CN107619050A - A kind of new bio charcoal ferro-aluminum composite preparation method - Google Patents
A kind of new bio charcoal ferro-aluminum composite preparation method Download PDFInfo
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- CN107619050A CN107619050A CN201710737554.3A CN201710737554A CN107619050A CN 107619050 A CN107619050 A CN 107619050A CN 201710737554 A CN201710737554 A CN 201710737554A CN 107619050 A CN107619050 A CN 107619050A
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Abstract
The invention provides a kind of new bio charcoal ferro-aluminum composite preparation method, the preparation method prepares Sheng Wutan ferro-aluminum composites using controllable stacking coating unit, controllable stacking coating unit includes the homogeneous electroplating reaction bed of graphitiferous tooth bed, reproducibility group mother liquor hold tank and spray head, reaction bed conductivity sensor and controller, connecting tube and pump.The preparation method of new bio Tan ferro-aluminum composites is carried out in controllable stacking coating unit, is comprised the following steps：S1, prepare ferro-aluminum base mother liquor；S2, prepare carbon-based dispersion liquid；S3, prepare reproducibility group mother liquor；S4, mixed liquor is obtained after mixing ferro-aluminum base mother liquor and carbon-based dispersion liquid, mixed liquor is filtrated to get and carries ferro-aluminum high-area carbon；S5 to carry iron carbon carrier sprinkling reproducibility group mother liquor with obtain charcoal ferro-aluminum composite.The new bio charcoal the preparation method of ferro-aluminum composite there is the advantages of process control, non-secondary pollution.
Description
Technical field
The present invention relates to the preparation of heavy metal repair materials in black foul sewage mud, soil and waste residue, and in particular to a kind of new
Charcoal ferro-aluminum composite preparation method.
Background technology
At present, environment functional material has become a global environmentally friendly study hotspot.Due to its have it is unique
Physics, chemical property, excellent depollution of environment effect, play a significant role in three-protection design technique.
Metal carbides functional form material has good hydrothermal stability, hierarchical porous structure and relatively large due to it
Specific surface area receives the extensive concern of researcher.Ferro-aluminum provides as a kind of metal with good characteristic in the whole world
Today of source increasingly reduction, iron and aluminium can be found everywhere, but also it is special cheap.With traditional heavy metal improvement side
Method bottleneck highlights, selection research and development efficiently, stably, recyclable and recycling ferro-aluminum magnetic material seem particularly urgent.
Carbon material repairs field using more in heavy metal, main cause be its there is comprehensive modifiability, can magnetic field
The features such as recyclability, huge theoretical specific surface area, excellent mechanical performance, hot property, inherently preferable heavy metal are inhaled
Enclosure material.In addition, magnetic Nano ferro-aluminum carbon can also realize large-scale production by the technique such as being simply co-precipitated, it is a kind of pole
Have the Low Cost Sorbents of application prospect.However, due to strong π-π phase interactions be present between magnetic ferro-aluminum carbon nano-particles
With, it is easy to reunite, and specific surface area caused by accumulating again declines even ten times of several times compared to theoretical value, caused absorption is held
Amount declines, furthermore the property such as single group of Armco magnetic iron carbon material surface also limits it in heavy metal complex and oxygen-containing acid group
Application in waste water.In addition can the absorption property of magnetic ferro-aluminum carbon material also in the liquid phase dispersed by it, low
Valency iron is easily reduced in water, causes magnetic Nano ferro-aluminum carbon material certain defect in practical application to be also present.For above-mentioned
Shortcoming, generally to ferro-aluminum carbon material surface carry out functional modification, the surface modification functionalization group of ferro-aluminum carbon material it is main
Form is non-covalent bond, has electrostatic interaction, pi-pi accumulation, Van der Waals force, hydrophobic effect in ferro-aluminum carbon material surface, so in aluminium
Iron carbon material surface introduces a number of functional group, so can not only strengthen its water-soluble surface, electrochemistry polarity and suction
Attached site, improve the absorption property of its heavy metal；The core of the stable protection ferro-aluminum carbon material of above-mentioned covalent bond can also be passed through
Core structure, keep the excellent mechanical performance of ferro-aluminum carbon material and chemically.
Conventional method is that ferro-aluminum carbon material is placed in into immersion in group mother liquor to obtain being modified ferro-aluminum carbon material, modified ferro-aluminum carbon
Material surface has a number of group, but this method is difficult to determine its modification time；Meanwhile for modified ferro-aluminum carbon material
Preparation technology is more coarse, and the deposition of its carbon surface iron of the iron carbon material of preparation is uneven, and coprecipitation uses dispersant, meeting
Produce secondary pollution.
