CN104229745A - Ultrasonic extraction method and process for processing slag containing elemental sulfur - Google Patents
Ultrasonic extraction method and process for processing slag containing elemental sulfur Download PDFInfo
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- CN104229745A CN104229745A CN201410437115.7A CN201410437115A CN104229745A CN 104229745 A CN104229745 A CN 104229745A CN 201410437115 A CN201410437115 A CN 201410437115A CN 104229745 A CN104229745 A CN 104229745A
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Abstract
The invention discloses an ultrasonic extraction method and process for processing slag containing elemental sulfur. One or a mixture of more of tetrachloroethylene, trichloro ethylene, methylbenzene and xylene is adopted as a solvent; ultrasonic extraction is carried out on the slag containing elemental sulfur; the ultrasonic frequency is 20-200KHz; and the sound intensity is 2.0-50w/cm<2>. According to the ultrasonic extraction method, low-temperature extraction can be achieved without high temperature, energy consumption can be greatly reduced, and the process is low in cost, simple and feasible in operation, high in extraction efficiency, large in raw material processing amount, low in extracting agent loss and significant in composite economic results.
Description
Technical field
The present invention relates to method and technique that a kind of process contains elemental sulfur slag, especially a kind of process contains ultrasonic extraction method and the technique of elemental sulfur slag, belongs to technical field of wet metallurgy.
Background technology
Adopt pressurization means of oxygen rich leaching method or normal pressure means of oxygen rich leaching method process zinc sulfide concentrates, the metals such as zinc, copper, cadmium, cobalt, nickel enter liquid phase, sulfur mineral main body enters slag phase with elemental sulfur, part with sulfide and metal sulfate form, and output is containing elemental sulfur and plumbous, silver-colored slag.Physical, chemical method and biological process is mainly contained from the method reclaiming elemental sulfur containing elemental sulfur slag.Physical mainly comprises heat filtering method, high pressure decantation method, vacuum distillation method, flotation process; Chemical method mainly comprises that sulphur method put forward by ammonium sulfide, dimethylbenzene carries sulphur method, CS
2put forward sulphur method.Wherein, heat filtering method energy consumption is high, and equipment is complicated, and filter residue sulfur-bearing is high; High pressure decantation method is difficult to effectively be separated because of elemental sulfur and sulfide, and sulfur product grade is low; Vacuum distillation method energy consumption is high, requires high to equipment airtight performance; Flotation process is separated not thorough to elemental sulfur, sulfur product grade is low; Sulphur method put forward by ammonium sulfide, and the smell is awful, severe operational environment; Dimethylbenzene carries sulphur method, CS
2put forward sulphur method, solvent is inflammable and explosive or poisonous, and production security is low; Biological process utilizes bacterium that sulfate reduction is become hydrogen sulfide, then changes into sulphur, technical sophistication by Crouse willow retrieving arrangement, and application difficulty is large.Therefore, necessary prior art to be improved.
Summary of the invention
In order to solve the problem, the present invention devises ultrasonic extraction method and the technique that a kind of process contains elemental sulfur slag, very efficiently, economically can extract elemental sulfur, is separated slag impurity, and raising sulphur quality and valuable metal go out the purity of product simultaneously.
The object of the present invention is achieved like this:
Process, containing a ultrasonic extraction method for elemental sulfur slag, is ultrasonic method and extracting process are combined, a kind of new opplication first in the extraction of non-metallic element elemental sulfur.The present invention adopts the mixture of one or more in zellon, trieline, toluene, dimethylbenzene as solvent, implements ultrasonic extraction to containing elemental sulfur slag.
Further, described contains elemental sulfur slag, at least comprises the leached mud adopting pressurization means of oxygen rich leaching method and normal pressure means of oxygen rich leaching method process zinc sulfide concentrates and lead sulfide zinc ore concentrate output.
Further, described ultrasonic extraction, its ultrasonic frequency is 20-200KHz, and the sound intensity is 2.0-50w/cm
2.
