CN105441685A - Method for recycling valuable metals in peracid waste fluid produced during copper anode mud treating process - Google Patents

Method for recycling valuable metals in peracid waste fluid produced during copper anode mud treating process Download PDF

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Publication number
CN105441685A
CN105441685A CN201510995426.XA CN201510995426A CN105441685A CN 105441685 A CN105441685 A CN 105441685A CN 201510995426 A CN201510995426 A CN 201510995426A CN 105441685 A CN105441685 A CN 105441685A
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arsenic
copper
slag
reaction
acid
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CN201510995426.XA
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CN105441685B (en
Inventor
柴立元
王庆伟
蒋国民
胡明
史美清
杨志辉
高伟荣
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Thiessens environmental Limited by Share Ltd
Central South University
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CHANGSHA SCIENCE ENVIRONMENTAL TECHNOLOGY Co Ltd
Central South University
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working 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
    • C22B7/006Wet processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B11/00Obtaining noble metals
    • C22B11/04Obtaining noble metals by wet processes
    • C22B11/042Recovery of noble metals from waste materials
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B15/00Obtaining copper
    • C22B15/0063Hydrometallurgy
    • C22B15/0084Treating solutions
    • C22B15/0089Treating solutions by chemical methods
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B19/00Obtaining zinc or zinc oxide
    • C22B19/30Obtaining zinc or zinc oxide from metallic residues or scraps
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00Obtaining nickel or cobalt
    • C22B23/04Obtaining nickel or cobalt by wet processes
    • C22B23/0453Treatment or purification of solutions, e.g. obtained by leaching
    • C22B23/0461Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B25/00Obtaining tin
    • C22B25/06Obtaining tin from scrap, especially tin scrap
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B30/00Obtaining antimony, arsenic or bismuth
    • C22B30/06Obtaining bismuth
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The invention discloses a method for recycling valuable metals in a peracid waste fluid produced during a copper anode mud treating process. The method mainly comprises the following steps: (1), selectively absorbing rare and precious metals such as gold, silver, platinum, palladium and the like; (2), carrying out diffusing and dialysis separation for recovering acid; (3), neutralizing and hydrolyzing to recover bismuth oxide chloride; (4), separating copper from arsenic to recover copper; (5), efficiently vulcanizing and deeply removing arsenic; (6), recovering metals such as zinc, nickel, tin and the like through a neutralization method; and (7), after neutralization, adopting multiple-effect evaporation for recovering salt from high salinity wastewater. The method provided by the invention achieves efficient separation and deep recycling to rare and precious metals, base metals, arsenic and acid, and achieves recycling of valuable elements and elimination of the harmful element arsenic, the running cost is saved, and the environment risk is lowered.

