CN105803209B - Method for recovering rare and precious metals from acid mud - Google Patents

Method for recovering rare and precious metals from acid mud Download PDF

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Publication number
CN105803209B
CN105803209B CN201610252644.9A CN201610252644A CN105803209B CN 105803209 B CN105803209 B CN 105803209B CN 201610252644 A CN201610252644 A CN 201610252644A CN 105803209 B CN105803209 B CN 105803209B
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filter residue
lead
mud
water
press filtration
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CN105803209A (en
Inventor
朱来东
鲁兴武
李彦龙
李俞良
陈博
陈一博
程亮
易超
马爱军
陈文波
张恩玉
曹桂银
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Gansu High Energy Zhongse Environmental Protection Technology Co ltd
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Northwest Research Institute of Mining and Metallurgy
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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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B19/00—Selenium; Tellurium; Compounds thereof
    • C01B19/02—Elemental selenium or tellurium
    • 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
    • C22B11/00—Obtaining noble metals
    • C22B11/02—Obtaining noble metals by dry processes
    • C22B11/021—Recovery of noble metals from waste materials
    • C22B11/023—Recovery of noble metals from waste materials from pyrometallurgical residues, e.g. from ashes, dross, flue dust, mud, skim, slag, sludge
    • 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
    • C22B13/02—Obtaining lead by dry processes
    • C22B13/025—Recovery from waste materials
    • 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
    • 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
    • C22B30/00—Obtaining antimony, arsenic or bismuth
    • C22B30/06—Obtaining bismuth
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

A method for recovering rare and precious metals from acid sludge and the technical field of precious metal acid sludge recovery and reuse, the method comprises the following steps: the method comprises the following steps of acid sludge pretreatment, copper recovery, lead recovery and selenium recovery, and is particularly suitable for acid sludge with the following characteristics: pb30-50%, Se2-15%, Bi1-5%, Cu2-10%, Au2-10g/t and Ag30-200 g/t. The invention has the beneficial effects that: the acid mud is washed to recover copper metal, the mixed acid is used for leaching, the lead is used for enriching gold, silver and bismuth by strong enriching capacity of lead, the fire smelting is used for preparing lead-bismuth alloy, rare and precious metals such as bismuth, gold and silver are recovered to the maximum extent, the sulfur dioxide is used for reducing and preparing selenium powder, and compared with a sodium sulfite process, sodium salt wastewater or sodium sulfate crystals are not formed. The solid waste generated in the process mainly comes from two solid-liquid separations: the filter residue after solid-liquid separation is rich in lead element and is used for pyrometallurgical smelting of lead to form lead-bismuth alloy, so that a closed circulating system is formed in the whole process, no pollution is caused to the environment, the production cost is reduced, and environment-friendly and clean production is realized.