Process, containing a ultrasonic extraction technique for elemental sulfur slag, is implemented according to the following steps:
(1) add containing elemental sulfur slag the ultrasonic wave Leaching reaction device that sulfur extraction agent is housed in advance, carry out reacting by heating;
(2) insulation is filtered;
(3) cool;
(4) sulfur product be extracted is refiltered.
Further, preferably can carry out drying, grinding, screening pre-treatment to containing elemental sulfur slag before the step (1), namely drying makes moisture be less than or equal to 10%, crosses 100 mesh sieves after grinding and sieve.
Further, described sulfur extraction agent is the mixture of one or more in zellon, trieline, toluene, dimethylbenzene, and measures by liquid-solid ratio 8-15.
Further, in described reacting by heating, ultrasonic frequency 20-200KHz, sound intensity 2.8-20w/cm
2, reaction 8-15 minute.
Further, it is centrifuging that described insulation is filtered, and carries out being incubated, airtight and Exhaust Gas cooling recycling during filtration.
Further, described cooling takes first naturally cooling to filtrate, and rear pressure cooling, makes sulphur separate out as far as possible, and complete crystal.
Further, separate out after sulphur refilter through cooling, can obtain regeneration sulfur extraction agent and return extraction sulphur operation, circulation participates in reaction, and cycle index can more than 20 times.
Further, described ultrasonic extraction technique also can be applicable in the comprehensive utilization operation of zinc ore concentrate or lead and zinc industry normal pressure/high-pressure oxygen-enriched direct leached mud, and the zinc in filter residue, lead, silver obtain enrichment, and lead system can be sent to reclaim zinc, lead, silver; Also crossing filter residue after first can leaching recovery zinc send lead system recovery plumbous, silver-colored, returns direct leaching system containing zinc filtrate.
The present invention utilizes elemental sulfur to be dissolved in sulfur extraction agent, and in certain temperature range, the solubleness of sulphur in sulfur extraction agent raises along with temperature and increases, and when temperature reduces, solubleness reduces, and separates out and reach separating-purifying object from sulfur extraction agent.Zellon boiling point in sulfur extraction agent 121.2 DEG C, stable in properties, toxicity is little, not volatile, water insoluble, dissolves in raw spirit, the solubleness temperature influence of sulphur in zellon, and its relation is as following table:
| Temperature DEG C | 30 | 50 | 60 | 70 | 80 | 90 | 100 | 110 |
| Solubleness g/l | 29.9 | 54.9 | 74.9 | 105 | 147 | 220 | 365 | 380 |
As seen from the table, along with temperature raises, the solubleness of sulphur increases, but sulfur recovery rate can't raise along with temperature and infinitely increase, and temperature makes the rate of recovery of sulphur reduce close to volatilizing due to zellon beginning during its boiling point.Therefore, molten sulphur temperature will suitably control.Dimethylbenzene in sulfur extraction agent, also has similar effect.
In order to improve the primary recovery of sulphur, extraction sulphur filtrate obtains sulfur product through naturally cooling with after forcing cooling to refilter, dry packing after sulfur product employing absolute ethanol washing.Thus, the sulphur grade of production is more than 98%.After washing, filtrate reclaims ethanol and zellon after treatment respectively.After desulfurization, sulfur extraction agent returns and recycles.
In the present invention, contain the valuable metals such as zinc, lead, silver with in the filter residue that washing with alcohol is good, because elemental sulfur is stripped of major part, the grade of zinc, lead, silver is also corresponding significantly to be raised.Usually, time not high containing zinc, after desulfurization, filter residue directly can return lead system and reclaim the valuable metals such as zinc, lead, silver after sulfur extraction agent and washing with alcohol; During containing zinc height, first can leach filter residue after reclaiming zinc send lead system to reclaim plumbous silver, namely adding one adds in the jacketed heating unit of dilute sulphuric acid and nitric acid mixing solutions in advance, heated and stirred reaction 1-2 hour, filtered filtration residue returns lead system again and reclaims plumbous, silver-colored, and zinc-containing solution returns direct leaching system.Like this, both improve the direct yield of zinc in zinc treatment system, and be also conducive to lead system and reclaim plumbous and silver-colored, avoid zinc in the side effect of lead system simultaneously.
