acid, hydrochloric acid, nitric acid, aqueous acetic acid；The concentration of sulphuric acid is 1 ~ 35g/L, and the concentration of hydrochloric acid is 1 ~ 20g/L, and concentration of nitric acid is 1 ~ 50g/L, and the concentration of acetic acid is 1 ~ 40g/L；The weight liquid-solid ratio of mud grog and dilute acid soln is 1 ~ 20:1.
The reaction temperature of described step (2) is 90 ~ 180 DEG C, and the response time is 1 ~ 4h, and reaction pressure is 0.1 ~ 3MPa.
The material of the compressive reaction still of described step (2) adopts Hastelloy.
The number of times of the washing of described step (3) is 3-5 time.
The filter plant of described step (3) is the one in filter press, band filter, Tao Shi filter.
The drying equipment of described step (3) is microwave drier, and its frequency range is 300GHz-3GHz, and the time that microwave field processes is 1-10min.
The mixture that filter aid is fatty alcohol-polyoxyethylene ether, alkylphenol polyoxyethylene of described step (3).
Embodiment 1
The content of zinc abstraction sludge water content is 63.56%, and the content of zinc is 8.94%.
Being loaded in homemade supersonic oscillations system by zinc abstraction mud, maintenance ultrasonic frequency is 80kHz, and the time of ultrasonic Treatment is 30min, obtains mud grog.The sulfuric acid solution of mud grog and 30g/L puts in Hastelloy pressure leaching tank according to weight liquid-solid ratio 1:10 simultaneously, keeps reaction temperature 160 DEG C, and pressure is 1.5MPa, is incubated 3h.Subsequently the zinc mud after pickling is imported in filter press and wash 4 times with clear water, add filter aid according to the amount of 50g/ ton simultaneously, and carry out filter pressing, it is achieved solid-liquor separation.Spent acid after separation is directly entered the cleaning system of zinc abstraction.Solid phase after separation enters microwave drier, and control frequency is 100GHz, and the process time is 10min.Just the moisture content clean mud lower than 5% can be obtained.
Result of implementation: in mud powder, zinc concentration is less than 0.005%, lower than the higher limit of hazardous waste.
Embodiment 2
The content of zinc abstraction sludge water content is 57.58%, and the content of zinc is 9.45%.
Being loaded in homemade supersonic oscillations system by zinc abstraction mud, maintenance ultrasonic frequency is 50kHz, and the time of ultrasonic Treatment is 20min, obtains mud grog.The hydrochloric acid solution of mud grog and 10g/L puts in Hastelloy pressure leaching tank according to weight liquid-solid ratio 1:5 simultaneously, keeps reaction temperature 130 DEG C, and pressure is 2.0MPa, is incubated 2h.Subsequently the zinc mud after pickling is imported in band filter and wash 5 times with clear water, add filter aid according to the amount of 80g/ ton simultaneously, and carry out filter pressing, it is achieved solid-liquor separation.Spent acid after separation is directly entered the cleaning system of zinc abstraction after ion exchange system processes.Solid phase after separation enters microwave drier, and control frequency is 150GHz, and the process time is 50min.Just the moisture content clean mud lower than 5% can be obtained.
Result of implementation: in mud powder, zinc concentration is less than 0.003%, lower than the higher limit of hazardous waste.
Embodiment 3
The content of zinc abstraction sludge water content is 48.76%, and the content of zinc is 7.34%.
Being loaded in homemade supersonic oscillations system by zinc abstraction mud, maintenance ultrasonic frequency is 70kHz, and the time of ultrasonic Treatment is 30min, obtains mud grog.The mixture (1:1) of the hydrochloric acid solution of mud grog and 5g/L and the sulfuric acid solution of 20g/L puts in Hastelloy pressure leaching tank according to weight liquid-solid ratio 1:8 simultaneously, keeps reaction temperature 180 DEG C, and pressure is 1.0MPa, is incubated 2.5h.Subsequently the zinc mud after pickling is imported in ceramic filter and wash 3 times with clear water, add filter aid according to the amount of 860g/ ton simultaneously, and carry out filter pressing, it is achieved solid-liquor separation.Spent acid after separation is directly entered the cleaning system of zinc abstraction after ion exchange system processes.Solid phase after separation enters microwave drier, and control frequency is 120GHz, and the process time is 30min.Just the moisture content clean mud lower than 5% can be obtained.
Result of implementation: in mud powder, zinc concentration is less than 0.006%, lower than the higher limit of hazardous waste.
Claims (10)
1. one kind is reclaimed the method for valuable metal in zinc abstraction mud, it is characterised in that comprise the steps:
(1) put in ultrasonic equipment after zinc abstraction system sludge being mixed with tap water, carry out supersonic oscillations, obtain mud grog；
(2) after the mud grog after oscillation treatment being mixed with dilute acid soln, put in compressive reaction still, control reaction temperature, response time and reaction pressure, dissolution valuable metal ions, obtain clean mud；
(3) cleaning mud is put in plate filtering equipment, add filter aid, scrubbed rear filtration drying, obtain the moisture content mud powder lower than 5%；
(4) reactant liquor after plate filter pressing returns in zinc abstraction system, carries out purifying, electrolysis, reclaims and obtains metallic zinc.
