CN107619050B - A kind of charcoal ferro-aluminum composite material preparation method - Google Patents
A kind of charcoal ferro-aluminum composite material preparation method Download PDFInfo
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- CN107619050B CN107619050B CN201710737554.3A CN201710737554A CN107619050B CN 107619050 B CN107619050 B CN 107619050B CN 201710737554 A CN201710737554 A CN 201710737554A CN 107619050 B CN107619050 B CN 107619050B
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Abstract
The present invention provides a kind of charcoal ferro-aluminum composite material preparation method, the preparation method prepares Sheng Wutan ferro-aluminum composite material 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 Sheng Wutan ferro-aluminum composite material carries out in controllably stacking coating unit, comprising the following steps: S1, prepares ferro-aluminum base mother liquor；S2, carbon-based dispersion liquid is prepared；S3, preparation reproducibility group mother liquor；S4, mixed liquor is obtained after ferro-aluminum base mother liquor and carbon-based dispersion liquid are mixed, mixed liquor is obtained by filtration and carries ferro-aluminum high-area carbon；S5 Xiang Zaitie carbon carrier sprays reproducibility group mother liquor to obtain Sheng Wutan ferro-aluminum composite material.The preparation method of Sheng Wutan ferro-aluminum composite material has the advantages that process control, without secondary pollution.
Description
Technical field
The present invention relates to the preparations of heavy metal repair materials in black foul sewage mud, soil and waste residue, and in particular to a kind of biology
Charcoal ferro-aluminum composite material preparation method.
Background technique
Currently, environment functional material has become a global environmentally friendly research 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 is since it is with good hydrothermal stability, hierarchical porous structure and relatively large
Specific surface area receives the extensive concern of researcher.Ferro-aluminum is provided as a kind of metal with good characteristic in the whole world
Iron and aluminium can be found everywhere today of source increasingly reduction, but also special cheap.With traditional heavy metal improvement side
Method bottleneck highlights, and selection research and development are efficient, stablize, recyclable and recycling ferro-aluminum magnetic material seems especially urgent.
Carbon material repairs field using more in heavy metal, main cause be it with comprehensive modifiability, can magnetic field
The features such as recyclability, huge theoretical specific surface area, excellent mechanical performance, hot property, inherently ideal heavy metal are inhaled
Enclosure material.In addition, magnetic Nano ferro-aluminum carbon can also realize large-scale production by the techniques such as being simply co-precipitated, it is a kind of pole
Have the Low Cost Sorbents of application prospect.However, since there are strong π-π phase interactions between magnetic ferro-aluminum carbon nano-particles
With, it is easy to reunite, and specific surface area caused by accumulating again is compared to even ten times of theoretical value decline several times, caused absorption appearance
Amount decline, furthermore the properties such as single group of Armco magnetic iron carbon material surface also limit it in heavy metal complex and oxygen-containing acid group
Application in waste water.In addition to this can the absorption property of magnetic ferro-aluminum carbon material also in the liquid phase evenly dispersed by it, low
Valence iron is easily reduced in water, and causing magnetic Nano ferro-aluminum carbon material, there is also certain defects in practical application.
For disadvantages mentioned above, functional modification, the surface modification of ferro-aluminum carbon material usually are carried out to ferro-aluminum carbon material surface
The principal mode of functionalization group is non-covalent bond, has electrostatic interaction, pi-pi accumulation, Van der Waals force, hydrophobic effect in ferro-aluminum carbon materials
Expect surface, so introduce a certain number of functional groups in ferro-aluminum carbon material surface, not only can enhance its surface it is water-soluble,
Electrochemistry polarity and adsorption site improve its absorption property to heavy metal；Protection that can also be stable by above-mentioned covalent bond
The nuclear structure of ferro-aluminum carbon material keeps the excellent mechanical performance of ferro-aluminum carbon material and chemically.
Conventional method is to be placed in ferro-aluminum carbon material in group mother liquor to impregnate to obtain modified ferro-aluminum carbon material, modified ferro-aluminum carbon
Material surface has a certain number of groups, but this method is difficult to determine its modification time；Meanwhile for modified ferro-aluminum carbon material
Preparation process is more coarse, and the deposition of its carbon surface iron of the iron carbon material of preparation is uneven, and coprecipitation uses dispersing agent, meeting
Generate secondary pollution.
Summary of the invention
In order to overcome the problems referred above, the present invention provides a kind of process control, charcoal without secondary pollution ferro-aluminum composite wood
The preparation method of material.
