CN104120272B - A kind of method of comprehensive utilization of zinc ore concentrate hyperbaric oxygen leaching sulphur slag - Google Patents
A kind of method of comprehensive utilization of zinc ore concentrate hyperbaric oxygen leaching sulphur slag Download PDFInfo
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- CN104120272B CN104120272B CN201410307879.4A CN201410307879A CN104120272B CN 104120272 B CN104120272 B CN 104120272B CN 201410307879 A CN201410307879 A CN 201410307879A CN 104120272 B CN104120272 B CN 104120272B
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Abstract
The present invention relates to the method for comprehensive utilization of a kind of zinc ore concentrate hyperbaric oxygen leaching sulphur slag, belong to the field of industrial residue comprehensive utilization in metallurgy industry.The inventive method is that sulphur slag is joined in the leaching vat containing water and dithiocarbonic anhydride, water plays sealing process, prevent dithiocarbonic anhydride volatilization in leaching process, obtain the sulfur product of high-quality through vacuum filtration, distillation after stirring reaction, filter residue obtains the enrichment slag of enrichment zinc-mercury after washing, drying; The sulfur product sulfur-bearing more than 99.5%, Hg adopting aforesaid method to obtain is less than 0.02mg/kg, and in enrichment slag, Zn content reaches about about 25%, more than Ag1600g/t, Hg0.5%; This technology not only can make full use of trade waste sulphur slag, is the application approach that the exploitation one of sulphur slag is new, turns waste into wealth, and can alleviate the environmental protection pressure of smeltery simultaneously, reduces environmental pollution, improves Business Economic Benefit.
Description
Technical field
The invention belongs to the research field that in metallurgy industry, solid waste utilizes, be specially the method for comprehensive utilization relating to the containing sulphur-slag produced in the dipped journey of zinc ore concentrate hyperbaric oxygen.
Background technology
Adopt hyperbaric oxygen soaking technology Leaching Zinc concentrate, zinc ore concentrate and oxygen in autoclave, the reactions such as electrolysis spent, control certain temperature and pressure, zinc ore concentrate directly can leach as ZnSO4 solution and produce simple substance sulphur, other insoluble impurities that simple substance sulphur and concentrate raw material are brought into mixes, oxygen leaching slag is obtained after being separated, the main component of this slag is sulfur-bearing 60 ~ 80%, Zn6 ~ 10%, Fe2 ~ 7%, Pb1 ~ 6%, Ag400 ~ 800g/t, Hg0.15 ~ 0.2% etc., so the main component of oxygen leaching slag is sulphur, wherein major part is elementary sulfur, content is greater than 60%, and it is plumbous containing heavy metal element, zinc, iron, silver and mercury etc.If the sulphur slag bulk deposition containing unstable element sulphur and heavy metal element, severe contamination can be caused to ecotope and waste has Sulphur ressource and the valuable metal element of higher-value.
The process of zinc ore concentrate hyperbaric oxygen leaching sulphur slag, mainly contains following several mode at present: as the raw material of pyrite relieving haperacidity factory, produce sulfuric acid after batching, but is subject to the restriction of the factors such as transport and price; Slag is obtained iron concentrate through flotation separation, then carries out molten sulphur, heat filter, packing granulation etc. to extract sulfur product to iron concentrate, it is comparatively large that the method realizes difficulty, and the sulfur product difficult quality guarantee obtained; Reclaim after sulphur being volatilized by vacuum distillation method and obtain sulfur product, but this method is while recovery sulphur, mercury can volatilize with sulphur and enter sulphur product, affects sulfur product quality, and this method is harsh to equipment requirements simultaneously, is difficult to realize industrial-scale production etc.
Zinc ore concentrate hyperbaric oxygen leaching sulphur slag belongs to secondary resource, be rich in the valuable constituent such as sulphur and zinc, lead, silver and mercury, object of the present invention is exactly that exploitation one is by extracting the elemental sulphur in sulphur slag, the proprietary technology of the valuable metals such as the lead in Sync enrichment slag, zinc, iron, silver, mercury.
Summary of the invention
The object of the present invention is to provide a kind of trade waste zinc ore concentrate hyperbaric oxygen leaching sulphur slag that utilizes to produce the operational path with the sulfur product of higher-value, reach utilization of waste material, realize recycling economy, energy-saving and emission-reduction object; The technological process that this treatment process adopts is simple, and mild condition, sulphur extraction yield is high, and sulphur, mercury good separating effect, processing cost is low, is easy to realize suitability for industrialized production.
