CN1381612A - Method for producing antimony by electrolyzing antimony-containing sulfide mineral pulp - Google Patents
Method for producing antimony by electrolyzing antimony-containing sulfide mineral pulp Download PDFInfo
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- CN1381612A CN1381612A CN02103704A CN02103704A CN1381612A CN 1381612 A CN1381612 A CN 1381612A CN 02103704 A CN02103704 A CN 02103704A CN 02103704 A CN02103704 A CN 02103704A CN 1381612 A CN1381612 A CN 1381612A
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Abstract
A method for producing antimony by electrolyzing antimony-containing sulfide mineral pulp relates to a hydrometallurgical process for extracting antimony from antimony-containing sulfide minerals, complex antimony/lead mixed minerals, antimony/gold mixed minerals and antimony concentrates. The method is characterized in that antimony-containing sulfide minerals are subjected to ore pulp electrolysis in a hydrochloric acid-ammonium chloride medium to produce the metal antimony plate, wherein the process conditions comprise that the hydrochloric acid concentration in the ore pulp is 15-40 g/L, the ammonium chloride concentration is 250g/L, the antimony concentration is 10-50 g/L, the temperature is room temperature to 70 ℃, and the cathode current density is 150-2. The method has short process flow, can produce the metal antimony plate by one step, has high metal recovery rate and low leaching temperature, can realize the selective leaching of antimony, lead and gold in complex minerals are inhibited in slag, sulfur exists in the leached slag in the form of elemental sulfur, most of harmful element arsenic also exists in the slag, and is an environment-friendly process.
Description
(1) technical field
The method of preparing antimony by electrolyzing slurry of sulfide ore containing antimony, relate to from antimony concentrate or the complicated unmanageable antimony sulfide mineral that contains, as jamesonite, antimony/golden collective concentrate or contain in the arsenic antimony concentrate method of extracting antimony, particularly from above-mentioned antimony-containing mineral, extract the method for antimony with the in-pulp electrolysis technology.
(2) background technology
Traditional wet method stibium smelting technology is to adopt antimony concentrate sodium sulphite leaching-purification of leaching liquor-diaphragm electrodeposition to produce electric antimony.But there is following shortcoming in it: 1) leaching process exists the hyperplasia accumulation of sodium sulphite, the oxidation of polysulfide and the accumulation problem of vitriol and sulphite; 2) current efficiency is low, is generally 70%, thereby power consumption height (3000-4000kWh/tSb); 3) extraction temperature height, the sodium sulphite volatilization is big, severe operational environment; 4) alkaline consumption height, complex technical process, antimony concentrate needs numerous and diverse sodium sulphite and removes and recovery system after leaching.At the deficiency of conventional wet stibium smelting technology, people have carried out the research of acid wet method antimony regulus in recent years, mainly contain: new chlorination-hydrolysis method, villaumite chlorination-low-temperature pyrolysis method and chlorine gas selecting lixiviation process, their common advantages are to have eliminated SO
2To the pollution problem of environment, antimony lead separates thoroughly, but shortcoming is also respectively arranged.It is higher that the stibium trioxide of new antimony that chlorination-hydrolysis method is produced contains arsenic, do not reach the zero level requirement, and the product weathering resistance is poor, because of product form is limit, also can't produce on a large scale; Villaumite chlorination-low-temperature pyrolysis method and chlorine gas selecting lixiviation process be to the seriously corroded of equipment, and do not have and similarly put into practice factory, still needs and carry out the pilot-plant test checking.
Slurry electrolysis is as emerging in recent years a kind of hydrometallurgical technology; integrate leaching-electrodeposition; mineral are leached in the anodic oxidation reactions oxidation that makes full use of electrolytic deposition process; not only simplified the hydrometallurgy flow process greatly; the metal recovery rate height; and make full use of the energy, and energy consumption is low, and environment protection is good.Slurry electrolysis also has following characteristics when keeping the metallurgical advantage of conventional wet:
1. one go on foot output metal and elementary sulfur, sulphur and poisonous impurity arsenic etc. enters in the leached mud with iron and gangue mineral, and process is simple.Because effects of ion concentration is low, leached mud is easy to filter and washing.The elementary sulfur that produces is convenient to store and transportation, has solved sulphuric acid output surplus in the world, sulfuric acid transportation and the difficult problem of sale.