2. the method for valuable metal in recovery zinc abstraction mud according to claim 1, it is characterised in that the described moisture in zinc abstraction system sludge is 25% ~ 55%, and the Zn content in mud is 5% ~ 15%.
3. the method for valuable metal in recovery zinc abstraction mud according to claim 1, it is characterised in that the supersonic oscillations frequency of described step (1) is 15 ~ 80kHz, and the supersonic oscillations time is 10 ~ 60min.
4. the method for valuable metal in recovery zinc abstraction mud according to claim 1, it is characterised in that the diluted acid of described step (2) is one or several mixing of sulphuric acid, hydrochloric acid, nitric acid, aqueous acetic acid；The concentration of sulphuric acid is 1 ~ 35g/L, and the concentration of hydrochloric acid is 1 ~ 20g/L, and concentration of nitric acid is 1 ~ 50g/L, and the concentration of acetic acid is 1 ~ 40g/L；The weight liquid-solid ratio of mud grog and dilute acid soln is 1 ~ 20:1.
5. the method for valuable metal in recovery zinc abstraction mud according to claim 1, it is characterised in that the reaction temperature of described step (2) is 90 ~ 180 DEG C, and the response time is 1 ~ 4h, and reaction pressure is 0.1 ~ 3MPa.
6. the method for valuable metal in recovery zinc abstraction mud according to claim 1, it is characterised in that the material of the compressive reaction still of described step (2) adopts Hastelloy.
7. the method for valuable metal in recovery zinc abstraction mud according to claim 1, it is characterised in that the number of times of the washing of described step (3) is 3-5 time.
8. the method for valuable metal in recovery zinc abstraction mud according to claim 1, it is characterised in that the filter plant of described step (3) is the one in filter press, band filter, Tao Shi filter.
9. the method for valuable metal in recovery zinc abstraction mud according to claim 1, it is characterised in that the drying equipment of described step (3) is microwave drier, and its frequency range is 300GHz-3GHz, the time that microwave field processes is 1-10min.
10. the method for valuable metal in recovery zinc abstraction mud according to claim 1, it is characterised in that the mixture that filter aid is fatty alcohol-polyoxyethylene ether, alkylphenol polyoxyethylene of described step (3).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610172381.0A CN105779771A (en) | 2016-03-24 | 2016-03-24 | Method for recycling valuable metal in zinc smelting sludge |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610172381.0A CN105779771A (en) | 2016-03-24 | 2016-03-24 | Method for recycling valuable metal in zinc smelting sludge |
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| Publication Number | Publication Date |
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| CN105779771A true CN105779771A (en) | 2016-07-20 |
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| CN201610172381.0A Pending CN105779771A (en) | 2016-03-24 | 2016-03-24 | Method for recycling valuable metal in zinc smelting sludge |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1286315A (en) * | 1999-08-26 | 2001-03-07 | 徐欣 | Process for comprehensive utilization of blast furnace top gas mud containing Zn |
| JP2011230074A (en) * | 2010-04-28 | 2011-11-17 | Hamada Heavy Industries Ltd | Method of treating wet dust generated in blast furnace |
| CN102912138A (en) * | 2012-10-19 | 2013-02-06 | 湖南有色金属研究院 | Method of recycling zinc, manganese, lead and silver from zinc electrowinning anode mud |
| CN103352127A (en) * | 2013-04-07 | 2013-10-16 | 昆明理工大学 | Method for recovering zinc from zinc flue dust leaching residue through ultrasonic wave assistance |
| CN105417908A (en) * | 2015-12-22 | 2016-03-23 | 云南省固体废物管理中心 | Method for harmlessly treating lead and zinc smelting sludge |
-
2016
- 2016-03-24 CN CN201610172381.0A patent/CN105779771A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1286315A (en) * | 1999-08-26 | 2001-03-07 | 徐欣 | Process for comprehensive utilization of blast furnace top gas mud containing Zn |
| JP2011230074A (en) * | 2010-04-28 | 2011-11-17 | Hamada Heavy Industries Ltd | Method of treating wet dust generated in blast furnace |
| CN102912138A (en) * | 2012-10-19 | 2013-02-06 | 湖南有色金属研究院 | Method of recycling zinc, manganese, lead and silver from zinc electrowinning anode mud |
| CN103352127A (en) * | 2013-04-07 | 2013-10-16 | 昆明理工大学 | Method for recovering zinc from zinc flue dust leaching residue through ultrasonic wave assistance |
| CN105417908A (en) * | 2015-12-22 | 2016-03-23 | 云南省固体废物管理中心 | Method for harmlessly treating lead and zinc smelting sludge |
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Application publication date: 20160720 |
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