CN106756047A - Debris silver anode slime high puies forward the processing method of gold - Google Patents

Debris silver anode slime high puies forward the processing method of gold Download PDF

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Publication number
CN106756047A
CN106756047A CN201611208766.4A CN201611208766A CN106756047A CN 106756047 A CN106756047 A CN 106756047A CN 201611208766 A CN201611208766 A CN 201611208766A CN 106756047 A CN106756047 A CN 106756047A
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silver
gold
debris
anode slime
liquid
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CN106756047B (en
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粟明辉
杨跃新
李环
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Chengzhou City Jingui Silver Co Ltd
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Chengzhou City Jingui Silver Co Ltd
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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
    • C22B7/007Wet processes by acid leaching
    • 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
    • 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

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

Abstract

The invention discloses the processing method that debris silver anode slime high carries gold;The method will the step of be mainly by debris silver anode slime high by wash remove soluble compound, then after acidleach is cooked off except base metal, then by alkaline oxygenated leaching, it is molten gold, reduction, washing, obtain 99.99% bronze.The method impurities removing efficiency is high, comprehensively recovering valuable metal, process.

Description

Debris silver anode slime high puies forward the processing method of gold
Technical field
The invention belongs to nonferrous metallurgy field, it is related to precious metal hydrometallurgy field, particularly a kind of debris silver anode high Mud puies forward the processing method of gold.
Background technology
During thick electrorefining of silver, the electrode potential metal more positive than silver is not dissolved and enters the earth of positive pole, same with this When the partial electrode current potential base metal impurity more negative than silver can also precipitate and enter the earth of positive pole because forming oxide or basic salt.This Class silver anode slime is generally higher containing gold and silver, also a small amount of impurity, is to extract gold and the main raw material(s) of other valuable metals.
Tradition mainly has from silver anode slime Method for extracting gold:Concentrated sulfuric acid digestion method, nitric acid oxidation method, chloroazotic acid method, electrolysis. Concentrated sulfuric acid digestion method and nitric acid oxidation method are needed to silver anode slime digestion repeatedly for a long time, and the fineness of gold for reclaiming is not high, expensive Metal level of aggregation is low.Although chloroazotic acid method can produce high-quality gold product, production process needs to carry out catching up with nitre, Operating process is complicated, and is only applicable to small-scale production.Electrolysis reclaims gold process from the earth of positive pole, produces Although gold purity is high, main drawback is that noble metal overstocks too many, the production cycle is more long, causes overstocking for fund for it.
By continuing to develop in recent years, the technique for carrying gold from silver anode slime is continued to develop, relatively conventional at present The handling process of gold is put forward generally using silver anode slime leaching-parting-gold reduction-washing founding.Golden reducing agent is generally Sodium sulfite, sodium hydrogensulfite, oxalic acid, sulfur dioxide etc., deoxidization terminal is by controlling control of Electric potentials.
The A of the Chinese invention patent application publication number CN of on December 2nd, 2015 105112669, by Yunnan Xi Ye groups(Control Stock)In the silver anode slime that Qian Ye branch companies of Co., Ltd are proposed in the comprehensive recovering process of platinum palladium, silver anode slime is used Nitric acid leaches a point silver, and nitric acid leached mud is further continued for chlorination parting, and parting liquid carries out golden reduction after removing bismuth, high in order to obtain purity Gold, chlorination parting liquid also needs to carry out removal of impurities, and process is cumbersome, and process time is long.