To achieve the above object, the present invention provides a kind of charcoal ferro-aluminum composite material preparation method, the preparation side
Method using charcoal ferro-aluminum composite material preparation facilities obtain charcoal ferro-aluminum composite material, the charcoal ferro-aluminum it is compound
Material preparation facilities include have open-topped reaction kettle, reproducibility group mother liquor hold tank and spray head, the reaction kettle with
The reproducibility group mother liquor hold tank connection, the reproducibility group mother liquor hold tank are connect with the spray head；The reaction
Pallet is equipped in kettle, the pallet is equipped with conductivity measuring instrument, and the preparation method comprises the following steps:
S1, it ferro-aluminum source is dissolved in deionized water obtains iron-based mother liquor, for use；S2, it will be obtained in carbon source addition deionized water
To suspension, the suspension pH value is adjusted to 1-4, obtains carbon-based dispersion after carrying out ultrasonic wave dispersion to the suspension
Liquid, for use；It is 30min-60min to the suspension ultrasonic dispersing time；S3, it dissolves reduce agent in deionized water and obtains
The reducing solution pH value is adjusted to obtain reproducibility group mother liquor after 3-4 by reducing solution, and the reproducibility group is female
Liquid should be configured in using preceding 20min；The reducing agent contains one of carboxyl, hydroxyl and sulfydryl or a variety of；S4, by institute
Ferro-aluminum carbon mixed liquor is obtained after stating ferro-aluminum base mother liquor and the carbon-based dispersion liquid mixing, the ferro-aluminum carbon mixed liquor is filtered
It obtains carrying ferro-aluminum carbon carrier；S5, the load ferro-aluminum carbon carrier is placed in the pallet, by the spray head to the load ferro-aluminum
Carbon carrier sprays the reproducibility group mother liquor and detects the conductance for carrying ferro-aluminum carbon carrier using the conductivity measuring instrument
Rate stops applying the reproducibility group mother liquor, and will apply when the conductivity for carrying ferro-aluminum carbon carrier reaches predetermined value
The load ferro-aluminum carbon carrier of the reproducibility group mother liquor it is dry with obtain the charcoal ferro-aluminum composite material；The biology
Tan ferro-aluminum composite material is one kind of modified ferro-aluminum carbon material.
Preferably, the pallet is equipped with the graphite rod 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, being equipped with oxidation-reduction potential monitor, the preparation method in the reproducibility group mother liquor hold tank
It include: to detect the oxidation of the reproducibility group mother liquor also using the oxidation-reduction potential monitor in the step S5
Former current potential, when the oxidation-reduction potential of the reproducibility group mother liquor is higher than 65mV, the addition of Xiang Suoshu reproducibility group mother liquor
Sodium borohydride is so that the oxidation-reduction potential of the reproducibility group mother liquor is reduced to 65mV or 65mV or less；The pallet overflows
The reproducibility group mother liquor flow into the reproducibility group mother liquor hold tank and be recycled.The described of recycling is kept to go back
The oxidation-reduction potential of originality group mother liquor is to ensure the reproducibility of the reproducibility group mother liquor, in this way can not only be maximum
Limit using the reproducibility group mother liquor, and the load ferro-aluminum carbon carrier and the reproducibility group mother liquor can be made to protect
Hold certain reaction speed, be conducive to zeroth order ferro-aluminum Quick uniform and be deposited on carbon, also can effectively control charcoal ferro-aluminum it is multiple
The preparation duration of condensation material；Sodium borohydride is strong reductant, can enhance the reproducibility of the reproducibility group mother liquor.
Preferably, being equipped 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, Xiang Suoshu reproducibility group mother liquor addition acid is so that the reproducibility group mother liquor pH value is 3-4.It is described acid be dilute sulfuric acid or
One of dust technology is a variety of.
Preferably, the reaction kettle 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 enclosure space with the base wall portion of the reaction kettle, described
The preferred G4 sand core filter of filter.
Preferably, the predetermined value is 0.85 × 102μs/cm-0.95×102μs/cm。
Preferably, further including following steps in the step S1: being carried out to the deionized water added with the ferro-aluminum source
Heating and stirring, and the temperature for controlling the deionized water is 413K-433K, and control stirring rate is 60r/min-120r/
A length of 30min-60min when min, stirring, so that source of iron can be quickly dissolved in deionized water；It, will be described in the step S4
Stirring rate when ferro-aluminum base mother liquor is mixed with the carbon-based dispersion liquid is a length of when being 60r/min-120r/min, stirring
60min-90min can make the ferro-aluminum base mother liquor and the carbon-based dispersion liquid be sufficiently mixed conducive to the load iron carbon carrier
Formation.The iron carbon mixed liquor can be placed a period of time (60min-90min) after stirring, adsorb carbon carrier sufficiently
Ferrous ion, aluminium ion.