In extraction sulphur process, in slag, when elemental sulfur and sulfur extraction agent temperature height, reaction is very fast, but it is large that sulfur extraction agent also can be caused to volatilize, and operating environment is severe, and cost increase needs insulation to filter simultaneously; The strong cavitation effect that ultrasonic extraction utilizes Ultrasonic Radiation pressure to produce, mechanical vibration, disturbance effect and high acceleration, emulsification, spread, smash and the multistage effects such as stirring action, increase molecular motion of material frequency and speed, increase solvent penetration power, thus acceleration target component enters solvent, the carrying out of facilitated extraction.
If ultrasonic energy is enough strong, expansion process can generate bubble in a liquid or liquid is torn into very little hole.These holes close instantaneously, and produce the instantaneous pressure up to 3000MPa time closed, whole process completes in 400 μ s.Cavatition refinement material and manufacture emulsion, accelerate target component and enter solvent, improve extraction yield.Except cavatition, hyperacoustic many second-order effects are also all conducive to transfer and the extraction of target component.Cavitation phenomena reacts when bubbles burst, and in some some positions, bubble no longer absorbs ultrasonic energy and produces implosion.Gas in bubble or hole and the compression of steam fast adiabatic, produce high temperature and pressure.Bubble volume relative liquid cumulative volume is atomic, and the heat therefore produced scatters and disappears instantaneously, can not produce obvious impact to envrionment conditions, cavitation bubbles break after speed of cooling estimate be about 1010 DEG C/s.Ultrasonic hole provides interaction unique between energy and material, and the High Temperature High Pressure of generation can cause the formation of radical and other component.In neat liquid, time breaking in hole, because environmental conditions is identical, therefore total maintenance is spherical; But near solid boundaries place, breaking of hole is heterogeneous, produces high velocity liquid jet, make the potential energy of expanding bubble become the kinetic energy of liquid jet, move in bubble and penetrate walls.Injection stream is very strong in the surging force of solid surface, can cause great destruction, thus produce highly active unsalted surface to impact zone.The large several times of the surging force that the surging force that arc bubble deformation produces from the teeth outwards produces than bubble resonance.Ultrasonic extraction method is creatively applied in extraction sulphur technique first time by the present invention, is very effective to extracting various subject component from dissimilar sulphur slag.Using ultrasound ripple strengthening in extraction process, high temperature, high pressure that organic solvent and direct leached mud solid particle contacts face produce, the energy of oxidation etc. of the radical of sonolysis generation in addition, can provide high extraction energy.
The present invention, relative to the routine extraction sulphur technology of field of hydrometallurgy, has quick, inexpensive, the efficient feature of extraction.Its unusual effect mainly contains: ultrasonic extraction sulphur, without the need to high temperature, can realize low-temperature extraction, significantly reduce energy consumption; Security is good, and operation is simple, and maintaining is convenient; Little to the character relation of solvent and target extract, extraction efficiency is high; Feed throughput is large, at double or several times improve, and product impurity is few, and effective constituent is easy to be separated, purification; Extraction agent loss is little, and extraction sulphur process costs is low, and overall economic efficiency is remarkable.
Accompanying drawing explanation
Fig. 1 is the best processing route figure of the present invention.
Embodiment
Embodiment one
Sulphur slag ingredient (processed 100 mesh sieves, butt): plumbous 1.22%, zinc 4.75%, indium 0.0029%, silver 0.0569%, sulphur 74.83%.Take 5.0000 grams of sulphur slags, 62.5ml(100 gram) mixed solution of zellon and toluene, 100 DEG C of heating in water bath 30min, filter immediately, obtain residue 3.2126 grams, are cooled to 27.5 DEG C, obtain 0.7483 gram, sulphur, and extraction sulphur rate is 32%.
