CN103352116A - Method for recovering zinc from high iron and high lead leaching residue through microwave-ultrasonic wave combination - Google Patents
Method for recovering zinc from high iron and high lead leaching residue through microwave-ultrasonic wave combination Download PDFInfo
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- CN103352116A CN103352116A CN2013101172509A CN201310117250A CN103352116A CN 103352116 A CN103352116 A CN 103352116A CN 2013101172509 A CN2013101172509 A CN 2013101172509A CN 201310117250 A CN201310117250 A CN 201310117250A CN 103352116 A CN103352116 A CN 103352116A
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- leached mud
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- 239000011701 zinc Substances 0.000 title claims abstract description 40
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 26
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title abstract description 24
- 238000002386 leaching Methods 0.000 title abstract description 21
- 229910052742 iron Inorganic materials 0.000 title abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 238000011084 recovery Methods 0.000 claims abstract description 15
- 230000005855 radiation Effects 0.000 claims abstract description 14
- 239000011259 mixed solution Substances 0.000 claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002253 acid Substances 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000000746 purification Methods 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims abstract description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 10
- 239000000428 dust Substances 0.000 claims description 7
- 238000004070 electrodeposition Methods 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 239000001117 sulphuric acid Substances 0.000 claims description 6
- 235000011149 sulphuric acid Nutrition 0.000 claims description 6
- 238000003912 environmental pollution Methods 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 150000002739 metals Chemical class 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 abstract 1
- 238000005363 electrowinning Methods 0.000 abstract 1
- 239000002699 waste material Substances 0.000 abstract 1
- 229910001308 Zinc ferrite Inorganic materials 0.000 description 7
- WGEATSXPYVGFCC-UHFFFAOYSA-N zinc ferrite Chemical compound O=[Zn].O=[Fe]O[Fe]=O WGEATSXPYVGFCC-UHFFFAOYSA-N 0.000 description 7
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- PIJPYDMVFNTHIP-UHFFFAOYSA-L lead sulfate Chemical compound [PbH4+2].[O-]S([O-])(=O)=O PIJPYDMVFNTHIP-UHFFFAOYSA-L 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 239000002893 slag Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000010310 metallurgical process Methods 0.000 description 1
- 150000004965 peroxy acids Chemical class 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229960001866 silicon dioxide Drugs 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000009858 zinc metallurgy Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention provides a method for recovering zinc from high iron and high lead leaching residue through microwave-ultrasonic wave combination, and belongs to the technical field of microwave and ultrasonic wave applications. The method comprises: taking high iron and high lead leaching residue, adding carbon powder, uniformly mixing, carrying out microwave heating to a temperature of 550-950 DEG C, carrying out constant temperature maintaining for 1-3 h, stopping heating, introducing a N2 protection atmosphere, cooling to a temperature of less than 100 DEG C to obtain after-reduction leaching residue, adding the after-reduction leaching residue to an acid liquid, carrying out ultrasonic wave radiation on the mixed solution at a temperature of 45-85 DEG C to carry out enhancement leaching, carrying out solid-liquid separation to obtain a leaching solution, carrying out subsequent purification on the leaching solution, and recovering metal zinc through electrowinning. Compared to the conventional hot acid leaching, the method of the present invention has the following characteristics that: a leaching time is significantly shortened, a leaching acidity and a leaching temperature are reduced, and 90-98% of zinc can be recovered. With the present invention, the difficult problem of low recovery rate of the high lead and high iron system is overcome, the process is simple, the treatment effect is good, zinc and other valuable metals can be efficiently recovered, and problems of environmental pollution and resource waste caused by stockpiling of a lot of abandoned residue are solved.
Description
Technical field
The invention provides a kind of microwave calcining that utilizes and leach the method that from high ferro, high plumbous leached mud, reclaims zinc in conjunction with intensified by ultrasonic wave, belong to the microwave and ultrasound applied technical field.
Background technology
The purposes of zinc is very extensive, occupies an important position in national economy, and the fusing point of zinc is lower; fluidity of molten is good, and preferably corrosion resistance is arranged, and is mainly used in zinc-plated industry; the protective layer of Chang Zuowei iron and steel, such as zinc-plated sheet material pipe fitting etc., its consumption accounts for 50% of world's zinc consumption.China is that the first in the world is produced zinc big country, and normal association has 8～15% iron in the common ore deposit of domestic zinc.The present conventional smelting technology of zinc factory: roasting-leachings-electrodeposition, in the roasting conventional process, the zinc oxidation generation zinc ferrite in the inevitable and calcining of iron.Because of the stable chemical nature of zinc ferrite, the acidleach in the conventional hydrometallurgy is difficult to dissolve zinc ferrite fully, often needs high temperature, and the high pressure leaching condition is processed; And in the zinc ore also common association lead is arranged, in roasting and leach and to generate the lead sulfate that is insoluble in acid in the engineering, in leaching process, cover particle surface, hinder zinc in the reaction of acid; Because of the existence of above-mentioned lead sulfate and zinc ferrite material, cause the overall rate of recovery of zinc only to have 75～80%, and produce a large amount of leached muds.
