CN104195344B - Method for recovering sulfur, lead, zinc and silver from oxygen-rich direct leaching residues of zinc concentrate or lead and zinc mixed ores by virtue of ultrasonic wave intensification - Google Patents
Method for recovering sulfur, lead, zinc and silver from oxygen-rich direct leaching residues of zinc concentrate or lead and zinc mixed ores by virtue of ultrasonic wave intensification Download PDFInfo
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Abstract
The invention discloses a method for recovering sulfur, lead, zinc and silver from oxygen-rich direct leaching residues of zinc concentrate or lead and zinc mixed ores by virtue of ultrasonic wave intensification, belonging to the field of comprehensive recycling of non-ferrous metal metallurgy. The method disclosed by the invention comprises the following steps: by using tetrachloroethylene or trichloro ethylene as a solvent, extracting elemental sulfur from the oxygen-rich direct leaching residues of zinc concentrate or lead and zinc mixed ores, which are dried, ground, and sieved by virtue of ultrasonic wave intensification, preserving heat and filtering, after naturally cooling and forcibly cooling the filtrate and filtering to obtain a sulfur product, and returning a regenerated sulfur extraction agent to a sulfur extraction step; and enriching zinc, lead and silver in the residues, wherein the residues can be directly fed to a lead system to recover zinc, lead and silver, or the residues are firstly leached to recover zinc, filter residues are fed to the lead system to recover silver, and zinc-containing filtrate is returned to a direct leaching system. The method disclosed by the invention is simple, energy-saving and high in sulfur recovery rate and product quality. The sulfur extraction process is sealed, so that the method is free from environmental pollution and is particularly suitable for comprehensively utilizing normal pressure/high pressure oxygen-rich direct leaching residues of zinc concentrate or lead and zinc mixed ores.
Description
Technical field
The invention belongs to non-ferrous metal metallurgy comprehensive reutilization field is and in particular to a kind of zinc concentrate or lead and zinc industry
Oxygen-enriched direct leached mud intensified by ultrasonic wave Recovered sulphur and lead, zinc, the method for silver.
Background technology
Current zinc more than 80% is the technique productions of roasting-leaching-purification-electrodeposition using fire-wet process integration.This technique
Maturation, technology controlling and process simple operationss are convenient, and metal recovery rate is high, the advantages of equipment requirements are high, but there is also baking flue gas
Sulfur dioxide pollution, producing flue gas needs antacid, consumes under-developed area for sulphuric acid, there is sulphuric acid market problem.In addition exist
Roasting process forms zinc ferrite unavoidably, and when calcining leaches, zinc leaching rate is not high, and only 70-80% causes a large amount of zinc to remain in leached mud
In, leached mud two is big simultaneously, and the slag of ton zinc output reaches 0.9 ton about, and factory has to store up in a large number or using works such as Rotary Kiln
Skill is processed.Meanwhile, it is unable to high-efficiency comprehensive utilization with the valuable metal of zinc association as silver, indium, germanium, both caused environmental pollution hidden danger,
Cause resource serious waste again.
The oxygen-enriched direct leaching-out technique of zinc sulfide concentrates is generally considered metallurgical the breaking through again of zinc, is known as third generation refining
Zinc technology.Oxygen-enriched direct leaching process mainly divides two big class: oxygen-enriched pressure leaching (abbreviation oxygen presses acidleach) and normal pressure means of oxygen rich leaching.
Compared with traditional smelting process, lack concentrate roasting and acid making system, advantageously reduce the air pollution of sulfur dioxide, also favorably
The recovery of valuable metal such as in, cu, ge and ga etc. in leached mud.
From the perspective of physical chemistry, normal pressure means of oxygen rich leaching and oxygen pressure acidleach do not have essential distinction.Simply oxygen pressure acidleach
It is to carry out under solution boiling point reaction temperature higher above and larger oxygen partial pressure in closed reactor, allow reaction energy
Effectively carry out at short notice；And normal pressure means of oxygen rich leaching is carried out under the following normal pressure of solution boiling point, thus with respect to oxygen pressure
The acid-leaching reaction time is longer.Zinc sulfide oxygen pressure acidleach and normal pressure means of oxygen rich leaching each depend on following reaction:
zns+h2so4+0.5h2=znso4+h2o+s0
It was found that zinc sulfide leaches the ferrum being by mean of dissolving does the carrier of oxygen to realize, leaching whole process should
It is decomposed into two reactions:
zns+fe2(so4)3→znso4+2feso4+s0
2feso4+h2so4+0.5o2→fe2(so4)3+h2o
The oxidation reaction mistake of the ferrum in the magnetic iron ore (fe7s8) containing in zinc concentrate and marmatite [(zn, fe) s]
Journey is similar with the zinc in sphalerite.And pyritous degree of oxidation is then relevant with leaching condition.