If in reacting by heating process, adopt ultrasonic extraction, ultrasonic frequency is 20KHz, and the sound intensity is at 2.0-50w/cm
2between, the reaction times is 8min, and at this moment the percentage extraction of sulphur sees the following form:
| The sound intensity (w/cm 2） | 2.0 | 2.8 | 10 | 20 | 35 | 50 |
| Output quality | 1.3843 | 1.5714 | 1.8410 | 2.1326 | 2.5442 | 2.6938 |
| Extraction sulphur rate | 37% | 42% | 49% | 57% | 68% | 72% |
If in reacting by heating process, adopt ultrasonic extraction, ultrasonic frequency is 100KHz, and the sound intensity is at 2.0-50w/cm
2between, the reaction times is 12min, and at this moment the percentage extraction of sulphur sees the following form:
| The sound intensity (w/cm 2） | 2.0 | 2.8 | 10 | 20 | 35 | 50 |
| Output quality | 1.4591 | 1.6836 | 1.9829 | 2.3197 | 2.6190 | 2.8061 |
| Extraction sulphur rate | 39% | 45% | 53% | 62% | 70% | 75% |
If in reacting by heating process, adopt ultrasonic extraction, ultrasonic frequency is 200KHz, and the sound intensity is at 2.0-50w/cm
2between, the reaction times is 15min, and at this moment the percentage extraction of sulphur sees the following form:
| The sound intensity (w/cm 2） | 2.0 | 2.8 | 10 | 20 | 35 | 50 |
| Output quality | 1.5714 | 1.7959 | 2.0578 | 2.4319 | 2.8435 | 2.9932 |
| Extraction sulphur rate | 42% | 48% | 55% | 65% | 76% | 80% |
Embodiment two
Sulphur slag ingredient (processed 100 mesh sieves, butt): plumbous 1.22%, zinc 4.75%, indium 0.0029%, silver 0.0569%, sulphur 74.83%.Take 10.0000 grams of sulphur slags, 125ml(100 gram) mixed solution of trieline and dimethylbenzene, 100 DEG C of heating in water bath 30min, filter immediately, obtain residue 6.3962 grams, are cooled to 27.5 DEG C, obtain 2.2449 grams, sulphur, and extraction sulphur rate is 30%.In the comprehensive utilization operation of zinc ore concentrate or lead and zinc industry normal pressure/high-pressure oxygen-enriched direct leached mud, zinc in filter residue, lead, silver obtain enrichment, directly returning lead system reclaims plumbous, silver-colored, and the rate of recovery of lead, silver, indium, zinc is respectively 110%, 34%, 89%, 113%.