The A of the Chinese invention patent application publication number CN of on November 16th, 2016 106119554, by Zijin Mining group share Co., Ltd;What is proposed prepares High Purity Gold from silver anode slime and is enriched with the method for silver, platinum and palladium, by silver anode slime nitre Ore Leaching point silver, parting liquid and parting slag are obtained by silver separating residues chloroazotic acid parting, add sodium hydrogensulfite to carry out toward parting liquid Reduction obtains reducing bronze, then washs, dries, obtaining ingot after founding, although the ingot purity for obtaining is high, but handling process Complexity, and treatment scale is partial to miniaturization.
In produce reality, some silver anode slimes often cause gold content low because of a variety of causes, and usually less than less than 10%, It is generally only, using acidleach removal of impurities, to cause subsequent handling to also need to further removal of impurities, and the Huang for obtaining and impurity is higher Golden purity does not often reach IC-Au99.99 standards.
The content of the invention
The deficiency that the purpose of the present invention exists aiming at above-mentioned existing technology, there is provided a kind of debris silver anode slime high is carried The processing method of gold, is further processed to debris silver anode slime high, and output meets the gold of IC-Au99.99 standards requirement Powder, the characteristics of with process.
The purpose of the present invention is achieved through the following technical solutions:
Debris silver anode slime high puies forward the processing method of gold, it is characterised in that following steps:
(1)The debris silver anode slime high of silver electrolysis output is washed first, liquid solid product mass ratio 2 ~ 3:1ml/g, temperature 95 ~ 100 DEG C, then 0.2 ~ 0.5h of mixing time filters, and obtains washing slag, and water lotion returns to silver electrolysis;
(2)By step(1)The washing slag for obtaining adds the nitric acid digestion of mass percent concentration 60 ~ 68%, liquid solid product mass ratio 2~3:Then 1 ml/g, 95 ~ 100 DEG C of temperature, 0.1 ~ 0.2h of reaction time is filtered, and obtains nitric acid leached mud, and leaching solution is returned Silver-colored system reclaims silver and other valuable metals;
(3)By step(2)The nitric acid leached mud for obtaining adds the concentrated sulfuric acid digestion of mass percent concentration 98%, the solid volume mass of liquid Than 1 ~ 2:Then 1 ml/g, 95 ~ 100 DEG C of temperature, 0.1 ~ 0.2h of reaction time filters, and obtains sulfuric acid leaching slag, sulphuric leachate Send water process;
(4)By step(3)The sulfuric acid leaching slag for obtaining adds alkali and oxidant, liquid solid product mass ratio 3 ~ 4:1 ml/g, temperature 85 ~ 95 DEG C of degree, the reaction time is 0.3 ~ 0.5h, is then filtrated to get alkali phase analysis, and water process is sent in alkali immersion liquid;
(5)By step(4)The alkali phase analysis for obtaining dissolve gold in 36% ~ 38% hydrochloric acid solution with oxidant, obtain parting liquid, parting Slag returns silver converter;
(6)By step(5)The parting liquid for obtaining adds reducing agent to be reduced after adjusting pH to 2 ~ 3 with NaOH, temperature 75 ~ 90 DEG C, reacted when current potential reaches 600 ~ 630mV and completed, then filter, the filter cake for obtaining is washed with pure water again after being washed with nitric acid Wash, four or nine bronzes are obtained after drying.
The step(4)Alkali and oxidant be potassium hydroxide and 30% hydrogen peroxide;Step(4)Alkali addition is theoretical amount 1.2 ~ 1.5 times, oxidant addition is 1.1 ~ 1.2 times of theoretical amount.
The step(5)Oxidant be also 30% hydrogen peroxide, its addition is 1.1 ~ 1.2 times of theoretical amount.
The step(6)Reducing agent be sodium sulfite.
Innovative point of the invention is, silver nitrate and soluble-salt, water in silver anode slime can be washed away with hot wash Nitric acid is added in washery slag, the metal such as most silver, copper, lead, bismuth, palladium, iron enters in leaching solution in slag, and gold is enriched in In nitric acid leached mud, sulfuric acid is added, it is main to remove the metal such as part silver, copper, iron of residual after nitric acid is leached, continuously add hydrogen Potassium oxide and hydrogen peroxide then mainly remove the foreign metals such as remaining antimony, silicon after digestion, realize the deep removal of foreign metal, By after removal of impurities, gold content can at least reach more than 90%, it is easy to the purification of subsequent handling gold to refine.
