CN106698615A - Method and equipment for efficiently recycling magnetic nano-particles from wastewater - Google Patents
Method and equipment for efficiently recycling magnetic nano-particles from wastewater Download PDFInfo
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- CN106698615A CN106698615A CN201710043865.XA CN201710043865A CN106698615A CN 106698615 A CN106698615 A CN 106698615A CN 201710043865 A CN201710043865 A CN 201710043865A CN 106698615 A CN106698615 A CN 106698615A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/48—Treatment of water, waste water, or sewage with magnetic or electric fields
- C02F1/481—Treatment of water, waste water, or sewage with magnetic or electric fields using permanent magnets
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/24—Treatment of water, waste water, or sewage by flotation
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- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Water Treatment By Electricity Or Magnetism (AREA)
Abstract
The invention relates to a method and equipment for efficiently recycling magnetic nano-particles from wastewater. The equipment comprises a gas-floating column with a gas inlet and a magnet suspended above the gas-floating column and capable of moving up and down freely, wherein the gas-floating column is filled with a wastewater solution; the magnet is in proper contact with an aqueous solution, so that gas is introduced into the gas-floating column from the gas inlet; generated gas bubbles apply acting force to the magnetic nano-particles for adsorbing contaminant components in the wastewater solution in a floating process, so that the magnetic nano-particles move upwards, and the magnetic nano-particles loaded with contaminants are efficiently recycled under co-action of magnetic force and the acting force after entering a magnet trapping area. The method can be adopted to efficiently recycle weakly magnetic nano-particles in wastewater; and compared with a high-gradient magnetic separating method which is commonly adopted at present, the method has the characteristics of being simple and quick, low in cost and easy to amplify, and can effectively solve the recycling problem of the weakly magnetic nano-particles in a wastewater treatment process.
Description
Technical field
The present invention relates to the treatment of Pollutants in Wastewater, more particularly to one kind high efficiente callback magnetic nanoparticle from waste water
Method and apparatus.
Background technology
The various pollutants in water body how to be removed to protection water environment and current water environment severe contamination tool is solved the problems, such as
There is important meaning.In numerous minimizing technologies, superparamagnetic isolation technics has simple, quick advantage, has turned into recent years
One important study hotspot, so-called superparamagnetic isolation technics refers to target contaminant by the superparamagnetism adsorbent for customizing
Adsorption is produced, the technology of these adsorbents is then simply and rapidly reclaimed from solution by externally-applied magnetic field.Superparamagnetic
It with the superparamagnetic nano particle less than 30nm is functionalization base core that property adsorbent refers to（By coated or directly in its table
Face is modified）Adsorbent, the superparamagnetism adsorbent of nanometer particle size not only the high absorption property with nano adsorber again with can
By the premium properties of externally-applied magnetic field low cost, quick recovery from solution, and without remanent magnetism after adsorbent recovery, it is easy to divide again
Dissipate（The essential characteristic of superparamagnetism）, thus it is easy to recycling, for example：Wassana etc. uses super-paramagnetism nano adsorbent
The removal of Hg, Pb, Cd and Ti in waste water, as a result finds that the adsorbent shows to be significantly better than the suction high of conventional resins adsorbent
Attached performance and can realize in 1min quickly being reclaimed from solution by magnetic field；Du Bin etc. receives the superparamagnetism of graphene modified
Rice adsorbent is used for the removal of Cr (VI), Pb (II), Hg (II), Cd (II) and Ni (II) in the aqueous solution, as a result shows the absorption
Agent shows good removal capacity to five heavy metal species ions, can quickly be reclaimed by magnetic field and adsorbent is easy to follow in itself
Ring is utilized.
