CN103482580A - Method for recycling elemental sulphur from ordinary-pressure oxygen-enrichment direct zinc hydrometallurgy high-sulphur residues - Google Patents
Method for recycling elemental sulphur from ordinary-pressure oxygen-enrichment direct zinc hydrometallurgy high-sulphur residues Download PDFInfo
- Publication number
- CN103482580A CN103482580A CN201310422340.9A CN201310422340A CN103482580A CN 103482580 A CN103482580 A CN 103482580A CN 201310422340 A CN201310422340 A CN 201310422340A CN 103482580 A CN103482580 A CN 103482580A
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- Prior art keywords
- oxygen
- pressure oxygen
- zinc hydrometallurgy
- elementary sulfur
- high sulphur
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 102
- 239000005864 Sulphur Substances 0.000 title claims abstract description 59
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 56
- 239000001301 oxygen Substances 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 42
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 32
- 239000011701 zinc Substances 0.000 title claims abstract description 32
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000009854 hydrometallurgy Methods 0.000 title claims abstract description 25
- 238000004064 recycling Methods 0.000 title abstract 2
- 238000007654 immersion Methods 0.000 claims abstract description 16
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract description 5
- 239000002893 slag Substances 0.000 claims description 48
- 229910052717 sulfur Inorganic materials 0.000 claims description 43
- 239000011593 sulfur Substances 0.000 claims description 42
- 238000002844 melting Methods 0.000 claims description 20
- 230000008018 melting Effects 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 15
- 238000007701 flash-distillation Methods 0.000 claims description 9
- 238000005188 flotation Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000009834 vaporization Methods 0.000 claims description 2
- 230000008016 vaporization Effects 0.000 claims description 2
- 239000012141 concentrate Substances 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000000630 rising effect Effects 0.000 abstract 2
- 238000001704 evaporation Methods 0.000 abstract 1
- 230000008020 evaporation Effects 0.000 abstract 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 229910052709 silver Inorganic materials 0.000 description 7
- 239000004332 silver Substances 0.000 description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000004821 distillation Methods 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 4
- 238000002386 leaching Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- -1 silver Chemical class 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
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Abstract
The invention relates to a method for recycling elemental sulphur from high-sulphur residues produced in an ordinary-pressure oxygen-enrichment direct zinc hydrometallurgy process. According to the technical scheme, rapid temperature and pressure rising is conducted on oxygen immersion during ordinary-pressure oxygen-enrichment direct zinc hydrometallurgy, flash evaporation is conducted, and then the melted elemental sulphur is cooled into granular solid elemental sulphur after the elemental sulphur is separated in a hot filtration mode. The method has the advantages that by means of rapid temperature and pressure rising, a small reactor is added to an existing ordinary-pressure oxygen-enrichment direct zinc hydrometallurgy system, equipment is simple, investment is low, the existing production system is not affected, process procedures are short, operation is easy, and the zinc concentrate ordinary-pressure oxygen-enrichment direct hydrometallurgy process is perfected.
Description
Technical field
The present invention relates to a kind of method that reclaims elementary sulfur from the high sulphur slag of the direct Zinc Hydrometallurgy Process output of normal pressure oxygen enrichment.
Background technology
In conventional zinc hydrometallurgy, zinc ore concentrate is adopted to fluidized bed roasting, the oxidized formation of sulphur SO
2enter flue gas and produce sulfuric acid.And in the direct zinc hydrometallurgy of normal pressure oxygen enrichment, to zinc ore concentrate, adopt the normal pressure oxygen enrichment directly to leach (95 ℃, normal atmosphere, pass into the dense oxygen of 98% above oxygen), the oxidized forming element sulphur of sulphur produces a large amount of high sulphur slags, both at home and abroad all less than reclaiming the industrial practice of elementary sulfur the high sulphur slag from the direct Zinc Hydrometallurgy Process output of normal pressure oxygen enrichment.This high sulphur slag mostly is placed on special slag field as waste abroad and stores up, and this high sulphur slag waits valuable metal because being rich in silver at home, need be by after recovery of elemental sulfur, and the valuable metals such as silver obtain enrichment and further reclaim.This high sulphur slag is to adopt the method for heat filtering after the steam heating melting to produce elementary sulfur, can not directly drop in a large number lead system because sulfur-bearing is too high and cause the sulphur imbalance simultaneously, this high sulphur slag can only adopt interim slag field to store up, and causes huge environmental protection pressure.The overstocked valuable metals such as silver of high sulphur slag can not reclaim simultaneously, cause deficiency in economic performance.