The content of the invention
To overcome above mentioned problem, the invention provides a kind of process control, non-secondary pollution new bio charcoal ferro-aluminum answer
The preparation method of condensation material.
To achieve the above object, the invention provides a kind of new bio charcoal ferro-aluminum composite preparation method, the system
Preparation Method using charcoal ferro-aluminum composite preparation facilities obtain charcoal ferro-aluminum composite, the charcoal ferro-aluminum
Composite preparation facilities includes having open-topped reactor, reproducibility group mother liquor hold tank and shower nozzle, the reaction
Kettle is connected with the reproducibility group mother liquor hold tank, and the reproducibility group mother liquor hold tank is connected with the shower nozzle；It is described
Pallet is provided with reactor, the pallet is provided with conductivity measuring instrument, and the preparation method comprises the following steps：
S1, ferro-aluminum source is dissolved in deionized water obtains iron-based mother liquor, it is stand-by；S2, carbon source is added in deionized water and hanged
Supernatant liquid, the suspension pH value is adjusted to 1-4, the suspension is carried out to obtain carbon-based dispersion liquid after ultrasonic wave is scattered, treated
With；It is 30min-60min to the suspension ultrasonic dispersing time；S3, dissolve reduce agent in deionized water and reduced
Property solution, the reducing solution pH value is adjusted to obtain reproducibility group mother liquor after 3-4, the reproducibility group mother liquor should
It should be configured in using preceding 20min；The reducing agent contains the one or more in carboxyl, hydroxyl and sulfydryl；S4, by the aluminium
Iron-based mother liquor obtains ferro-aluminum carbon mixed liquor after being mixed with the carbon-based dispersion liquid, and the ferro-aluminum carbon mixed liquor is filtrated to get
Carry ferro-aluminum carbon carrier；S5, the load ferro-aluminum carbon carrier is placed in the pallet, carried by the shower nozzle to the load ferro-aluminum carbon
Body sprays the reproducibility group mother liquor and detects the electrical conductivity for carrying ferro-aluminum carbon carrier using the conductivity measuring instrument, when
When the electrical conductivity for carrying ferro-aluminum carbon carrier reaches predetermined value, stop applying the reproducibility group mother liquor, and institute will be applied with
State the load ferro-aluminum carbon carrier drying of reproducibility group mother liquor with obtain the charcoal ferro-aluminum composite；The charcoal aluminium
Iron composite material is one kind of modified ferro-aluminum carbon material.
Preferably, the pallet is provided with the graphite rod for being used for being in contact with the load ferro-aluminum carbon carrier, the graphite rod connects
Power cathode is connect so that electronics can be provided to the load ferro-aluminum carbon carrier.The graphite rod provides electricity to the load ferro-aluminum carbon carrier
Son can make Zero-valent Iron uniform deposition on carbon.The graphite rod quantity is not limited to one.
Preferably, it is provided with oxidation-reduction potential monitor, the preparation method in the reproducibility group mother liquor hold tank
Including：In the step S5, the oxidation of the reproducibility group mother liquor is detected also using the oxidation-reduction potential monitor
Former current potential, when the oxidation-reduction potential of the reproducibility group mother liquor is higher than 65mV, added to the reproducibility group mother liquor
Sodium borohydride is so that the oxidation-reduction potential of the reproducibility group mother liquor is reduced to 65mV or below 65mV；The pallet overflows
The reproducibility group mother liquor flow into the reproducibility group mother liquor hold tank and recycle.The described of recycling is kept to go back
The oxidation-reduction potential of originality group mother liquor is that ensure that the reproducibility of the reproducibility group mother liquor, so can not only be maximum
The application reproducibility group mother liquor of limit, and the load ferro-aluminum carbon carrier can be made to be protected with the reproducibility group mother liquor
Hold certain reaction speed, be advantageous to zeroth order ferro-aluminum Quick uniform and be deposited on carbon, also can effectively control charcoal ferro-aluminum answer
Condensation material prepares duration；Sodium borohydride is strong reductant, can strengthen the reproducibility of the reproducibility group mother liquor.
Preferably, being provided with pH meter in the reproducibility group mother liquor hold tank, the preparation method includes：In the step
In S5, the pH value of the reproducibility group mother liquor is detected using the pH meter, when the reproducibility group mother liquor pH value is higher than 3-4
When, acid is added so that the reproducibility group mother liquor pH value is 3-4 to the reproducibility group mother liquor.The acid for dilute sulfuric acid or
One or more in dust technology.
Preferably, the reactor is internally provided with for filtering the reproducibility group mother liquor overflowed from the pallet
Filter, the filter is located at below the pallet and forms closing space with the base wall portion of the reactor, described
The preferred G4 sand core filters of filter.