2. operation under the condition of normal pressure and intimate normal temperature, equipment can be used polyphenoils corrosion materials such as cheap glass reinforced plastic, polypropylene.
3. the required bath voltage of electrolysis is lower, owing to made full use of the oxygen reduction voltinism of anode and cathode, whole process power consumption is few.
4. reagent consumption is few, the metal recovery rate height.
Handle sulphide ores with slurry electrolysis, done many research work at home and abroad.Just began one's study in 1978 behavior of different material in in-pulp electrolysis of elements such as containing Cu, Pb, Zn, Bi, Mn, Au, Ag, Ni, Co of Beijing Mine and Metallurgy General Inst, and obtained remarkable progress, as the in-pulp electrolysis in the in-pulp electrolysis of chalcopyrite, the in-pulp electrolysis of cupric secondary material, plumbous zinc-silver mixing ore deposit, the in-pulp electrolysis of pyrolusite and the in-pulp electrolysis repercussion study of lithium bismuthinite.
Traditional in-pulp electrolysis technology, utilize the higher characteristic of most metal ions solubleness in chloride system, mostly adopt hydrochloric acid-sodium-chlor (or calcium chloride) system, to eliminate the anodic oxygen evolution reaction, reduce bath voltage, cut down the consumption of energy, this not only helps the formation of elemental sulfur in the sulfide mineral, also helps the leaching that mineral itself have valence component simultaneously.In-pulp electrolysis as mineral such as bismuthinite, chalcopyrite, lead glances.But concerning Refractory Sb-Pb Concentrate, it is unfavorable adopting hydrochloric acid-sodium-chlor (or calcium chloride) system.This system is when the in-pulp electrolysis of antimony lead ore deposit, antimony and lead can leach simultaneously fully, antimony after the leaching, lead will generate antimony, plumbous chloro-complex with the chlorion complexing in the solution, cause the plumbous bigger solubleness that in this system, has, because the redox potential difference of antimony, lead is little, antimony and lead can be separated out simultaneously at negative electrode, can't realize effective separation of antimony, lead.
(3) summary of the invention
The objective of the invention is the deficiency that exists in the above-mentioned technology, it is effective to provide a kind of antimony selectivity to leach, and extraction temperature is low, the method from preparing antimony by electrolyzing slurry of sulfide ore containing antimony that technology is simple, flow process is short.
The objective of the invention is to be achieved through the following technical solutions.
The method of preparing antimony by electrolyzing slurry of sulfide ore containing antimony, it is characterized in that to contain the antimony sulphide concentrate and in hydrochloric acid-ammonium chloride medium, carry out in-pulp electrolysis, contain antimony in the antimony sulfide mineral, lead, sulphur at anode generation electro-chemical reaction, generate antimony ion, lead chloride and elemental sulfur respectively, antimony ion directly obtains the metallic antimony plate on the positive plate of cathodic electricity, the PbCl of generation
2, elemental sulfur precipitation enters in the slag, again with the electrolytic slag that obtains through the carbon ammonium transform, extraction carries sulphur, obtains lead ore concentrate and elemental sulfur respectively; The processing condition of control electrolysis leaching process are: concentration of hydrochloric acid is 15-40g/L in the in-pulp electrolysis liquid, and ammonium chloride concentration is 150-250g/L, and antimony concentration is 10-50g/L, and temperature is a room temperature to 70 ℃, cathode current density 150-200A/m
2
In the method for the present invention, when electrolysis was leached, the acidity that improves ore pulp helped the leaching of antimony, prevents the hydrolysis of antimony, but peracid is spent then acid mist increase of height, and loss through volatilization increases, and controls best concentration of hydrochloric acid 20-30g/L, and ammonium chloride concentration is 180-220g/L.
In the solution antimony concentration from theory keep high dense will be favourable to this electrolytic deposition process, but be subjected to the handled restriction that contains antimony sulfide mineral antimony content to be generally 50g/L, separating out with tabular for assurance negative electrode antimony, for the concentration in the electrolytic solution should be higher than 10g/L, is good with 30-50g/L.
Method of the present invention, the control extraction temperature is good at 60 ℃, realizes that the low temperature of antimony ore leaches, and can reduce the loss through volatilization of acid, guarantee that the sulphur in the mineral is oxidized to elementary sulfur rather than sulfuric acid, and pyrite is not oxidized substantially.