The present invention realizes the object of the invention by following method:
A, by liquid addition pipe, water is joined in leaching vat, leaching vat volume 60% place is provided with middle spacer web, then dithiocarbonic anhydride is added in the bottom of water, zinc ore concentrate hyperbaric oxygen leaching sulphur slag is added under 100rpm agitation condition, the mass ratio of zinc ore concentrate hyperbaric oxygen leaching sulphur slag and dithiocarbonic anhydride is 1:2 ~ 1:4, under the condition of water seal under room temperature, 250-400rpm stirring reaction 0.5 ~ 1.0h, leach the sulphur in sulphur slag material; Wherein all cumulative volumes (namely the solid-liquid mixture of water, dithiocarbonic anhydride, zinc ore concentrate hyperbaric oxygen leaching sulphur slag amasss) adding material are the 75-85% of leaching vat volume, and the solid-liquid volume of zinc ore concentrate hyperbaric oxygen leaching sulphur slag and dithiocarbonic anhydride is the 50-60% of leaching vat volume;
(B) to the solid-liquid mixture that steps A obtains, the sub-bottom of the vacuum filtration groove being added with water is in advance passed into by the discharge nozzle bottom leaching vat, filter under the condition of water seal, filter residue washes the enrichment slag obtaining Zn accumulation, mercury etc. for 3 times with water, merges all filter liquors; The effect of water is the volatilization avoiding dithiocarbonic anhydride at the water seal layer of vacuum filtration groove top formation certain altitude, being separated of residue and liquid phase (dithiocarbonic anhydride and water) is leached in filtration, utilize the water of the superiors to wash the dithiocarbonic anhydride that may exist in residue during filtration, reuse to reclaim dithiocarbonic anhydride.
(C) after the filtrate stratification that step B obtains, collect dithiocarbonic anhydride organic phase, and import in distiller by pipeline, distillation of heating under normal pressure, temperature 50 ~ 80 DEG C of conditions, the solid materials obtained after steaming dithiocarbonic anhydride is the sulfur product of high-quality; The dithiocarbonic anhydride employing temperature steamed is that the water of about 10 DEG C cools in eluting column, drip washing returns step A after collecting and reclaiming and recycles.
Leaching vat described in the present invention comprise cell body, liquid addition pipe, solid addition tube, airway, middle graticule mesh, discharge nozzle, wherein the position of middle spacer web is positioned at long-pending 60% place of leaching vat cell body, middle spacer web is 80 ~ 200 object screen clothes, the flowing of top and the bottom liquid can be ensured, the effect of middle spacer web ensures in agitation leach reaction process, water base of middle spacer web top keeps laminar flow regime that is static or that do not mix with lower liquid phase, thus reach the object of sealed lower portion liquid phase, to prevent the effusion of dithiocarbonic anhydride as far as possible; Liquid addition pipe and solid addition tube are arranged in cell body, and exit end is positioned at cell body inner bottom part, and leaching vat are tightness system, and airway is arranged on cell body top, and discharge nozzle is arranged on bottom cell body.
In the inventive method when adding material in leaching vat, first water is added, and then inject dithiocarbonic anhydride organic phase in the bottom of water, finally under the condition of low stirring velocity, add solid materials sulphur slag, the cumulative volume of sulphur slag and dithiocarbonic anhydride just in time reaches the bottom of middle spacer web, make water just in time on the top of middle spacer web, thus ensure that in reactor, water is to the water seal effect of dithiocarbonic anhydride.
In the present invention, leaching vat, filter vat are tightness system, and a small amount of carbon disulfide gas of overflowing in equipment is introduced centralized collection in eluting column by pipeline and recycled.
Effect of the present invention and advantage: the sulfur product sulfur-bearing more than 99.5, Hg adopting aforesaid method to obtain is less than 0.02mg/kg, and in enrichment slag, Zn content reaches about about 25%, more than Ag1600g/t, Hg0.5%.This technology not only can make full use of trade waste sulphur slag, is the application approach that the exploitation one of sulphur slag is new, turns waste into wealth, and can alleviate the environmental protection pressure of smeltery simultaneously, reduces environmental pollution, improves Business Economic Benefit; The internal structure of leaching vat of the present invention can meet the leaching completing sulphur in sulphur slag under agitation, simultaneously owing to there is metastable water layer height (effect of middle spacer web), can avoid the volatilization of leaching process dithiocarbonic anhydride.