Preferably, the predetermined value is 0.85 × 102μs/cm-0.95×102μs/cm。
Preferably, in the step S1, also comprise the following steps：Deionized water added with the ferro-aluminum source is carried out
Heating and stirring, and it be 413K-433K to control the temperature of the deionized water, control stir speed (S.S.) be 60 r/min-
A length of 30 min -60min when 120r/min, stirring, so that source of iron can be quickly dissolved in deionized water；In the step S4,
Stir speed (S.S.) when the ferro-aluminum base mother liquor is mixed with the carbon-based dispersion liquid is 60 r/min -120r/min, stirring
Shi Changwei 60min-90min, the ferro-aluminum base mother liquor can be caused to be sufficiently mixed with the carbon-based dispersion liquid beneficial to the load iron
The formation of carbon carrier.The iron carbon mixed liquor can be placed a period of time by stirring after terminating（60min-90min）, fill carbon carrier
Divide absorption ferrous ion, aluminium ion.
Preferably, the total concentration of ferro-aluminum is carbon in 150g/L-250 g/L, the carbon-based dispersion liquid in the iron-based mother liquor
Concentration for 100g/L-250 g/L, ferro-aluminum base mother liquor and the mass ratio with the carbon-based dispersion liquid in the ferro-aluminum carbon mixed liquor
For 2:1-5:1.
Preferably, in the step S3, the reducing agent contains sodium citrate, ascorbic acid, sodium sulfite and boron hydrogen
Change sodium, the sodium citrate, the ascorbic acid and the sodium sulfite mol ratio are 2.0-3.0:0.5-1.5:1.0-2.0
The mixture of the sodium citrate, the ascorbic acid and the sodium sulfite three is 1 with the mass ratio of the deionized water:
100-2:100, concentration of the sodium borohydride in the reproducibility group mother liquor is 3g/L-5g/L；The sodium citrate, institute
State ascorbic acid, the sodium sulfite is weak reductant, the sodium citrate, the ascorbic acid, the sodium sulfite with
The load iron carbon carrier reaction speed is slower, in order to accelerate its reaction speed, it is necessary to strengthen the reproducibility of reproducibility group mother liquor,
So containing a small amount of strong reductant sodium borohydride in reproducibility group mother liquor, a small amount of strong reductant will not destroy the citric acid
Sodium, the ascorbic acid and the sodium sulfite.
Preferably, the ferro-aluminum source be ferrous nitrate, ferrous sulfate heptahydrate, bodied ferric sulfate, potassium ferrate, aluminum sulfate,
One or more in aluminum nitrate, aluminium chloride, polyaluminium sulfate；The carbon source has microcosmic hexagonal structure unit, the carbon
Source is the one or more in charcoal, CNT, graphene, graphene oxide, lamellar graphite powder, and the carbon source is preferably raw
Thing charcoal, the charcoal enter after high temperature pyrolysis what is generated by bio-organic materials in the environment of anoxic or anoxybiotic.Charcoal
It is a kind of functional material with controllable conductance and property stabilization, charcoal atom is good for big π and the rule of the plane net of extension
The property regular three-dimensional structure of arrangement form.During material functional, introducing iron can be with the irregular arrangement of microcrystalline carbon interlayer
" random layer distorted-structure ", foreign atom（Such as nitrogen, oxygen）And surface amino groups, C=O are coordinated, metal active can be promoted
Center is uniformly distributed with molecular level in biological carbon surface, is advantageous to the formation of ferro-aluminum carbon catalysis structure.Charcoal is by rich
Rich unsaturated double strong, substantial amounts of surface groups, which form to be formed with the metal of variable valency, has d, positive the six of pi-conjugated coordination
Face body stacking mesh-like configuration, and charcoal also has stable doping electric conductivity, energy-storage property and adjustable oxidationreduction in itself
Performance, the oxidationreduction chain with Reversible Cycle can be formed with metal ion, be advantageous to metal and carried out between various valence states
Conversion.
It is currently preferred from microcosmic hexagonal structure unit carbon source, obtained charcoal ferro-aluminum composite wood
Material is in processing procedure is polluted, Fe2+Etching electronic transmission, Fe can be formed in waste water with carbon or carbon compound2+With carbon or carbonization
There is very high electrical potential difference so that hydroxyl radical free radical is produced at the microcosmic hexagonal margin of carbon or carbon compound and is surpassed between compound
Oxygen radical, hydroxyl radical free radical and superoxide radical can resolve into the organic matter in waste water harmless material.
New bio charcoal provided by the invention ferro-aluminum composite preparation method to carry iron carbon carrier carry out electrical conductivity enter
Row detection reacts whether reach terminal to judge to carry iron carbon carrier with reproducibility group mother liquor so that whole preparation process is easy to grasp
Control；Simultaneously the preparation method be not required to add dispersant, so new bio charcoal ferro-aluminum composite preparation method without secondary dirt
Dye.
