CN85106670A - Extract precious metal with the CONTROLLED POTENTIAL method from the anode sludge - Google Patents
Extract precious metal with the CONTROLLED POTENTIAL method from the anode sludge Download PDFInfo
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- CN85106670A CN85106670A CN198585106670A CN85106670A CN85106670A CN 85106670 A CN85106670 A CN 85106670A CN 198585106670 A CN198585106670 A CN 198585106670A CN 85106670 A CN85106670 A CN 85106670A CN 85106670 A CN85106670 A CN 85106670A
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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
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Abstract
Extract precious metal with the CONTROLLED POTENTIAL method from the anode sludge.The invention belongs to precious metal hydrometallurgy.Its method is that material is placed HCl and NaCl medium.In 75~85 ℃, add NaClO and make the oxidation reduction potential control of system in 400~460 millivolts, select to leach.The leached mud that leaves precious metal can adopt in 600~650 millivolts of current potentials according to its characteristics and leach once more; Or with the leached mud dissolving, the precious metal in the solution is reduced respectively, settles out, with the crude metal or the precious metal concentrate that obtain purity>95%, the rate of recovery can reach more than 98%.Present method is mainly used in the precious metals metallurgy process and extracts, the high and low metal separation of enrichment and purified.
Description
The wet method that the invention relates to precious metal is extracted metallurgical.
To so far, the application of known relevant controlling potentiometry on hydrometallurgy all is separating copper, nickel from matte, sulphide ores or alloy, extracts precious metal.With CONTROLLED POTENTIAL method logical chlorine in the HCl medium, in 350~450 millivolts of scopes of current potential, handle matte under 80 ℃ of temperature as (Journal of metals, 1975, Vol.27, No.5,6~9) such as L.R.Hougen, reclaim copper, nickel and precious metal; (non-ferrous metal (smelting part) such as Xiong Zongguo, 1980, No2,21~26) with CONTROLLED POTENTIAL method logical chlorine in the HCl medium, in 400 ± 10 millivolts of scopes of current potential, handling the copper ashes of the high floating magnetic cupronickel that is produced of ice nickel mill after HCl leaches nickel under 80 ℃ of temperature, reclaim copper, nickel and precious metal.The leached mud of aforesaid method gained is to adopt the method for repeated calcination or vitriol oil digestion and obtain concentrate.About using the CONTROLLED POTENTIAL method from the anode sludge, particularly from lead, antimony anode mud, extract the method for precious metal, be not reported so far.The shortcoming of aforesaid method is, and is poor to leaching effect plumbous, antimony, if be used for lead, antimony anode mud is handled, and then can not separate expensive, base metal effectively, in addition the aforesaid method cycle longer, environmental pollution is heavier relatively.
The object of the present invention is to provide a kind of full wet process method of extracting precious metal (Au, Ag, Pt, Pd, Os, Ir, Ru, Rh) with the CONTROLLED POTENTIAL method from lead, antimony, nickel anode mud, this method can be separated expensive, base metal effectively, cycle is short, cost is low, environmental pollution is little, precious metal rate of recovery height.
Method provided by the present invention, be with said anode sludge material in 4~6NHCl, 1~1.4N NaCl medium, at 75~85 ℃, preferably in 80 ± 2 ℃ of temperature ranges, in solid (weight): liquid (volume)=1: 8~15, preferably under 1: 10 the condition, stir adding oxygenant NaClO down, the oxidation reduction potential control that makes system is selected to leach in 400~460 millivolts of scopes, make base metal change leach liquor over to, precious metal is stayed in the leached mud.Make oxygenant with NaClO, base metals such as lead that logical chlorine is difficult to thoroughly remove, antimony can thoroughly be removed.After selecting to leach, the base metal more than 98% changes leach liquor over to.The oxidation reduction potential control scope of said system changes with the difference of material composition, and, precious metal stripping rate the highest with the base metal solubility rate is minimum to be its optimum range, and the best potential range of different material needs specifically determine according to experiment.Common best potential range is: 430~460 millivolts (to Au, Ag, Pt, Pd), or 400~420 millivolts (to Os, Ir, Ru, Rh).Potential value can be measured saturated calomel electrode with platinum electrode.The control of best potential range, when leaching continuously be with material, solution and oxygenant by a certain percentage, the given pace adding, can make current potential remain on predetermined scope; Be interrupted when grasping, only need the add-on of controlled oxidation agent NaClO can make current potential remain on pre-determined range.If after stopping to add NaClO, current potential did not descend in 20~30 minutes or descends seldom, was its reaction end, can filter.The acidity of medium is looked material and is contained the antimony amount and increase and decrease, and contains antimony 20~40%, is advisable with 6N HCl, if surpass 60%, then is advisable with 4N HCl.The adding of NaCl can increase plumbous leaching effect, and its consumption can change at 1~1.4N according to the content of lead, if plumbous 20~30%, is advisable with 1.2N.
