CN85106670B - Process for extraction of noble metal from anode mud by method of controlling potential - Google Patents
Process for extraction of noble metal from anode mud by method of controlling potential Download PDFInfo
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- CN85106670B CN85106670B CN198585106670A CN85106670A CN85106670B CN 85106670 B CN85106670 B CN 85106670B CN 198585106670 A CN198585106670 A CN 198585106670A CN 85106670 A CN85106670 A CN 85106670A CN 85106670 B CN85106670 B CN 85106670B
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Abstract
The present invention relates to a method for extracting noble metals from anode mud by a potential controlling method, which belongs to noble metal hydrometallurgy. The method comprises the steps: materials are put into an HCl and NaCl medium; at the temperature of 75 to 85 DEG C, NaClO is added to control the systemic oxidation-reduction potential to be within 400 to 460 mv so as to being precipitated selectively; the precipitated slag containing noble metals can be precipitated again at the potential of 600 to 650 mv according to the characteristics, or the precipitated slag is dissolved, and the noble metals in the solution are respectively reduced and precipitated to obtain coarse metal or noble metal ore concentrate with the purity of more than 95%; the recovery rate can reach more than 98%. The method is mainly used for the extraction and the enrichment of noble metals, and the separation of the refined noble metals and the refined base metals in the metallurgical process.
Description
The wet method that the invention relates to precious metal is extracted metallurgical.
To so far, the application of known relevant controlling potentiometry in hydrometallurgy, is all separating copper, nickel from matte, sulphide ores or alloy, extracts precious metal.If (Journal of metals, 1975, vol.27, № .5,6～9) such as L.R.Hougen are with controlling potentiometry logical chlorine in HCl medium, within the scope of 350～450 millivolts of current potentials, at 80 DEG C of temperature, process matte, reclaim copper, nickel and precious metal; (the non-ferrous metal (Smelting Part) such as Xiong Zongguo, 1980, № 2,21～26) with controlling potentiometry logical chlorine in HCl medium, within the scope of 400 ± 10 millivolts of current potentials, at 80 DEG C of temperature, process the copper ashes of the floating Magnetic Copper nickelalloy producing of high ice nickel mill after HCl leaching nickel, 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 with controlling potentiometry from the anode sludge, particularly from lead, antimony anode mud, extract the method for precious metal, so far there are no reports.The shortcoming of aforesaid method is, poor to leaching effect plumbous, antimony, if for plumbous, antimony anode mud processing, can not effectively separate expensive, base metal, in addition the aforesaid method cycle longer, environmental pollution is relatively heavier.
The object of the present invention is to provide a kind of with controlling the full wet process method of potentiometry from lead, antimony, nickel anode mud extraction precious metal (Au, Ag, Pt, Pd, Os, Ir, Ru, Rh), the method can separate expensive, base metal effectively, cycle is short, and cost is low.Environmental pollution is little, and the precious metal rate of recovery is high.
Method provided by the present invention, be by said anode sludge material in 4～6NHCl, 1～1.4NNaCl medium, at 75～85 DEG C, preferably in 80 ± 2 DEG C of temperature ranges, in solid (weight): liquid (volume)=1: 8～15, preferably under the condition of 1: 10, under stirring, add oxygenant NaClO, make the oxidation reduction potential control of system within the scope of 400～400 millivolts, carry out selectively leaching, make base metal proceed to leach liquor, precious metal is stayed in leached mud.Make oxygenant with NaClO, the base metal such as lead, antimony that just can make logical chlorine be difficult to thoroughly remove can thoroughly be removed.After selectively leaching, more than 98% base metal proceeds to leach liquor.The oxidation reduction potential control scope of said system, changes with the difference of material composition, and, precious metal stripping rate the highest taking base metal solubility rate is minimum is its optimum range, and the best potential range of different material need specifically be determined according to experiment.Common best potential range is: 430～460 millivolts (to Au, Ag, Pt, Pd), or 400～420 millivolts (to Oa, Ir, Ru, Rh).Potential value can be measured saturated calomel electrode with platinum electrode.The control of best potential range, while leaching continuously, be by material, solution and oxygenant by a certain percentage, given pace adds, and can make current potential remain on predetermined scope; Be interrupted while behaviour, only need the add-on of controlling oxygenant NaClO can make current potential remain on pre-determined range.Add after NaClO if stop, current potential did not decline or declines seldom in 20～30 minutes, was its reaction end, can filter.The acidity of medium increases and decreases containing antimony amount depending on material, containing antimony 20～40%, is advisable with 6NHCl, if exceed 60%, is advisable with 4NHCl.Adding of NaCl can increase plumbous leaching effect, and its consumption can change at 1～1.4N according to plumbous content, if plumbous 20～30%, is advisable with 1.2N.