Brief description of the drawings
Fig. 1 be new bio charcoal provided by the invention ferro-aluminum composite preparation method process chart；
Fig. 2 be charcoal provided by the invention ferro-aluminum composite preparation facilities；
Fig. 3 be charcoal made from embodiment 1 ferro-aluminum composite electron-microscope scanning figure.
Embodiment
The present invention is described in detail with reference to the accompanying drawings and examples.If it should be noted that do not conflicted, this hair
Each feature in bright embodiment and embodiment can be combined with each other, within protection scope of the present invention.
Embodiment 1
Reference picture 2, to charcoal ferro-aluminum composite preparation facilities be described in detail：
A kind of charcoal ferro-aluminum composite preparation facilities, including open-topped reactor 1, reproducibility group mother liquor storage
Tank 2 and shower nozzle 3, for reactor 1 by being connected with valvular pipeline with reproducibility group mother liquor hold tank 2, reproducibility group is female
Liquid holding vessel 2 is connected by the pipeline with circulating pump with shower nozzle 3, and pallet 4 is provided with reactor 1, and pallet 4 is surveyed provided with electrical conductivity
Determine instrument 5 and several graphite rods 6, graphite rod 6 is connected with power cathode, and oxidation is provided with reproducibility group mother liquor hold tank 2
Reduction potential monitor 7 and pH meter 8.The bottom of reactor 1 is provided with filter 9, filter 9 be located at the lower section of pallet 4 and with reactor 1
Base wall portion forms closing space, and the preferred G4 sand core filters of filter 9, filter is sand core filter, and the quantity of shower nozzle 3 is unlimited
In one, reactor 1 is preferably shaped to infundibulate.
Embodiment 2
With reference to Fig. 1, Fig. 2 to new bio charcoal provided by the invention the preparation method of ferro-aluminum composite be described in detail：
A kind of new bio charcoal the preparation method of ferro-aluminum composite comprise the following steps：
S1, certain ferrous nitrate, polyaluminium sulfate is taken to add deionized water, then to the deionized water added with ferrous nitrate
Heated and stirred, the temperature for controlling deionized water is 413K, control stir speed (S.S.) for 60 r/min, stirring when it is a length of
30min, it is 200g/L ferro-aluminum base mother liquors that stirring obtains alferric amount after terminating, stand-by；
S2, take a certain amount of charcoal to add in deionized water to obtain the suspension that charcoal concentration is 200 g/L, by suspension
PH value be adjusted to 3 or so, then to pH value be 3 or so suspension carry out ultrasonic wave disperse 30min after obtain carbon-based dispersion liquid,
It is stand-by；
S3, by mol ratio be 2.5:1:1.5 sodium citrate, ascorbic acid and sodium sulfite, which is added in deionized water, to be reduced
Property solution, solvent and Solute mass ratio are 1 in reducing solution:100；By the pH value of reducing solution be adjusted to 3 or so it is backward its
Add sodium borohydride and obtain reproducibility group mother liquor, it is stand-by；Wherein, sodium borohydride concentration is 4g/L in reproducibility group mother liquor；
Reproducibility group mother liquor need to charcoal ferro-aluminum composite prepare before prepare in 20min；
S4, by ferro-aluminum base mother liquor and carbon-based dispersion liquid with 3:1 mass ratio is mixed to get ferro-aluminum carbon mixed liquor, and ferro-aluminum carbon is mixed
Liquid is stirred, and it is 60 r/min to control stir speed (S.S.), a length of 60min when control is stirred, and stirring stands iron carbon after terminating
It is filtrated to get after mixed liquor 60min and carries ferro-aluminum carbon carrier；
S5, by carry ferro-aluminum carbon carrier be placed in pallet 4, pallet 4 is positioned in reactor 1, and reactor 1 is provided with filter 9, filter
The preferred G4 sand core filters of device 9, pallet 4 is interior to be provided with multiple graphite rods 6, and graphite rod 6 is connected with power cathode, carries ferro-aluminum carbon and carries
Body contacts with graphite rod 6；Then reproducibility group mother liquor is slowly sprayed to ferro-aluminum carbon carrier is carried by shower nozzle 5, during sprinkling
To the detection for carrying ferro-aluminum carbon carrier and carrying out electrical conductivity in pallet 4（Detected using conductivity measuring instrument 5）, the interior spilling of pallet 4
The reproducibility group mother liquor inflow bottom of reactor 1 filters to be collected into again by filter 9 to be stored equipped with reproducibility group mother liquor
Recycled in tank 2, now the reproducibility group mother liquor in reproducibility group mother liquor hold tank 2 carries out oxidation-reduction potential detection
（Oxidation reduction potential determination instrument 7 detects the oxidation-reduction potential of reproducibility group mother liquor）And pH value（PH meter 8 detects reproducibility base
Group's mother liquor pH value）Detection, when the oxidation-reduction potential of reproducibility group mother liquor is higher than 65mV, add to reproducibility group mother liquor
Add sodium borohydride so that oxidation-reduction potential is reduced to 65mV or below 65mV；While by detecting the pH of reproducibility group mother liquor