If in reacting by heating process, adopt ultrasonic extraction, ultrasonic frequency is 30KHz, and the sound intensity is at 2.0-50w/cm
2between, the reaction times is 9min, and at this moment the percentage extraction of sulphur sees the following form:
| The sound intensity (w/cm 2） | 2.0 | 2.8 | 10 | 20 | 35 | 50 |
| Output quality | 2.6190 | 2.9932 | 3.5170 | 4.1156 | 4.9387 | 5.2381 |
| Extraction sulphur rate | 35% | 40% | 47% | 55% | 66% | 70% |
If in reacting by heating process, adopt ultrasonic extraction, ultrasonic frequency is 120KHz, and the sound intensity is at 2.0-50w/cm
2between, the reaction times is 11min, and at this moment the percentage extraction of sulphur sees the following form:
| The sound intensity (w/cm 2） | 2.0 | 2.8 | 10 | 20 | 35 | 50 |
| Output quality | 2.7687 | 3.1428 | 3.8163 | 4.4898 | 5.0084 | 5.4625 |
| Extraction sulphur rate | 37% | 42% | 51% | 60% | 68% | 73% |
If in reacting by heating process, adopt ultrasonic extraction, ultrasonic frequency is 180KHz, and the sound intensity is at 2.0-50w/cm
2between, the reaction times is 14min, and at this moment the percentage extraction of sulphur sees the following form:
| The sound intensity (w/cm 2） | 2.0 | 2.8 | 10 | 20 | 35 | 50 |
| Output quality | 2.9932 | 3.4421 | 3.9659 | 4.7142 | 5.5374 | 5.8367 |
| Extraction sulphur rate | 40% | 46% | 53% | 63% | 74% | 78% |
Embodiment three
Sulphur slag ingredient (processed 100 mesh sieves, butt): plumbous 1.22%, zinc 4.75%, indium 0.0029%, silver 0.0569%, sulphur 74.83%.Take 10.0000 grams of sulphur slags, 125ml(100 gram) zellon, 100 DEG C of heating in water bath 30min, filter immediately, obtain residue 6.3962 grams, are cooled to 27.5 DEG C, obtain 2.0952 grams, sulphur, and extraction sulphur rate is 28%.In the comprehensive utilization operation of zinc ore concentrate or lead and zinc industry normal pressure/high-pressure oxygen-enriched direct leached mud, the zinc in filter residue, lead, silver obtain enrichment, first leach to cross filter residue after reclaiming zinc to send lead system to reclaim plumbous, silver-colored, return direct leaching system containing zinc filtrate.At this moment, the rate of recovery of lead, silver, indium, zinc is respectively 120%, 36%, 85%, 124%.
If in reacting by heating process, adopt ultrasonic extraction, ultrasonic frequency is 40KHz, and the sound intensity is at 2.0-50w/cm
2between, the reaction times is 8min, and at this moment the percentage extraction of sulphur sees the following form:
| The sound intensity (w/cm 2） | 2.0 | 2.8 | 10 | 20 | 35 | 50 |
| Output quality | 2.69381 | 3.0680 | 3.5918 | 4.1904 | 5.0136 | 5.3129 |
| Extraction sulphur rate | 36% | 41% | 48% | 56% | 67% | 71% |
If in reacting by heating process, adopt ultrasonic extraction, ultrasonic frequency is 130KHz, and the sound intensity is at 2.0-50w/cm
2between, the reaction times is 12min, and at this moment the percentage extraction of sulphur sees the following form:
| The sound intensity (w/cm 2） | 2.0 | 2.8 | 10 | 20 | 35 | 50 |
| Output quality | 2.8435 | 3.2925 | 3.8911 | 4.5646 | 5.1632 | 5.5374 |
| Extraction sulphur rate | 38% | 44% | 52% | 61% | 69% | 74% |
If in reacting by heating process, adopt ultrasonic extraction, ultrasonic frequency is 160KHz, and the sound intensity is at 2.0-50w/cm
2between, the reaction times is 15min, and at this moment the percentage extraction of sulphur sees the following form:
| The sound intensity (w/cm 2） | 2.0 | 2.8 | 10 | 20 | 35 | 50 |
| Output quality | 3.0680 | 3.5170 | 3.9659 | 4.7891 | 5.6122 | 5.9115 |
| Extraction sulphur rate | 41% | 47% | 53% | 64% | 75% | 79% |
Claims (10)
1. process is containing a ultrasonic extraction method for elemental sulfur slag, it is characterized in that: the mixture of one or more in employing zellon, trieline, toluene, dimethylbenzene, as solvent, implements ultrasonic extraction to containing elemental sulfur slag.
2. a kind of process according to claim 1 is containing the ultrasonic extraction method of elemental sulfur slag, and it is characterized in that: described ultrasonic extraction, its ultrasonic frequency is 20-200KHz, and the sound intensity is 2.0-50w/cm
2.