When in said anode, contain needs reclaim silver-colored time, leach medium and only use 4～6NHCl, extraction temperature is 85～95 DEG C, all the other terms and conditions and operation steps are same as described above.
The processing of leached mud, can adopt diverse ways processing according to material feature.As the precious metal (Au in leached mud, Pt, Pd, at least one element in Rh) grade is more than 30～70%, and when insoluble impurity is less, can adopt control potentiometry again to leach, be placed in 2～3NHCl medium (also can add the NaCl of 0～0.5N according to the number of lead tolerance) by said leached mud, with above-mentioned identical temperature and solid-to-liquid ratio (solid-to-liquid ratio is preferably 1: 15) under, under stirring, add NaClO, make the oxidation reduction potential control of system at 600～650 millivolts, preferably in 630～650 millivolts, again carry out selectively leaching, high and low metal is further separated.In leaching for the second time, there is a small amount of precious metal to proceed to together in leach liquor together with base metal, available known, suitable reductive agent and precipitation agent (for example gold Na
2sO
3reduction, Cu reduction or NH for platinum
4cl precipitation etc.) respectively by precious metal reduction, settle out, filter, wash, dry with together with soluble noble metal not, to obtain thick gold or the precious metal concentrate of purity > 95%.For the leached mud except above-mentioned situation, add NaClO or Cl with HCl
2at 80 ± 2 DEG C, dissolved, with known, suitable reductive agent and precipitation agent reduce the precious metal in solution, settle out respectively, then filter, wash, be dried, and can obtain thick gold or the precious metal concentrate of purity > 96%.
Advantage of the present invention is: (1) full wet process, and operation is few, the cycle short (when particularly application controls current potential secondary leaches, the cycle can shorten 8～10 times), expensive, base metal good separating effect, the precious metal rate of recovery is high; (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, except processing lead, antimony, nickel anode mud, also can process other material containing precious metal.To copper anode mud, present method can be used for leaching copper, nickel wherein, but effect is poor to selenium, tellurium.
Embodiment mono-, with composition be (% by weight) Au3.99, Cu14.05, Ni4.17, Pb21.18, the antimony anode mud of Sb38.00 is that raw material extracts gold, in 6NHCl, 1.2NNaCl medium, at 80 DEG C of temperature, add NaClO and make system oxidation reduction potential control in 430～450 millivolts, carry out selectively leaching, separate expensive, base metal.Gained leached mud, in 3NHCl, 0.5NNaCl medium, adds NaClO and makes system oxidation reduction potential control selectively leaching again under 630～650 millivolts, adjusts solution acidity at 1～2N, uses Na
2sO
3reduction enters a small amount of gold in solution, filters, and obtains the thick gold of purity > 95%.Process 9964 grams of antimony anode muds, to obtain purity be 98.8% thick golden 396.36 grams, the rate of recovery 98.5%.
Embodiment bis-, using composition is (% by weight) Au0.89, Cu3.18, Ni0.67, Pb12.60, the lead anode slurry of Sb69.94, at 4NHCl, in 1.2NNaCl medium, add NaClO hierarchy of control redox potential at 440～460 millivolts, carry out selectively leaching, separate high and low metal.Leached mud is dissolved, use Na
2sO
3reduction, the thick gold of acquisition purity > 96%.Process 19500 grams of lead anode slurries, to obtain purity be 96.7% thick golden 178.64 grams, the rate of recovery 99.5%.