For solving the recovery problem of zinc in the wet-leaching slag zinc ferrite, main wet method and thermal process has fuming process (201010286118.7) at present, reducing roasting (201110096566.5), electric heating process (91107379.5), hot acid lixiviation process (201110286158.6), but all perfect not, thermal process generally exists labour intensity larger, zinc recovery is not high, energy consumption is large, the problems such as environmental pollution is serious, and in conventional heating process need higher temperature and long reaction times (201010611028.0), and because the formed sosoloid of high temperature has higher hardness, bring certain difficulty for the later stage ore grinding, follow-uply be difficult to adopt ordinary method to reclaim wherein valuable metal, cause a large amount of slags to pile up; The problems such as there is complex process in existing wet processing, and equipment requirements is high, and input cost is higher.And peracid, hot conditions has improved running cost, and so that a large amount of ferro elements enters solution, causes electric effusion processing load and technical load to increase, and simultaneously the existence of lead sulfate is not had preferably treatment process yet.Therefore, the zinc metallurgy industry is at present in the urgent need to a kind of processing method that can effectively address the above problem.
Summary of the invention
The present invention is directed to the problem and the deficiency that exist in the existing production process, the processing method that a kind of microwave reducing roasting leaches in conjunction with intensified by ultrasonic wave has been proposed, take the Zn dust leached mud as raw material, join carbon reducting roast through microwave first, destroy the structure of zinc ferrite, reduced the required condition of follow-up leaching, the recycling ultrasonic cavitation produce mechanical effect, lead sulfate to the acidleach particle surface is peeled off, thereby so that the rate of recovery of zinc improves greatly, present method has not only proposed microwave for the zinc ferrite that exists in the zinc metallurgical process and lead sulfate respectively and has joined carbon reduction and intensified by ultrasonic wave extract technology, and reduces a large amount of leached muds and store up the problem of environmental pollution that causes.
The present invention realizes by following technical proposal: the method for zinc in a kind of microwave-ultrasonic combined recovery high ferro, the high plumbous leached mud, and following each step of process:
(1) get high ferro, high plumbous leached mud, add the carbon dust of its quality 1～7% again, mixing is by constant temperature behind microwave heating to 550～950 ℃ 1～3 hour, stopped heating then, and pass into N
2Protective atmosphere to be preventing the Z 250 oxidation, until temperature is down to below 100 ℃, obtains reducing rear leached mud;
(2) with leached mud after the reduction of step (1) gained, add concentration take liquid-solid ratio as 3～8:1 and be the acid solution of 70～170g/L, under 45～85 ℃, again mixed solution is strengthened with Ultrasonic Radiation and leached 1～3h, obtain leach liquor through solid-liquid separation, again leach liquor is carried out follow-up purification, reclaim metallic zinc through electrodeposition.
The acid solution of described step (2) is sulphuric acid soln.
The condition of the Ultrasonic Radiation of described step (2) is: ultrasonic frequency is 20～25KHz, every liter of ultrasonic power 40～160W that mixed solution distributes.
Advantage of the present invention:
(1) microwave has the characteristics of penetrance, selectivity heating, can act directly on the metal oxide, reduces required temperature of reaction, and Reaction time shorten is saved the energy, reduces cost, has the very strong market competitiveness.
(2) because carbon is strong wave absorbtion material, can so that material heats up evenly, avoid the local sintering phenomenon so evenly join carbon.
(3) the Ultrasonic Radiation stage produces a large amount of heat, and the acidleach temperature condition is provided, and need not extra heating.
(4) compare conventional hot acid and leach, obviously shortened extraction time, reduced leaching acidity and extraction temperature, can reclaim 90～98% zinc.
(5) the present invention has overcome high lead, the low difficult problem of zinc recovery under the high ferro system, and flow process is simple, and treatment effect is good, and the valuable metals such as energy high efficiente callback zinc solve a large amount of castaway slags and store up environmental pollution and the wasting of resources problem that causes.
Description of drawings
Fig. 1 is process flow sheet of the present invention;
Fig. 2 is the XRD figure spectrum of high ferro, high plumbous leached mud.
Embodiment
The present invention will be further described below by embodiment.