But after the target contaminant in magnetic nanoparticle Adsorption waste water, how efficiently to be returned from waste water solution
It is still a prominent problem to receive these weak magnetic nanoparticles.According to Magneto separate principle：The magnetic force acted on magnetic particle must
Fluid drag, extension and the gravity being applied to it need be more than.Magnetic field and magnetic field gradient expression formula are substituted into magnetic force formula
Magnetic force can be obtained（FM）And separating distance（r）Relational expression：FM = μ0χVpH▽H= -2μ0χVpK2Q2/r5, it is known that, for superparamagnetic
The magnetic force of property particle capture is a kind of short-range contingence, and five powers with separating distance are inversely proportional, and due to magnetic nanoparticle in itself
Magnetic is weak, and the separating distance that its effectively capture is capable of achieving under magnetic field is extremely limited, this severely limits recovery magnetic Nano
The scale and separative efficiency of grain.Although the high-gradient magnetic separation unit for generally using at present can be by improving magnetic field intensity, increasing
The density of addition polymerization magnetizing mediums is made up in the way of improving magnetic field gradient etc. and improving magnetic trapping power and is remarkably decreased because of distance increase
Magnetic force, but this effect is extremely limited and separator cost can be caused to dramatically increase.
The bubble adsorption separation technology for for particle rich in the aqueous solution separate that recent decades grow up, abbreviation air supporting
Isolation technics, it is the principle according to surface interaction force between bubble and particle, the glue in making solution as carrier using bubble
Body particle etc. adhere to or adsorb " solution-air " interface and with mother liquor quick separating so as to realize particle rich and at a distance capture
Method.It has that device is simple, be easy to amplify, can operate continuously, low power consumption and other advantages, in particles such as mineral, coal and plastics
FLOTATION SEPARATION aspect have a wide range of applications.
Early stage patent ZL201110289043.2 " a kind of gas helps superparamagnetism extracting process " is proposed in surfactant
Under booster action, using air flotation technology by the magnetic particle rich in weak solution to foam phase, from small part liquid after defoaming treatment
Magneto separate reclaims these magnetic particles in body, is separated with the scale for realizing the product such as biology, ion in weak solution, this coupling
Method shows good effect, and can solve the scale recovery problem of magnetic particle in weak solution really, but the method is still deposited
Need in two steps complete to cause the defects such as separative efficiency decline using surfactant, air supporting and Magneto separate.
Based on this, the present invention proposes directly to be total to the magnetic force of the surface reaction forces auxiliary magnetic field of supperparamagnetic particles in bubble
The same capture for being used for magnetic nanoparticle, to strengthen Magneto separate process significantly, i.e.,：Using bubble to the long distance of supperparamagnetic particles
Limitation of the magnetic force on separating distance is broken through from efficient capture effect, while greatly accelerating magnetic by this increased external force
The separative efficiency of grain.This new method is not based on highly enriched effect of the bubble to magnetic particle, but based on bubble to magnetic
The surface reaction forces of particle, thus surfactant generation foam phase need not be added, and air supporting is carried out simultaneously with Magneto separate process,
One step is completed.The method without by increasing magnetic field intensity or magnetic field gradient, only need to by simple aeration with it is common
Low field magnet combines and is capable of achieving to reclaim the high efficiency of weak magnetic nanoparticle in solution, and it is unrestricted to separate scale.This
The proposition of inventive method will greatly promote the extensive use of magnetic separation technique various pollutant processes in waste water, particularly scale
Change application, it is significant to the current increasingly serious water body environment pollution problem of protection.
The content of the invention
It is an object of the invention to provide a kind of method and apparatus of the high efficiente callback magnetic nanoparticle from waste water, fully
Gas magnetic assist isolation technics is make use of, the efficient of magnetic nanoparticle returns in can realizing waste water solution using the method for the present invention
Receive, solve the recovery problem of weak magnetic nanoparticle in wastewater treatment process.