Accompanying drawing explanation
Fig. 1 is the structural representation of leaching vat in the present invention;
In figure: 1-cell body; 2-liquid addition pipe; 3-solid addition tube; 4-airway; Graticule mesh in the middle of 5-; 6-discharge nozzle; 7-agitator.
Embodiment
Below by drawings and Examples, the present invention is described in further detail, but protection scope of the present invention is not limited to described content.
embodiment 1:by liquid addition pipe, water is joined in leaching vat, long-pending 60% place of leaching vat cell body is provided with middle spacer web, then dithiocarbonic anhydride is added in the bottom of water, the zinc ore concentrate hyperbaric oxygen leaching sulphur slag containing 74.58% sulphur, 8.25%Zn, 527g/tAg and 0.17%Hg is added under 100rpm agitation condition, the mass ratio of zinc ore concentrate hyperbaric oxygen leaching sulphur slag and dithiocarbonic anhydride is 1:2, after reinforced, improve stirring velocity to 250rpm, under the condition of water seal, leach the sulphur in sulphur slag material in stirred at ambient temperature reaction 1.0h; Wherein all cumulative volumes adding material are 85% of leaching vat volume, and the solid-liquid volume of zinc ore concentrate hyperbaric oxygen leaching sulphur slag and dithiocarbonic anhydride is 60% of leaching vat volume;
Then passed into the sub-bottom of the vacuum filtration groove being added with water in advance by the discharge nozzle bottom leaching vat, under the condition of water seal, carry out vacuum filtration (solid-liquor separation), filter residue washes 3 times with water, obtains the enrichment slag of zinc, mercury etc., merges all filter liquors; After filtrate stratification, collect dithiocarbonic anhydride organic phase, and dithiocarbonic anhydride organic phase is sent into distiller by pipeline, distill in 50 DEG C at ambient pressure, steam whole liquid, obtain sulfur product; The dithiocarbonic anhydride that steams imports in eluting column, adopts temperature to be that water cooling, the drip washing of 10 DEG C returns leaching vat after collecting and reclaiming and recycles; Analysis shows, sulfur product is containing S99.74%, Hg0.17mg/kg, and outward appearance is yellow, and the yield of sulphur is 95.32%; Enrichment slag is containing Zn26.95%, Hg0.54%, Ag1748g/t.
The leaching vat that the present embodiment uses comprise cell body 1, liquid addition pipe 2, solid addition tube 3, airway 4, middle graticule mesh 5, discharge nozzle 6, agitator 7, wherein the position of middle spacer web 5 is positioned at long-pending 60% place of leaching vat cell body, liquid addition pipe 2 and solid addition tube 3 are arranged in cell body 1, and exit end is positioned at cell body inner bottom part, leaching vat are tightness system, airway 4 is arranged on cell body 1 top, and discharge nozzle 6 is arranged on bottom cell body, and agitator 7 is arranged on cell body inner bottom part (see figure 1).
embodiment 2:by liquid addition pipe, water is joined in leaching vat, long-pending 60% place of leaching vat cell body is provided with middle spacer web, then dithiocarbonic anhydride is added in the bottom of water, the zinc ore concentrate hyperbaric oxygen leaching sulphur slag containing 74.58% sulphur, 8.25%Zn, 527g/tAg and 0.17%Hg is added under 100rpm agitation condition, the mass ratio of zinc ore concentrate hyperbaric oxygen leaching sulphur slag and dithiocarbonic anhydride is 1:4, after reinforced, improve stirring velocity to 400rpm, under the condition of water seal, leach the sulphur in sulphur slag material in stirred at ambient temperature reaction 0.5h; Wherein all cumulative volumes adding material are 80% of leaching vat volume, and the solid-liquid volume of zinc ore concentrate hyperbaric oxygen leaching sulphur slag and dithiocarbonic anhydride is 55% of leaching vat volume;
Then passed into the sub-bottom of the vacuum filtration groove being added with water in advance by the discharge nozzle bottom leaching vat, under the condition of water seal, carry out vacuum filtration (solid-liquor separation), filter residue washes 3 times with water, obtains the enrichment slag of zinc, mercury etc., merges all filter liquors; After filtrate stratification, collect dithiocarbonic anhydride organic phase, and dithiocarbonic anhydride organic phase is sent into distiller by pipeline, distill in 70 DEG C at ambient pressure, steam whole liquid, obtain sulfur product; The dithiocarbonic anhydride that steams imports in eluting column, adopts temperature to be that water cooling, the drip washing of 10 DEG C returns leaching vat after collecting and reclaiming and recycles.Analysis shows, sulfur product is containing S99.62%, Hg0.02mg/kg, and outward appearance is yellow, and the yield of sulphur is 95.89%; Enrichment slag is containing Zn25.32%, Hg0.50%, Ag1674g/t.