Preferably, in the iron-based mother liquor total concentration of ferro-aluminum be 150g/L-250g/L, carbon in the carbon-based dispersion liquid
Concentration is 100g/L-250g/L, ferro-aluminum base mother liquor with the mass ratio with the carbon-based dispersion liquid is in the ferro-aluminum carbon mixed liquor
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 molar 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 and the mass ratio of the deionized water are 1:
100-2:100, concentration of the sodium borohydride in the reproducibility group mother liquor are 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, needs to reinforce 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 of aluminum nitrate, aluminium chloride, polyaluminium sulfate are a variety of；The carbon source has microcosmic hexagonal structure unit, the carbon
Source is one of charcoal, carbon nanotube, graphene, graphene oxide, lamellar graphite powder or a variety of, and the carbon source is preferably raw
Object charcoal, the charcoal is by bio-organic materials into generating after high temperature pyrolysis in the environment of anoxic or anoxybiotic.Charcoal
It is a kind of functional material stable with controllable conductance and property, charcoal atom is with the rule for the plane net that big π is strong and extends
Property arranges to form regular three-dimensional structure.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 be coordinated, metal can be promoted living
Property center is uniformly distributed with molecular level in biological carbon surface, is conducive to the formation of ferro-aluminum carbon catalysis structure.Charcoal by
Unsaturated double strong, a large amount of surface groups abundant, which constitute to be formed with the metal of variable valency, has d, pi-conjugated coordination just
Mesh-like configuration is laminated in hexahedron, and charcoal itself also has stable doping electric conductivity, energy-storage property and adjustable oxidation-also
Originality energy, can with metal ion formed have Reversible Cycle oxidationreduction chain, be conducive to metal between various valence states into
Row conversion.
It is currently preferred select have microcosmic hexagonal structure unit carbon source, charcoal obtained ferro-aluminum composite wood
Material is in pollution treatment process, Fe2+It will form etching electronic transmitting, Fe in waste water with carbon or carbon compound2+With carbon or carbonization
Closing has very high potential difference between object, so that generating hydroxyl radical free radical at the microcosmic hexagonal margin of carbon or carbon compound and surpassing
Organic matter in waste water can be resolved into harmless substance by oxygen radical, hydroxyl radical free radical and superoxide radical.
Charcoal provided by the invention ferro-aluminum composite material preparation method to carry iron carbon carrier carry out conductivity examine
It surveys to judge to carry iron carbon carrier with reproducibility group mother liquor and react whether reach terminal, so that whole preparation process is easily manipulated；
Simultaneously the preparation method be not required to addition dispersing agent, so charcoal ferro-aluminum composite material preparation method it is without secondary pollution.
Detailed description of the invention
Fig. 1 be charcoal provided by the invention ferro-aluminum composite material preparation method process flow chart；
Fig. 2 be charcoal provided by the invention ferro-aluminum composite material preparation facilities；
Fig. 3 be embodiment 1 made from charcoal ferro-aluminum composite material electron-microscope scanning figure.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawings and examples.It should be noted that if do not conflicted, this hair
Each feature in bright embodiment and embodiment can be combined with each other, within the scope of the present invention.
Embodiment 1
Referring to Fig. 2, to charcoal ferro-aluminum composite material preparation facilities be described in detail:
A kind of charcoal ferro-aluminum composite material preparation facilities, including open-topped reaction kettle 1, reproducibility group mother liquor
Holding vessel 2 and spray head 3, reaction kettle 1 with valvular pipeline with reproducibility group mother liquor hold tank 2 by connecting, reproducibility base
Group's mother liquor hold tank 2 is connect by the pipeline with circulating pump with spray head 3, and pallet 4 is equipped in reaction kettle 1, and pallet 4 is equipped with conductance
Rate analyzer 5 and several graphite rods 6, graphite rod 6 connect with power cathode, are equipped in reproducibility group mother liquor hold tank 2
Oxidation-reduction potential monitor 7 and pH meter 8.1 bottom of reaction kettle is equipped with filter 9, filter 9 be located at below pallet 4 and with it is anti-
1 base wall portion of kettle is answered to form enclosure space, the preferred G4 sand core filter of filter 9, filter is sand core filter, the number of spray head 3
Amount is not limited to one, and reaction kettle 1 is preferably shaped to infundibulate.