Embodiment 1
(1) get the boiler dirt high ferro of 250g Yunnan Metallurgical Factory, high plumbous leached mud, contain zinc 12.34%, iron 20.85%, lead 12.20%, silicon-dioxide 6.12%, indium 1091.9g/t, wherein main containing metal material is ZnFe
2O
4, PbSO
4, as shown in Figure 2.The carbon dust that adds again its quality 1%, mixing be by constant temperature after the microwave heating to 600 ℃ 2 hours, stopped heating then, and pass into N
2Protective atmosphere to be preventing the Z 250 oxidation, until temperature is down to below 100 ℃, obtains reducing rear leached mud;
(2) with leached mud after the reduction of step (1) gained, add concentration take liquid-solid ratio (L/Kg) as 8:1 and be the sulphuric acid soln of 150g/L, under 75 ℃, again mixed solution is strengthened with Ultrasonic Radiation and leached 3h, the condition of Ultrasonic Radiation is: ultrasonic frequency is 20KHz, and every liter of ultrasonic power 40W that mixed solution distributes obtains leach liquor through solid-liquid separation, again leach liquor is carried out follow-up purification, reclaim metallic zinc through electrodeposition.The rate of recovery of zinc reaches 92%, iron leaching rate 32%.
Embodiment 2
(1) get 250g high ferro, high plumbous leached mud, add the carbon dust of its quality 5% again, mixing is by constant temperature after the microwave heating to 800 ℃ 1 hour, stopped heating then, and pass into N
2Protective atmosphere to be preventing the Z 250 oxidation, until temperature is down to below 100 ℃, obtains reducing rear leached mud;
(2) with leached mud after the reduction of step (1) gained, add concentration take liquid-solid ratio as 5:1 and be the sulphuric acid soln of 70g/L, under 85 ℃, again mixed solution is strengthened with Ultrasonic Radiation and leached 2h, the condition of Ultrasonic Radiation is: ultrasonic frequency is 22KHz, and every liter of ultrasonic power 100W that mixed solution distributes obtains leach liquor through solid-liquid separation, again leach liquor is carried out follow-up purification, reclaim metallic zinc through electrodeposition.The rate of recovery of zinc reaches 95%, iron leaching rate 39%.
Embodiment 3
(1) get 250g high ferro, high plumbous leached mud, add the carbon dust of its quality 7% again, mixing is by constant temperature after the microwave heating to 550 ℃ 3 hours, stopped heating then, and pass into N
2Protective atmosphere to be preventing the Z 250 oxidation, until temperature is down to below 100 ℃, obtains reducing rear leached mud;
(2) with leached mud after the reduction of step (1) gained, add concentration take liquid-solid ratio as 3:1 and be the sulphuric acid soln of 170g/L, under 45 ℃, again mixed solution is strengthened with Ultrasonic Radiation and leached 1h, the condition of Ultrasonic Radiation is: ultrasonic frequency is 25KHz, and every liter of ultrasonic power 160W that mixed solution distributes obtains leach liquor through solid-liquid separation, again leach liquor is carried out follow-up purification, reclaim metallic zinc through electrodeposition.The rate of recovery of zinc reaches 97%, iron leaching rate 40%.
Embodiment 4
(1) get high ferro, high plumbous leached mud, add the carbon dust of its quality 6% again, mixing is by constant temperature after the microwave heating to 950 ℃ 3 hours, stopped heating then, and pass into N
2Protective atmosphere to be preventing the Z 250 oxidation, until temperature is down to below 100 ℃, obtains reducing rear leached mud;
(2) with leached mud after the reduction of step (1) gained, add concentration take liquid-solid ratio as 8:1 and be the sulphuric acid soln of 100g/L, under 55 ℃, again mixed solution is strengthened with Ultrasonic Radiation and leached 3h, the condition of Ultrasonic Radiation is: ultrasonic frequency is 22KHz, and every liter of ultrasonic power 80W that mixed solution distributes obtains leach liquor through solid-liquid separation, again leach liquor is carried out follow-up purification, reclaim metallic zinc through electrodeposition.The rate of recovery of zinc reaches 92%, and the iron leaching rate only has 36%.
Claims (3)
1. the method for zinc in a microwave-ultrasonic combined recovery high ferro, the high plumbous leached mud is characterized in that through following each step:
(1) get high ferro, high plumbous leached mud, add the carbon dust of its quality 1～7% again, mixing is by constant temperature behind microwave heating to 550～950 ℃ 1～3 hour, stopped heating then, and pass into N
2Protective atmosphere until temperature is down to below 100 ℃, obtains reducing rear leached mud;
(2) with leached mud after the reduction of step (1) gained, add concentration take liquid-solid ratio as 3～8:1 and be the acid solution of 70～170g/L, under 45～85 ℃, again mixed solution is strengthened with Ultrasonic Radiation and leached 1～3h, obtain leach liquor through solid-liquid separation, again leach liquor is carried out follow-up purification, reclaim metallic zinc through electrodeposition.
