CN1057865A - A kind of solder anode slime nitric acid slag extracts the method for silver and gold - Google Patents

A kind of solder anode slime nitric acid slag extracts the method for silver and gold Download PDF

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Publication number
CN1057865A
CN1057865A CN90103200A CN90103200A CN1057865A CN 1057865 A CN1057865 A CN 1057865A CN 90103200 A CN90103200 A CN 90103200A CN 90103200 A CN90103200 A CN 90103200A CN 1057865 A CN1057865 A CN 1057865A
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silver
gold
nitric acid
anode slime
weight
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CN90103200A
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CN1023025C (en
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何国华
王延岭
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Kunming Precious Metals Research Inst Of China Nonferrous Metals Industry Co (
KUNMING NOBLE METAL INST CHINA NONFERROUS METAL INDUSTRY GENERAL Co
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Kunming Precious Metals Research Inst Of China Nonferrous Metals Industry Co (
KUNMING NOBLE METAL INST CHINA NONFERROUS METAL INDUSTRY GENERAL Co
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Priority to CN90103200A priority Critical patent/CN1023025C/en
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    • 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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  • Manufacture And Refinement Of Metals (AREA)

Abstract

A kind of solder anode slime nitric acid slag extracts the method for silver and gold.Its treatment step is: raw material is through sulfurization roasting, and the secondary selectivity leaches, and makes silver change solution over to, again through precipitation and reduce fine silver.Selective leaching is slagged tap and is carried out chloridized and make gold change solution over to, gets proof gold through displacement and wet processing again.Flow process is simple, and the cycle is short, and cost is low, silver-colored and golden yield height (Ag~95, Au~100%).The purity height (Ag99.9%, Au99.99%).