Value control（Add dust technology, the pH value of dilute sulfuric acid control reproducibility group mother liquor）Reproducibility group mother liquor pH is in the range of 3-4；
When the electrical conductivity for carrying ferro-aluminum carbon carrier reaches 0.91 × 102During more than μ s/cm, stop to load ferro-aluminum carbon carrier sprinkling reduction
Property group mother liquor, now load ferro-aluminum carbon carrier in pallet 4 is collected obtained after drying charcoal ferro-aluminum composite, obtain
Charcoal in ferro-aluminum composite the mass ratio of ferro-aluminum and carbon be 1:4, charcoal in ferro-aluminum composite carbon be loaded with two
Valency iron, Zero-valent Iron, zeroth order aluminium, sulfydryl, carboxyl and hydroxyl etc., zeroth order ferro-aluminum uniform deposition is on carbon.
Fig. 3 be embodiment 1 charcoal ferro-aluminum composite electron-microscope scanning figure.
Embodiment 3
With reference to Fig. 1, Fig. 2 to new bio charcoal provided by the invention the preparation method of ferro-aluminum composite be described in detail：
A kind of new bio charcoal the preparation method of ferro-aluminum composite comprise the following steps：
S1, take certain ferrous nitrate, aluminum sulfate add deionized water, then to added with ferrous nitrate, aluminum sulfate go from
Sub- water is heated and stirred, and the temperature for controlling deionized water is 433K, controls stir speed (S.S.) as 120 r/min, stirring duration
For 60min, it is 250g/L ferro-aluminum base mother liquors that stirring obtains iron-holder after terminating, stand-by；
S2, take a certain amount of graphene to add in deionized water to obtain the suspension that graphene concentration is 250 g/L, by suspension
PH value be adjusted to 3 or so, then to pH value be 3 or so suspension carry out ultrasonic wave disperse 60min after obtain carbon-based dispersion liquid,
It is stand-by；
S3, by mol ratio be 2.5:1:1.5 sodium citrate, ascorbic acid and sodium sulfite, which is added in deionized water, to be reduced
Property solution, solvent and Solute mass ratio are 1 in reducing solution:100；By the pH value of reducing solution be adjusted to 3 or so it is backward its
Add sodium borohydride and obtain reproducibility group mother liquor, it is stand-by；Wherein, sodium borohydride concentration is 4g/L in reproducibility group mother liquor；
Reproducibility group mother liquor need to charcoal ferro-aluminum composite prepare before 20min prepare；
S4, by ferro-aluminum base mother liquor and carbon-based dispersion liquid with 5:1 mass ratio is mixed to get ferro-aluminum carbon mixed liquor, and ferro-aluminum carbon is mixed
Liquid is stirred, and it is 120r/min to control stir speed (S.S.), and a length of 90min when control is stirred, stirring stands ferro-aluminum after terminating
It is filtrated to get after carbon mixed liquor 90min and carries ferro-aluminum carbon carrier；
S5, by carry ferro-aluminum carbon carrier be placed in pallet 4, pallet 4 is positioned in reactor 1, and reactor 1 is provided with filter 9, filter
The preferred G4 sand core filters of device 9, pallet 4 is interior to be provided with multiple graphite rods 6, and graphite rod 6 is connected with power cathode, carries ferro-aluminum carbon and carries
Body contacts with graphite rod 6；Then reproducibility group mother liquor is slowly sprayed to iron carbon carrier is carried by shower nozzle 5, it is right during sprinkling
The detection for carrying iron carbon carrier and carrying out electrical conductivity in pallet 4（Detected using conductivity measuring instrument 5）, the interior reduction overflowed of pallet 4
Property group mother liquor flow into the bottom of reactor 1 and filtered by filter 9 and be collected into again equipped with reproducibility group mother liquor hold tank 2
Recycle, now the reproducibility group mother liquor in reproducibility group mother liquor hold tank 2 carries out oxidation-reduction potential detection（Oxidation
Reduction potential analyzer 7 detects the oxidation-reduction potential of reproducibility group mother liquor）And pH value（It is female that pH meter 8 detects reproducibility group
Liquid pH value）Detection, when the oxidation-reduction potential of reproducibility group mother liquor is higher than 65mV, to reproducibility group mother liquor add boron
Sodium hydride causes oxidation-reduction potential to be reduced to 65mV or below 65mV；While by detecting the pH value control of reproducibility group mother liquor
System（Add dust technology, the pH value of dilute sulfuric acid control reproducibility group mother liquor）Reproducibility group mother liquor pH is in the range of 3-4；
When the electrical conductivity for carrying ferro-aluminum carbon carrier reaches 0.85 × 102During more than μ s/cm, stop to load ferro-aluminum carbon carrier sprinkling reduction
Property group mother liquor, now load ferro-aluminum carbon carrier in pallet 4 is collected obtained after drying charcoal ferro-aluminum composite, obtain
Charcoal in ferro-aluminum composite the mass ratio of iron and carbon be 1:3, charcoal in ferro-aluminum composite carbon be loaded with divalence
Iron, Zero-valent Iron, zeroth order aluminium, sulfydryl, carboxyl and hydroxyl etc., Zero-valent Iron, zeroth order aluminium uniform deposition are on carbon.