The leaching vat structure that the present embodiment uses is with embodiment 1.
embodiment 3:by liquid addition pipe, water is joined in leaching vat, long-pending 60% place of leaching vat cell body is provided with middle spacer web, then dithiocarbonic anhydride is added in the bottom of water, the zinc ore concentrate hyperbaric oxygen leaching sulphur slag containing 74.58% sulphur, 8.25%Zn, 527g/tAg and 0.17%Hg is added under 100rpm agitation condition, the mass ratio of zinc ore concentrate hyperbaric oxygen leaching sulphur slag and dithiocarbonic anhydride is 1:3, after reinforced, improve stirring velocity to 300rpm, under the condition of water seal, leach the sulphur in sulphur slag material in stirred at ambient temperature reaction 0.75h; Wherein all cumulative volumes adding material are 75% of leaching vat volume, and the solid-liquid volume of zinc ore concentrate hyperbaric oxygen leaching sulphur slag and dithiocarbonic anhydride is 50% of leaching vat volume;
Then passed into the sub-bottom of the vacuum filtration groove being added with water in advance by the discharge nozzle bottom leaching vat, under the condition of water seal, carry out vacuum filtration (solid-liquor separation), filter residue washes 3 times with water, obtains the enrichment slag of zinc, mercury etc., merges all filter liquors; After filtrate stratification, collect dithiocarbonic anhydride organic phase, and dithiocarbonic anhydride organic phase is sent into distiller by pipeline, distill in 80 DEG C at ambient pressure, steam whole liquid, obtain sulfur product; The dithiocarbonic anhydride that steams imports in eluting column, adopts temperature to be that water cooling, the drip washing of 10 DEG C returns leaching vat after collecting and reclaiming and recycles; Analysis shows, sulfur product is containing S99.58%, Hg0.02mg/kg, and outward appearance is yellow, and the yield of sulphur is 94.85%; Enrichment slag is containing Zn26.17%, Hg0.58%, Ag1723g/t.
The leaching vat structure that the present embodiment uses is with embodiment 1.
embodiment 4:by liquid addition pipe, water is joined in leaching vat, long-pending 60% place of leaching vat cell body is provided with middle spacer web, then dithiocarbonic anhydride is added in the bottom of water, the zinc ore concentrate hyperbaric oxygen leaching sulphur slag containing 74.58% sulphur, 8.25%Zn, 527g/tAg and 0.17%Hg is added under 100rpm agitation condition, the mass ratio of zinc ore concentrate hyperbaric oxygen leaching sulphur slag and dithiocarbonic anhydride is 1:3, after reinforced, improve stirring velocity to 350rpm, under the condition of water seal, leach the sulphur in sulphur slag material in stirred at ambient temperature reaction 1h; Wherein all cumulative volumes adding material are 75% of leaching vat volume, and the solid-liquid volume of zinc ore concentrate hyperbaric oxygen leaching sulphur slag and dithiocarbonic anhydride is 60% of leaching vat volume;
Then passed into the sub-bottom of the vacuum filtration groove being added with water in advance by the discharge nozzle bottom leaching vat, under the condition of water seal, carry out vacuum filtration (solid-liquor separation), filter residue washes 3 times with water, obtains the enrichment slag of zinc, mercury etc., merges all filter liquors; After filtrate stratification, collect dithiocarbonic anhydride organic phase, and dithiocarbonic anhydride organic phase is sent into distiller by pipeline, distill in 60 DEG C at ambient pressure, steam whole liquid, obtain sulfur product; The dithiocarbonic anhydride that steams imports in eluting column, adopts temperature to be that water cooling, the drip washing of 10 DEG C returns leaching vat after collecting and reclaiming and recycles; Analysis shows, sulfur product is containing S99.69%, Hg0.12mg/kg, and outward appearance is yellow, and the yield of sulphur is 96.15%; Enrichment slag is containing Zn24.83%, Hg0.62%, Ag1643g/t.