Description

A kind of method that rare precious metal is reclaimed in sour mud
Technical field
The present invention relates to noble metal acid mud utilization and recycle technical field, the side of rare precious metal is reclaimed in specifically a kind of sour mud Method.
Background technology
In sulphide ore pyrometallurgical smelting acid manufacturing processes, the tiny grit that the metal of some low melting points is formed usually can be with cigarette Gas enters smoke exhaust barrel, and with the application of current wet cleaning flue gas process, this kind of grit accumulates over a long period, formd with heavy metal lead Based on, the sour mud of the rare precious metal such as Enriching Selenium, bismuth, gold, silver.This kind of resource is because Main Ingredients and Appearance is lead, current most of factories and miness Pyrometallurgical smelting of lead enterprise is sold to as lead skim, in processing procedure, lead base therein is originally recycled, but other for Lian Qian enterprises Rare precious metal is largely dispersed in flue dust and Water Quenching Slag, can not be reclaimed.As the available mineral products class resource of non-ferrous metal is more next Fewer, the comprehensive utilization of secondary resource increasingly attracts people's attention；And sour mud yield is big, there will be heap in sale Put（It is outdoor）And the process of long-distance transport, due to wherein containing various heavy harmful element, long-time solar exposure, rainwater punching Surrounding enviroment are brought serious secondary pollution by brush, strong wind airborne dust, therefore, environmental protection, effective exploitation are carried out to sour mud, is made Its huge economic value contained is embodied, and has been the task of top priority.Utilization for caused sour mud in smelting acid making system, Such as big, high energy consumption, metal recovery rate are invested using side-blown melting, side-blown reduction, fuming furnace technical finesse acid mud, this kind of method not Enough ideals；Wet processing is and for example utilized, the technique is not suitable for handling leaded and rare precious metal acid mud, and too long in flow；For another example Using sodium sulfite lixiviation process, this kind of method can only be extracted selenium therein.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of method that rare precious metal is reclaimed in sour mud, existing to solve Technological investment is big, high energy consumption, metal recovery rate are not ideal enough, too long in flow, the problem of can only extracting single metal.
The present invention solve technical problem technical scheme be：A kind of method that rare precious metal is reclaimed in sour mud, methods described Comprise the following steps.
Sour mud pretreatment.
Water is added into sour mud, is stirred pulp, mixing time 0.5-3 hours, the mass ratio of sour mud and water is 1:3, Temperature maintains 25-90 degrees Celsius, and stirring carries out press filtration processing after terminating to mud, obtains filtrate A and filter residue A.Into filter residue A Water is added, is stirred, mixing time 0.5-3 hours, the mass ratio of filter residue A and water is 1:1, stir after terminating to mud through row Press filtration is handled, and obtains liquor B and filter residue B.Liquor B and filtrate A are mixed to get liquor C.
Copper reclaims.
Ammonium sulfide or vulcanized sodium are added in liquor C, untill blueness not being presented in liquor C, wherein ammonium sulfide or sulphur Change sodium with reference to 1.1-1.5 times that addition is theoretical reacting dose.Press filtration processing, the filter after press filtration are carried out to reacted mixture Slag is the copper concentrate rich in copper sulfide.
Lead reclaims.
By filter residue B and water mixing pulp, the mass ratio of filter residue B and water is 3-8:1, the mixed acid added afterwards after dilution, Mixed acid addition after dilution is 50-300g/L；Temperature maintains 40-90 degrees Celsius, hour time 1.5-5；In mixed acid The quality of nitric acid accounts for the 20-50% of gross mass, and remaining is sulfuric acid, the mixed acid volumetric concentration 200-300g/L after dilution；Reaction Reactant press filtration is handled after end to obtain filtrate D and filter residue C, wherein filter residue C is the lead skim for being enriched gold and silver.
Selenium reclaims.
Sulfur dioxide gas, 1-5 cubes m/min of control sulfur dioxide flow, temperature 25-60 are added in filtrate D Degree Celsius, control terminal PH maintains 0.5-2, sustained response 2-4 hours, during which with uniform stirring；Stir after terminating to anti- Thing is answered to be handled through row press filtration, the filter residue obtained afterwards is the powder rich in selenium.
Methods described is particularly suitable for use in the sour mud of following feature：Pb30-50%、Se2-15%、Bi1-5%、Cu2-10%、Au2- 10g/t、Ag30-200g/t。
The beneficial effects of the present invention are：Sour mud washing is recycled copper metal therein, is leached, utilized using nitration mixture Lead produces lead bismuth alloy to gold, silver, the strong accumulation ability of bismuth, pyrometallurgical smelting, has at utmost reclaimed your dilute gold such as bismuth, gold, silver Category, produces selenium powder using sulphur dioxide reduction, than sodium sulfite technique, does not form sodium salt waste water or sulfate crystal.Technique In caused solid waste mostly come from separation of solid and liquid twice：The filter residue of separation of solid and liquid is rich in lead element, the pyrogenic process for lead Smelting forms lead bismuth alloy, thus whole technical process forms closed circulation system, does not form pollution to environment, reduces production Cost, realize environment-protecting clean production.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described.
Embodiment 1.
Sour mud composition is：Pb32.56%、Se5.66%、Bi2.38%、Cu3.62%、Au2.6g/t、Ag46.8g/t.
Sour mud pretreatment.
