CN103352116B - The method of zinc in microwave-ultrasonic combined recovery high ferro, high plumbous leached mud - Google Patents
The method of zinc in microwave-ultrasonic combined recovery high ferro, high plumbous leached mud Download PDFInfo
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- CN103352116B CN103352116B CN201310117250.9A CN201310117250A CN103352116B CN 103352116 B CN103352116 B CN 103352116B CN 201310117250 A CN201310117250 A CN 201310117250A CN 103352116 B CN103352116 B CN 103352116B
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- zinc
- leached mud
- microwave
- ultrasonic
- plumbous
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- 239000011701 zinc Substances 0.000 title claims abstract description 38
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000011084 recovery Methods 0.000 title claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 239000011259 mixed solution Substances 0.000 claims abstract description 13
- 230000005855 radiation Effects 0.000 claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 11
- 239000000428 dust Substances 0.000 claims abstract description 8
- 238000004070 electrodeposition Methods 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 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
- 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
- 239000002253 acid Substances 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 4
- 238000000605 extraction Methods 0.000 abstract description 4
- 239000002893 slag Substances 0.000 abstract description 4
- 239000000243 solution Substances 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 150000002739 metals Chemical class 0.000 abstract description 2
- 238000002604 ultrasonography Methods 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 16
- 229910052742 iron Inorganic materials 0.000 description 8
- 238000002386 leaching Methods 0.000 description 8
- 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
- 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
- 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
- 239000002245 particle Substances 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 230000035484 reaction time Effects 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
- 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
- 238000005272 metallurgy Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction 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
- 238000009858 zinc metallurgy Methods 0.000 description 1
Classifications
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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
Abstract
The invention provides the method for zinc in a kind of microwave-ultrasonic combined recovery high ferro, high plumbous leached mud, belong to microwave and ultrasound applied technical field.Get high ferro, high plumbous leached mud, then add carbon dust, after mixing behind microwave heating to 550 ~ 950 DEG C constant temperature 1 ~ 3 hour, then stop heating, and pass into N
2protective atmosphere, until temperature is down to less than 100 DEG C, obtains reducing rear leached mud; Leached mud after reducing, adds acid solution, at 45 ~ 85 DEG C, then carries out Strengthen education to mixed solution with Ultrasonic Radiation, obtain leach liquor through solid-liquid separation, then carry out subsequent purification to leach liquor, through electrodeposition Footwall drift zinc.Compare conventional hot acid to leach, obviously shorten extraction time, reduce and leach acidity and extraction temperature, the zinc of 90 ~ 98% can be reclaimed.The valuable metals such as instant invention overcomes high plumbous, the difficult problem that under high ferro system, zinc recovery is low, flow process is simple, and treatment effect is good, energy high efficiente callback zinc, solve a large amount of castaway slag and store up the environmental pollution and problem of resource waste that cause.
Description
Technical field
The invention provides a kind of microwave calcining that utilizes and leach the method reclaiming zinc from high ferro, high plumbous leached mud in conjunction with intensified by ultrasonic wave, belong to microwave and ultrasound applied technical field.
Background technology
The purposes of zinc is very extensive, and occupy an important position in national economy, the fusing point of zinc is lower; fluidity of molten is good, has good corrosion resistance, is mainly used in zinc-plated industry; the protective layer of Chang Zuowei iron and steel, as zinc-plated sheet material pipe fitting etc., its consumption accounts for 50% of world's zinc consumption.China is the first in the world Chan Xin big country, and in the common ore deposit of domestic zinc, normal association has the iron of 8 ~ 15%.The conventional smelting technology of current zinc factory: roasting-leaching-electrodeposition, in roasting conventional process, the zinc oxidation of iron unavoidably and in calcining generates zinc ferrite.Because of the stable chemical nature of zinc ferrite, the acidleach in conventional wet lay metallurgy is difficult to dissolve zinc ferrite completely, and often need high temperature, high pressure leaching condition processes; And in zinc ore also common association have lead, in roasting and leach the lead sulfate generating in engineering and be insoluble in acid, 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 mud.