2. the method for zinc in microwave-ultrasonic combined recovery high ferro according to claim 1, the high plumbous leached mud, it is characterized in that: the acid solution of described step (2) is sulphuric acid soln.
3. the method for zinc in microwave-ultrasonic combined recovery high ferro according to claim 1 and 2, the high plumbous leached mud, it is characterized in that: the condition of the Ultrasonic Radiation of described step (2) is: ultrasonic frequency is 20～25KHz, every liter of ultrasonic power 40～160W that mixed solution distributes.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104131176A (en) * | 2014-08-01 | 2014-11-05 | 昆明理工大学 | Method for recovery of zinc by ultrasonic neutral leaching of zinc oxide flue dust |
| CN105349777A (en) * | 2015-10-19 | 2016-02-24 | 昆明理工大学 | Method for conducting microwave low temperature activation and ultrasonic coupling coupling leaching on oxygen vulcanization mixed ore |
| CN108070712A (en) * | 2017-12-15 | 2018-05-25 | 郴州市金贵银业股份有限公司 | The recovery method of valuable metal in a kind of silver electrolysis mother liquor purification slag |
| CN108754151A (en) * | 2018-06-23 | 2018-11-06 | 铜仁学院 | A kind of leaching method of manganese in electrolytic manganese residues |
| CN109735700A (en) * | 2019-03-13 | 2019-05-10 | 安徽工业大学 | A kind of method that microwave reducing roasting-sulfuric acid leaching recycles copper and zinc deposit in Bellamya aeruginosa |
| CN111485098A (en) * | 2020-04-15 | 2020-08-04 | 湘潭高新区风动机械有限公司 | Method for dezincification of converter mud by microwave reduction roasting |
| CN111961860A (en) * | 2020-08-21 | 2020-11-20 | 昆明理工大学 | Method for recovering lithium ion battery by ultrasonic-microwave assistance |
| CN113846233A (en) * | 2021-10-20 | 2021-12-28 | 辽宁石油化工大学 | Method for directly reducing and treating waste CRT glass by utilizing microwaves |
| CN115652100A (en) * | 2022-10-25 | 2023-01-31 | 昆明理工大学 | Method for efficiently and comprehensively treating reclaimed copper smelting fly ash |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104131176A (en) * | 2014-08-01 | 2014-11-05 | 昆明理工大学 | Method for recovery of zinc by ultrasonic neutral leaching of zinc oxide flue dust |
| CN104131176B (en) * | 2014-08-01 | 2016-09-21 | 昆明理工大学 | A kind of ultrasound wave neutrality leaches the method that zinc oxide fumes reclaims zinc |
| CN105349777A (en) * | 2015-10-19 | 2016-02-24 | 昆明理工大学 | Method for conducting microwave low temperature activation and ultrasonic coupling coupling leaching on oxygen vulcanization mixed ore |
| CN108070712A (en) * | 2017-12-15 | 2018-05-25 | 郴州市金贵银业股份有限公司 | The recovery method of valuable metal in a kind of silver electrolysis mother liquor purification slag |
| CN108070712B (en) * | 2017-12-15 | 2019-12-03 | 郴州市金贵银业股份有限公司 | A kind of silver is electrolysed the recovery method of valuable metal in mother liquor purification slag |
| CN108754151A (en) * | 2018-06-23 | 2018-11-06 | 铜仁学院 | A kind of leaching method of manganese in electrolytic manganese residues |
| CN109735700A (en) * | 2019-03-13 | 2019-05-10 | 安徽工业大学 | A kind of method that microwave reducing roasting-sulfuric acid leaching recycles copper and zinc deposit in Bellamya aeruginosa |
| CN111485098A (en) * | 2020-04-15 | 2020-08-04 | 湘潭高新区风动机械有限公司 | Method for dezincification of converter mud by microwave reduction roasting |
| CN111961860A (en) * | 2020-08-21 | 2020-11-20 | 昆明理工大学 | Method for recovering lithium ion battery by ultrasonic-microwave assistance |
| CN113846233A (en) * | 2021-10-20 | 2021-12-28 | 辽宁石油化工大学 | Method for directly reducing and treating waste CRT glass by utilizing microwaves |
| CN115652100A (en) * | 2022-10-25 | 2023-01-31 | 昆明理工大学 | Method for efficiently and comprehensively treating reclaimed copper smelting fly ash |
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