Water is added into sour mud, is stirred pulp, mixing time 0.5 hour, the mass ratio of sour mud and water is 1:3, temperature Degree maintains 25 degrees Celsius, and stirring carries out press filtration processing after terminating to mud, obtains filtrate A and filter residue A.Added into filter residue A Water, it is stirred, mixing time 0.5 hour, the mass ratio of filter residue A and water is 1:1, stirring terminate after to mud through row press filtration at Reason, obtains liquor B and filter residue B.Liquor B and filtrate A are mixed to get liquor C.
Copper reclaims.
Ammonium sulfide or vulcanized sodium are added in liquor C, untill blueness not being presented in liquor C, wherein ammonium sulfide or sulphur Change sodium with reference to 1.1 times that addition is theoretical reacting dose.Press filtration processing is carried out to reacted mixture, the filter residue after press filtration is For the copper concentrate rich in copper sulfide.
Lead reclaims.
By filter residue B and water mixing pulp, the mass ratio of filter residue B and water is 3:1, the mixed acid added afterwards after dilution is dilute Mixed acid addition after releasing is 50g/L；Temperature maintains 40 degrees Celsius, 1.5 hours time；The quality of nitric acid accounts in mixed acid The 20% of gross mass, remaining is sulfuric acid, the mixed acid volumetric concentration 200g/L after dilution；React after terminating to reactant press filtration Processing obtains filtrate D and filter residue C, and wherein filter residue C is the lead skim for being enriched gold and silver.
Selenium reclaims.
Sulfur dioxide gas is added in filtrate D, 1 cube m/min of control sulfur dioxide flow, temperature 25 is Celsius Degree, control terminal PH maintain 0.5, sustained response 2 hours, during which with uniform stirring；Stir after terminating to reactant through row Press filtration is handled, and the filter residue obtained afterwards is the powder rich in selenium.
The direct yield of calculating is：Selenium 88.6%, gold 99%, silver 98%, lead 98.6%, bismuth 99.6%.
Embodiment 2.
Sour mud composition is：Pb42.36%、Se2.36%、Bi3.28%、Cu4.32%、Au5.2g/t、Ag56.6g/t.
Sour mud pretreatment.
Water is added into sour mud, is stirred pulp, mixing time 2.5 hours, the mass ratio of sour mud and water is 1:3, temperature Degree maintains 65 degrees Celsius, and stirring carries out press filtration processing after terminating to mud, obtains filtrate A and filter residue A.Added into filter residue A Water, it is stirred, mixing time 2.5 hours, the mass ratio of filter residue A and water is 1:1, stirring terminate after to mud through row press filtration at Reason, obtains liquor B and filter residue B.Liquor B and filtrate A are mixed to get liquor C.
Copper reclaims.
Ammonium sulfide or vulcanized sodium are added in liquor C, untill blueness not being presented in liquor C, wherein ammonium sulfide or sulphur Change sodium with reference to 1.3 times that addition is theoretical reacting dose.Press filtration processing is carried out to reacted mixture, the filter residue after press filtration is For the copper concentrate rich in copper sulfide.
Lead reclaims.
By filter residue B and water mixing pulp, the mass ratio of filter residue B and water is 6:1, the mixed acid added afterwards after dilution is dilute Mixed acid addition after releasing is 150g/L；Temperature maintains 70 degrees Celsius, 4 hours time；The quality of nitric acid accounts in mixed acid The 30% of gross mass, remaining is sulfuric acid, the mixed acid volumetric concentration 260g/L after dilution；React after terminating to reactant press filtration Processing obtains filtrate D and filter residue C, and wherein filter residue C is the lead skim for being enriched gold and silver.
Selenium reclaims.
Sulfur dioxide gas is added in filtrate D, 3 cubes ms/min of control sulfur dioxide flow, temperature 45 is Celsius Degree, control terminal PH maintain 1.2, sustained response 3 hours, during which with uniform stirring；Stir after terminating to reactant through row Press filtration is handled, and the filter residue obtained afterwards is the powder rich in selenium.
The direct yield of calculating is：Selenium 91.6%, gold 97.5%, silver 96.8%, lead 98.3%, bismuth 99.2%.
Embodiment 3.
Sour mud composition is：Pb36.1%、Se9.56%、Bi4.68%、Cu8.82%、Au8.6g/t、Ag128.6g/t.
Sour mud pretreatment.
Water is added into sour mud, is stirred pulp, mixing time 3 hours, the mass ratio of sour mud and water is 1:3, temperature 90 degrees Celsius are maintained, stirring carries out press filtration processing after terminating to mud, obtains filtrate A and filter residue A.Water is added into filter residue A, It is stirred, mixing time 3 hours, the mass ratio of filter residue A and water is 1:1, stirring is handled mud after terminating through row press filtration, is obtained To liquor B and filter residue B.Liquor B and filtrate A are mixed to get liquor C.
Copper reclaims.
Ammonium sulfide or vulcanized sodium are added in liquor C, untill blueness not being presented in liquor C, wherein ammonium sulfide or sulphur Change sodium with reference to 1.5 times that addition is theoretical reacting dose.Press filtration processing is carried out to reacted mixture, the filter residue after press filtration is For the copper concentrate rich in copper sulfide.
Lead reclaims.
By filter residue B and water mixing pulp, the mass ratio of filter residue B and water is 8:1, the mixed acid added afterwards after dilution is dilute Mixed acid addition after releasing is 300g/L；Temperature maintains 90 degrees Celsius, 5 hours time；The quality of nitric acid accounts in mixed acid The 50% of gross mass, remaining is sulfuric acid, the mixed acid volumetric concentration 300g/L after dilution；React after terminating to reactant press filtration Processing obtains filtrate D and filter residue C, and wherein filter residue C is the lead skim for being enriched gold and silver.
Selenium reclaims.
Sulfur dioxide gas is added in filtrate D, 5 cubes ms/min of control sulfur dioxide flow, temperature 60 is Celsius Degree, control terminal PH maintain 2, sustained response 4 hours, during which with uniform stirring；Stirring is pressed reactant after terminating through row Filter is handled, and the filter residue obtained afterwards is the powder rich in selenium.
The direct yield of calculating is：Selenium 93.5%, gold 98.3%, silver 98.5%, lead 99.2%, bismuth 99.7%.