For solving the recovery problem of zinc in wet-leaching slag zinc ferrite, wet method main at present and thermal process have fuming process (201010286118.7), reducing roasting (201110096566.5), electric heating process (91107379.5), hot acid lixiviation process (201110286158.6), but it is perfect all not, it is larger generally to there is labour intensity in thermal process, zinc recovery is not high, energy consumption is large, the problems such as environmental pollution is serious, and need higher temperature and longer reaction times (201010611028.0) at regular heating process, and the sosoloid formed due to high temperature has higher hardness, certain difficulty is brought to later stage ore grinding, follow-up being difficult to adopts ordinary method recovery valuable metal wherein, a large amount of slag is caused to pile up, there is complex process in existing wet processing, equipment requirements is high, the problem such as input cost is higher.And peracid, hot conditions improves running cost, and makes a large amount of ferro elements enter solution, causes electric effusion processing load and technical load to increase, does not also have good treatment process to the existence of lead sulfate simultaneously.Therefore, zinc metallurgy industry is at present in the urgent need to a kind of processing method that can effectively solve the problem.
Summary of the invention
The present invention is directed to Problems existing and deficiency in existing production process, propose the processing method that a kind of microwave reducing roasting leaches in conjunction with intensified by ultrasonic wave, with Zn dust leached mud for raw material, first join carbon reducting roast through microwave, destroy the structure of zinc ferrite, reduce the condition needed for follow-up leaching, recycling ultrasonic cavitation produce mechanical effect, the lead sulfate of acidleach particle surface is peeled off, thus the rate of recovery of zinc is improved greatly, present method not only proposes microwave for the zinc ferrite existed in zinc metallurgical process and lead sulfate respectively and joins carbon reduction and intensified by ultrasonic wave extract technology, and reduce a large amount of leached mud and store up the problem of environmental pollution caused.
The present invention is realized by following technical proposal: a kind of method of zinc in microwave-ultrasonic combined recovery high ferro, high plumbous leached mud, through following each step:
(1) get high ferro, high plumbous leached mud, then add the carbon dust of its quality 1 ~ 7%, after mixing behind microwave heating to 550 ~ 950 DEG C constant temperature 1 ~ 3 hour, then stop heating, and pass into N
2protective atmosphere is oxidized to prevent Z 250, until temperature is down to less than 100 DEG C, obtains reducing rear leached mud;
(2) by leached mud after the reduction of step (1) gained, be the acid solution that 3 ~ 8:1 adds that concentration is 70 ~ 170g/L with liquid-solid ratio, at 45 ~ 85 DEG C, again with Ultrasonic Radiation, Strengthen education 1 ~ 3h is carried out to mixed solution, leach liquor is obtained through solid-liquid separation, again subsequent purification is carried out to leach liquor, through electrodeposition Footwall drift zinc.
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, ultrasonic power 40 ~ 160W that often liter of mixed solution distributes.
Advantage of the present invention:
(1) microwave has the feature of penetrance, selectivity heating, and on an metal oxide, the temperature of reaction needed for reduction, Reaction time shorten, saves the energy, reduce costs, have the very strong market competitiveness energy direct effect.
(2) because carbon is strong wave absorbtion material, material can be made to heat up evenly so evenly join carbon, avoid local sintering phenomenon.
(3) the Ultrasonic Radiation stage produces a large amount of heat, provides acidleach temperature condition, without the need to extra heating.
(4) compare conventional hot acid to leach, obviously shorten extraction time, reduce and leach acidity and extraction temperature, the zinc of 90 ~ 98% can be reclaimed.
(5) valuable metals such as instant invention overcomes high lead, the difficult problem that under high ferro system, zinc recovery is low, flow process is simple, and treatment effect is good, energy high efficiente callback zinc, solve a large amount of castaway slag and store up the environmental pollution and problem of resource waste that cause.
Accompanying drawing explanation
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
Below by embodiment, the present invention will be further described.
Embodiment 1
(1) get the boiler dirt high ferro of 250g Yunnan Metallurgical Factory, high plumbous leached mud, containing 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.Add the carbon dust of its quality 1% again, after mixing after microwave heating to 600 DEG C constant temperature 2 hours, then stop heating, and pass into N
2protective atmosphere is oxidized to prevent Z 250, until temperature is down to less than 100 DEG C, obtains reducing rear leached mud;
(2) by leached mud after the reduction of step (1) gained, with liquid-solid ratio (L/Kg) for 8:1 adds the sulphuric acid soln that concentration is 150g/L, at 75 DEG C, again with Ultrasonic Radiation, Strengthen education 3h is carried out to mixed solution, the condition of Ultrasonic Radiation is: ultrasonic frequency is 20KHz, the ultrasonic power 40W that often liter of mixed solution distributes, and obtains leach liquor through solid-liquid separation, again subsequent purification is carried out to leach liquor, through electrodeposition Footwall drift zinc.The rate of recovery of zinc reaches 92%, the leaching yield 32% of iron.
