CN1088266A - The method and apparatus of leaching and recoverying copper, silver, gold, lead, iron, sulphur from sulphuretted copper ore - Google Patents
The method and apparatus of leaching and recoverying copper, silver, gold, lead, iron, sulphur from sulphuretted copper ore Download PDFInfo
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- CN1088266A CN1088266A CN93115993A CN93115993A CN1088266A CN 1088266 A CN1088266 A CN 1088266A CN 93115993 A CN93115993 A CN 93115993A CN 93115993 A CN93115993 A CN 93115993A CN 1088266 A CN1088266 A CN 1088266A
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Abstract
The present invention is a kind of method and equipment thereof that adopts hydrochloric acid, oxygen, sodium hydroxide leaching and recoverying copper, silver, gold, lead, iron, sulphur from complicated sulphuretted copper ore.Be short matchmaker in the small amounts agent, from immersion liquid, reclaim multiple element, recovery sulphur, gold and Sulfothiorine from soak slag, all renewable circulation of immersion liquid; Electrolyzer adopts separates cucurbit groove recovery copper.This method is improved with the nontoxic efficient of extracting gold of low price, and technology is reinforced, and adopts all reagent nontoxic, inexpensive, and the loss of gold reduces in the treating processes, and multiple element all obtains the high-level efficiency recovery.This method is pollution-free not to produce any toxicity or harmful waste.
Description
The present invention relates to a kind of hydrometallurgical processes, the equipment that it is used, particularly a kind of from sulphuretted copper ore the method and the equipment thereof of leaching and recoverying copper, silver, gold, lead, iron, sulphur.
At present, reclaim valuable element from sulphuretted copper ore stone or copper fine-powdery, traditional method is that the method for roasting, melting realizes, but these methods just seem inconvenient to handling the low-grade complex copper-sulphide ores, and has brought environmental pollution.So people's active development wet process smelting technique.Though handling sulphuretted copper ore stone, adopt chlorination technique to obtain proof aborning, the method for lixiviate and reaction are complicated difficulties.As the patent No. by retrieval be: US37675430, US3896208, CA-985508, US3901776, BE-840820, US4053305, the described patent of US4063933, CA1065615, U.S. Patent number: US4053305 wherein, title is " reclaiming the method for copper and silver-by getting with ferrous aqueous fusion liquid of oxychlorination and oxygen lixiviate from sulfide concentrate ".
Content is: except that cupric and silver, the sulfide ore or the concentrate that also contain the complexity of lead, zinc, arsenic, antimony and iron are combined filtration with iron protochloride and oxygen, reclaim copper and silver.
Ore grinds to form the particle of 80 sieve meshes at first, be mixed into semi-fluid lean mixture slurry with solution of ferrous chloride then, slurry concentration 60%, generally comparatively desirable at the 20-400 grams per liter, insert in the closed reactor then, press certain speed and add oxygen, make temperature rise to 100-115 ℃, pressure remains on 20-80 pound/square inch in the reactor, behind the stop oxygen consumption, generally need through 1-6 hour, filter, the flushing residue, residue that reflects and concentration are about 1.0-5.0 sodium cyanide solution and 0.2-1.0 sodium hydroxide and other substrate value, after the lime dissolving, with electrolytic recovery silver, copper solidifies precipitation with iron plate and reclaims.
Get copper-sulphide ores by above-described iron protochloride and oxygen lixiviate, its weak point: though ore can be dissolved, when leaching, need a large amount of oxygen and long duration to finish, get off to finish as needs 6 hours and high pressure.Reclaiming the more imperfection that just seems aspect silver-colored, the cyaniding violent in toxicity leach residue that is adopted has brought inconvenience, and as: contaminate environment and low-grade silver ore that contains is not just had recovery value, cost is too high.