Reclaim the method for plumbous and sulphur in the method in-pulp electrolysis leached mud of the present invention, electrolysis leached mud after the liquid-solid separation is added in the ammonium bicarbonate soln, lead chloride is converted into lead carbonate to be stayed in the slag, the ammonium chloride that generates enters solution, carry out again adopting after the solid-liquid separation conventional sulphur solvent extraction with the sulphur content in the slag from obtaining elemental sulfur, obtain lead ore concentrate.
Method from preparing antimony by electrolyzing slurry of sulfide ore containing antimony of the present invention based on the in-pulp electrolysis novel process, is carried out in-pulp electrolysis to containing the antimony sulfide mineral in hydrochloric acid-ammonium chloride medium, directly obtain the metallic antimony plate at negative electrode, and makes plumbous with PbCl
2Form be precipitated into slag.The in-pulp electrolysis slag obtains lead ore concentrate and elemental sulfur product respectively through carbon ammonium conversion-abstraction desulfurization, low, the leaded height of the lead ore concentrate sulfur-bearing that produces, the elementary sulfur that produces is convenient to store and transportation.This technology can be connected effectively with traditional plumbous pyrometallurgical smelting process, all has very strong competitive power aspect economic benefit and the environmental protection.
Method of the present invention has realized finishing containing the selective extraction of antimony in the antimony sulfide mineral under low extraction temperature and acidity.Sulphur in the mineral is oxidized into elemental sulfur rather than sulfuric acid.Antimony in the mineral is efficiently leached, and lead then stays in slag, and other harmful element such as arsenic also major part are solidificated in the leached mud.Be one and be used to contain the simple, efficient of antimony sulfide mineral extraction antimony, eco-friendly technology.
Adopt method of the present invention, the leaching yield of antimony does not produce the problem of sulphur parcel greater than 96%, and the sulphur in the concentrate is oxidized to elementary sulfur, realizes antimony, the plumbous separation in leaching, and most of lead enters in the slag.Realized that antimony, a plumbous step separate.The antimony that is leached is separated out with the form of metallic antimony antimony plate at negative plate, has realized that a step of antimony extracts.Another characteristics wide adaptability of method of the present invention can be handled complexity and contain the antimony sulfide mineral, the leaching yield height of antimony.
(4) description of drawings
Fig. 1 is the principle flow chart of method of the present invention.
(5) embodiment
Method from preparing antimony by electrolyzing slurry of sulfide ore containing antimony, at first preparation contains hydrochloric acid-ammonium chloride medium solution of antimony 10-50g/L, hydrochloric acid 15-40g/L, ammonium oxide 150-250g/L, sulphide ores is carried out ore pulp leach electrolysis in medium, antimony electrodeposition in the ore pulp directly obtains the metallic antimony plate on negative plate, the lead in the ore pulp is with PbCl
2Form, sulphur generate elemental sulfur form precipitation and enter in the slag, with the electrolytic slag that obtains through the carbon ammonium transform, extraction carries sulphur, obtains lead ore concentrate and elemental sulfur respectively; Keeping the processing condition that in-pulp electrolysis leaches is: concentration of hydrochloric acid is 15-40g/L in the in-pulp electrolysis liquid, and ammonium chloride concentration is 150-250g/L, and antimony concentration is, temperature is a room temperature to 70 ℃, cathode current density 150-200A/m
2Electrolysis leached mud after the liquid-solid separation is added in the ammonium bicarbonate soln, lead chloride is converted into lead carbonate to be stayed in the slag, the ammonium chloride that generates enters solution, carry out again adopting after the solid-liquid separation conventional sulphur solvent extraction agent with the sulphur content in the slag from obtaining elemental sulfur, obtain lead ore concentrate.
With following indefiniteness embodiment technology of the present invention is further described, helping understanding of the present invention and advantage, and as the qualification to protection domain of the present invention, protection scope of the present invention is determined by claims.
Example 1
Used complicated antimony concentrate is formed: Sb23.4%, Fe14.7%, S23.57%, Pb27.8%.The in-pulp electrolysis leaching condition is: antimony concentrate granularity-50 μ m accounts for more than 90%, gets the 100g sample ore and carry out electrolysis in 5L in-pulp electrolysis groove, 60 ℃ of extraction temperatures, concentration of hydrochloric acid 30g/L, ammonium chloride concentration is 200g/L, and antimony concentration is 50g/L, cathode current density 150A/m
2Feeding electric weight is the required theoretical amount of weisspiessglanz.