To the direct zinc hydrometallurgy high sulphur slag of this normal pressure oxygen enrichment, can adopt traditional fluidized bed roasting to carry out desulfurization, sulfur-containing smoke gas send relieving haperacidity to produce sulfuric acid, slag send lead system to reclaim the valuable metals such as silver, the integral production technical process is complete, but do not reach the purpose that reclaims elementary sulfur from high sulphur slag, just the roasting relieving haperacidity of zinc ore concentrate is changed into to the roasting relieving haperacidity of high sulphur slag, a kind of simple short processes flow process is reduced into again to a kind of traditional farm labourer's process flow of complexity.Owing to the high sulphur slag from the direct Zinc Hydrometallurgy Process output of normal pressure oxygen enrichment, can not reclaiming elementary sulfur, thereby this zinc ore concentrate normal pressure oxygen enrichment direct leaching process is incomplete.
Summary of the invention
The purpose of this invention is to provide and a kind ofly from the direct zinc hydrometallurgy high sulphur slag of normal pressure oxygen enrichment, reclaim elementary sulfur, greatly reduce the sulphur of high sulphur slag, and be beneficial to further recovery for further improving the valuable metal grades such as silver, perfect zinc ore concentrate normal pressure oxygen enrichment direct leaching process.
Technical scheme of the present invention is:
1), by the oxygen immersion liquid in the direct zinc hydrometallurgy of normal pressure oxygen enrichment, pass into oxygen and steam and be rapidly heated and boost in reactor; Wherein temperature is 110～150 ℃, pressure 450～1100Kpa, and oxygen partial pressure is 250～800Kpa;
2) the High Temperature High Pressure oxygen immersion liquid obtained in step 1) is carried out to flash distillation by flash drum;
3) the oxygen immersion liquid after flash distillation is carried out to flotation and obtain high sulphur slag;
4) the high sulphur slag heating is obtained to the elementary sulfur of molten state;
5) step 4) is obtained to high sulphur slag and carry out heat filtering output melting elementary sulfur.
6) adopt nodulizer, to the melting elementary sulfur, adopt water cooling to become the particulate solid elementary sulfur.
The applicant finds by research: the high sulphur slag sulfur-bearing that the direct Zinc Hydrometallurgy Process of normal pressure oxygen enrichment produces reaches 70～80%, and at the temperature of 150 ℃ of left and right, the sulphur in these high sulphur slags can not separate in melting; Be greater than at the temperature of 400 ℃, elementary sulfur distillation in high sulphur slag can be being become to gaseous state, under the condition of isolated air, through condensation, can obtain elementary sulfur.But adopt this distillation method to reclaim elementary sulfur from high sulphur slag and bring two vital problems, the one, the equipment complexity, quantity is many, and investment is large, especially requires to distill in isolated air conditions, is applied to large-scale industrial production unrealistic; The 2nd, distillation method running cost is high, for the sulfur recovery of low value, adopts distillation method to lose more than gain.
The applicant finds by research: in the high sulphur slag produced at the direct Zinc Hydrometallurgy Process of normal pressure oxygen enrichment, in element sulphur, 10～20% be the vitriol form, 90～80% is the elementary sulfur form.Elementary sulfur crystal formation difference in high sulphur slag, make at 150 ℃ of temperature just, and in these high sulphur slags, elementary sulfur can not melting, also just can't adopt the mode of heat filtering after simple steam heating to reclaim elementary sulfur from high sulphur slag.
Therefore, the applicant proposes first the normal pressure oxygen immersion liquid in the direct zinc hydrometallurgy of normal pressure oxygen enrichment to be carried out to pyroprocessing, and the oxygen immersion liquid under High Temperature High Pressure is carried out to flash distillation by flash drum, the crystalline structure of element sulphur is wherein changed, then the oxygen immersion liquid after flash distillation is obtained to high sulphur slag by flotation separation, again the high sulphur slag after this processing is heated, melting sulphur wherein, and separated.
Due to the pressure general control when the oxygen immersion liquid is carried out to high temperature high pressure process at 450～1100Kpa, therefore, pressure in flash drum will be starkly lower than 450Kpa, 200Kpa for example, the oxygen immersion liquid that is high-temperature pressure by the oxygen immersion liquid step-down of High Temperature High Pressure by flash distillation, the requirement of processing to meet subsequent handling.