Analyze according to reliable patent report, its content mostly adopts iron trichloride, iron protochloride, cupric chloride, sodium cyanide and chlorine to reclaim Jin Heyin, more than used high price salt handle copper sulfide ore.But these iron content, copper bearing high price salt, commercially available costing an arm and a leg; Since the very easily hydrolysis of high price molysite, thus effective ingredient reduced, in order to prevent iron salt hydrolysis, to often replenish hydrochloric acid in process of production, keep the pH value of solution stable within the specific limits, in fact just at consumption acids.
The purpose of this invention is to provide a kind ofly from the sulphuretted copper ore stone of complexity, adopt the processing method and the equipment of hydrochloric acid, oxygen, sodium hydroxide leaching and recoverying copper, silver, gold, lead, iron, sulphur.
The present invention adopts such method to realize: the present invention is from the sulphuretted copper ore stone of complexity, adopts the method and apparatus of hydrochloric acid, oxygen, sodium hydroxide leaching and recoverying copper, silver, gold, lead, iron, sulphur.It is to utilize the cupric ion iron ion that self contains in the copper mine to pass through leaching process, plays the transmission electronic action, thereby causes the generation of redox reaction.But because the copper-sulphide ores structure has center of area tetrahedron lattice.Metallic element is relatively stable in this lattice, and the cupric ion that only inspires in copper mine stone or the copper fine-powdery is active.This is main key point.Simple hydrochloric acid and oxygen are not enough to destroy the molecular structure in copper sulfide ore or the copper fine-powdery.Can find by experiment to do under short matchmaker's the condition in the small amounts agent, molecular structure is very fast destroyed in copper-sulphide ores or the copper fine-powdery.So that copper mine decomposes rapidly.Metallic element in the copper mine is dissolved in the hydrochloric acid, generates corresponding chloride soln, and cupric ion and iron ion transmit electronics in the solution between copper mine and oxygen, and then causes redox reaction to take place.Metallic element in the copper mine is dissolved in the vat liquor fully and reaches the purpose of leaching.
Reaction mechanism of the present invention is by following step-by-step instructions:
In reactor, at first oxidized dose of (sodium chlorate) oxidation of hydrochloric acid produces chlorine.
Chlorine with copper mine generation redox reaction, is produced Cu by the absorption of the ore pulp of suspended state in encloses container
2+And Fe
3+, the sulphur in the copper mine is separated out with the elementary sulfur state.
The CU that generates
2+With Fe
3+Further reaction produces Cu to ion with copper mine
+And Fe
2+, the lead sulfide in the copper mine, silver sulfide are also simultaneously by Cu
2+And Fe
3+Oxidation, generting element sulphur and lead chloride, silver chloride.
The cuprous chloride that generates, lead chloride, silver chloride are produced complexing ion and are dissolved in the solution by the acid chlorization sodium complexing in the solution.
The Fe that is reduced in the solution
2+, under High Temperature High Pressure, use the gaseous oxygen oxidation, produce Fe
3+Continue and the copper mine reaction, cause copper mine all to decompose.
Owing to have a large amount of sodium-chlor to exist in the solution, in Oxidation of Fe
2+The time, prevent that effectively cuprous chloride and elementary sulfur are by the gaseous oxygen oxidation.
Behind system's stop oxygen consumption, (generally need 2 hours),, use the soluble salt in the normal saline washing residue again the reaction mixture filtered while hot.In leaching reaction process, copper, silver, lead, iron are soluble, and golden being retained in the leaching slag with sulphur is able to enrichment.
From leach liquor, separate lead salt, silver salt, adopt the crystallisation by cooling method, make and plumbously separate out from the solution intercrystalline with muriate, and then from crystal, dissolve silver chloride, obtain silver powder with the aldehyde reduction again, through fusion, ingot casting, be the finished product silver ingot at last with ammonia solution with silver.
Reaction formula is as follows:
Remaining chlorination lead skim behind the desilver adopts iron replacement to go out spongy lead after acid is molten, through melting, ingot casting, is finished product lead at last.Displacement waste back-cycling leaching section and vat liquor are merged as the solvent that soaks copper.