The leaching vat structure that the present embodiment uses is with embodiment 1.
Claims (3)
1. a method of comprehensive utilization for zinc ore concentrate hyperbaric oxygen leaching sulphur slag, is characterized in that through following process steps:
A, by liquid addition pipe, water is joined in leaching vat, long-pending 60% place of leaching vat cell body is provided with middle spacer web, then dithiocarbonic anhydride is added in the bottom of water, zinc ore concentrate hyperbaric oxygen leaching sulphur slag is added under 100rpm agitation condition, the mass ratio of zinc ore concentrate hyperbaric oxygen leaching sulphur slag and dithiocarbonic anhydride is 1:2 ~ 1:4, the sulphur under the condition of water seal under room temperature, in 250 ~ 400rpm stirring reaction, 0.5 ~ 1.0h leaching sulphur slag material; Wherein all cumulative volumes adding material are the 75-85% of leaching vat volume, and the solid-liquid volume of zinc ore concentrate hyperbaric oxygen leaching sulphur slag and dithiocarbonic anhydride is the 50-60% of leaching vat volume;
B, the solid-liquid mixture obtained steps A, imported the sub-bottom of the vacuum filtration groove being added with water in advance, filter under the condition of water seal by pipeline, filter residue washes the enrichment slag obtaining Zn accumulation, mercury for 3 times with water, merges all filter liquors;
After the filtrate stratification that C, step B obtain, collect dithiocarbonic anhydride organic phase, and import in distiller by pipeline, to heat under normal pressure, temperature 50 ~ 80 DEG C of conditions distillation, the solid materials obtained after steaming dithiocarbonic anhydride is sulfur product, and the dithiocarbonic anhydride employing temperature steamed is that the water of 10 DEG C cools in eluting column, drip washing returns steps A after collecting and reclaiming and recycles.
2. the method for comprehensive utilization of zinc ore concentrate hyperbaric oxygen leaching sulphur slag according to claim 1, it is characterized in that: leaching vat comprise cell body, liquid addition pipe, solid addition tube, airway, middle spacer web, discharge nozzle, agitator, wherein the position of middle spacer web is positioned at long-pending 60% place of leaching vat cell body, liquid addition pipe and solid addition tube are arranged in cell body, and exit end is positioned at cell body inner bottom part, leaching vat are tightness system, airway is arranged on cell body top, discharge nozzle is arranged on bottom cell body, and agitator is arranged on cell body inner bottom part.
3. the method for comprehensive utilization of zinc ore concentrate hyperbaric oxygen leaching sulphur slag according to claim 1, is characterized in that: middle spacer web is 80 ~ 200 object screen clothes.
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| CN108977656A (en) * | 2018-08-24 | 2018-12-11 | 淄博淦达环保科技有限公司 | A kind of lixiviation process preparation process of Zinc in Zinc Concentrates and sulphur |
| CN108706546A (en) * | 2018-08-24 | 2018-10-26 | 淄博淦达环保科技有限公司 | A kind of leaching liquid of sulphur and sulphur technique processed |
| CN109590107B (en) * | 2019-01-02 | 2020-09-04 | 长沙有色冶金设计研究院有限公司 | Process for recovering sulfur and valuable metals from copper oxygen pressure leaching slag |
| CN112375916B (en) * | 2020-11-04 | 2022-07-15 | 昆明理工精诚技术开发有限公司 | Copper-cobalt hydrometallurgy filtering and washing system and operation mode thereof |
| CN113774221A (en) * | 2021-07-29 | 2021-12-10 | 广东邦普循环科技有限公司 | Method for extracting valuable metals and sulfur elements by leaching low grade nickel matte |
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| CN101503761B (en) * | 2009-03-24 | 2010-10-27 | 中南大学 | Method for separating and recycling valuable metal from pressure leached high sulphur slag |
| JP2013028520A (en) * | 2011-06-24 | 2013-02-07 | Jfe Steel Corp | Method for extracting sulfur from sulfur-containing slag and method for recycling hot metal desulfurization slag |
| CN103194621A (en) * | 2013-04-23 | 2013-07-10 | 吴鋆 | Method for treating sulfur slag |
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