The high sulphur slag obtained according to the inventive method is carried out to heat treatment, to obtain molten sulfur, while being convenient to further separate, preferably adopt steam-heated method.Those skilled in the art can also adopt additive method heating high sulphur slag.
The equipment of fractional melting sulphur can select the blade pressure filter to carry out heat filtering output melting elementary sulfur.Filter residue after separate sulfur is rich in the valuable metals such as silver simultaneously, in order to further reclaim.
By nodulizer, adopt water cooling to become the particulate solid elementary sulfur melting elementary sulfur.
The invention has the advantages that:
1) utilize the method that is rapidly heated and boosts, increase the reactor of small volume in the existing direct wet zinc-making system of normal pressure oxygen enrichment, equipment is simple, and less investment does not affect existing production system.
2) utilize flash vaporization process, elementary sulfur crystalline structure in high sulphur slag is transformed, can melting at 150 ℃ of temperature.
3) owing to having changed elementary sulfur crystalline structure in high sulphur slag, after the employing steam heating, the method for heat filtering reclaims elementary sulfur, belongs to physical process, and technical process is short, and equipment is simple, processing ease, and production cost is low.
4) from the direct zinc hydrometallurgy high sulphur slag of normal pressure oxygen enrichment sulphur to elementary sulfur product direct yield>85%, S>99.5%.
5) perfect zinc ore concentrate normal pressure oxygen enrichment direct leaching process.
The accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Embodiment 1
The technique of the direct zinc hydrometallurgy of normal pressure oxygen enrichment is: zinc ore concentrate enters reactor through ore grinding, adds waste electrolyte, passes into oxygen and steam that 98% above oxygen is dense, carries out the normal pressure oxygen enrichment and directly leaches, and controls 95 ℃ of temperature, normal atmosphere, reaction times>24h.
Briefly introduce technique and the parameter of the direct zinc hydrometallurgy of normal pressure oxygen enrichment
1) by (95 ℃ of the high-temperature pressure oxygen immersion liquid in the direct zinc hydrometallurgy of normal pressure oxygen enrichment of above-mentioned acquisition, normal atmosphere) be placed in reactor, pass into oxygen and steam, be rapidly heated and boosted, reaction times 20～40min, 110～150 ℃ of temperature, pressure 450～1100Kpa, wherein oxygen partial pressure is 250～800Kpa.
2) the above-mentioned High Temperature High Pressure oxygen immersion liquid be rapidly heated after boosting is placed in to flash drum and carries out flash distillation, in flash drum, temperature is 102～120 ℃, pressure 200Kpa.
3) the oxygen immersion liquid after flash distillation is carried out to flotation, flotation divide roughly select, selected, scan three sections operations, control 60～80 ℃ of flotation temperatures, inflation pressure 100～300Kpa.(please supplement disclosed flotation conditions in concrete prior art) obtains high sulphur slag, and output low-sulfur slag send slag to process simultaneously.
4) above-mentioned high sulphur slag is added in sulfur melting pool, pass into steam heating and carry out melting, control 150 ℃ of temperature.
5) adopt the blade pressure filter, the melting high sulphur slag is carried out to heat filtering, filter pressure 500～800Kpa, 150 ℃ of temperature, output melting elementary sulfur, the hot filter residue of while output is rich in silver and waits valuable metal further to reclaim.
6) adopt nodulizer, to the melting elementary sulfur, adopt water cooling to become the particulate solid elementary sulfur.
Claims (2)
1. reclaim the method for elementary sulfur from the direct zinc hydrometallurgy high sulphur slag of normal pressure oxygen enrichment, it is characterized in that comprising the steps:
1), by the oxygen immersion liquid in the direct zinc hydrometallurgy of normal pressure oxygen enrichment, pass into oxygen and steam and be rapidly heated and boost in reactor; Wherein temperature is 110～150 ℃, pressure 450～1100Kpa, and oxygen partial pressure is 250～800KPa;
2) the High Temperature High Pressure oxygen immersion liquid obtained in step 1) is carried out to flash distillation by flash drum;
3) the oxygen immersion liquid after flash distillation is carried out to flotation and obtain high sulphur slag;
4) high sulphur slag is passed in sulfur melting pool to steam and carry out melting;
5) the melting high sulphur slag is carried out to heat filtering output melting elementary sulfur by the blade pressure filter;
6) adopt nodulizer, to the melting elementary sulfur, adopt water cooling to become the particulate solid elementary sulfur.