From leached mud, reclaim elementary sulfur and Precious Metals-Gold, conventional method is with organic solvent lixiviate elementary sulfur, with sodium cyanide or gas chlorine lixiviate gold, because organic solvent is inflammable, volatile, and price is more expensive, using aspects such as storing recovery, also exist the problem that is difficult to overcome, cyanide process, chlorination process are carried gold and silver, because the medicine severe toxicity, very harmful to the lixiviate operation, severe contamination.People are studying with the golden solvent of soaking of nontoxic or low toxicity and are substituting sodium cyanide for this reason.But these nontoxic or low toxicities soak golden solvent and cost an arm and a leg, and less stable, and also there is insoluble technical problem in penetration and promotion, and the cost height.
The present invention extracts recovery sulphur and gold copper, lead, silver, the iron leached mud afterwards from sulphuretted copper ore stone or copper fine-powdery, adopts sodium hydroxide leaching medicament, and under the condition that catalyzer (oxygen) is arranged, golden and sulphur reaches synchronous leaching.Changed the prior art organic solvent extraction
See shown in Figure 1: ore grinds to form the particle that size is 120 eye mesh screens at first, is mixed into the semi-fluid mixed pulp with hydrochloric acid soln then, and concentration is 30-50%, and best pulp density should change according to the character of ore.
With copper ore powder 25-30%, hydrochloric acid 65-75%, oxygenant (sodium chlorate) 1-5% is mixed into the semi-fluid mixed pulp, sends in the reactor 1, and heating maintains the temperature at 138-140 ℃, and oxygenation surpasses 3 hours, by solid-liquid separation 2, filters and wash residue then.Separate back solution and residue, residue soaks 11 by 5-10% sodium hydroxide solution maintenance leaching in 3 hours by alkali, through solid-liquid separation 12, filters to isolate waste residue and solution, and solution reclaims gold by carbon absorption 13.Adopt conventional method (activated carbon adsorption) to carry golden carbon 17, carry gold 18.
Carbon adsorbs the oxidizing reaction 14 that 13 isolated solution adopt the gaseous oxidation technology, and general temperature is at 90-100 ℃, pressure 2Kg/cm
2, kept 1 hour, through solid-liquid separation 15, isolate sulphur then.
Solid-liquid separation 15 isolated solution obtain Sulfothiorine (hypo) by freezing and crystallizing 16.
Solid-liquid separation 2 isolated solution are passed through freezing and crystallizing 3, produce crystal and solution, crystal carries out ammonia with solution of ammonium hydroxide and soaks 5, this moment, silver was complexed in the ammonia, filter by solid-liquid separation 6 again, solid dissolving with hydrochloric acid after the filtration, it is molten 8 to carry out acid, adds the iron replacement lead 9 with electrolytic recovery then;
Add acetaldehyde solution reduction silver 7 from solid-liquid separation 6 isolated solution.
Get the solution of crystallization 3 and send in the electrolyzer 4, carry out the decopper(ing) liquid that electrodeposition deposition copper powder produces, enter flat electrolyzer 10 electrodeposition and reclaim iron powder; Reclaim plumbous the using of plumbous 9 displacements for displacement.
Extracting the equipment that copper adopted is:
Chemical equation of the present invention is:
Specific embodiments of the invention are provided by accompanying drawing.
Fig. 1 is a process flow sheet of the present invention.
Fig. 2 is a copper electrodeposition electrolytic cell equipment synoptic diagram of the present invention.
The drawing explanation: 1 among Fig. 1 is reactor, and 2 is solid-liquid separation, and 3 are crystallization, 4 is copper electrodeposition electrolyzer, and 5 for ammonia soaks, and 6 is solid-liquid separation, 7 is reduction silver, and 8 are acidleach, and 9 are iron displacement lead, 10 is ferroelectric long-pending, and 11 for alkali soaks, and 12 is solid-liquid separation, 13 are carbon absorption, and 14 is oxidizing reaction, and 15 is solid-liquid separation, 16 are crystallization, 17 years golden carbon, and 18 for carrying gold;
Among Fig. 2 19 is the barrier film cloth bag, and 20 is the anolyte compartment, and 21 is cathode compartment, and 22 is electrolyzer, and 23 is the electrolytic solution import, and 24 is butterfly valve, and 25 is the copper powder collecting chamber, and 26 emit butterfly valve for copper powder, and 27 is electrolyte outlet, and 28 is negative electrode graphite carbon plate, and 29 is the anode graphite carbon plate;
Below in conjunction with accompanying drawing specific embodiments of the invention are further described.