When containing silver-colored that needs reclaim in the said anode, then leach medium and only use 4~6N HCl, extraction temperature is 85~95 ℃, all the other terms and conditions and operation steps are same as described above.
The processing of leached mud can adopt diverse ways to handle according to material feature.Precious metal (Au in leached mud, Pt, Pd, at least a element among the Rh) grade is more than 30~70%, and insoluble impurity more after a little while, then can adopt the CONTROLLED POTENTIAL method to leach once more, be about to said leached mud and place 2~3N HCl medium (according to the NaCl that how much also can add 0~0.5N of lead tolerance), with above-mentioned identical temperature and solid-to-liquid ratio (solid-to-liquid ratio is preferably 1: 15) under, stir and add NaClO down, the oxidation reduction potential control that makes system is at 600~650 millivolts, preferably in 630~650 millivolts, select once more to leach, high and low metal is further separated.In leaching for the second time, there is small amount of precious metals to change over to together in the leach liquor, available known, suitable reductive agent and precipitation agent (gold Na for example together with base metal
2SO
3Reduction, platinum reduces or NH with Cu
4Cl precipitation etc.) respectively with the precious metal reduction, settle out, filter, wash, dry with soluble noble metal not, to obtain the thick gold or the precious metal concentrate of purity>95%.For the leached mud except that above-mentioned situation, then add NaClO or Cl with HCl
2Under 80 ± 2 ℃,, respectively the precious metal in the solution is reduced, settles out, filter then, wash, drying, can obtain the thick gold or the precious metal concentrate of purity>96% with known, suitable reductive agent and precipitation agent with its dissolving.
Advantage of the present invention is: (1) full wet process, and operation is few, cycle short (when particularly application controls current potential secondary leached, the cycle can shorten 8~10 times), expensive, base metal good separating effect, precious metal rate of recovery height; (2) operating process is simple, is easy to realize automatic control; (3) agents useful for same is inexpensive, operational condition good, and contaminate environment is very little; (4) the present invention also can handle the material that other contains precious metal except that handling lead, antimony, nickel anode mud.To copper anode mud, present method can be used for leaching copper, nickel wherein, but then effect is relatively poor to selenium, tellurium.
Embodiment one, with composition is (weight %) Au3.99, Cu14.05, Ni4.17, Pb21.18, the antimony anode mud of Sb38.00 are that raw material extracts gold, in 6N HCl, 1.2N NaCl medium, under 80 ℃ of the temperature, add NaClO and make the system oxidation reduction potential control in 430~450 millivolts, select to leach, separate expensive, base metal.The gained leached mud adds NaClO and makes the system oxidation reduction potential control select once more to leach under 630~650 millivolts in 3N HCl, 0.5N NaCl medium, adjusts solution acidity at 1~2N, uses Na
2SO
3Reduction enters a small amount of gold in the solution, filters, and obtains the thick gold of purity>95%.Handle antimony anode mud 9964 grams, acquisition purity is 98.8% thick golden 396.36 grams, the rate of recovery 98.5%.
Embodiment two, are (weight %) Au0.89 with composition, Cu3.18, Ni0.67, Pb12.60, the lead anode slurry of Sb69.94 is at 4N HCl, in the 1.2N NaCl medium, add NaClO hierarchy of control redox potential at 440~460 millivolts, select to leach, separate high and low metal.With the leached mud dissolving, use Na
2SO
3Reduction, the thick gold of acquisition purity>96%.Handle lead anode slurry 19500 grams, acquisition purity is 96.7% thick golden 178.64 grams, the rate of recovery 99.5%.
The present invention is not limited to the foregoing description.