3. a kind of process according to claim 1 is containing the ultrasonic extraction method of elemental sulfur slag, it is characterized in that: described contains elemental sulfur slag, at least comprises the leached mud adopting pressurization means of oxygen rich leaching method and normal pressure means of oxygen rich leaching method process zinc sulfide concentrates and lead sulfide zinc ore concentrate output.
4. process is containing a ultrasonic extraction technique for elemental sulfur slag, it is characterized in that: implement according to the following steps,
(1) add containing elemental sulfur slag the ultrasonic wave Leaching reaction device that sulfur extraction agent is housed in advance, carry out reacting by heating;
(2) insulation is filtered;
(3) cool;
(4) sulfur product be extracted is refiltered.
5. a kind of process according to claim 4 is containing the ultrasonic extraction technique of elemental sulfur slag, it is characterized in that: before extractive reaction, carry out drying, grinding, screening pre-treatment to containing elemental sulfur slag, make moisture be less than or equal to 10%, after grinding, cross 100 mesh sieve screenings.
6. a kind of process according to claim 4 is containing the ultrasonic extraction technique of elemental sulfur slag, it is characterized in that: described sulfur extraction agent is the mixture of one or more in zellon, trieline, toluene, dimethylbenzene, measures by liquid-solid ratio 8-15.
7. a kind of process according to claim 4 is containing the ultrasonic extraction technique of elemental sulfur slag, it is characterized in that: in described reacting by heating, ultrasonic frequency 20-200KHz, sound intensity 2.8-20w/cm
2, reaction 8-15 minute.
8. a kind of process according to claim 4 is containing the ultrasonic extraction technique of elemental sulfur slag, it is characterized in that: it is centrifuging that described insulation is filtered, and carries out being incubated, airtight and Exhaust Gas cooling recycling during filtration; Described cooling is to the first naturally cooling of filtrate, then forces cooling.
9. a kind of process according to any one of claim 4 to 8 is containing the ultrasonic extraction technique of elemental sulfur slag, it is characterized in that: described ultrasonic extraction technique is also applied in the comprehensive utilization of zinc ore concentrate or lead and zinc industry means of oxygen rich leaching slag, filtrate is separated out after sulphur through cooling, obtain regenerating sulfur extraction agent, return extraction sulphur operation; Zinc in filter residue, lead, silver obtain enrichment, send lead system to reclaim zinc, lead, silver.
10. a kind of process according to any one of claim 4 to 8 is containing the ultrasonic extraction technique of elemental sulfur slag, it is characterized in that: described ultrasonic extraction technique is also applied in the comprehensive utilization of zinc ore concentrate or lead and zinc industry means of oxygen rich leaching slag, filtrate is separated out after sulphur through cooling, obtain regenerating sulfur extraction agent, return extraction sulphur operation; Zinc in filter residue, lead, silver obtain enrichment, cross filter residue and send lead system recovery plumbous, silver-colored, return direct leaching system containing zinc filtrate after first leaching recovery zinc.
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| CN104831062A (en) * | 2015-03-26 | 2015-08-12 | 武汉钢铁(集团)公司 | A method of extracting valuable elements by utilization of sulfur concentrate |
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| CN112198081A (en) * | 2020-10-12 | 2021-01-08 | 长沙矿冶研究院有限责任公司 | Method for measuring elemental sulfur content in ore |
| CN113549760A (en) * | 2021-08-02 | 2021-10-26 | 中国科学院过程工程研究所 | Method for improving divalent metal extraction separation difference |
| 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 |
| CN115921123A (en) * | 2022-10-11 | 2023-04-07 | 昆明理工大学 | Novel galena-chalcopyrite separation composite inhibitor and application thereof |
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| CN115921123B (en) * | 2022-10-11 | 2024-04-05 | 昆明理工大学 | Novel composite inhibitor for galena-chalcopyrite separation and application thereof |
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Application publication date: 20141224 |