2. the method that reclaims elementary sulfur from the direct zinc hydrometallurgy high sulphur slag of normal pressure oxygen enrichment according to claim 1, is characterized in that the flash vaporization point in step 3) is 102～120 ℃, pressure 200Kpa.
3. the method that reclaims elementary sulfur from the direct zinc hydrometallurgy high sulphur slag of normal pressure oxygen enrichment according to claim 1, is characterized in that step 4) the middle method that heats high sulphur slag is to pass into steam, and the control temperature is 145～155 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310422340.9A CN103482580B (en) | 2013-09-17 | 2013-09-17 | Method for recycling elemental sulphur from ordinary-pressure oxygen-enrichment direct zinc hydrometallurgy high-sulphur residues |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310422340.9A CN103482580B (en) | 2013-09-17 | 2013-09-17 | Method for recycling elemental sulphur from ordinary-pressure oxygen-enrichment direct zinc hydrometallurgy high-sulphur residues |
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| Publication Number | Publication Date |
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| CN103482580A true CN103482580A (en) | 2014-01-01 |
| CN103482580B CN103482580B (en) | 2015-04-29 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104445083A (en) * | 2014-11-25 | 2015-03-25 | 株洲冶炼集团股份有限公司 | Comprehensive recovery method for sulfur ore concentrate |
| CN104445084A (en) * | 2014-11-25 | 2015-03-25 | 株洲冶炼集团股份有限公司 | Method for recovering sulfur from zinc-leached sulfur-containing residues |
| CN109593959A (en) * | 2018-12-24 | 2019-04-09 | 重庆工程职业技术学院 | A kind of pyrolusite and zincblende joint oxygen press acid leaching process |
| CN111392696A (en) * | 2020-04-26 | 2020-07-10 | 中国恩菲工程技术有限公司 | Device and method for recovering elemental sulfur in sulfur-containing hydrometallurgy slag |
| CN111874870A (en) * | 2020-08-11 | 2020-11-03 | 中南大学 | Device and method for regulating and controlling crystallization transformation of element sulfur in high-sulfur slag in zinc smelting |
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| CN101734626A (en) * | 2009-11-23 | 2010-06-16 | 长沙有色冶金设计研究院 | Method for recovering sulfur element from zinc sulphide concentrate direct leaching residues |
| CN102796868A (en) * | 2012-09-12 | 2012-11-28 | 长沙有色冶金设计研究院有限公司 | Production process for directly leaching zinc from zinc sulfide concentrate |
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2013
- 2013-09-17 CN CN201310422340.9A patent/CN103482580B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101734626A (en) * | 2009-11-23 | 2010-06-16 | 长沙有色冶金设计研究院 | Method for recovering sulfur element from zinc sulphide concentrate direct leaching residues |
| CN102796868A (en) * | 2012-09-12 | 2012-11-28 | 长沙有色冶金设计研究院有限公司 | Production process for directly leaching zinc from zinc sulfide concentrate |
Non-Patent Citations (1)
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| 邓孟俐: "硫化锌精矿加压浸出元素硫的形成机理及硫回收工艺的研究", 《工程设计与研究》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104445083A (en) * | 2014-11-25 | 2015-03-25 | 株洲冶炼集团股份有限公司 | Comprehensive recovery method for sulfur ore concentrate |
| CN104445084A (en) * | 2014-11-25 | 2015-03-25 | 株洲冶炼集团股份有限公司 | Method for recovering sulfur from zinc-leached sulfur-containing residues |
| CN109593959A (en) * | 2018-12-24 | 2019-04-09 | 重庆工程职业技术学院 | A kind of pyrolusite and zincblende joint oxygen press acid leaching process |
| CN111392696A (en) * | 2020-04-26 | 2020-07-10 | 中国恩菲工程技术有限公司 | Device and method for recovering elemental sulfur in sulfur-containing hydrometallurgy slag |
| CN111874870A (en) * | 2020-08-11 | 2020-11-03 | 中南大学 | Device and method for regulating and controlling crystallization transformation of element sulfur in high-sulfur slag in zinc smelting |
| CN111874870B (en) * | 2020-08-11 | 2023-08-18 | 中南大学 | Device and method for regulating and controlling element sulfur crystallization transformation in zinc smelting high-sulfur slag |
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| CN103482580B (en) | 2015-04-29 |
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