The technical scheme is that：
A kind of method of the high efficiente callback magnetic nanoparticle from waste water, using gas magnetic assist separation equipment, the equipment includes bottom
Portion carries the air-flotation column of gas access and hangs on the magnet that can be freely moved up and down on air-flotation column, will contain and adsorb pollutant
The waste water solution of the magnetic nanoparticle of component is filled in air-flotation column, and magnet is contacted with waste water solution, and gas is entered from gas
Mouth is passed through in air-flotation column, and the gas being passed through carries out bubbling by entering in waste water solution after gas distributor, and the bubble of generation exists
Magnetic nanoparticle in floating-upward process to the absorption contaminant component applies active force, promotes its upward motion, into magnetic
Realize under the surface force collective effect that magnetic force and bubble apply it catching above-mentioned magnetic nanoparticle after iron capture zone
Collection, then takes out magnet, scrapes magnetic nanoparticle, realizes its removal process.
Further, the flow of the gas being passed through is controlled to 0 ~ 1000ml/min, and does not include 0（It is more than 0）.It is passed through
Gas flow need to be according to the gas distribution area of the size of air-flotation column and gas distributor depending on, the more big then gas flow of gas distribution area
It is bigger, the gas flow being passed through flow preferably higher.Described gas can be selected from not with water phase substance reaction it is any
Gas, under preferable case, described gas is selected from air or inert gas（Such as nitrogen, argon gas）In one or more.
Further, the groups of contaminants be selected from heavy metal ion, dyestuff, organic pollution and applied other
To the pollutant of environmental danger.
Further, the magnetic nanoparticle is selected from by base core of superparamagnetic nano particle and is repaiied by embedding or surface
The obtained nano particle of decorations, or the nano particle that by magnetic field can separate with other magnetic, particle diameter is 5 ~ 500nm.
The method of the present invention is preferably in the way of intermittent feeding, is first added appropriate magnetic nanoparticle pending
In waste water, be slowly injected into the mixed solution in air-flotation column up to after balancing by absorption pollutant, is then passed through from the bottom of air-flotation column
Gas carries out bubbling, and the magnetic nanoparticle applying of the bubble of generation to being adsorbed with contaminant component in floating-upward process is acted on
Power, promotes its upward motion, into magnet capture zone after it is real under the surface force collective effect that magnetic force and bubble apply to it
Now to the trapping of these magnetic nanoparticles, magnet is finally taken out, scrape magnetic nanoparticle, realize that it is reclaimed.
A kind of gas magnetic assist separation equipment for above-mentioned method, including air-flotation column and the side of being suspended over magnet, institute
The magnet stated can be moved up and down, and described air supporting column bottom is provided with gas access.
Further, also including gas distributor, the gas distributor is arranged at the top of gas access in air-flotation column.
Further, the magnet is selected from the permanent magnet or electromagnet of various different sizes, and freely can adjust up and down, from
The angle of energy-conservation, preferably permanent magnet；For the ease of freely upper and lower quick regulation magnet, a small-sized regulation up and down also can be set
Device, upper and lower adjuster is connected with magnet.
Further, described gas distributor is selected from the sand core funnel of different model or the micropore of suitable air supporting post shapes
The sand core funnel of gas distributing pipeline, such as model G1, G2 commonly used in the art, G3, G4 and G5 series；Or various sizes micropore
The gas pipe that footpath pipeline is made, can preferably produce the small-bore pipeline of micro-bubble.
Further, the gas magnetic assist separation equipment can also include auxiliary equipment, such as spinner flowmeter, surge tank and
Gas cylinder；Wherein, described gas cylinder is connected by pipeline with the air inlet of described surge tank, and decompression can be also installed on the pipeline
Valve, the gas vent of surge tank is connected by pipeline with the gas access of air supporting column bottom, to providing gas in air-flotation column；Institute
The spinner flowmeter stated is installed on the pipeline that the gas vent of surge tank is connected with the gas access of air supporting column bottom, while
Control valve further can be installed on the pipeline, it is possible to which gas flow is controlled by spinner flowmeter.Additionally, bubble is big
It is small to realize control by adjusting the pore size and gas flow of gas distributor, it is easily manufactured.
