CN104195339A - Method for separating copper from iron in sludge by virtue of hydrodynamic cavitation-assisted extraction - Google Patents

Method for separating copper from iron in sludge by virtue of hydrodynamic cavitation-assisted extraction Download PDF

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Publication number
CN104195339A
CN104195339A CN201410415972.7A CN201410415972A CN104195339A CN 104195339 A CN104195339 A CN 104195339A CN 201410415972 A CN201410415972 A CN 201410415972A CN 104195339 A CN104195339 A CN 104195339A
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Prior art keywords
iron
slurry
copper
leaching
sludge
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CN201410415972.7A
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Chinese (zh)
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谢逢春
伍琳瑛
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South China University of Technology SCUT
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South China University of Technology SCUT
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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Abstract

The invention provides a method for separating copper from iron in sludge and belongs to the technical field of environment friendliness. The method can be used for recycling the heavy metal sludge. The method comprises the following steps of firstly slurrying the sludge and oxidizing, and then adding an acid into the sludge, pre-extracting, and then carrying out cavitation treatment on the pre-extracted mixture by virtue of a hydrodynamic cavitation reactor, reinforcing the extraction process by virtue of the effect generated by the hydrodynamic cavitation to extract a majority of copper to enter a liquid phase and retain iron in a solid phase and then completing the separation process of iron in the solid phase from copper in the liquid phase by virtue of solid-liquid separation. The method disclosed by the invention has the characteristics of high energy conversion efficiency, good separation effect, less usage of acid and the like and is very suitable for the resource recycling of copper and iron in the heavy metal sludge.