In normal pressure/high-pressure oxygen-enriched acid leaching process, in leached mud, contain a certain amount of metal sulphurizing salt and simple substance elementary sulfur,
Wherein it is mainly the simple substance elementary sulfur that lead in raw ore, silver-colored and unreacted zinc and reaction produce.Some factories enter to leached mud
Go process, such as flotation is reclaimed and isolated sulfur slag, but effect is bad, and energy consumption is also big, and the impure height of sulfur slag remains a need for further
Process；Then temporary transient heap stores away for some factories, causes fund to overstock and environment hidden danger.
At present, the conventional method reclaiming the elemental sulfur in zinc sulfide concentrates or the direct leached mud of lead and zinc industry mainly has:
Heat filtering method, high pressure decantation method, vacuum distillation method, floatation, ammonium sulfide put forward sulfur method, dimethylbenzene carries sulfur method, cs2Propose sulfur method, life
Thing method etc..Above method all haves the shortcomings that certain, and such as floatation separates thorough, and sulfur grade is not high；Heat filtering method profit
At 125-158 DEG C, there is preferable mobility, high energy consumption with sulfur, equipment is complicated, need insulation to filter, filtering residue sulfur-bearing is high；High pressure
, because unreacted metal sulfide is melted in sulfur in removal process, therefore sulfur grade is not also high for decantation；Vacuum is steamed
Evaporate method high energy consumption, equipment seal has high demands；The raw material taste that ammonium sulfide proposes the use of sulfur method is smelly, severe operational environment；Dimethylbenzene carries
Sulfur method, cs2The shortcoming putting forward sulfur method is that these organic solvents are inflammable and explosive or poisonous, and device security has high demands；Bioanalysises are profits
With sulfate reducting bacteria, sulfate reduction is become hydrogen sulfide gas, then sulfur, technology are changed into by Crouse's willow retracting device
Complexity is it is impossible to be widely popularized.
Content of the invention
Contain outside 40-60% sulfur for zinc concentrate or lead and zinc industry normal pressure/high-pressure oxygen-enriched direct leached mud, still contain one
The valuable metals such as quantitative zinc, lead and silver, presently, there are difficult treatment, fund overstocks and the problems such as environment hidden danger, the present invention sets
A kind of zinc concentrate or the oxygen-enriched direct leached mud intensified by ultrasonic wave Recovered sulphur of lead and zinc industry and lead, zinc, the method for silver are counted.
The object of the present invention is achieved like this:
A kind of zinc concentrate or the oxygen-enriched direct leached mud intensified by ultrasonic wave Recovered sulphur of lead and zinc industry and lead, zinc, the side of silver
Method, with tetrachloroethylene or trichloro ethylene as solvent, to through being dried, grinding, sieve the good zinc concentrate of pretreatment or the mixing of lead zinc
The oxygen-enriched direct leached mud of ore deposit adopts intensified by ultrasonic wave to extract the elemental sulfur in slag, and insulation is filtered, and filtrate is through natural cooling and pressure
Cooling obtains sulfur product after refiltering, regeneration sulfur extraction agent returns extraction sulfur operation；Zinc in filtering residue, lead, silver are enriched with, can be straight
Pick lead system and reclaim zinc, lead, silver, cross filtering residue after also can first leaching recovery zinc and send lead system to reclaim lead silver, filtrate containing zinc returns
Directly leaching system.
Further, above-mentioned pretreatment refers to that direct leached mud oxygen-enriched to zinc concentrate or lead and zinc industry is dried
Moisture is made after being less than or equal to 10%, grinding, to cross 100 mesh sieves screenings.