The present invention is not limited to above-described embodiment.
Claims (3)
1. with controlling the method for potentiometry from lead, antimony, nickel anode mud extraction precious metal, it is characterized in that:
A, said anode sludge material is placed in to 4～6NHCl and 1～1.4NNaCl medium, in solid (weight): under the condition of liquid (volume)=1: 8～15, by adding oxygenant NaClO to make the oxidation reduction potential control of system within the scope of 400～460 millivolts, carry out selectively leaching;
B, when in the said anode sludge, contain needs reclaim silver-colored time, the said anode sludge is placed in to 4～6NHCl medium, at 85～95 DEG C of temperature, under other conditions condition identical with A, carry out selectively leaching;
C, precious metal in the leached mud obtaining is (only to Au, Pt, Pd, at least one element in Rh) grade is more than 30～70%, and when insoluble impurity is less, said leached mud is placed in to 2～3NHCl medium, in 75～85 DEG C of temperature, in solid (weight): under the condition of liquid (volume)=1: 8～15, add NaClO to make the oxidation reduction potential control of system within the scope of 600～650 millivolts, again carry out selectively leaching, make expensive, base metal one step separates, proceed to a small amount of precious metal in leach liquor with known, suitable reductive agent and precipitation agent reduce respectively, settle out, filter with together with soluble noble metal not, washing, dry,
D, leached mud except C situation, add NaClO or Cl with HCl
2at 80 ± 2 DEG C, dissolved, the precious metal in solution is reduced respectively, settled out with known suitable reductive agent and precipitation agent.
2. the method for claim 1, it is characterized in that, said system is controlling for the first time in current potential selectively leaching process, the oxidation reduction potential control of said system is (to Au, Pt, Pd, Ag) within the scope of 430～460 millivolts, or within the scope of 400～420 millivolts (to Os, Ir, Ru, Rh), temperature is controlled within the scope of 80 ± 2 DEG C, solid: liquid=1: 10.
3. method as claimed in claim 1 or 2, it is characterized in that, in the time that said system is controlled current potential selectively leaching for the second time, the redox potential (to Au, Pt, Pd, Rh) of said system is controlled within the scope of 630～650 millivolts, temperature is controlled in 80 ± 2 DEG C, solid: liquid=1: 15.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN198585106670A CN85106670B (en) | 1985-08-31 | 1985-08-31 | Process for extraction of noble metal from anode mud by method of controlling potential |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN198585106670A CN85106670B (en) | 1985-08-31 | 1985-08-31 | Process for extraction of noble metal from anode mud by method of controlling potential |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN85106670A CN85106670A (en) | 1987-03-11 |
| CN85106670B true CN85106670B (en) | 1988-06-15 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN198585106670A Expired 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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| CN (1) | CN85106670B (en) |
Families Citing this family (15)
| 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 |
| 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 |
| RU2670117C2 (en) * | 2013-09-27 | 2018-10-18 | Текникас Реунидас, С.А. | Process for the selective recovery of lead and silver and carbonate lead and silver concentrate, obtained by the method above |
| JP6652741B2 (en) | 2014-12-25 | 2020-02-26 | 三菱マテリアル株式会社 | Leaching method of valuable metals contained in copper removal slime |
| 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 |
| CN105779766A (en) * | 2016-03-23 | 2016-07-20 | 江西铜业集团公司 | Method for gathering platinum and palladium in solution |
| 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 |
| 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 |
| CN106498168B (en) * | 2016-11-16 | 2018-01-23 | 广东先导稀材股份有限公司 | The method that gallium is reclaimed 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 |
| 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 |
| 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 |
| 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 |
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1985
- 1985-08-31 CN CN198585106670A patent/CN85106670B/en not_active Expired
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| CN85106670A (en) | 1987-03-11 |
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