Embodiment 4
With reference to Fig. 1, Fig. 2 to new bio charcoal provided by the invention the preparation method of ferro-aluminum composite be described in detail：
A kind of new bio charcoal the preparation method of ferro-aluminum composite comprise the following steps：
S1, take certain ferrous nitrate, aluminum nitrate add deionized water, then to added with ferrous nitrate, aluminum nitrate go from
Sub- water is heated and stirred, and the temperature for controlling deionized water is 423K, control stir speed (S.S.) for 80 r/min, stirring when it is a length of
50min, stirring obtains the ferro-aluminum base mother liquor that alferric amount is 150g/L after terminating, stand-by；
S2, take a certain amount of CNT to add in deionized water to obtain the suspension that carbon nanotube concentration is 100 g/L, will be outstanding
The pH value of supernatant liquid is adjusted to 3 or so, and then the suspension that pH value is 3 or so is carried out to obtain carbon-based point after ultrasonic wave disperses 50min
Dispersion liquid, it is stand-by；
S3, by mol ratio be 2.5:1:1.5 sodium citrate, ascorbic acid and sodium sulfite, which is added in deionized water, to be reduced
Property solution, solvent and Solute mass ratio are 1 in reducing solution:100；By the pH value of reducing solution be adjusted to 3 or so it is backward its
Add sodium borohydride and obtain reproducibility group mother liquor, it is stand-by；Wherein, sodium borohydride concentration is 4g/L in reproducibility group mother liquor；
Reproducibility group mother liquor need to charcoal ferro-aluminum composite prepare before 20min prepare；
S4, by ferro-aluminum base mother liquor and carbon-based dispersion liquid with 2:1 mass ratio is mixed to get ferro-aluminum carbon mixed liquor, and ferro-aluminum carbon is mixed
Liquid is stirred, and it is 70 r/min to control stir speed (S.S.), and a length of 70min when control is stirred, stirring stands ferro-aluminum after terminating
It is filtrated to get after carbon mixed liquor 90min and carries ferro-aluminum carbon carrier；
S5, by carry ferro-aluminum carbon carrier be placed in pallet 4, pallet 4 is positioned in reactor 1, and reactor 1 is provided with filter 9, filter
The preferred G4 sand core filters of device 9, pallet 4 is interior to be provided with multiple graphite rods 6, and graphite rod 6 is connected with power cathode, carries ferro-aluminum carbon and carries
Body contacts with graphite rod 6；Then reproducibility group mother liquor is slowly sprayed to ferro-aluminum carbon carrier is carried by shower nozzle 5, during sprinkling
To the detection for carrying ferro-aluminum carbon carrier and carrying out electrical conductivity in pallet 4（Detected using conductivity measuring instrument 5）, the interior spilling of pallet 4
The reproducibility group mother liquor inflow bottom of reactor 1 filters to be collected into again by filter 9 to be stored equipped with reproducibility group mother liquor
Recycled in tank 2, now the reproducibility group mother liquor in reproducibility group mother liquor hold tank 2 carries out oxidation-reduction potential detection
（Oxidation reduction potential determination instrument 7 detects the oxidation-reduction potential of reproducibility group mother liquor）And pH value（PH meter 8 detects reproducibility base
Group's mother liquor pH value）Detection, when the oxidation-reduction potential of reproducibility group mother liquor is higher than 65mV, add to reproducibility group mother liquor
Add sodium borohydride so that oxidation-reduction potential is reduced to 65mV or below 65mV；While by detecting the pH of reproducibility group mother liquor
Value control（Add dust technology, the pH value of dilute sulfuric acid control reproducibility group mother liquor）Reproducibility group mother liquor pH is in the range of 3-4；
When the electrical conductivity for carrying ferro-aluminum carbon carrier reaches 0.95 × 102During more than μ s/cm, stop to load ferro-aluminum carbon carrier sprinkling reduction
Property group mother liquor, now load ferro-aluminum carbon carrier in pallet 4 is collected obtained after drying charcoal ferro-aluminum composite, obtain
Charcoal in ferro-aluminum composite the mass ratio of iron and carbon be 1:5, charcoal in ferro-aluminum composite carbon be loaded with divalence
Iron, Zero-valent Iron, zeroth order aluminium, sulfydryl, carboxyl and hydroxyl etc., Zero-valent Iron uniform deposition is on carbon.