Further, this invention is to add oxygen-enriched to zinc concentrate or lead and zinc industry direct leached mud to be pre-loaded with by liquid
Gu in the ultrasound wave leaching reactor than the sulfur extraction agent of 8-15 metering, reacting by heating 8-15 minute.Using ultrasonic cavitation effect
Strengthening dissolving in tetrachloroethylene or trichloro ethylene for the elemental sulfur, its ultrasonic frequency is 20-200khz, and the sound intensity is 2.0-50w/
cm2.
Further, it is centrifugal filtration that above-mentioned insulation is filtered, and carries out being incubated, airtight and discharge gas cooling during filtration
Recycling；Above-mentioned cooling is that filtrate is taken with first natural cooling, forces cooling afterwards, so that sulfur is separated out as far as possible, and completely
Crystallization.
Further, refilter after cooled precipitation sulfur, can obtain regenerating sulfur extraction agent and returning extracting sulfur operation, circulation
Participate in reaction, cycle-index can be more than 20 times.Finally, sulfur product adopts dry packing after absolute ethanol washing.
Further, above-mentioned sulfur extraction agent can also be one of tetrachloroethylene, trichloro ethylene, toluene, dimethylbenzene
Or several mixture.
The present invention is dissolved in sulfur extraction agent using elemental sulfur, in certain temperature range dissolubility in sulfur extraction agent for the sulfur with
Temperature raises and increases, and when temperature reduces, dissolubility reduces, and separates out and reach separating-purifying purpose from sulfur extraction agent.In sulfur extraction agent
121.2 DEG C of tetrachloroethylene boiling point, stable in properties, small toxicity, not volatile, water insoluble, dissolve in anhydrous alcohol, sulfur is in tetrachloro
Dissolubility temperature influence in ethylene, its relation is as follows:
| Temperature DEG C | 30 | 50 | 60 | 70 | 80 | 90 | 100 | 110 |
| Dissolubility g/l | 29.9 | 54.9 | 74.9 | 105 | 147 | 220 | 365 | 380 |
As seen from the table, raise with temperature, the dissolubility of sulfur increases, but sulfur recovery rate can't be with temperature rising
Unlimited increase, temperature close to its boiling point when the response rate of sulfur is reduced due to the volatilization of tetrachloroethylene beginning.Therefore, molten sulfur
Temperature wants suitable control.Dimethylbenzene in sulfur extraction agent, it may have similar effect.
In order to improve the primary recovery of sulfur, extraction sulfur filtrate through natural cooling and forces cooling to obtain sulfur product after refiltering
Product, the sulfur grade thus producing is more than 98%.After washing, filtrate is separately recovered ethanol and tetrachloroethylene after treatment.Desulfurization
Afterwards, sulfur extraction agent returns and recycles.
In the present invention, with containing the valuable metal such as zinc, lead, silver in the good filtering residue of washing with alcohol, due to elemental sulfur removing
Major part, zinc, lead, the grade of silver also accordingly significantly raise.Generally, containing zinc high when, after desulfurization, filtering residue is through sulfur extraction agent and second
Lead system can directly be returned after alcohol washing and reclaim the valuable metals such as zinc, lead, silver；Containing zinc high when, can first leach recovery zinc after
Filtering residue send lead system to reclaim lead silver, that is, add a jacketed heater being previously added dilute sulfuric acid and nitric acid mixed solution
In, heated and stirred reacts 1-2 hour, and filtered filtration residue returns again to lead system and reclaims lead, silver, and zinc-containing solution returns and directly leaches system
System.So, both improve the direct yield in zinc processing system for the zinc, and be also beneficial to lead system and reclaim lead and silver, avoid zinc to exist simultaneously
The side effect of lead system.
In extraction sulfur process, when in slag, elemental sulfur and sulfur extraction agent temperature are high, reaction is very fast, but will also result in sulfur extraction agent and wave
Send out big, working environment is severe, cost increases simultaneously need to insulation is filtered；Ultrasonic extraction utilizes Ultrasonic Radiation pressure to produce
Strong cavitation effect, mechanical vibration, disturbance effect and high acceleration, emulsifying, spread, smash and the multistage effects such as stirring action
Should, increasing molecular motion of material frequency and speed, increase solvent penetration power, thus accelerating target component to enter solvent, promoting extraction
The carrying out taking.