Description

The method of copper iron in the auxiliary leaching of a kind of Hydrodynamic cavitation separated sludge
[technical field]
The method that the present invention relates to copper iron separation in a kind of mud, can be used for the recycling of heavy metal sewage sludge, belongs to environmental technology field.
[background technology]
Heavy metal sewage sludge is a kind of mud that some industrial enterprise's wastewater treatments produce, it is the trade waste that a kind of pollution is larger, its composition is the mixture of various heavy metal hydroxide precipitations or carbonate deposition, if it not carried out to recycling treatment, must cause environmental pollution and the wasting of resources.At present most domestic is engaged in technique that producer that heavy metal sewage sludge processes adopts and can be divided into two kinds of pyrogenic process and wet methods.A kind of front method causes larger secondary pollution, and resource utilization is not thorough.A kind of rear method is first mud to be dissolved completely with acid, and then employing ammonia soaks or the method for fractional precipitation or extraction is carried out separation, adopt this technique if obtain good resource utilization, innoxious effect, higher processing cost will be paid, and also easily produce secondary pollution, thereby its economic benefit and social benefit are restricted.Therefore be necessary to set up that a set of processing cost is low, treatment capacity is large, treatment process is simple, stop secondary pollution the recycling treatment process of heavy metal sewage sludge, and the core of the resource utilization of heavy metal sewage sludge, innoxious treatment technology is the separation of different metal component in mud, set up the separation method of different metal component in an advanced heavy metal sewage sludge, can greatly improve the recycling treatment of heavy metal sewage sludge, the effect of harmless treatment.
If sour leaching process reaches after thermodynamic(al)equilibrium (being reaction end), be to make the cupric ion dissolving of large (being that solubleness is larger) and the ferric iron of solubility product less (being that solubleness is less) is insoluble reaches separated object of solubility product by controlling suitable acid concentration (as pH value) theoretically.But this is difficult to realize in actual leaching operating process, on the one hand, because actual leaching process is difficult to reach thermodynamic(al)equilibrium (being reaction end) in finite time, the larger cupric ion of solubility product is owing to being wrapped in solid phase by other components, if do not have be difficult to dissolve completely superacid adding, simultaneously, in sour adition process, because the acid adding can not mix with whole reaction system instantaneous, thereby a little often form temporary transient high concentration region around in adding of acid, this temporary transient local overrich is also partly dissolved the ferric iron that solubility product is less, after mixing local overrich disappearance, the iron ion of these dissolvings is condensed into tiny crystal grains formation colloidal sol and is difficult for same liquid phase separation, like this, the sepn process of different metal is difficult to occur in actual leaching process.
[summary of the invention]
The object of the invention is to overcome the shortcoming of prior art, propose effectively to solve the separation problem of copper iron in above-mentioned heavy metal sewage sludge, provide that a kind of processing cost is low, treatment capacity is large, treatment process is simple, avoid the recycling treatment process of the heavy metal sewage sludge of secondary pollution.
The cavatition that Hydrodynamic cavitation produces can produce local high speed micro jet flow, this high speed micro jet flow can activate solid phase surface, solid phase particles is accelerated owing to having been abolished by ultrasonic wave to wrap up other components on its surface and fully contact with the leaching agent in liquid phase the speed that makes its dissolving enter liquid phase, the micelle of colloidal sol is same under Hydrodynamic cavitation effect to be wrapped up its surface and makes its stable Charge stripping and unstability and then acceleration coagulation, thereby whole leaching process can reach thermodynamic(al)equilibrium (being reaction end) faster, and the oxyhydroxide of different metal or the solubility product of carbonate are different, equilibrium concentration at the lower different metal ion of certain leaching agent concentration (pH value) in liquid phase is also different, the equilibrium concentration of the large metal ion of solubility product in liquid phase is large, thereby most of dissolving, the equilibrium concentration of the little metal ion of solubility product in liquid phase is little, thereby most of insoluble and remain in solid phase, like this, the different heavy metal components of solubility product has reached separated object with regard to beening separated in solid-liquid two-phase.For example, if control pH value, in 3 left and right, carry out acidleach, under Hydrodynamic cavitation effect, the copper overwhelming majority in mud is dissolved and is entered liquid phase, and most iron is retained in solid phase, and like this, these two kinds of components of copper and iron are just separated in leaching process.So not only can be issued at lower cost good separating effect, but also can reduce energy consumption, and realize the target of zero release.
Therefore present method can be divided into following steps:
1, mud slurrying: first solid waste is put into slurrying still and added water fully to stir and obtain the well-mixed slurry of solid-liquid.
2, slurry screening: the slurry mixing is screened by 600 order vibratory screening apparatuss.The coarse fodder sifting out is got back to the slurrying again of slurrying still.The slurry having screened adds a certain amount of oxygenant to be oxidized.
3, leaching in advance: the screened stock material that completes oxidation is divided into two portions, first part, in well-beaten situation, adds excessive acid, obtains high acidity slurry, and then in well-beaten situation, second section is added in the high acidity slurry of first part gradually and control suitable pH value.
4, cavitation leaching: under the condition arranging in best Hydrodynamic cavitation parameter, slurry is passed through to Hydrodynamic cavitation reactor repeatedly, the accumulation residence time of control slurry in cavitation reactor reaches after certain value, make slurry obtain the required cavitation process time, reinforced leaching effect, obtain higher leaching rate and separating effect, the most of leaching of copper is entered to liquid phase, and iron is retained in solid phase.
5, solid-liquid separation, makes iron in solid phase and the copper in liquid phase complete sepn process.
The present invention has following features with respect to prior art: the features such as effciency of energy transfer is high, good separating effect, sour consumption are few, are well suited for the copper in heavy metal sewage sludge and iron are carried out to resource utilization recovery.
[embodiment]
With following indefiniteness embodiment, further illustrate the specific embodiment of the present invention and effect:
Embodiment 1
The wastewater treatment mud copper content of certain circuit board plant is 3.5%, and iron-holder is 4.2%, and water content is 76.3%, and its separating copper iron process is as follows:
1. first mud added to slurrying still and add water to make its total water content reach 90%, fully stirring half an hour, then it is evacuated to 600 order vibratory screening apparatuss with underflow pump screens, the coarse fodder sifting out is got back to the slurrying again of slurrying still.The hydrogen peroxide that the slurry having screened adds 20ml/L again stirs half an hour.。
2. the fines filtering out is divided into two portions, first part is in well-beaten situation, add 20% sulfuric acid to leach in advance, leaching time is one hour, the pH value of controlling leaching terminal is 1.5, and then in well-beaten situation, second section is added in the high acidity slurry of first part gradually, the pH value of controlling after the amount adding completes whole leaching process is 2.9.
3, reaction mass is inputted to Hydrodynamic cavitation reactor repeatedly and carry out cavitation process, Hydrodynamic cavitation reactor adopts venturi arrangement, controlling inlet feed pressure is 0.90Mpa, top hole pressure is 0.15Mpa, the accumulated process time of slurry in cavitation reactor reaches one hour, the most of leaching of copper is entered to liquid phase, and iron is retained in solid phase.
4, solid-liquid separation, makes iron in solid phase and the copper in liquid phase complete sepn process.
According to above-mentioned steps, carry out the separation of copper iron, in solid phase, the rate of recovery of iron reaches 99.6, and in liquid phase, the rate of recovery of copper reaches 98.3%.
Embodiment 2
The wastewater treatment mud copper content of certain Electroplate Factory is 2.3%, and iron-holder is 3.2%, and water content is 82.3%, and its separating copper iron process is as follows:
1.1. first mud added to slurrying still and add water to make its total water content reach 90%, fully stirring half an hour, then it is evacuated to 600 order vibratory screening apparatuss with underflow pump screens, the coarse fodder sifting out is got back to the slurrying again of slurrying still.The hydrogen peroxide that the slurry having screened adds 15ml/L again stirs half an hour.
2. the fines filtering out is divided into two portions, first part is in well-beaten situation, add 31% hydrochloric acid to leach in advance, leaching time is one hour, the pH value of controlling leaching terminal is 1.5, and then in well-beaten situation, second section is added in the high acidity slurry of first part gradually, the pH value of controlling after the amount adding completes whole leaching process is 3.0.
3, reaction mass is inputted to Hydrodynamic cavitation reactor repeatedly and carry out cavitation process, Hydrodynamic cavitation reactor adopts liquid whistle device, controlling cavitation reactor inlet feed pressure is 0.85Mpa, top hole pressure is 0.15Mpa, the accumulated process time of reaction mass in cavitation reactor reaches one hour, the most of leaching of copper is entered to liquid phase, and iron is retained in solid phase.
4, solid-liquid separation, makes iron in solid phase and the copper in liquid phase complete sepn process.
According to above-mentioned steps, carry out the separation of copper iron, in solid phase, the rate of recovery of iron reaches 98.6, and in liquid phase, the rate of recovery of copper reaches 97.3%.
Embodiment 3
Certain metal product plant acid washing water lignin-sludge copper content is 5.2%, and iron-holder is 4.5%, and water content is 70.3%, and its separating copper iron process is as follows:
1. first mud added to slurrying still and add water to make its total water content reach 90%, fully stirring half an hour, then it is evacuated to 600 order vibratory screening apparatuss with underflow pump screens, the coarse fodder sifting out is got back to the slurrying again of slurrying still.The hydrogen peroxide that the slurry having screened adds 30ml/L again stirs half an hour.
2. the fines filtering out is divided into two portions, first part is in well-beaten situation, add 31% hydrochloric acid to leach in advance, leaching time is one hour, the pH value of controlling leaching terminal is 1.5, and then in well-beaten situation, second section is added in the high acidity slurry of first part gradually, the pH value of controlling after the amount adding completes whole leaching process is 2.8.
3, reaction mass is inputted to Hydrodynamic cavitation reactor repeatedly and carry out cavitation process, Hydrodynamic cavitation reactor adopts porous plate device, porous plate aperture 2.5mm, thickness of slab 10mm, the ratio 0.125 that hole area is long-pending with cavitation reactor cross-section of pipeline, cavitation reactor inlet feed pressure is 1.05Mpa, top hole pressure is 0.15Mpa, the accumulated process time of control slurry in cavitation reactor reaches 2 hours, the most of leaching of copper is entered to liquid phase, and iron is retained in solid phase.
4, solid-liquid separation, makes iron in solid phase and the copper in liquid phase complete sepn process.
According to above-mentioned steps, carry out the separation of copper iron, in solid phase, the rate of recovery of iron reaches 98.2, and in liquid phase, the rate of recovery of copper reaches 98.1%.
Above-described embodiment has only expressed the preferred embodiment of the present invention, can not be interpreted as the restriction to the scope of the claims of the present invention, so the present invention is not limited to this concrete technical process.Those skilled in the art, according to technical scheme of the present invention and design, can also make some distortion and improvement, and these all belong to protection scope of the present invention.So all other embodiments that draw according to the claims in the present invention scope, all should belong to the scope that the present invention is contained.