Claims (3)
1, with the method for CONTROLLED POTENTIAL method, it is characterized in that from lead, antimony, nickel anode mud extraction precious metal:
A, said anode sludge material is placed 4~6NHCl and 1~1.4NNaCl medium, in solid (weight): under the condition of liquid (volume)=1: 8~15, by adding oxidation reduction potential control that oxygenant NaClO makes system in 400~460 millivolts of scopes, select to leach;
B, when containing silver-colored that needs reclaim in the said anode sludge, then the said anode sludge is placed 4~6NHCl medium, under 85~95 ℃ of temperature, under other conditions condition identical, select leaching with A;
C, precious metal in the resulting leached mud is (only to Au, Pt, Pd, at least a element among the Rh) grade is more than 30~70%, and insoluble impurity more after a little while, then said leached mud is placed 2~3NHCl medium, in 75~85 ℃ of temperature, in solid (weight): under the condition of liquid (volume)=1: 8~15, adding NaClO makes the oxidation reduction potential control of system in 600~650 millivolts of scopes, select once more to leach, make expensive, one step of base metal separates, change small amount of precious metals in the leach liquor over to known, suitable reductive agent and precipitation agent reduce respectively, settle out, filter with soluble noble metal not, washing, oven dry;
D, the leached mud except that the C situation add NaClO or Cl with HCl
2Under 80 ± 2 ℃,, the precious metal in the solution is reduced respectively, settles out with known suitable reductive agent and precipitation agent with its dissolving.
2, the method for claim 1, it is characterized in that, said system is in carrying out CONTROLLED POTENTIAL selection first time leaching process, the oxidation reduction potential control of said system is (to Au, Pt, Pd, Ag) in 430~460 millivolts of scopes, or 400~420 millivolts of scopes interior (to Os, Ir, Ru, Rh), temperature is controlled in 80 ± 2 ℃ of scopes, solid: liquid=1: 10.
3, method as claimed in claim 1 or 2, it is characterized in that, when said system carries out that the second time, CONTROLLED POTENTIAL select to leach, the redox potential of said system (to Au, Pt, Pd, Rh) is controlled in 630~650 millivolts of scopes, temperature is controlled in 80 ± 2 ℃, solid: liquid=1: 15.
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CN198585106670A CN85106670B (en) | 1985-08-31 | 1985-08-31 | Process for extraction of noble metal from anode mud by method of controlling potential |
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CN198585106670A CN85106670B (en) | 1985-08-31 | 1985-08-31 | Process for extraction of noble metal from anode mud by method of controlling potential |
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CN85106670B CN85106670B (en) | 1988-06-15 |
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Cited By (15)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1045794C (en) * | 1996-09-16 | 1999-10-20 | 昆明贵金属研究所 | Method for extracting gold, silver and valuable metals from high-arsenic lead anode mud |
CN102978414A (en) * | 2012-11-28 | 2013-03-20 | 大连东泰产业废弃物处理有限公司 | Method for precipitating gold from cyanogen-containing gold-plated waste liquid |
CN104894383A (en) * | 2015-06-09 | 2015-09-09 | 上海交通大学 | Leaching method of gold and copper in gold-contained electronic waste |
CN105300961A (en) * | 2015-10-16 | 2016-02-03 | 贵研检测科技(云南)有限公司 | Separation and enrichment determination method for Ir, Rh, Pt, Pd and Au in secondary resource material |
CN105705664A (en) * | 2013-09-27 | 2016-06-22 | 西班牙联合技术公司 | Process for the selective recovery of lead and silver |
CN105779765A (en) * | 2016-03-23 | 2016-07-20 | 江西铜业集团公司 | Method for separating and recovering rare and precious metals in chlorination leaching liquid |
CN105779766A (en) * | 2016-03-23 | 2016-07-20 | 江西铜业集团公司 | Method for gathering platinum and palladium in solution |
CN106319224A (en) * | 2016-08-08 | 2017-01-11 | 广东先导稀材股份有限公司 | Indium recovery method |
CN106498168A (en) * | 2016-11-16 | 2017-03-15 | 广东先导稀材股份有限公司 | The method for reclaiming gallium from oil-containing GaAs mud |
CN107447107A (en) * | 2017-08-23 | 2017-12-08 | 中南大学 | A kind of method that rich and honour antimony control current potential is separated and recovered from base metal |