Claims (1)

1. reclaiming the method for rare precious metal in a kind of sour mud, methods described comprises the following steps：
Sour mud pretreatment：
Water is added into sour mud, is stirred pulp, mixing time 0.5-3 hours, the mass ratio of sour mud and water is 1:3, temperature 25-90 degrees Celsius is maintained, stirring carries out press filtration processing after terminating to mud, obtains filtrate A and filter residue A；
Water is added into filter residue A, is stirred, mixing time 0.5-3 hours, the mass ratio of filter residue A and water is 1:1, stirring knot Mud is handled through row press filtration after beam, obtains liquor B and filter residue B；
Liquor B and filtrate A are mixed to get liquor C；
Copper reclaims：
Ammonium sulfide or vulcanized sodium are added in liquor C, untill blueness not being presented in liquor C, wherein ammonium sulfide or vulcanized sodium With reference to 1.1-1.5 times that addition is theoretical reacting dose；
Press filtration processing is carried out to reacted mixture, the filter residue after press filtration is the copper concentrate rich in copper sulfide；
Lead reclaims：
By filter residue B and water mixing pulp, the mass ratio of filter residue B and water is 3-8:1, the mixed acid added afterwards after dilution, dilution Mixed acid addition afterwards is 50-300g/L；Temperature maintains 40-90 degrees Celsius, hour time 1.5-5；Nitric acid in mixed acid Quality account for the 20-50% of gross mass, remaining is sulfuric acid, the mixed acid volumetric concentration 200-300g/L after dilution；Reaction terminates Reactant press filtration is handled afterwards to obtain filtrate D and filter residue C, wherein filter residue C is the lead skim for being enriched gold and silver；
Selenium reclaims：
Sulfur dioxide gas is added in filtrate D, 1-5 cubes m/min of control sulfur dioxide flow, temperature 25-60 is Celsius Degree, control terminal pH maintain 0.5-2, sustained response 2-4 hours, during which with uniform stirring；Stir after terminating to reactant Handled through row press filtration, the filter residue obtained afterwards is the powder rich in selenium；
Methods described is directed to the sour mud of following feature：Pb30-50%、Se2-15%、Bi1-5%、Cu2-10%、Au2-10g/t、 Ag30-200g/t, using effect are more preferable.
CN201610252644.9A 2016-04-21 2016-04-21 Method for recovering rare and precious metals from acid mud Active CN105803209B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106219500B (en) * 2016-08-04 2018-09-28 西北矿冶研究院 Method for preparing sodium selenite by utilizing selenium dioxide containing bismuth and copper and application
CN108913909B (en) * 2018-08-30 2024-01-30 西北矿冶研究院 Black copper mud arsenic removal device and method

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* Cited by examiner, † Cited by third party
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CN102583264B (en) * 2012-02-03 2014-01-22 昆明冶金研究院 Method for leaching selenium in acid mud by using sodium sulfite
RU2534093C2 (en) * 2013-03-12 2014-11-27 Открытое акционерное общество "Уралэлектромедь" Method of copper-electrolyte processing
CN103435016B (en) * 2013-08-16 2016-08-17 云南铜业股份有限公司 A kind of method extracting selenium from acid mud
CN103496676A (en) * 2013-10-11 2014-01-08 金川集团股份有限公司 Method for recovering selenium from acid mud wastes of acid production with copper smelting smoke
CN105463197A (en) * 2015-12-02 2016-04-06 昆明理工大学 Method for recycling valuable metal from copper smelting white smoke

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