Adopt this method effectively further to purify to debris silver anode slime high, and removal of impurity is high, can comprehensively return Valuable metal is received, flowage structure is simple, and reaction is efficient, process, it is easy to commercial Application.
Brief description of the drawings
Fig. 1 is process chart of the invention.
Specific embodiment
Described in detail with reference to embodiment and invented
Embodiment 1
Debris silver anode slime high puies forward the processing method of gold, comprises the following steps that:
(1)The debris silver anode slime 3kg high of silver electrolysis output is washed first, wherein Au10.7%, Ag, 5.54%, Cu1.13%, Fe2.01%, Pb1.97%, Sb1.96%, Si2.17%, liquid-solid ratio 3:1,90 DEG C of temperature, mixing time 0.3h, then Filtering, obtains washing slag, and water lotion returns to silver electrolysis;
(2)By step(1)The washing slag for obtaining adds 68% nitric acid digestion, liquid-solid ratio 2:1,100 DEG C of temperature, reaction time 0.2h, then filters, and obtains nitric acid leached mud, and leaching solution returns silver-colored system and reclaims silver and other valuable metals;
(3)By step(2)The nitric acid leached mud for obtaining adds 98% concentrated sulfuric acid digestion, liquid-solid ratio 2:1 100 DEG C of temperature, reaction time 0.2h, then filters, and obtains sulfuric acid leaching slag, and sulphuric leachate send water process;
(4)By step(3)The sulfuric acid leaching slag for obtaining adds 45g potassium hydroxide and 30% hydrogen peroxide 30mL, liquid-solid ratio 3:1, temperature 95 DEG C, the reaction time is 0.4h, is then filtrated to get alkali phase analysis, and water process is sent in alkali immersion liquid;
(5)By step(4)The alkali phase analysis for obtaining add 50mL30% dioxygens water dissolves gold in 75mL38% hydrochloric acid solutions, are divided Golden liquid, parting slag returns silver converter;
(6)By step(5)The parting liquid for obtaining adds 48g NaOH to add 90g sodium sulfites to be reduced after adjusting pH to 3, 85 DEG C of temperature, reacts when current potential reaches 630mV and completes, and then filters, and the filter cake for obtaining uses pure water again after being washed with nitric acid Washing, obtains four or nine bronzes after drying.
Embodiment 2
Debris silver anode slime high puies forward the processing method of gold, comprises the following steps that:
(1)The debris silver anode slime 1kg high of silver electrolysis output is washed first, wherein Au11.3%, Ag, 6.12%, Cu1.98%, Fe1.96%, Pb1.55%, Sb2.64%, Si2.02%, liquid-solid ratio 2:1,95 DEG C of temperature, mixing time 0.3h, then Filtering, obtains washing slag, and water lotion returns to silver electrolysis;
(2)By step(1)The washing slag for obtaining adds 65% nitric acid digestion, liquid-solid ratio 3:1,98 DEG C of temperature, reaction time 0.4h, Then filter, obtain nitric acid leached mud, leaching solution returns silver-colored system and reclaims silver and other valuable metals;
(3)By step(2)The nitric acid leached mud for obtaining adds 98% concentrated sulfuric acid digestion, liquid-solid ratio 2:1 100 DEG C of temperature, reaction time 0.1h, then filters, and obtains sulfuric acid leaching slag, and sulphuric leachate send water process;
(4)By step(3)The sulfuric acid leaching slag for obtaining adds 16g potassium hydroxide and 30% hydrogen peroxide 12mL, liquid-solid ratio 4:1, temperature 90 DEG C, the reaction time is 0.5h, is then filtrated to get alkali phase analysis, and water process is sent in alkali immersion liquid;
(5)By step(4)The alkali phase analysis for obtaining add 18mL30% dioxygens water dissolves gold in 12mL36% hydrochloric acid solutions, are divided Golden liquid, parting slag returns silver converter;
(6)By step(5)The parting liquid for obtaining adds 20g NaOH to add 32g sodium sulfites to be gone back after adjusting pH to 2.5 Original, 90 DEG C of temperature is reacted when current potential reaches 620mV and is completed, and is then filtered, the filter cake for obtaining washed with nitric acid after again with pure Water washing, obtains four or nine bronzes after drying.