If ultrasonic energy is sufficiently strong, the sky that expansion process can generate bubble in a liquid or liquid tears into very little
Cave.These hole moments close, and produce the instantaneous pressure being up to 3000mpa during closure, and whole process completes in 400 μ s.
Cavitation refinement material and manufacture emulsion, accelerate target component to enter solvent, improve extraction ratio.In addition to cavitation, surpass
Many second order effects of sound wave are also all conducive to transfer and the extraction of target component.Cavitation phenomena occurs in bubbles burst instead
Should, some put position, bubble not re-absorption ultrasonic energy and produce implosion.Gas in bubble or hole and steam are quickly exhausted
Hot compression, produces high temperature and pressure.Atomic for bubble volume relative liquid cumulative volume, the heat moment of therefore generation
Scatter and disappear, environmental condition will not be produced and significantly affect, the rate of cooling after the follicular rupture of hole is estimated to be about 1010 DEG C/s.Ultrasonic
Hole provides unique interaction between energy and material, and the High Temperature High Pressure of generation can lead to free radical and the shape of other component
Become.In neat liquid, during the rupture of hole, because ambient conditions is identical, therefore total holding is spherical；But at solid boundaries, empty
The rupture in cave is heterogeneous, produces high velocity liquid jet, makes the potential energy of expanding bubble become the kinetic energy of liquid jet, in gas
Move in bubble and penetrate walls.Injection stream is very strong in the impulsive force of the surface of solids, can impact zone be caused greatly destroy,
Thus producing highly active unsalted surface.The impact that the impulsive force that arc bubble deformation produces from the teeth outwards produces than bubble resonance
Power will big several times.The present invention creatively ultrasonic extraction method is applied in extraction sulfur technique for the first time, to from dissimilar
Sulfur slag in extract various subject component be very effective.Apply intensified by ultrasonic wave in extraction process, in organic solvent
With the high temperature producing on direct leached mud solid particle contact surface, high pressure, the oxidation of the free radical that sonolysis produce in addition
Energy waits the extraction energy it is provided that high.
The present invention, with respect to the conventional extraction sulfur technology of field of hydrometallurgy, has quick, inexpensive, the efficient feature of extraction.
Its remarkable result mainly has: ultrasonic extraction sulfur is without high temperature, it is possible to achieve low-temperature extraction, and energy consumption is greatly decreased；Safety is good, operation
Simple, maintaining is convenient；Little to the property relation of solvent and target extract, extraction efficiency is high；Feed throughput is big,
At double or several times improve, and product impurity is few, and effective ingredient is easily isolated, purifies；Sulfur extraction agent loss is little, extracts sulfur process costs
Low, overall economic efficiency is notable.
Brief description
Fig. 1 is the best processing route figure of the present invention.
Specific embodiment
Embodiment one
Sulfur slag ingredient (machined mistake 100 mesh sieve, butt): lead 1.22%, zinc 4.75%, indium 0.0029%, silver 0.0569%, sulfur
74.83%.Weigh 5.0000 grams of sulfur slags, 1.0000 grams of a# additives, 62.5ml(100 gram) mixed liquor of tetrachloroethylene and toluene,
100 DEG C of heating in water bath 30min, filter immediately, obtain 3.2126 grams of residue, are cooled to 27.5 DEG C, with ultrasonic frequency, the sound intensity and anti-
Difference between seasonable, the sulfur product quality obtaining is also different.
If during reacting by heating, using intensified by ultrasonic wave, supersonic frequency is 20khz, and the sound intensity is in 2.0-50w/cm2
Between, the response time is 8min, and at this moment the extraction yield of sulfur see table:
If during reacting by heating, using intensified by ultrasonic wave, supersonic frequency is 100khz, and the sound intensity is in 2.0-50w/
cm2Between, the response time is 12min, and at this moment the extraction yield of sulfur see table:
If during reacting by heating, using intensified by ultrasonic wave, supersonic frequency is 200khz, and the sound intensity is in 2.0-50w/
cm2Between, the response time is 15min, and at this moment the extraction yield of sulfur see table:
The filtering residue having washed directly return lead system reclaim lead, silver, lead, silver, indium, zinc the response rate be respectively 110%,
34%、89%、113%.