Description

A kind of solder anode slime nitric acid slag extracts the method for silver and gold
A kind of solder anode slime nitric acid slag extracts the method for silver and gold, the invention relates to precious metals metallurgy.
The solder electrolytic anode sludge is one of raw material that extracts precious metal.Solder anode slime nitric acid slag is that solder anode slime leaches the last residue in extraction silver back with nitric acid, and generally consist of (except the %, Au): Au 250~260g/T, Ag 7.5~7.6, Sb~8.02, Pb~3.02, Sn~2.52, As~2.33, Bi~2.02, SiO 2~8.15, S~6, Fe~0.7, Se~0.42.This material feature is that bullion content is low, base metal content height, and complicated component, and also amphoteric element is more, and high and low metal is difficult to separate, and still this type of waste residue of non-processor extracts successful methods silver-colored and gold both at home and abroad.Residue is stacked for a long time, and the precious metal that country is badly in need of be cannot take out, and influences the business capital turnover, again contaminate environment.
The objective of the invention is to propose the general flow that a solder anode slime nitric acid slag extracts silver and gold, can from waste residue, extract silver and gold effectively, turn waste into wealth, and the rate of recovery height of silver and gold, the purity height, reagent consumes low, and equipment solves easily.
Method provided by the present invention, (1) be with said solder anode slime nitric acid leached mud material, adding the vitriol oil stirs, 500~700 ℃ of temperature, best 550~600 ℃, 2~4 hours time, best 3 hours, carry out sulfurization roasting, make the silver-colored Sulfuric acid disilver salt state that can leach that is converted in the slag.(2) the gained fired slags is levigate, and is best<80 orders, at sulfuric acid concentration 0~6N, best 0.5~1N, and solid (weight, g): liquid (volume, ml)=1: 8~20, best 1: 15,40~85 ℃ of temperature, best~80 ℃, carrying out the secondary selectivity leaches, one-level 2 hours, secondary 1 hour, the enrichment of dilute sulphuric acid leach liquor silver.(3) leach liquor is the AgCl state with the NaCl precipitated silver, and hydrazine hydrate reduction AgCl is a sponge silver, Ag purity 99.9%, direct yield 93~96%.(4) the sulfurization roasting leached mud is at HCl1N+H 2SO 4The nitration mixture medium of 1N, (weight, g): (volume, ml)=1: 3~8, best 1: 5,50~80 ℃ of temperature, were used NaClO to liquid to solid by best 70 ℃ 3Carry out chlorination, make Au change solution over to, NaClO 3The best 20%(material of consumption is heavy), gradation adds, 4~10 hours time, best 6 hours.(5) after chlorated liquid filters, get thick bronze (gold mud) with zinc dust precipitation, thick bronze gets high-purity cake of gold, Au purity 99.99%, direct yield~100% through simple wet processing.Chloride residue returns sulfurization roasting, and waste liquid contains Ag and Au is the 0.000Xg/l level, can discharge.
Advantage of the present invention is: (1) flow process is simple, and the treatment process process cycle is short.(2) precious metal direct yield height, Au~100%, Ag~95%; The high Au 99.99% of purity, Ag99.9%.(3) must directly not obtain the satisfactory precious metal product of purity with golden refining procedure through traditional silver such as electrolysis or extraction.(4) used chemical reagent is general reagent, and is cheap and easy to get.(5) equipment is general device, and smeltery's off-the-shelf equipment all can utilize.(6) cost is low, handles one ton of nitric acid leached mud and can make a profit more than 60,000 yuan.(7) present method can be directly used in tin anode mud and handle the acquisition precious metal.(8) turn waste into wealth, reduced environmental pollution again.
Embodiment one, and content is (removing Au, weight %): Au 260g/T, and Ag 7.6, Sb8.02, Pb3.02, Sn 2.52, Ax2.33, Bi2.02 SiO 28.15 S 6, Fe 0.7, and the solder anode slime nitric acid leached mud 4kg of Se0.42 adds the vitriol oil and stirs after the pre-treatment, put into retort furnace in the Sheng iron pan and carry out sulfurization roasting, 500~600 ℃ of temperature, 3 hours.Fired slags is levigate to<80 orders, with 0.5N industry H 2SO 4, solid (weight, g): liquid (volume, ml)=1: 15, temperature~90 ℃ are carried out secondary and are leached, and 2 hours for the first time, 1 hour for the second time, rare H 2SO 4It is the AgCl state that leach liquor adds the NaCl precipitated silver, and hydrazine hydrate reduction gets sponge silver powder, silver powder weight 289g, direct yield 95.06%, purity 99.9%, rare H 2SO 4Leached mud 1N industry H 2SO 4+ 1N industry HCl, (weight, g): (volume, ml)=1: 6, NaClO is used in temperature~70 ℃ to liquid at solid 3Carry out chlorination, gradation adds, 6 hours time.After chlorated liquid filtered, zinc dust precipitation got thick bronze (gold mud), and gold mud gets proof gold powder 1.06g, direct yield 101.9%, purity 99.99% through wet processing.
Embodiment two, the solder anode slime nitric acid leached mud 4kg that content and example one are identical, through and example one, behind the same treatment step, silver powder weight 293g, direct yield 96.38% purity 99.9%; Get bronze 1.04g, direct yield 100%, purity 99.99%

Claims (4)