New bio charcoal provided by the invention the preparation method of ferro-aluminum composite there is process control, non-secondary pollution
The advantages of.
Although having been described for the preferred embodiment of the embodiment of the present invention, those skilled in the art once know base
This creative concept, then other change and modification can be made to these embodiments.So appended claims are intended to be construed to
Including preferred embodiment and fall into having altered and changing for range of embodiment of the invention.
Claims (10)
1. a kind of preparation method of new bio Tan ferro-aluminum composites, it is characterised in that the preparation method uses controllable stacking
Coating unit obtains Sheng Wutan ferro-aluminum composites, and the controllable stacking coating unit includes homogeneous with graphitiferous tooth bed
Electroplating reaction bed, reproducibility group mother liquor hold tank and spray head, reaction bed conductivity sensor and controller, connecting tube and are followed
Ring pump, the electroplating reaction bed are connected with the reproducibility group mother liquor hold tank, the reproducibility group mother liquor hold tank with
The spray head connection；Pallet is provided with the reactor, the pallet is provided with conductivity measuring instrument, the preparation method bag
Include following steps：
S1, ferro-aluminum source is dissolved in deionized water obtains ferro-aluminum base mother liquor；
S2, suspension will be obtained in carbon source addition deionized water, the suspension pH value is adjusted to 1-4, to the suspension
Carry out obtaining charcoal base dispersion liquid after ultrasonic wave is scattered；
S3, the reducing agent containing group is dissolved in deionized water obtains reproducibility radical solution, by the reducing solution pH value
Reproducibility group mother liquor is obtained after being adjusted to 3-4（Configured before synthesis）；The reducing agent is rich in carboxyl, hydroxyl and sulfydryl；
S4, ferro-aluminum carbon mixed liquor is obtained after the ferro-aluminum base mother liquor is mixed with the carbon-based dispersion liquid, to the ferro-aluminum
Carbon mixed liquor, which is filtrated to get, carries ferro-aluminum carbon carrier；
S5, the load ferro-aluminum carbon carrier is placed in the pallet, institute is sprayed to the load ferro-aluminum carbon carrier by the shower nozzle
Reproducibility group mother liquor is stated and using the conductivity measuring instrument detection electrical conductivity for carrying ferro-aluminum carbon carrier, when the load aluminium
When the electrical conductivity of iron carbon carrier reaches predetermined value, stop applying the reproducibility group mother liquor, and the reproducibility will be applied with
The load ferro-aluminum carbon carrier of group mother liquor is dried, obtain the charcoal ferro-aluminum composite.
2. new bio charcoal according to claim 1 ferro-aluminum composite preparation method, it is characterised in that it is described
Phase electroplating reaction bed is provided with the graphite tooth plate for being used for mutually uniformly contacting with the load ferro-aluminum carbon carrier, the graphite truss plate connection electricity
Source negative electrode to the load ferro-aluminum carbon carrier can provide electronics.
3. new bio charcoal according to claim 1 ferro-aluminum composite preparation method, it is characterised in that it is described also
Oxidation-reduction potential monitor is provided with originality group mother liquor hold tank, the preparation method includes：In the step S5, make
The oxidation-reduction potential of the reproducibility group mother liquor is detected with the oxidation-reduction potential monitor, when the reproducibility group
When the oxidation-reduction potential of mother liquor is higher than 65mV, to the reproducibility group mother liquor add citric acid and sodium borohydride weak solution with
The oxidation-reduction potential of the reproducibility group mother liquor is set to be reduced to 65mV or below 65mV.
4. new bio charcoal according to claim 3 ferro-aluminum composite preparation method, it is characterised in that it is described also
PH meter is provided with originality group mother liquor hold tank, the preparation method includes：In the step S5, detected using the pH meter
The pH value of the reproducibility group mother liquor, when the reproducibility group mother liquor pH value is higher than 4, to the reproducibility group mother liquor
Diluted acid is added so that the reproducibility group mother liquor pH value is 3-4.