Detailed process is as follows：
Gas in gas cylinder is being passed through by showing its flow by spinner flowmeter after the gentle velocity modulation section Valve controlling of pressure-reducing valve
Many micro-bubbles are broken up into during the gas distributor of air supporting column bottom, these rising bubbles can need to neighbouring absorption
Except the magnetic nanoparticle of target contaminant applies surface reaction forces, acted on by one or many and promote it to move up to
The capture zone of square magnet, finally traps magnetic under the surface reaction forces collective effect of magnetic force and bubble by magnetic nanoparticle
On iron.
For different pollution objects systems to be removed and different types of magnetic nanoparticle, can be by adjusting external process
Parameter is such as：Gas flow rate, Air Bubble Size, pH value, ionic strength etc. provide greater number and smaller bubble or enable bubble right
Magnetic nanoparticle applies bigger surface reaction forces, so as to reach faster recovery rate and more thoroughly recovery.
The beneficial effects of the present invention are：
Bubble is introduced Magneto separate process to the surface reaction forces of particle by the present invention, and this surface reaction forces are strong, cheap and energy is real
Now the magnetic nanoparticle to weak magnetic is efficiently trapped, and trap time is short, can just be completed within short tens seconds, and separative efficiency is high,
And the rate of recovery is very high, 96.8% even more high can be up to, limitation of the magnetic force on engagement range be overcome well and need to be led to
Crossing increases magnetic field intensity or this high cost mode of gradient and could obtain the defect of active force high, produced by this coupling process
New gas magnetic assist separation equipment, compares with existing high gradient magnetic separating apparatus, with low cost, efficiently, be easy to be carried out continuously,
It is easy to the advantages such as amplification, especially the trapping aspect of weak magnetic nanoparticle has broad application prospects in aqueous.
Brief description of the drawings
Fig. 1 is the structural representation for including the gas magnetic assist separation equipment of the invention of auxiliary equipment, wherein, 1. gas cylinder, 2.
Pressure-reducing valve, 3. surge tank, 4. spinner flowmeter, 5. gas distributor, 6. magnetic nanoparticle, 7. bubble, 8. on lower
Device is saved, 9. air-flotation column.
Specific embodiment
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art are it will be clearly understood that the implementation
Example is used only for help and understands the present invention, is not construed as to concrete restriction of the invention.
Embodiment 1
Referring to Fig. 1, gas magnetic assist separation equipment of the present invention, including air-flotation column 9 of the bottom with gas access（In air-flotation column
Footpath is 16mm, and overall length is 500mm）, the top of described air-flotation column 9 is provided with ferromagnetic permanent magnet, magnet can be by upper
Lower adjuster 8 is freely adjusted up and down；The air-flotation column is filled with the waste water solution containing magnetic nanoparticle, the bottom of air-flotation column 9
Gas distributor 5 uses the aperture of model G4 specifications commonly used in the art for 4~7 microns of sand core funnel.
The gas outlet of gas cylinder 1 is connected by pressure-reducing valve 2, pipeline with the air inlet of surge tank 3, and the gas of surge tank 3 goes out
Mouth is connected by pipeline with the gas access of the described bottom of air-flotation column 9, by the gas distributor 5 to air-flotation column
Gas is provided in 9；Rotor is installed on the pipeline that the gas vent of described surge tank 3 is connected with described air-flotation column 9
Flowmeter 4.
Magnetic nanoparticle is reclaimed from waste water using above-mentioned gas magnetic assist separation equipment：
To having adsorbed Cu2+Magnetic nanoparticle reclaimed from waste water solution, the magnetic nanoparticle is chosen and uses PEG
The superparamagnetism Fe of modification3O4Nano particle, average grain diameter is 10nm, and the waste water chooses heavy metal Cu containing 30mg/L2+It is useless
Water.