See shown in Figure 1: the present invention adopts the method that adopts hydrochloric acid, oxygen, sodium hydroxide leaching and recoverying copper, silver, gold, lead, iron, sulphur from complicated sulphuretted copper ore stone, adopt the used typical feedstock of production technique of the present invention to comprise sulphuretted copper ore stone, copper fine-powdery and cupric oxide ore, three kinds or one raw material comprise: 1-30% copper, 1-20% lead, 1-15% zinc, 10-40% iron, 2-1000 gram/ton gold, 5-3000 gram/ton silver, 1-30% sulphur.In the powder collecting chamber 25, electrolytic solution is progressively headed in the cathode compartment 21 of upper end, when the copper powder for the treatment of the lower end reaches a certain amount of, close butterfly valve 24, open the butterfly valve 26 of lower end and emit copper powder.Electrolytic solution enters cathode compartment 21 by the import 23 of lower end.Waste electrolyte is flowed out by anolyte compartment's outlet 27.
Be to reduce the concentration polarization phenomenon, the speed of circulation of electrolytic solution is controlled at 50-100 liter/minute groove, does not have cupric ion and exceeds to be recycled to electrolytic solution.The temperature of electrolytic solution produces favourable influence along with the electrolysis time temperature remains on about 50 ℃ to metal precipitate.Adopt automatic control cathode electropotential electrolyzer, to reach isolating purpose.Whole electrolyzer all adopts series system, the tandem feed flow.Bath voltage is the 2-3 volt, current density 200A/m
2Cu because of leach liquor
+Be 1 valency, so reduce half than the conventional method power consumption during electrolysis.Current utilization rate reaches 90%.
Electrolytic solution behind the electrolysis decopper(ing) enters and carries out electrolytic iron in the flat electrolyzer, reclaims iron powder, and plumbous with iron displacement 9 for displacement, waste electrolyte Returning reactor 1 recycles.
Reclaim the copper electrode plate, cathode-anode plate is the graphite carbon plate.Reclaim electrolytic iron slot number plate, anode is the graphite carbon plate, and negative electrode is an iron plate.Diaphragm material is synthon.Immersion liquid reprocessing cycle when electrodeposition reclaims iron.
Reclaiming zinc is to adopt conventional method, and the present invention does not repeat to introduce.
Calabash shape electrolyzer of the present invention reclaims copper, unlike the prior art, its advantage be make simple, easy to operate, can continuous and automatic and be convenient to miniaturization production.
Prior art is to adopt to separate the pond or separate flat pan, and getting copper powder is to adopt conveying belt to carry copper powder continuously from the bottom of electrolytic solution, and this method manufacturing technology requires very high, and the cost costliness.Compare with the present invention, the calabash shape electrolyzer has obvious superiority.
Method of the present invention has nontoxic at a low price, and the efficient of extracting gold is improved, and technology is reinforced, all reagent that adopt are nontoxic inexpensive, the loss of gold reduces in the treating processes, and multiple element all obtains high recovery, and this method is pollution-free not to produce any toxicity or harmful waste.