Claims (3)

1. Hydrodynamic cavitation is assisted a method for copper iron in leaching separated sludge, it is characterized in that comprising following steps:
(1), mud slurrying: first solid waste is put into slurrying still and added water fully to stir and obtain the well-mixed slurry of solid-liquid.
(2), slurry screening: the slurry mixing is screened by 600 order vibratory screening apparatuss.The coarse fodder sifting out is got back to the slurrying again of slurrying still, and the slurry having screened adds a certain amount of oxygenant to be oxidized.。
(3), leaching in advance: the screened stock material that completes oxidation is divided into two portions, first part is in well-beaten situation, add excessive acid, obtain high acidity slurry, and then in well-beaten situation, second section is added in the high acidity slurry of first part gradually, and control suitable pH value.
(4), cavitation leaching: under the condition arranging in best Hydrodynamic cavitation parameter, slurry is passed through to Hydrodynamic cavitation reactor repeatedly, the accumulation residence time of control slurry in cavitation reactor reaches after certain value, make slurry obtain the required cavitation process time, reinforced leaching effect, obtain higher leaching rate and separating effect, the most of leaching of copper is entered to liquid phase, and iron is retained in solid phase.
(5), solid-liquid separation, make iron in solid phase and the copper in liquid phase complete sepn process.
2. treatment process according to claim 1, is characterized in that: described Hydrodynamic cavitation reactor is a kind of in orifice plate, Venturi tube, the liquid whistle.
3. method according to claim 1, is characterized in that: described acid is the mixture of one or more compositions in sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid etc.
CN201410415972.7A 2014-08-21 2014-08-21 Method for separating copper from iron in sludge by virtue of hydrodynamic cavitation-assisted extraction Pending CN104195339A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106517708A (en) * 2016-12-15 2017-03-22 宁波宝力农环境技术开发有限公司 Ultrasonic reinforced acid dissolution electroplating sludge device

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101538651A (en) * 2009-04-22 2009-09-23 上海第二工业大学 Method for recycling metal
CN102534224A (en) * 2012-02-09 2012-07-04 华南理工大学 Method for separating heavy metal components from solid waste

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101538651A (en) * 2009-04-22 2009-09-23 上海第二工业大学 Method for recycling metal
CN102534224A (en) * 2012-02-09 2012-07-04 华南理工大学 Method for separating heavy metal components from solid waste

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106517708A (en) * 2016-12-15 2017-03-22 宁波宝力农环境技术开发有限公司 Ultrasonic reinforced acid dissolution electroplating sludge device

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Application publication date: 20141210