Concrete operations mode is：In the case of intermittently operated, the magnetic nanoparticle that 100mg PEG are modified is added to
Heavy metal Cu containing 30mg/L2+200mL waste water solutions in, be stirred continuously it is lower absorption 0.5 hour, then by solution pass through air supporting
Column top is slowly injected in air-flotation column 9；Gas cylinder is opened, the flow velocity of spinner flowmeter is adjusted, under the gas velocity of 50ml/min, by nitrogen
Gas is from the continuous air-blowing into air-flotation column in the gas access of air supporting column bottom, and the nitrogen being passed through is substantial amounts of by being produced after sand core funnel
Micro-bubble, these rising bubbles can be adsorbed with Cu to neighbouring2+PEG modification magnetic nanoparticle apply surface action
Power, the capture zone for promoting it to move up to upper magnets, by magnetic under the surface reaction forces collective effect of magnetic force and bubble
Property nano particle is trapped on magnet.In removal process, solution colour change is paid close attention to, when solution becomes transparent immediately
Stop air-blowing and record duration of ventilation, then take the concentration of remanent magnetization nano particle in supernatant measurement solution, calculate magnetic
The rate of recovery and the rate of departure of magnetic nanoparticle of property nano particle.
Result shows：Recovery to magnetic nanoparticle in the above-mentioned waste water solution of 200ml, required time is only 40 seconds,
Its rate of departure is up to 300ml/min, and its rate of recovery is：95.2%.
Embodiment 2
The recovery of magnetic nanoparticle in waste water, difference therein are carried out using the gas magnetic assist separation equipment and technique of embodiment 1
Part is：Pending waste water is changed to waste water from dyestuff by heavy metal wastewater thereby, and superparamagnetic nano particle is：The Fe of polypyrrole modifying3O4
Particle, average grain diameter is 25nm.
Concrete operations mode is：In the case of intermittently operated, the magnetic nanoparticle of 200mg polypyrrole modifyings is added
Enter in the 400mL waste water solutions containing 10mg/L congo reds, be stirred continuously lower absorption 1 hour, then pass through solution
Air-flotation column top is slowly in injection air-flotation column 9；Gas cylinder is opened, the flow velocity of spinner flowmeter is adjusted, in the gas velocity of 100ml/min
Under, by nitrogen from the continuous air-blowing into air-flotation column in the gas access of air supporting column bottom, the nitrogen being passed through after sand core funnel by producing
The substantial amounts of micro-bubble of life, these rising bubbles can be to the neighbouring magnetic nanoparticle for being adsorbed with Congo red polypyrrole modifying
Apply surface reaction forces, the capture zone for promoting it to move up to upper magnets is total in the surface reaction forces of magnetic force and bubble
Magnetic nanoparticle is trapped on magnet under same-action.In removal process, solution colour change is paid close attention to, treat that solution becomes
It is transparent when stop air-blowing immediately and record duration of ventilation, then take remanent magnetization nano particle in supernatant measurement solution
Concentration, calculates the rate of recovery of magnetic nanoparticle and the rate of departure of magnetic nanoparticle.
Result shows：Recovery to magnetic nanoparticle in the above-mentioned waste water solution of 400ml, required time is only 1min,
Its rate of departure is up to 400ml/min, and its rate of recovery is：96.8%.
Applicant states that the present invention illustrates detailed process equipment of the invention and technological process by above-described embodiment,
But the invention is not limited in above-mentioned detailed process equipment and technological process, that is, do not mean that the present invention has to rely on above-mentioned detailed
Process equipment and technological process could be implemented.Person of ordinary skill in the field it will be clearly understood that any improvement in the present invention,
Addition, the selection of concrete mode to the equivalence replacement and auxiliary element of each raw material of product of the present invention etc., all fall within of the invention
Within protection domain.