The technology of the present invention detects the yield table
Cu Pb Fe A
Au S
Copper powder analytical element content % 18 8 16 300g/t 40g/t 20
Leaching yield % 96.5 97 90 98 93 96
Claims (3)
1, a kind of from sulphuretted copper ore leaching and recoverying copper, silver, gold, plumbous, iron, the method of sulphur and equipment thereof, it reclaims the method for copper and silver-by getting with ferrous aqueous fusion liquid of oxychlorination and oxygen lixiviate from sulfide concentrate, its technology is to adopt ore to grind to form the particle of 80 sieve meshes at first, be mixed into semi-fluid lean mixture slurry with solution of ferrous chloride then, slurry concentration 60%, generally comparatively desirable at the 20-400 grams per liter, insert in the closed reactor then, press certain speed and add oxygen, make temperature rise to 100-115 ℃, pressure remains on 20-80 pound/square inch in the reactor, behind the stop oxygen consumption, generally need through 1-6 hour, filter, the flushing residue, residue that reflects and concentration are about 1.0-5.0 sodium cyanide solution and 0.2-1.0 sodium hydroxide and other substrate value, after the lime dissolving, with electrolytic recovery silver, copper solidifies precipitation with iron plate and reclaims; The invention is characterized in: from complicated sulphuretted copper ore stone, adopt hydrochloric acid, oxygen, the sodium hydroxide leaching and recoverying copper, silver, gold, plumbous, iron, the processing method of sulphur and equipment, technology is with copper ore powder 25-30%, hydrochloric acid 65-75%, oxygenant such as sodium chlorate 1-5%, be mixed into semi-fluid and mix slurry, send in the reactor (1), heating maintains the temperature at 138-140 ℃, and oxygenation surpasses 3 hours, then by solid-liquid separation (2), filter and wash residue, decomposite solution and residue, residue soaks (11) by alkali and is kept leaching in 3 hours by the 5-10% sodium hydroxide solution, through solid-liquid separation (12), filter to isolate waste residue and solution, reclaim gold by carbon absorption (13);
The isolated solution of carbon absorption (13) adopts the oxidizing reaction (14) of gaseous oxidation technology, and general temperature is at 90-100 ℃, pressure 2Kg/cm
2, kept 1 hour, through solid-liquid separation (15), isolate sulphur then;
The isolated solution of solid-liquid separation (15) obtains Sulfothiorine by freezing and crystallizing (16);
The isolated solution of solid-liquid separation (2) is passed through freezing and crystallizing (3), produce crystal and solution, crystal carries out ammonia with solution of ammonium hydroxide and soaks (5), this moment, silver was complexed in the ammonia, filter by solid-liquid separation (6) again, solid dissolving with hydrochloric acid after the filtration carries out acid molten (8), adds the iron replacement lead (9) with electrolytic recovery then;
The solution isolated from solid-liquid separation (6) adds acetaldehyde solution reduction silver (7);
Get the solution of crystallization (3) and send in the electrolyzer (4), carry out the decopper(ing) liquid that electrodeposition deposition copper powder produces, enter flat electrolyzer (10) electrodeposition and reclaim iron powder; Reclaim plumbous (9) for displacement and replace plumbous using.
2, according to claim 1 from sulphuretted copper ore stone leaching and recoverying copper, silver, gold, plumbous, iron, the method and apparatus of sulphur, it is characterized in that: copper electrodeposition electrolyzer (4) adopts calabash shape, electrolyzer (22) anolyte compartment (20) separates with barrier film cloth bag (19) with cathode compartment (21), copper powder after the electrolysis falls in the copper powder collecting chamber (25) of lower end, electrolytic solution is progressively headed in the cathode compartment (21) of upper end, when the copper powder for the treatment of the lower end reaches a certain amount of, close butterfly valve (24), open the butterfly valve (26) of lower end and emit copper powder, electrolytic solution enters cathode compartment (21) by (23) import of lower end, waste electrolyte is flowed out by anolyte compartment's outlet (27), for reducing the concentration polarization phenomenon, the speed of circulation of electrolytic solution is controlled at 50-100 liter/minute groove, do not have cupric ion and exceed to be recycled to electrolytic solution, the temperature of electrolytic solution is along with the electrolysis time temperature remains on about 50 ℃, metal precipitate is produced favourable influence, adopt automatic control cathode electropotential electrolyzer, to reach isolating purpose, whole electrolyzer all adopts the parallel-series mode, the tandem feed flow, bath voltage is the 2-3 volt, current density 200A/m
2, because of the Cu of leach liquor
+Be 1 valency, so reduce half than the conventional method power consumption during electrolysis, current utilization rate reaches 90%.