Embodiment two
Sulfur slag ingredient (machined mistake 100 mesh sieve, butt): lead 1.22%, zinc 4.75%, indium 0.0029%, silver 0.0569%, sulfur
74.83%.Weigh 10.0000 grams of machined sample sulfur slags, 125ml trichloro ethylene, 100 DEG C of heating in water bath 25min, filter immediately,
Obtain 6.3962 grams of residue, be cooled to 27.5 DEG C, with the difference in ultrasonic frequency, the sound intensity and response time, the sulfur product obtaining
Quality is also different.
If during reacting by heating, using ultrasonic extraction, supersonic frequency is 30khz, and the sound intensity is in 2.0-50w/cm2It
Between, the response time is 9min, and at this moment the extraction yield of sulfur see table:
If during reacting by heating, using ultrasonic extraction, supersonic frequency is 120khz, and the sound intensity is in 2.0-50w/cm2
Between, the response time is 11min, and at this moment the extraction yield of sulfur see table:
If during reacting by heating, using ultrasonic extraction, supersonic frequency is 180khz, and the sound intensity is in 2.0-50w/cm2
Between, the response time is 14min, and at this moment the extraction yield of sulfur see table:
Zinc in filtering residue, lead, silver are enriched with, first leach reclaim zinc after cross filtering residue send lead system reclaim lead silver, lead, silver,
The response rate of indium is respectively 114%, 30%, 79%；Zinc-containing solution returns direct leaching stage, and the response rate of zinc is 116%.
Embodiment three
Sulfur slag ingredient (machined mistake 100 mesh sieve, butt): lead 1.22%, zinc 4.75%, indium 0.0029%, silver 0.0569%, sulfur
74.83%.Weigh 10.0000 grams of sulfur slags, 125ml(100 gram) tetrachloroethylene, 100 DEG C of heating in water bath 30min, filter immediately, obtain
6.3962 grams of residue, is cooled to 27.5 DEG C, with the difference in ultrasonic frequency, the sound intensity and response time, the sulfur product matter obtaining
Amount is also different.
If during reacting by heating, using ultrasonic extraction, supersonic frequency is 40khz, and the sound intensity is in 2.0-50w/cm2It
Between, the response time is 8min, and at this moment the extraction yield of sulfur see table:
If during reacting by heating, using ultrasonic extraction, supersonic frequency is 130khz, and the sound intensity is in 2.0-50w/cm2
Between, the response time is 12min, and at this moment the extraction yield of sulfur see table:
If during reacting by heating, using ultrasonic extraction, supersonic frequency is 160khz, and the sound intensity is in 2.0-50w/cm2
Between, the response time is 15min, and at this moment the extraction yield of sulfur see table:
Zinc in filtering residue, lead, silver are enriched with, and cross filtering residue and send lead system to reclaim lead, silver, containing zinc filter after first leaching recovery zinc
Liquid returns direct leaching system.At this moment, lead, silver, indium, the response rate of zinc are respectively 120%, 36%, 85%, 124%.
Claims (6)
1. a kind of zinc concentrate or the oxygen-enriched direct leached mud intensified by ultrasonic wave Recovered sulphur of lead and zinc industry and lead, zinc, the method for silver,
It is characterized in that: with tetrachloroethylene or trichloro ethylene as solvent, by through being dried, grinding, the screening good zinc concentrate of pretreatment or
The oxygen-enriched direct leached mud of lead and zinc industry adds the ultrasound wave Leach reaction being pre-loaded with the sulfur extraction agent by the metering of liquid-solid ratio 8-15
In device, reacting by heating 8-15 minute, the elemental sulfur in slag is extracted using intensified by ultrasonic wave, ultrasonic frequency is 20-200khz, sound
It is by force 2.0-50w/cm2；Carry out centrifugation insulation again to filter, carry out during filtration being incubated, airtight and discharge gas cooling recycling,
Filtrate elder generation natural cooling obtains sulfur product after being refiltered after forcing cooling again；Regeneration sulfur extraction agent returns extraction sulfur operation, filter
Zinc in slag, lead, silver are enriched with, and directly send lead system to reclaim zinc, lead, silver.