Claims (10)
1. a kind of method of the high efficiente callback magnetic nanoparticle from waste water, it is characterised in that use gas magnetic assist separation equipment, institute
State air-flotation column of the equipment including bottom with gas access and hang on the magnet that can be freely moved up and down on air-flotation column, will contain
The waste water solution for having adsorbed the magnetic nanoparticle of contaminant component is filled in air-flotation column, and magnet is contacted with waste water solution, will
Gas is passed through in air-flotation column from gas access, and the gas being passed through carries out bubbling by entering in waste water solution after gas distributor,
Magnetic nanoparticle of the bubble of generation to adsorbing contaminant component in floating-upward process applies active force, promotes its upward fortune
It is dynamic, into magnet capture zone after realized to above-mentioned magnetic Nano under the surface force collective effect that magnetic force and bubble apply to it
The trapping of particle, then takes out magnet, scrapes magnetic nanoparticle, realizes that it is reclaimed.
2. method according to claim 1, it is characterised in that the groups of contaminants be selected from heavy metal ion, dyestuff and
One or more in organic pollution.
3. method according to claim 1, it is characterised in that the magnetic nanoparticle is selected from super-paramagnetism nano
The nano particle that grain is obtained by base core by embedding or surface modification, or the nanometer by magnetic field separate with other magnetic properties
Particle, particle diameter is 5nm-500nm.
4. method according to claim 1, it is characterised in that the flow of the gas being passed through is controlled to 0 ~ 1000ml/min,
And do not include 0；Described gas is selected from air or inert gas.
5. the gas magnetic assist separation equipment of a kind of method for described in any one of Claims 1-4, it is characterised in that including gas
Floating post and the magnet of the side of being suspended over, described magnet can be moved up and down, and described air supporting column bottom is provided with gas access.
6. equipment according to claim 5, it is characterised in that also including gas distributor, the gas distributor is set
In the top of gas access in air-flotation column.
7. equipment according to claim 5, it is characterised in that the magnet is selected from the permanent magnet or electricity of various different sizes
Magnet.
8. equipment according to claim 5, it is characterised in that also including upper and lower adjuster, upper and lower adjuster and magnet phase
Even.
9. equipment according to claim 5, it is characterised in that the core that described gas distributor is selected from different model leaks
The micropore gas distributing pipeline of bucket or suitable air supporting post shapes.
10. equipment according to claim 5, it is characterised in that also the spinner flowmeter including auxiliary equipment, surge tank and
Gas cylinder；Described gas cylinder is connected by pipeline with the air inlet of described surge tank, and the gas vent of surge tank passes through pipeline
Gas access with air supporting column bottom is connected；Described spinner flowmeter is installed on gas vent and the air-flotation column bottom of surge tank
On the pipeline that the gas access in portion is connected.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710043865.XA CN106698615A (en) | 2017-01-21 | 2017-01-21 | Method and equipment for efficiently recycling magnetic nano-particles from wastewater |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710043865.XA CN106698615A (en) | 2017-01-21 | 2017-01-21 | Method and equipment for efficiently recycling magnetic nano-particles from wastewater |
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| CN106698615A true CN106698615A (en) | 2017-05-24 |
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| CN201710043865.XA Pending CN106698615A (en) | 2017-01-21 | 2017-01-21 | Method and equipment for efficiently recycling magnetic nano-particles from wastewater |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108245930A (en) * | 2018-02-10 | 2018-07-06 | 湘潭大学 | A kind of gas helps adsorption separating method and device |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102500460A (en) * | 2011-09-26 | 2012-06-20 | 中国科学院过程工程研究所 | Air-assist superparamagnetic extraction method |
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2017
- 2017-01-21 CN CN201710043865.XA patent/CN106698615A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102500460A (en) * | 2011-09-26 | 2012-06-20 | 中国科学院过程工程研究所 | Air-assist superparamagnetic extraction method |
Non-Patent Citations (1)
| Title |
|---|
| TINGTING DONG ET AL: ""Removal of cadmium(II) from wastewater with gas-assisted magnetic separation"", 《CHEMICAL ENGINEERING JOURNAL》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108245930A (en) * | 2018-02-10 | 2018-07-06 | 湘潭大学 | A kind of gas helps adsorption separating method and device |
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