Antimony leaching yield result is 99.12%, and negative electrode antimony contains antimony 98.78%, leaded 0.02%.
Embodiment 2
Used complicated antimony concentrate is formed: Sb16.1%, Fe11.2%, S18.8%, Pb19.8%.The in-pulp electrolysis leaching condition is: antimony concentrate granularity-74 μ m accounts for more than 70%, gets the 100g sample ore and carry out electrolysis in 5L in-pulp electrolysis groove, 30 ℃ of extraction temperatures, concentration of hydrochloric acid 20g/L, ammonium chloride concentration is 150g/L, and antimony concentration is 40g/L, cathode current density 160A/m
2Feeding electric weight is the required theoretical amount of weisspiessglanz.
Antimony leaching yield result is 96.58%, and negative electrode antimony contains antimony 98.98%, leaded 0.021%.
Embodiment 3
Used complicated antimony concentrate is formed: Sb28.5%, Fe16.5%, S24.7%, Pb34.6%.The in-pulp electrolysis leaching condition is: antimony concentrate granularity-74 μ m accounts for more than 70%, gets the 100g sample ore and carry out ore pulp leaching electrolysis, 50 ℃ of extraction temperatures in 5L in-pulp electrolysis groove, concentration of hydrochloric acid 15g/L, ammonium chloride concentration is 250g/L, and antimony concentration is 30g/L, cathode current density 180A/m
2Feeding electric weight is the required theoretical amount of weisspiessglanz.
Antimony leaching yield result is 97.18%, and negative electrode antimony contains antimony 97.57%, leaded 0.024%.
Embodiment 4
Used complicated antimony concentrate is formed: Sb25.1%, Fe18.2%, S28.8%.
The in-pulp electrolysis leaching condition is: antimony concentrate granularity-74 μ m accounts for more than 70%, gets the 100g sample ore and carry out in-pulp electrolysis in 5L in-pulp electrolysis groove, 50 ℃ of extraction temperatures, concentration of hydrochloric acid 40g/L, ammonium chloride concentration is 180g/L, and antimony concentration is 10g/L, cathode current density 200A/m
2Feeding electric weight is the required theoretical amount of weisspiessglanz.
Antimony leaching yield result 96.53%, negative electrode antimony contains antimony 98.46%.
Embodiment 5
Used complicated antimony concentrate is formed: Sb28.5%, Fe16.5%, S24.7%, Pb34.6%.The in-pulp electrolysis leaching condition is: antimony concentrate granularity-74 μ m accounts for more than 70%, gets the 100kg sample ore at 2.5m
3Carry out in-pulp electrolysis in the in-pulp electrolysis groove, 65 ℃ of extraction temperatures, concentration of hydrochloric acid 40g/L, ammonium chloride concentration are 200g/L, antimony concentration is 35g/L, cathode current density 200A/m
2Feeding electric weight is the required theoretical amount of weisspiessglanz.
Antimony leaching yield result is 96.14%, and negative electrode antimony contains antimony 97.57%, leaded 0.026%.
Claims (4)
1. the method for preparing antimony by electrolyzing slurry of sulfide ore containing antimony, it is characterized in that to contain the antimony sulphide concentrate and in hydrochloric acid-ammonium chloride medium, carry out in-pulp electrolysis, contain antimony in the antimony sulfide mineral, lead, sulphur at anode generation electro-chemical reaction, generate antimony ion, lead chloride and elemental sulfur respectively, antimony ion directly obtains the metallic antimony plate on the positive plate of cathodic electricity, the PbCl of generation
2, elemental sulfur precipitation enters in the slag, again with the electrolytic slag that obtains through the carbon ammonium transform, extraction carries sulphur, obtains lead ore concentrate and elemental sulfur respectively; The processing condition of control electrolysis leaching process are: concentration of hydrochloric acid is 15-40g/L in the in-pulp electrolysis liquid, and ammonium chloride concentration is 150-250g/L, and antimony concentration is 10-50g/L, and temperature is a room temperature to 70 ℃, cathode current density 150-200A/m
2
2. method according to claim 1 is characterized in that: concentration of hydrochloric acid is 20-30g/L in the ore pulp leach liquor, and ammonium chloride concentration is 180-220g/L, and antimony concentration is 30-50g/L.