3, according to claim 2 from sulphuretted copper ore stone the method and apparatus of leaching and recoverying copper, silver, gold, lead, iron, sulphur, it is characterized in that: reclaim the copper electrode plate, cathode-anode plate is the graphite carbon plate, reclaim electrolytic iron slot number plate, anode is the graphite carbon plate, negative electrode is an iron plate, and diaphragm material is synthon, immersion liquid reprocessing cycle when electrode reclaims iron.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93115993A CN1088266A (en) | 1993-12-27 | 1993-12-27 | The method and apparatus of leaching and recoverying copper, silver, gold, lead, iron, sulphur from sulphuretted copper ore |
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|---|---|---|---|
| CN93115993A CN1088266A (en) | 1993-12-27 | 1993-12-27 | The method and apparatus of leaching and recoverying copper, silver, gold, lead, iron, sulphur from sulphuretted copper ore |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100378233C (en) * | 2004-08-30 | 2008-04-02 | 金川集团有限公司 | Process for cleaning decopper nickel electrolytic solution |
| CN100485059C (en) * | 2005-02-16 | 2009-05-06 | 奥图泰有限公司 | Method for recovering gold from sulphide concentrate |
| CN101555551B (en) * | 2009-05-22 | 2011-05-18 | 昆明理工大学 | Method for comprehensively recovering Fe, Cu and Si from copper smelting slag |
| CN103074488A (en) * | 2013-01-31 | 2013-05-01 | 谷盾 | Oxidation leaching method and system |
| CN103757420A (en) * | 2014-01-20 | 2014-04-30 | 北京矿冶研究总院 | Method for recovering lead and silver from zinc leaching residues |
| CN101421426B (en) * | 2006-03-03 | 2015-05-27 | 鑫亚国际有限公司 | Process for extracting gold from gold-bearing ore |
| US10400306B2 (en) | 2014-05-12 | 2019-09-03 | Summit Mining International Inc. | Brine leaching process for recovering valuable metals from oxide materials |
| CN114407237A (en) * | 2022-01-21 | 2022-04-29 | 重庆金美新材料科技有限公司 | Waste composite copper film recovery processing method |
-
1993
- 1993-12-27 CN CN93115993A patent/CN1088266A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100378233C (en) * | 2004-08-30 | 2008-04-02 | 金川集团有限公司 | Process for cleaning decopper nickel electrolytic solution |
| CN100485059C (en) * | 2005-02-16 | 2009-05-06 | 奥图泰有限公司 | Method for recovering gold from sulphide concentrate |
| CN101421426B (en) * | 2006-03-03 | 2015-05-27 | 鑫亚国际有限公司 | Process for extracting gold from gold-bearing ore |
| CN101555551B (en) * | 2009-05-22 | 2011-05-18 | 昆明理工大学 | Method for comprehensively recovering Fe, Cu and Si from copper smelting slag |
| CN103074488A (en) * | 2013-01-31 | 2013-05-01 | 谷盾 | Oxidation leaching method and system |
| CN103757420A (en) * | 2014-01-20 | 2014-04-30 | 北京矿冶研究总院 | Method for recovering lead and silver from zinc leaching residues |
| CN103757420B (en) * | 2014-01-20 | 2016-09-21 | 北京矿冶研究总院 | Method for recovering lead and silver from zinc leaching residues |
| US10400306B2 (en) | 2014-05-12 | 2019-09-03 | Summit Mining International Inc. | Brine leaching process for recovering valuable metals from oxide materials |
| CN114407237A (en) * | 2022-01-21 | 2022-04-29 | 重庆金美新材料科技有限公司 | Waste composite copper film recovery processing method |
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