Embodiment 2
(1) get 250g high ferro, high plumbous leached mud, then add the carbon dust of its quality 5%, after mixing after microwave heating to 800 DEG C constant temperature 1 hour, then stop heating, and pass into N
2protective atmosphere is oxidized to prevent Z 250, until temperature is down to less than 100 DEG C, obtains reducing rear leached mud;
(2) by leached mud after the reduction of step (1) gained, take liquid-solid ratio as the sulphuric acid soln that 5:1 adds that concentration is 70g/L, at 85 DEG C, again with Ultrasonic Radiation, Strengthen education 2h is carried out to mixed solution, the condition of Ultrasonic Radiation is: ultrasonic frequency is 22KHz, the ultrasonic power 100W that often liter of mixed solution distributes, and obtains leach liquor through solid-liquid separation, again subsequent purification is carried out to leach liquor, through electrodeposition Footwall drift zinc.The rate of recovery of zinc reaches 95%, the leaching yield 39% of iron.
Embodiment 3
(1) get 250g high ferro, high plumbous leached mud, then add the carbon dust of its quality 7%, after mixing after microwave heating to 550 DEG C constant temperature 3 hours, then stop heating, and pass into N
2protective atmosphere is oxidized to prevent Z 250, until temperature is down to less than 100 DEG C, obtains reducing rear leached mud;
(2) by leached mud after the reduction of step (1) gained, take liquid-solid ratio as the sulphuric acid soln that 3:1 adds that concentration is 170g/L, at 45 DEG C, again with Ultrasonic Radiation, Strengthen education 1h is carried out to mixed solution, the condition of Ultrasonic Radiation is: ultrasonic frequency is 25KHz, the ultrasonic power 160W that often liter of mixed solution distributes, and obtains leach liquor through solid-liquid separation, again subsequent purification is carried out to leach liquor, through electrodeposition Footwall drift zinc.The rate of recovery of zinc reaches 97%, the leaching yield 40% of iron.
Embodiment 4
(1) get high ferro, high plumbous leached mud, then add the carbon dust of its quality 6%, after mixing after microwave heating to 950 DEG C constant temperature 3 hours, then stop heating, and pass into N
2protective atmosphere is oxidized to prevent Z 250, until temperature is down to less than 100 DEG C, obtains reducing rear leached mud;
(2) by leached mud after the reduction of step (1) gained, take liquid-solid ratio as the sulphuric acid soln that 8:1 adds that concentration is 100g/L, at 55 DEG C, again with Ultrasonic Radiation, Strengthen education 3h is carried out to mixed solution, the condition of Ultrasonic Radiation is: ultrasonic frequency is 22KHz, the ultrasonic power 80W that often liter of mixed solution distributes, and obtains leach liquor through solid-liquid separation, again subsequent purification is carried out to leach liquor, through electrodeposition Footwall drift zinc.The rate of recovery of zinc reaches 92%, and the leaching yield of iron only has 36%.
Claims (1)
1. the method for zinc in microwave-ultrasonic combined recovery high ferro, high plumbous leached mud, is characterized in that through following each step:
(1) get high ferro, high plumbous leached mud, then add the carbon dust of its quality 1 ~ 7%, after mixing behind microwave heating to 550 ~ 950 DEG C constant temperature 1 ~ 3 hour, then stop heating, and pass into N
2protective atmosphere, until temperature is down to less than 100 DEG C, obtains reducing rear leached mud;
(2) by leached mud after the reduction of step (1) gained, count 3 ~ 8:1 with liquid-solid ratio L/Kg and add the sulphuric acid soln that concentration is 70 ~ 170g/L, at 45 ~ 85 DEG C, again with Ultrasonic Radiation, Strengthen education 1 ~ 3h is carried out to mixed solution, obtain leach liquor through solid-liquid separation, then subsequent purification is carried out to leach liquor, through electrodeposition Footwall drift zinc, wherein ultrasonic frequency is 20 ~ 25KHz, ultrasonic power 40 ~ 160W that often liter of mixed solution distributes.
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| 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 |
| CN105349777B (en) * | 2015-10-19 | 2018-03-06 | 昆明理工大学 | A kind of method that microwave low-temperature activation ultrasonic wave-coupled leaches oxygen vulcanization composite ore |
| 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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| JP2004292901A (en) * | 2003-03-27 | 2004-10-21 | Dowa Mining Co Ltd | Leaching method for zinc concentrate |
| CN1710116A (en) * | 2005-06-09 | 2005-12-21 | 昆明理工大学 | Method for extracing zinc from waste zinc acetate |
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