3. method according to claim 1 is characterized in that: leaching electrolysis temperature is 60 ℃.
4. method according to claim 1, it is characterized in that: reclaiming plumbous in the in-pulp electrolysis leached mud is that the electrolysis leached mud after liquid-solid the separation is added in the ammonium bicarbonate soln with the method for sulphur, lead chloride is converted into lead carbonate to be stayed in the slag, the ammonium chloride that generates enters solution, carry out again adopting after the solid-liquid separation conventional sulphur solvent extraction with the sulphur content in the slag from obtaining elemental sulfur, obtain lead ore concentrate.
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| CNB021037043A CN1173077C (en) | 2002-03-11 | 2002-03-11 | Method for producing antimony by electrolyzing antimony-containing sulfide mineral pulp |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103757439A (en) * | 2014-01-20 | 2014-04-30 | 北京矿冶研究总院 | Method for recovering antimony and lead from antimony-lead-containing complex sulfide ore |
| CN106422716A (en) * | 2016-08-25 | 2017-02-22 | 昆明理工大学 | Method and device for removing SO2 in flue gas with copper extracting tailings and recycling copper extracting tailings |
| CN108221000A (en) * | 2018-01-08 | 2018-06-29 | 昆明理工大学 | A kind of electrolyte and application for electrorefining needle antimony or electro-deposition antimony |
| CN111020635A (en) * | 2019-12-19 | 2020-04-17 | 新邵辰州锑业有限责任公司 | Novel be arranged in ore pulp electrolysis antimony smelting hydrochloric acid recovery device |
| CN113089026A (en) * | 2021-03-17 | 2021-07-09 | 磨名言 | Method for electrolyzing and recovering antimony from antimony sulfide ore |
| CN113102110A (en) * | 2021-04-16 | 2021-07-13 | 中南大学 | Inhibitor for sorting molybdenum-bismuth ore and application thereof |
| CN115323435A (en) * | 2022-09-02 | 2022-11-11 | 昆明理工大学 | Electrochemical metallurgy method for extracting metal and sulfur from metal sulfide |
-
2002
- 2002-03-11 CN CNB021037043A patent/CN1173077C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103757439A (en) * | 2014-01-20 | 2014-04-30 | 北京矿冶研究总院 | Method for recovering antimony and lead from antimony-lead-containing complex sulfide ore |
| CN103757439B (en) * | 2014-01-20 | 2015-12-09 | 北京矿冶研究总院 | Method for recovering antimony and lead from antimony-lead-containing complex sulfide ore |
| CN106422716A (en) * | 2016-08-25 | 2017-02-22 | 昆明理工大学 | Method and device for removing SO2 in flue gas with copper extracting tailings and recycling copper extracting tailings |
| CN108221000A (en) * | 2018-01-08 | 2018-06-29 | 昆明理工大学 | A kind of electrolyte and application for electrorefining needle antimony or electro-deposition antimony |
| CN108221000B (en) * | 2018-01-08 | 2019-09-27 | 昆明理工大学 | A kind of electrolyte and application for electrorefining needle antimony or electro-deposition antimony |
| CN111020635A (en) * | 2019-12-19 | 2020-04-17 | 新邵辰州锑业有限责任公司 | Novel be arranged in ore pulp electrolysis antimony smelting hydrochloric acid recovery device |
| CN113089026A (en) * | 2021-03-17 | 2021-07-09 | 磨名言 | Method for electrolyzing and recovering antimony from antimony sulfide ore |
| CN113102110A (en) * | 2021-04-16 | 2021-07-13 | 中南大学 | Inhibitor for sorting molybdenum-bismuth ore and application thereof |
| CN113102110B (en) * | 2021-04-16 | 2022-11-04 | 中南大学 | Inhibitor for sorting molybdenum-bismuth ore and application thereof |
| CN115323435A (en) * | 2022-09-02 | 2022-11-11 | 昆明理工大学 | Electrochemical metallurgy method for extracting metal and sulfur from metal sulfide |
| WO2024045447A1 (en) * | 2022-09-02 | 2024-03-07 | 昆明理工大学 | Electrochemical metallurgy method for extracting metal and sulfur from metal sulfide |
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