2. a kind of zinc concentrate or the oxygen-enriched direct leached mud intensified by ultrasonic wave Recovered sulphur of lead and zinc industry and lead, zinc, the method for silver,
It is characterized in that: with tetrachloroethylene or trichloro ethylene as solvent, by through being dried, grinding, the screening good zinc concentrate of pretreatment or
The oxygen-enriched direct leached mud of lead and zinc industry adds the ultrasound wave Leach reaction being pre-loaded with the sulfur extraction agent by the metering of liquid-solid ratio 8-15
In device, reacting by heating 8-15 minute, the elemental sulfur in slag is extracted using intensified by ultrasonic wave, ultrasonic frequency is 20-200khz, sound
It is by force 2.0-50w/cm2；Carry out centrifugation insulation again to filter, carry out during filtration being incubated, airtight and discharge gas cooling recycling,
Filtrate elder generation natural cooling obtains sulfur product after being refiltered after forcing cooling again；Regeneration sulfur extraction agent returns extraction sulfur operation, filter
Zinc in slag, lead, silver are enriched with, and cross filtering residue and send lead system to reclaim lead silver, filtrate containing zinc returns direct after first leaching recovery zinc
Leaching system.
3. a kind of zinc concentrate according to claim 1 and 2 or the oxygen-enriched direct leached mud intensified by ultrasonic wave of lead and zinc industry return
Receive sulfur and lead, zinc, silver method it is characterised in that: described pretreatment be oxygen-enriched to zinc concentrate or lead and zinc industry directly
Leached mud is dried so that moisture crosses 100 mesh sieve screenings after being less than or equal to 10%, grinding.
4. a kind of zinc concentrate according to claim 1 and 2 or the oxygen-enriched direct leached mud intensified by ultrasonic wave of lead and zinc industry return
Receive sulfur and lead, zinc, silver method it is characterised in that: described is strong using ultrasonic cavitation effect using intensified by ultrasonic wave
Change dissolving in tetrachloroethylene or trichloro ethylene for the elemental sulfur.
5. a kind of zinc concentrate according to claim 1 and 2 or the oxygen-enriched direct leached mud intensified by ultrasonic wave of lead and zinc industry return
Receive sulfur and lead, zinc, silver method it is characterised in that: described sulfur extraction agent is tetrachloroethylene, trichloro ethylene, toluene, dimethylbenzene
One or more of mixture.
6. a kind of zinc concentrate according to claim 1 and 2 or the oxygen-enriched direct leached mud intensified by ultrasonic wave of lead and zinc industry return
Receive sulfur and lead, zinc, silver method it is characterised in that: described sulfur product adopts dry packing after absolute ethanol washing.
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| CN106315517A (en) * | 2016-08-21 | 2017-01-11 | 株洲冶炼集团股份有限公司 | Method for recycling sulphur from sulphur-containing residue |
| CN109750173A (en) * | 2017-11-07 | 2019-05-14 | 呼伦贝尔驰宏矿业有限公司 | A kind of high-iron sphalerite zinc metallurgy and the system and technique for handling associated metal altogether |
| CN108002350B (en) * | 2017-11-20 | 2020-11-06 | 浙江海洋大学 | Composite extractant and method for separating and recovering sulfur by using same |
| CN110898987B (en) * | 2019-11-13 | 2021-06-22 | 鞍钢集团矿业有限公司 | Oxidation desulfurization method of high-sulfur magnetite concentrate |
| CN111638244B (en) * | 2020-06-05 | 2021-05-11 | 中南大学 | Safety analysis method for zinc concentrate oxygen pressure acid leaching high-sulfur slag |
| CN114772558A (en) * | 2022-04-27 | 2022-07-22 | 长沙华时捷环保科技发展股份有限公司 | Process for extracting elemental sulfur from high-sulfur ore/slag |
| CN115445776B (en) * | 2022-08-11 | 2023-05-26 | 昆明理工大学 | Separation method applied to copper-lead bulk concentrate |
| CN115637327B (en) * | 2022-10-28 | 2024-06-04 | 昆明理工大学 | Coupling device for extracting lithium from salt lake based on ultrasonic assistance and application method thereof |
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| CN103172218B (en) * | 2013-03-06 | 2015-03-25 | 北京赛科康仑环保科技有限公司 | Method and device for recovery and purifying elemental sulfur from high-concentration sulfate wastewater |
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