Claims (4)

1. a debris silver anode slime high puies forward the processing method of gold, it is characterised in that following steps:
(1)The debris silver anode slime high of silver electrolysis output is washed first, liquid solid product mass ratio 2 ~ 3:1ml/g, temperature 95 ~ 100 DEG C, then 0.2 ~ 0.5h of mixing time filters, and obtains washing slag, and water lotion returns to silver electrolysis;
(2)By step(1)The washing slag for obtaining adds the nitric acid digestion of mass percent concentration 60 ~ 68%, liquid solid product mass ratio 2~3:Then 1 ml/g, 95 ~ 100 DEG C of temperature, 0.1 ~ 0.2h of reaction time is filtered, and obtains nitric acid leached mud, and leaching solution is returned Silver-colored system reclaims silver and other valuable metals;
(3)By step(2)The nitric acid leached mud for obtaining adds the concentrated sulfuric acid digestion of mass percent concentration 98%, the solid volume mass of liquid Than 1 ~ 2:Then 1 ml/g, 95 ~ 100 DEG C of temperature, 0.1 ~ 0.2h of reaction time filters, and obtains sulfuric acid leaching slag, sulphuric leachate Send water process;
(4)By step(3)The sulfuric acid leaching slag for obtaining adds alkali and oxidant, liquid solid product mass ratio 3 ~ 4:1 ml/g, temperature 85 ~ 95 DEG C of degree, the reaction time is 0.3 ~ 0.5h, is then filtrated to get alkali phase analysis, and water process is sent in alkali immersion liquid;
(5)By step(4)The alkali phase analysis for obtaining dissolve gold in 36% ~ 38% hydrochloric acid solution with oxidant, obtain parting liquid, parting Slag returns silver converter;
(6)By step(5)The parting liquid for obtaining adds reducing agent to be reduced after adjusting pH to 2 ~ 3 with NaOH, temperature 75 ~ 90 DEG C, reacted when current potential reaches 600 ~ 630mV and completed, then filter, the filter cake for obtaining is washed with pure water again after being washed with nitric acid Wash, four or nine bronzes are obtained after drying.
2. debris silver anode slime high according to claim 1 puies forward the processing method of gold, it is characterised in that:The step(4) Alkali and oxidant be potassium hydroxide and 30% hydrogen peroxide;Step(4)Alkali addition is 1.2 ~ 1.5 times of theoretical amount, oxidant Addition is 1.1 ~ 1.2 times of theoretical amount.
3. debris silver anode slime high according to claim 1 puies forward the processing method of gold, it is characterised in that:The step(5) Oxidant be also 30% hydrogen peroxide, its addition is 1.1 ~ 1.2 times of theoretical amount.
4. debris silver anode slime high according to claim 1 puies forward the processing method of gold, it is characterised in that:It is described to state step (6)Reducing agent be sodium sulfite.
CN201611208766.4A 2016-12-23 2016-12-23 High sundries silver anode slime puies forward the processing method of gold Active CN106756047B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107460324A (en) * 2017-08-23 2017-12-12 中南大学 A kind of method that silver anode slime control current potential prepares four or nine gold medals
CN114113041A (en) * 2021-11-29 2022-03-01 昆山鸿福泰环保科技有限公司 Method for testing gold and palladium by gold and palladium-containing material

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4293332A (en) * 1977-06-08 1981-10-06 Institute Of Nuclear Energy Research Hydrometallurgical process for recovering precious metals from anode slime
CN1442498A (en) * 2003-04-11 2003-09-17 山东黄金集团有限公司焦家金矿 Method of crude gold purification
CN104328284A (en) * 2014-11-17 2015-02-04 中南大学 Method for enriching and purifying gold
CN105274351A (en) * 2015-10-12 2016-01-27 湖南金旺铋业股份有限公司 Process for recycling high-purity gold from anode slime through organic reduction method
CN106065434A (en) * 2016-07-11 2016-11-02 郴州市金贵银业股份有限公司 A kind of method of the wet method direct purifying gold of synthetical recovery silver anode slime
CN106119554A (en) * 2016-08-18 2016-11-16 紫金矿业集团股份有限公司 High Purity Gold the method being enriched with silver, platinum and palladium is prepared from silver anode slime

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4293332A (en) * 1977-06-08 1981-10-06 Institute Of Nuclear Energy Research Hydrometallurgical process for recovering precious metals from anode slime
CN1442498A (en) * 2003-04-11 2003-09-17 山东黄金集团有限公司焦家金矿 Method of crude gold purification
CN104328284A (en) * 2014-11-17 2015-02-04 中南大学 Method for enriching and purifying gold
CN105274351A (en) * 2015-10-12 2016-01-27 湖南金旺铋业股份有限公司 Process for recycling high-purity gold from anode slime through organic reduction method
CN106065434A (en) * 2016-07-11 2016-11-02 郴州市金贵银业股份有限公司 A kind of method of the wet method direct purifying gold of synthetical recovery silver anode slime
CN106119554A (en) * 2016-08-18 2016-11-16 紫金矿业集团股份有限公司 High Purity Gold the method being enriched with silver, platinum and palladium is prepared from silver anode slime

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107460324A (en) * 2017-08-23 2017-12-12 中南大学 A kind of method that silver anode slime control current potential prepares four or nine gold medals
CN114113041A (en) * 2021-11-29 2022-03-01 昆山鸿福泰环保科技有限公司 Method for testing gold and palladium by gold and palladium-containing material

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