Description

The method of valuable metal recovery in the high acid waste liquid that a kind of copper anode mud treating processes produces
Technical field
The invention belongs to metallurgical engineering and environmental engineering crossing domain, be specifically related to a kind of method reclaiming valuable metal in the high acid waste liquid of copper anode mud treating processes generation.
Background technology
In Copper making process, create a certain amount of insolubles when electrorefining, be copper anode mud.Copper anode cement copper arsenic content is higher, simultaneously containing a large amount of valuable metals, is the important source material extracting the precious metal such as gold and silver and platinum.At present, most smelting enterprise all adopts the technique of high temperature pyrogenic process roasting to extract the precious metal in the anode sludge, therefore in pyrogenic process process, creates a large amount of flue gas during smeltings, defines the high acid waste liquid of washing after washing with water of flue gas.Washing peracid component of effluent is complicated, copper arsenic and acidity higher, also have a certain amount of valuable metal simultaneously.High owing to washing high acid waste liquid acidity, complicated component, has to pass through further process and just can arrange outward, otherwise can cause serious environmental pollution, and can cause the loss in vain of acid wherein and valuable metal.
At present, the method for the high acid waste liquid of domestic process mainly contains limestone vegetation method, in and ?molysite coprecipitation method and sulfuration method.Limestone vegetation method adds lime directly in high acid waste liquid, in and ?molysite method be add molysite on the basis regulating peracid waste liquor PH, sulfuration method adds vulcanizing agent as sodium sulphite, hydrogen sulfide etc. directly in high acid waste liquid.Above-mentioned three kinds of methods all can reach good arsenic removal removing heavy metals effect.But in scavenging process, the valuable metal in high acid waste liquid is sunken in waste residue together, waste residue amount is large, and valuable metal grade is low, causes being difficult to reclaim, and enterprise all makes landfill disposal, causes the waste of resource.Meanwhile, the acid in high acid waste liquid is not also reclaimed, and have lost a large amount of acid, increases the production cost of enterprise.Therefore, the recovery how realizing valuable metal and acid from the high acid waste liquid of the washing of copper anode mud smoke treatment is a great problem that enterprise needs to solve.
Summary of the invention
The present invention is directed in the high acid waste liquid of washing of copper anode mud smoke treatment valuable metal and acid cannot efficient recovery, causes the defect of serious waste of resources, provides a kind ofly to wash the method reclaiming valuable metal and acid in high acid waste liquid.After process of the present invention, wash the rare precious metals such as the Gold, Silver, Platinum, Palladium in high acid waste liquid, the metals such as copper, bismuth, nickel, tin, zinc, harmful element arsenic and acid all achieve recovery.
A method for valuable metal recovery in the high acid waste liquid that copper anode mud treating processes produces, comprises the following steps:
(1) high acid waste liquid successively enters quartz sand and the cotton metre filter of PP, and aperture is 0.5-10 μm, and filtrate enters selective adsorption tank and carries out rare precious metal adsorption and enrichment;
(2) spent acid after absorption rare precious metal and heavy metal is separated by diffusion dialysis;
(3) adopt neutralizing agent to neutralize containing the stoste of heavy metal after diffusion dialysis, after solid-liquid separation, obtain bismuth oxychloride slag;
(4) step (3) filtrate adds red arsenic or arsenic sulfide slag, carries out the separation of copper arsenic, obtains sulfuration copper ashes after solid-liquid separation;
(5) copper arsenic be separated after liquid add vulcanizing agent and carry out deeply removing arsenic, obtain arsenic sulfide slag after solid-liquid separation, arsenic sulfide slag is back to step (4);
(6) step (5) filtrate adopts neutralizing agent neutralization, reclaims slag and comprises nickel, zinc, tin at interior heavy metal element, and after neutralization is separated, salt is reclaimed in the crystallization of liquid multiple-effect evaporation, and recycling condensing water is in system.
Extraordinary sorbing material is filled in selective adsorption tank in step (1), comprise: one or more in gac, strongly basic anion exchange resin, resin, coutroi velocity is 5 ~ 20BV/h, and temperature is 25 ~ 60 DEG C, adsorbs one or more in gold and silver, platinum.
In step (2), the condition of diffusion dialysis is coutroi velocity 7 ~ 15cm/h, and temperature is 25 ~ 60 DEG C.
In controlling in step (3) and pH value be 0.5 ~ 3, temperature of reaction is 40 ~ 90 DEG C, and the reaction times is 10 ~ 30min.
In step (4) according to As/Cu mol ratio be 1 ?the ratio of 5:1 add red arsenic or arsenic sulfide slag.Step (4) copper arsenic separating reaction condition is temperature of reaction 50 ~ 90 DEG C, and the reaction times is 0.5 ~ 3h.
In step (5), vulcanizing agent is one or more in hydrogen sulfide, Sodium sulfhydrate, sodium sulphite, barium sulphide, sulfurated lime.The ratio being 1-10 according to S/As mol ratio adds vulcanizing agent.
Neutralizing agent in step (3) (6) is NaOH, Na 2cO 3, NaHCO 3, CaO, CaCO 3, MgO, MgCO 3, one or more in carbide slag, the pH scope of neutralization is 5.50 ~ 9.50.