CN107849636A (en) * | 2014-12-25 | 2018-03-27 | 三菱综合材料株式会社 | The leaching method of valuable metal contained by decopper(ing) mud |
CN108034821A (en) * | 2017-11-14 | 2018-05-15 | 河南中原黄金冶炼厂有限责任公司 | A kind of wet processing process of earth of positive pole smelting slag |
CN111593203A (en) * | 2020-05-20 | 2020-08-28 | 金川集团股份有限公司 | Method for separating and extracting gold and palladium from high-palladium-content silver anode mud |
CN115323187A (en) * | 2022-08-19 | 2022-11-11 | 中南大学 | Method for removing SnPbFe impurity in copper anode mud rich in platinum group metal |
CN117887977A (en) * | 2024-01-12 | 2024-04-16 | 武汉理工大学 | Method for selectively leaching Au and Ag in electronic waste step by electrochemical oxidation |
-
1985
- 1985-08-31 CN CN198585106670A patent/CN85106670B/en not_active Expired
Cited By (24)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1045794C (en) * | 1996-09-16 | 1999-10-20 | 昆明贵金属研究所 | Method for extracting gold, silver and valuable metals from high-arsenic lead anode mud |
CN102978414A (en) * | 2012-11-28 | 2013-03-20 | 大连东泰产业废弃物处理有限公司 | Method for precipitating gold from cyanogen-containing gold-plated waste liquid |
CN102978414B (en) * | 2012-11-28 | 2015-02-18 | 大连东泰产业废弃物处理有限公司 | Method for precipitating gold from cyanogen-containing gold-plated waste liquid |
CN105705664A (en) * | 2013-09-27 | 2016-06-22 | 西班牙联合技术公司 | Process for the selective recovery of lead and silver |
US10151015B2 (en) | 2014-12-25 | 2018-12-11 | Mitsubishi Materials Corporation | Method for leaching precious metal contained in decopperized anode slime |
CN107849636A (en) * | 2014-12-25 | 2018-03-27 | 三菱综合材料株式会社 | The leaching method of valuable metal contained by decopper(ing) mud |
CN104894383A (en) * | 2015-06-09 | 2015-09-09 | 上海交通大学 | Leaching method of gold and copper in gold-contained electronic waste |
CN105300961A (en) * | 2015-10-16 | 2016-02-03 | 贵研检测科技(云南)有限公司 | Separation and enrichment determination method for Ir, Rh, Pt, Pd and Au in secondary resource material |
CN105779765B (en) * | 2016-03-23 | 2018-03-27 | 江西铜业集团公司 | A kind of method by rare precious metal separation and recovery in chloridizing leach solution |
CN105779765A (en) * | 2016-03-23 | 2016-07-20 | 江西铜业集团公司 | Method for separating and recovering rare and precious metals in chlorination leaching liquid |
CN105779766A (en) * | 2016-03-23 | 2016-07-20 | 江西铜业集团公司 | Method for gathering platinum and palladium in solution |
CN106319224B (en) * | 2016-08-08 | 2018-01-23 | 广东先导稀材股份有限公司 | The recovery method of indium |
CN106319224A (en) * | 2016-08-08 | 2017-01-11 | 广东先导稀材股份有限公司 | Indium recovery method |
CN106498168A (en) * | 2016-11-16 | 2017-03-15 | 广东先导稀材股份有限公司 | The method for reclaiming gallium from oil-containing GaAs mud |
CN107447107B (en) * | 2017-08-23 | 2018-11-09 | 中南大学 | A kind of method that wealth and rank antimony control current potential is separated and recovered from base metal |
CN107447107A (en) * | 2017-08-23 | 2017-12-08 | 中南大学 | A kind of method that rich and honour antimony control current potential is separated and recovered from base metal |
CN108034821A (en) * | 2017-11-14 | 2018-05-15 | 河南中原黄金冶炼厂有限责任公司 | A kind of wet processing process of earth of positive pole smelting slag |
CN108034821B (en) * | 2017-11-14 | 2019-08-02 | 河南中原黄金冶炼厂有限责任公司 | A kind of wet processing process of earth of positive pole smelting slag |
CN111593203A (en) * | 2020-05-20 | 2020-08-28 | 金川集团股份有限公司 | Method for separating and extracting gold and palladium from high-palladium-content silver anode mud |
CN111593203B (en) * | 2020-05-20 | 2022-03-15 | 金川集团股份有限公司 | Method for separating and extracting gold and palladium from high-palladium-content silver anode mud |
CN115323187A (en) * | 2022-08-19 | 2022-11-11 | 中南大学 | Method for removing SnPbFe impurity in copper anode mud rich in platinum group metal |
CN115323187B (en) * | 2022-08-19 | 2023-08-22 | 中南大学 | Method for removing SnPbFe impurities in platinum group metal-rich copper anode slime |
CN117887977A (en) * | 2024-01-12 | 2024-04-16 | 武汉理工大学 | Method for selectively leaching Au and Ag in electronic waste step by electrochemical oxidation |
CN117887977B (en) * | 2024-01-12 | 2024-10-18 | 武汉理工大学 | Method for selectively leaching Au and Ag in electronic waste step by electrochemical oxidation |
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