1, a kind of solder anode slime nitric acid slag extracts silver and golden method, it is characterized in that:
A will add dense stream acid through pretreated solder anode slime nitric acid slag and stir, and 500~700 ℃ of temperature, carry out sulfurization roasting, 2~4 hours time, make that silver is converted into the state that can leach in the slag;
B with the sizing of A gained thin after, at sulfuric acid concentration 0~6N, solid (weight, g): liquid (volume, ml)=1: 8~20, temperature is carried out the secondary selectivity for 40~85 ℃ and is leached, the leach liquor enrichment silver;
C adds NaCl with B gained leach liquor, and precipitated silver is the AgCl state, gets high-purity sponge silver product with hydrazine hydrate reduction again;
D with B gained leached mud at HClIN+H 2SO 4IN nitration mixture medium, (weight, g): (volume, ml)=1: 3~8, NaClO is used in temperature .50~80 ℃ to liquid to solid 3, carry out chlorination and leach gold, NaClO, consumption 10~20% (weight of material), time of chlorinating 4~10 hours;
E obtains thick bronze (gold mud) with D gained solution zinc dust precipitation, and thick bronze gets high-purity cake of gold through wet processing.
2, solder anode slime nitric acid slag as claimed in claim 1 is got the method for silver and gold, and when it is characterized in that carrying out the 1A process, temperature is 550~600 ℃, 3 hours time.
3, solder anode slime nitric acid slag as claimed in claim 1 extracts silver and golden method, when it is characterized in that carrying out the 1B process, slag particle degree<80 orders, sulfuric acid concentration 0.5~1N, and solid (weight, g): liquid (volume, ml)=1: 15, temperature~80 ℃, the first step leached 2 hours, and leached 1 hour the second stage.
4, solder anode slime nitric acid slag as claimed in claim 1 extracts silver and golden method, when it is characterized in that carrying out the 1D process, solid (weight, g): liquid (volume, ml)=1: 5, temperature~70 ℃, 5~6 hours time, NaClO 3Consumption 20%(solid material weight), gradation adds.
CN90103200A 1990-06-23 1990-06-23 Method of extracting silver and gold from anode argillaceous nitric acidic residue of tin soldering Expired - Fee Related CN1023025C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN90103200A CN1023025C (en) 1990-06-23 1990-06-23 Method of extracting silver and gold from anode argillaceous nitric acidic residue of tin soldering

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN90103200A CN1023025C (en) 1990-06-23 1990-06-23 Method of extracting silver and gold from anode argillaceous nitric acidic residue of tin soldering

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CN1057865A true CN1057865A (en) 1992-01-15
CN1023025C CN1023025C (en) 1993-12-08

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1043787C (en) * 1996-11-21 1999-06-23 招远市北截金矿 Technical process for extracting valuable metal from gold slime
CN1045795C (en) * 1996-09-16 1999-10-20 昆明贵金属研究所 Method for recovering platinum and lead from anode slime of hydrogen peroxide production by electrolysis
CN102560141A (en) * 2012-02-28 2012-07-11 江西铜业股份有限公司 Full-wet method for producing high-grade silver product
CN102787240A (en) * 2012-07-18 2012-11-21 云南锡业集团有限责任公司研究设计院 Method for comprehensive recovery of valuable metals from tin anode mud
CN104046784A (en) * 2014-07-07 2014-09-17 扬州宁达贵金属有限公司 Method of recycling silver-containing soldering tin slag
CN104212976A (en) * 2014-08-30 2014-12-17 广东省工业技术研究院(广州有色金属研究院) Method for recovering silver from wet zinc smelting waste slag
CN111705216A (en) * 2020-06-16 2020-09-25 云南锡业股份有限公司锡业分公司 Treatment process of tin soldering electrolytic anode mud

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1045795C (en) * 1996-09-16 1999-10-20 昆明贵金属研究所 Method for recovering platinum and lead from anode slime of hydrogen peroxide production by electrolysis
CN1043787C (en) * 1996-11-21 1999-06-23 招远市北截金矿 Technical process for extracting valuable metal from gold slime
CN102560141A (en) * 2012-02-28 2012-07-11 江西铜业股份有限公司 Full-wet method for producing high-grade silver product
CN102787240A (en) * 2012-07-18 2012-11-21 云南锡业集团有限责任公司研究设计院 Method for comprehensive recovery of valuable metals from tin anode mud
CN104046784A (en) * 2014-07-07 2014-09-17 扬州宁达贵金属有限公司 Method of recycling silver-containing soldering tin slag
CN104212976A (en) * 2014-08-30 2014-12-17 广东省工业技术研究院(广州有色金属研究院) Method for recovering silver from wet zinc smelting waste slag
CN104212976B (en) * 2014-08-30 2016-08-17 广东省工业技术研究院(广州有色金属研究院) The method reclaiming silver from wet method zinc abstraction waste residue
CN111705216A (en) * 2020-06-16 2020-09-25 云南锡业股份有限公司锡业分公司 Treatment process of tin soldering electrolytic anode mud

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