Multiple-effect evaporation described in step (6) is triple effect evaporation or MVR evaporation, and evaporator material used is titanium alloy or titanium composite panel.
Beneficial effect of the present invention
1, by incorporating selectively sorbing material, rare precious metal in the spent acid produced in antianode mud treating processes carries out effective separation and consentration, has fully reclaimed the high added value component in spent acid, process cleans, non-secondary pollution, process is efficient, reclaims considerable benefit.
2, by the introducing of diffusion dialysis membrane technique, for the recovery of bismuth creates condition, a large amount of consumption of reclaiming neutralizing agent in bismuth process are avoided, with the generation of slag in decreasing, improve the grade reclaiming slag, reclaimed the acid in high acid waste liquid simultaneously, and reduced running cost.
3, neutralizing experiment is adopted to reclaim bismuth, the rate of recovery of bismuth is higher than traditional method, and purity is higher, better can realize being separated of bismuth and copper arsenic, simultaneously by vulcanized slag circumfluence method high efficiency separation copper arsenic, achieve effectively being separated of copper and arsenic, classification is achieved to valuable resource and reclaims, decrease subsequent disposal operation, successful.
4, after process of the present invention, the rare precious metals such as the Gold, Silver, Platinum, Palladium in high acid waste liquid, the metals such as copper, bismuth, nickel, tin, zinc, harmful element arsenic and acid all achieve recovery.
Accompanying drawing explanation
Fig. 1 present invention process schema.
Embodiment:
Be intended to further illustrate the present invention below in conjunction with embodiment, and unrestricted the present invention.
Embodiment 1
The ANODE SLIME TREATMENT of getting certain copper smelting plant produces high acid waste liquid 500ml, H +concentration is 4.0mol/L, other principal elements and content as follows:
Table 1 ANODE SLIME TREATMENT produces high acid waste liquid principal element and concentration (g/L)
Get above-mentioned high acid waste liquid by after quartz sand and the cotton metre filter of PP, then carry out selective adsorption through the adsorption column that resin is filled, control volumetric flow rate is 10BV, and after adsorption selection, in solution, Ag is less than 0.1mg/L, and Pd is less than 0.05mg/L.After absorption, solution enters diffusion dialysis device with the flow velocity of 10m/s, and most of acid is moved into concentration compartments, and recovered acid hydrogen ion concentration is 3.4mol/L, and heavy metal ion mobility is 6%.Diffusion dialysis stoste adds sodium carbonate and carries out neutralizing hydrolysis recovery bismuth, and control ph is 3.0, temperature of reaction 50 DEG C, reaction times 30min, solid-liquid separation reclaims bismuth oxychloride slag, and in slag, bi content is 67%, in filtrate, the content of bismuth is 20mg/L, and the rate of recovery of bismuth is greater than 99%.After heavy bismuth, liquid adds arsenic sulfide slag according to As/Cu metering than for 1.2:1, reaction 30min, obtain the higher-grade sulfuration copper ashes that copper content is 50%, in filtrate, copper is less than 5mg/L, hydrogen sulfide is added than for 1.1:1 according to S/As metering, carry out vulcanization reaction, the grade of having reacted arsenic in rear slag can reach 50%, and in filtrate, the concentration of arsenic is 0.8mg/L.After deeply removing arsenic, filtrate adopts liquid caustic soda to neutralize, in and pH be 9.5, obtain zinc, nickel slag that zinc content is greater than 40%, last saline solns adopts triple-effect evaporator to evaporate, and reclaims sodium-chlor and sodium sulfate, steams Condensate reuse in system.
Embodiment 2
The ANODE SLIME TREATMENT of getting certain copper smelting plant produces high acid waste liquid 500ml, H +concentration is 4.2mol/L, other principal elements and content as follows:
Table 2 ANODE SLIME TREATMENT produces high acid waste liquid principal element and concentration (g/L)
Get above-mentioned high acid waste liquid by after quartz sand and the cotton metre filter of PP, then carry out selective adsorption through the adsorption column that resin is filled, control volumetric flow rate is 10BV, and after adsorption selection, in solution, Ag is less than 0.1mg/L, and Pd is less than 0.05mg/L.After absorption, solution enters diffusion dialysis device with the flow velocity of 10m/s, and most of acid is moved into concentration compartments, and recovered acid hydrogen ion concentration is 3.6mol/L, and heavy metal ion mobility is 5%.Diffusion dialysis stoste adds sodium carbonate and carries out neutralizing hydrolysis recovery bismuth, and control ph is 3.0, temperature of reaction 40 DEG C, reaction times 60min, solid-liquid separation reclaims bismuth oxychloride slag, and in slag, bi content is 65.7%, in filtrate, the content of bismuth is 22mg/L, and the rate of recovery of bismuth is greater than 99%.After heavy bismuth, liquid adds arsenic sulfide slag according to As/Cu metering than for 1.3:1, reaction 60min, obtain the higher-grade sulfuration copper ashes that copper content is 51.3%, in filtrate, copper is less than 5mg/L, sodium sulphite is added than for 1.2:1 according to S/As metering, carry out vulcanization reaction, the grade of having reacted arsenic in rear slag can reach 50%, and in filtrate, the concentration of arsenic is 0.8mg/L.After deeply removing arsenic, filtrate adopts liquid alkali to neutralize, in and pH be 9.0, obtain zinc, nickel slag that zinc content is greater than 41%, last saline solns adopts triple-effect evaporator to evaporate, and reclaims sodium-chlor and sodium sulfate, steams Condensate reuse in system.

