CN1023025C - Method of extracting silver and gold from anode argillaceous nitric acidic residue of tin soldering - Google Patents
Method of extracting silver and gold from anode argillaceous nitric acidic residue of tin soldering Download PDFInfo
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- CN1023025C CN1023025C CN90103200A CN90103200A CN1023025C CN 1023025 C CN1023025 C CN 1023025C CN 90103200 A CN90103200 A CN 90103200A CN 90103200 A CN90103200 A CN 90103200A CN 1023025 C CN1023025 C CN 1023025C
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- silver
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- nitric acid
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- 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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Abstract
The present invention relates to a method for extracting silver and gold from nitric acid slag of anode mud for soldering tin, which comprises the treating steps: raw material is roasted in a sulfurization mode, and is selectively leached twice so that the silver is transferred to a solution, and pure silver is obtained by deposit and reduction; leached slag is selectively chlorinated so that the gold is transferred to the solution, and pure gold is obtained by displacement and wet treatment. The present invention has the advantages of simple flow path, short period, low cost, and high recovery rates and purity of the silver and the gold, wherein the recovery rates of the silver and the gold are respectively 95% and 100%, and the purity of the silver and the gold is respectively 99.9% and 99.99%.
Description
A kind of solder anode slime nitric acid slag extracts the method for silver and gold, the invention relates to precious metals metallurgy.
Association has silver and trace gold in the tin ore of Yunnan Tin Industrial Corp., and silver and gold are enriched in the anode sludge after smelting the tin electrolysis.Past is to adopt the nitric acid lixiviation process that most of silver is wherein extracted, remaining solder anode slime nitric acid slag, and it consists of (except the wt%, 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 the solder anode slime nitric acid slag retained for many years at Gejiu cloud tin company or the metallurgical intermediates of analogous components, a comprehensive interflow journey of extracting silver and gold is proposed, 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 ℃, time 2-4 hour, 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, granularity＜0.18mm(international standard sieve mesh＜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%(solid of consumption material 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 the vitriol oil 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
4LN nitration mixture medium, (weight, g): (volume, ml)=1: 3～8,50～80 ℃ of temperature are used NaClO to liquid to solid
3Carry out chlorination and leach gold, NaClO
3Best 20% (the solid material weighs) of consumption, 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, it is characterized in that carrying out 1A.During 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, it is characterized in that carrying out 1B.During process, slag particle degree＜0.18mm, sulfuric acid concentration 0.5～1N, 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, it is characterized in that carrying out 1D.During process, and solid (weight, g): liquid (volume, ml)=1: 5, temperature～70 ℃, 5～6 hours time, NaClO
3Consumption 20%(solid material weight), gradation adds.
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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1057865A CN1057865A (en) | 1992-01-15 |
| CN1023025C true CN1023025C (en) | 1993-12-08 |
Family
ID=4877966
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN90103200A Expired - Fee Related CN1023025C (en) | 1990-06-23 | 1990-06-23 | Method of extracting silver and gold from anode argillaceous nitric acidic residue of tin soldering |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1023025C (en) |
Families Citing this family (7)
| 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 |
| CN104046784B (en) * | 2014-07-07 | 2019-02-12 | 扬州宁达贵金属有限公司 | A kind of recovery method of argentiferous scolding tin 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 |
| CN111705216B (en) * | 2020-06-16 | 2021-12-03 | 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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1990
- 1990-06-23 CN CN90103200A patent/CN1023025C/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| CN1057865A (en) | 1992-01-15 |
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