5. new bio charcoal according to claim 3 ferro-aluminum composite preparation method, it is characterised in that the stone
Bottom is provided with the filter for filtering the reproducibility group mother liquor overflowed from the pallet, the mistake below black fluted disc
Filter is used to filter reproducibility group mother liquor and be drained in group mother liquor hold tank.
6. new bio charcoal according to claim 1 ferro-aluminum composite preparation method, it is characterised in that it is described pre-
Definite value is the μ s/cm of 0.85 × 102 μ s/cm-0.95 × 102.
7. new bio charcoal according to claim 1 ferro-aluminum composite preparation method, it is characterised in that described
In step S1, also comprise the following steps：Deionized water added with the ferro-aluminum source is heated and stirred, and controls institute
The temperature for stating deionized water is 413K-433K, control stir speed (S.S.) for 60 r/min -120r/min, stirring when a length of 30min-
60min, so that source of iron is dissolved in deionized water；In the step S4, the ferro-aluminum base mother liquor and the carbon-based dispersion liquid are mixed
Close stirring when stir speed (S.S.) for 60 r/min -120r/min, stirring when a length of 60min-90min.
8. new bio charcoal according to claim 1 ferro-aluminum composite preparation method, it is characterised in that the aluminium
The total concentration of ferro-aluminum is 150g/L-250g/L in iron-based mother liquor, the concentration of carbon is 100g/L-250g/ in the carbon-based dispersion liquid
L, ferro-aluminum base mother liquor and the mass ratio with the carbon-based dispersion liquid are 2 in the ferro-aluminum carbon mixed liquor:1-5:1.
9. new bio charcoal according to claim 1 ferro-aluminum composite preparation method, it is characterised in that described
In step S3, the reducing agent contains sodium citrate, ascorbic acid, sodium sulfite and sodium borohydride, the sodium citrate, described
Ascorbic acid and the sodium sulfite mol ratio are 2.0-3.0:0.5-1.5:1.0-2.0, the sodium citrate, the Vitamin C
The mixture of sour and described sodium sulfite three is 1 with the mass ratio of the deionized water:100-2:100, the sodium borohydride
Concentration in the reproducibility group mother liquor is 3g/L-5g/L.
10. new bio charcoal according to any one of claim 1-9 ferro-aluminum composite preparation method, its feature
It is, the ferro-aluminum source is ferrous nitrate, ferrous sulfate heptahydrate, bodied ferric sulfate, potassium ferrate, aluminum sulfate, aluminum nitrate, chlorination
One or more in aluminium, polyaluminium sulfate；The carbon source has a microcosmic hexagonal structure unit, the carbon source be charcoal,
One or more in CNT, graphene, graphene oxide, lamellar graphite powder.
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| CN111807449A (en) * | 2020-07-17 | 2020-10-23 | 长沙理工大学 | Device and method for in-situ treatment of natural water pollution |
| CN114405471A (en) * | 2022-01-27 | 2022-04-29 | 东南大学 | Aluminum-iron bimetal modified biochar phosphorus removal material and preparation method thereof |
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| WO2013126477A1 (en) * | 2012-02-22 | 2013-08-29 | University Of Florida Research Foundation, Inc. | Biochar/metal composites, methods of making biochar/metal composites, and methods of removing contaminants from water |
| CN103623824A (en) * | 2012-08-23 | 2014-03-12 | 华东师范大学 | Magnetic iron-carbon composite material, preparation method and application thereof |
| US20160229709A1 (en) * | 2015-02-06 | 2016-08-11 | Biochar Now, Llc | Contaminant removal from water bodies with biochar |
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| WO2013126477A1 (en) * | 2012-02-22 | 2013-08-29 | University Of Florida Research Foundation, Inc. | Biochar/metal composites, methods of making biochar/metal composites, and methods of removing contaminants from water |
| CN103623824A (en) * | 2012-08-23 | 2014-03-12 | 华东师范大学 | Magnetic iron-carbon composite material, preparation method and application thereof |
| US20160229709A1 (en) * | 2015-02-06 | 2016-08-11 | Biochar Now, Llc | Contaminant removal from water bodies with biochar |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111807449A (en) * | 2020-07-17 | 2020-10-23 | 长沙理工大学 | Device and method for in-situ treatment of natural water pollution |
| CN114405471A (en) * | 2022-01-27 | 2022-04-29 | 东南大学 | Aluminum-iron bimetal modified biochar phosphorus removal material and preparation method thereof |
| CN114405471B (en) * | 2022-01-27 | 2023-12-22 | 东南大学 | Aluminum-iron bimetal modified biochar dephosphorizing material and preparation method thereof |
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