Claims (10)

1. the method for valuable metal recovery in the high acid waste liquid that produces of copper anode mud treating processes, is characterized in that, comprise the following steps:
(1) high acid waste liquid successively enters quartz sand and the cotton metre filter of PP, and aperture is 0.5-10 μm, and filtrate enters selective adsorption tank and carries out rare precious metal adsorption and enrichment;
(2) spent acid after absorption rare precious metal and heavy metal is separated by diffusion dialysis;
(3) adopt neutralizing agent to neutralize containing the stoste of heavy metal after diffusion dialysis, after solid-liquid separation, obtain bismuth oxychloride slag;
(4) step (3) filtrate adds red arsenic or arsenic sulfide slag, carries out the separation of copper arsenic, obtains sulfuration copper ashes after solid-liquid separation;
(5) copper arsenic be separated after liquid add vulcanizing agent and carry out deeply removing arsenic, obtain arsenic sulfide slag after solid-liquid separation, arsenic sulfide slag is back to step (4);
(6) step (5) filtrate adopts neutralizing agent neutralization, reclaims slag and comprises nickel, zinc, tin at interior heavy metal element, and after neutralization is separated, salt is reclaimed in the crystallization of liquid multiple-effect evaporation, and recycling condensing water is in system.
2. method according to claim 1, it is characterized in that, extraordinary sorbing material is filled in selective adsorption tank in step (1), comprise: one or more in gac, strongly basic anion exchange resin, resin, coutroi velocity is 5 ~ 20BV/h, temperature is 25 ~ 60 DEG C, adsorbs one or more in gold and silver, platinum.
3. method according to claim 1, is characterized in that, in step (2), the condition of diffusion dialysis is coutroi velocity 7 ~ 15cm/h, and temperature is 25 ~ 60 DEG C.
4. method according to claim 1, is characterized in that, in controlling in step (3) and pH value be 0.5 ~ 3, temperature of reaction is 40 ~ 90 DEG C, and the reaction times is 10 ~ 30min.
5. method according to claim 1, is characterized in that, in step (4) according to As/Cu mol ratio be 1 ?the ratio of 5:1 add red arsenic or arsenic sulfide slag.
6. method according to claim 1 or 5, it is characterized in that, step (4) copper arsenic separating reaction condition is temperature of reaction 50 ~ 90 DEG C, and the reaction times is 0.5 ~ 3h.
7. method according to claim 1, is characterized in that, in step (5), vulcanizing agent is one or more in hydrogen sulfide, Sodium sulfhydrate, sodium sulphite, barium sulphide, sulfurated lime.
8. the method according to claim 1 or 7, is characterized in that, the ratio being 1-10 according to S/As mol ratio adds vulcanizing agent.
9. method according to claim 1, is characterized in that, the neutralizing agent in step (3) (6) is NaOH, Na 2cO 3, NaHCO 3, CaO, CaCO 3, MgO, MgCO 3, one or more in carbide slag, the pH scope of neutralization is 5.50 ~ 9.50.
10. method according to claim 1, is characterized in that, the multiple-effect evaporation described in step (6) is triple effect evaporation or MVR evaporation, and evaporator material used is titanium alloy or titanium composite panel.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106119547A (en) * 2016-07-20 2016-11-16 中国恩菲工程技术有限公司 A kind of method reclaiming copper in the outer waste discharge acid of Copper making system for preparing sulfuric acid
CN106566927A (en) * 2016-10-14 2017-04-19 铜陵有色金属集团股份有限公司 Efficient gradient separation recovery process for copper anode slime leachate
CN108358343A (en) * 2018-02-13 2018-08-03 武汉船用机械有限责任公司 Electroplating sewerage processing method

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CN101759250A (en) * 2009-12-31 2010-06-30 南京工业大学 Process for recovering heavy metallic salt and inorganic acid in pickling waste liquid
CN103014355A (en) * 2012-12-13 2013-04-03 马永涛 Multi-metal comprehensive recycling process for copper smelting ash

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CN101759250A (en) * 2009-12-31 2010-06-30 南京工业大学 Process for recovering heavy metallic salt and inorganic acid in pickling waste liquid
CN103014355A (en) * 2012-12-13 2013-04-03 马永涛 Multi-metal comprehensive recycling process for copper smelting ash

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106119547A (en) * 2016-07-20 2016-11-16 中国恩菲工程技术有限公司 A kind of method reclaiming copper in the outer waste discharge acid of Copper making system for preparing sulfuric acid
CN106566927A (en) * 2016-10-14 2017-04-19 铜陵有色金属集团股份有限公司 Efficient gradient separation recovery process for copper anode slime leachate
CN108358343A (en) * 2018-02-13 2018-08-03 武汉船用机械有限责任公司 Electroplating sewerage processing method

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