Embodiment 2
In conjunction with Fig. 1, Fig. 2 to charcoal provided by the invention the preparation method of ferro-aluminum composite material be described in detail:
A kind of charcoal ferro-aluminum composite material preparation method the following steps are included:
S1, take certain ferrous nitrate, polyaluminium sulfate be added deionized water, then to added with ferrous nitrate go from
Sub- water is heated and is stirred, and the temperature for controlling deionized water is 413K, and control stirring rate is a length of when being 60r/min, stirring
30min, it is 200g/L ferro-aluminum base mother liquor that alferric amount is obtained after stirring, for use；
S2, it takes a certain amount of charcoal that the suspension for obtaining charcoal concentration in deionized water as 200g/L is added, will hang
The pH value of supernatant liquid is adjusted to 3 or so, and the suspension for being then 3 or so to pH value carries out obtaining carbon-based point after ultrasonic wave disperses 30min
Dispersion liquid, for use；
S3, the sodium citrate, ascorbic acid and sodium sulfite that are 2.5:1:1.5 by molar ratio are added in deionized water and obtain
Reducing solution, solvent and Solute mass ratio are 1:100 in reducing solution；After the pH value of reducing solution is adjusted to 3 or so
Sodium borohydride is added to it and obtains reproducibility group mother liquor, for use；Wherein, sodium borohydride concentration is in reproducibility group mother liquor
4g/L；Reproducibility group mother liquor need to charcoal ferro-aluminum composite material prepare before prepare in 20min；
S4, ferro-aluminum base mother liquor and carbon-based dispersion liquid are mixed to get ferro-aluminum carbon mixed liquor with the mass ratio of 3:1, to ferro-aluminum carbon
Mixed liquor is stirred, and controlling stirring rate is 60r/min, and control a length of 60min when stirring stands iron after stirring
It is obtained by filtration after carbon mixed liquor 60min and carries ferro-aluminum carbon carrier；
S5, load ferro-aluminum carbon carrier being placed in pallet 4, pallet 4 is placed in reaction kettle 1, and reaction kettle 1 is equipped with filter 9,
The preferred G4 sand core filter of filter 9, pallet 4 is interior to be equipped with multiple graphite rods 6, and graphite rod 6 is connect with power cathode, carries ferro-aluminum
Carbon carrier is contacted with graphite rod 6；Then reproducibility group mother liquor is slowly sprayed to ferro-aluminum carbon carrier is carried by spray head 5, sprayed
The detection (detecting using conductivity measuring instrument 5) of conductivity is carried out in journey to the load ferro-aluminum carbon carrier in pallet 4, is overflow in pallet 4
Reproducibility group mother liquor out flows into 1 bottom of reaction kettle and is collected into again through the filtering of filter 9 equipped with reproducibility group mother liquor
It is recycled in holding vessel 2, the reproducibility group mother liquor in reproducibility group mother liquor hold tank 2 carries out oxidation-reduction potential at this time
Detection (oxidation-reduction potential of the detection reproducibility group mother liquor of oxidation reduction potential determination instrument 7) and pH value (the detection reduction of pH meter 8
Property group mother liquor pH value) detection, it is female to reproducibility group when the oxidation-reduction potential of reproducibility group mother liquor is higher than 65mV
Liquid addition sodium borohydride makes oxidation-reduction potential be reduced to 65mV or 65mV or less；Pass through detection reproducibility group mother liquor simultaneously
PH value control (pH value of addition dust technology, dilute sulfuric acid control reproducibility group mother liquor) reproducibility group mother liquor pH is in 3-4 model
In enclosing；
When the conductivity for carrying ferro-aluminum carbon carrier reaches 0.91 × 102When μ s/cm or more, stop to load ferro-aluminum carbon carrier sprinkling
Reproducibility group mother liquor, at this time by the load ferro-aluminum carbon carrier in pallet 4 collect it is dry after obtain charcoal ferro-aluminum composite material,
Obtained charcoal in ferro-aluminum composite material the mass ratio of ferro-aluminum and carbon be 1:4, charcoal carbon load in ferro-aluminum composite material
There are ferrous 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 material electron-microscope scanning figure.
Embodiment 3
In conjunction with Fig. 1, Fig. 2 to charcoal provided by the invention the preparation method of ferro-aluminum composite material be described in detail:
A kind of charcoal ferro-aluminum composite material preparation method the following steps are included:
S1, take certain ferrous nitrate, aluminum sulfate that deionized water is added, then to added with ferrous nitrate, aluminum sulfate
Deionized water is heated and is stirred, and the temperature for controlling deionized water is 433K, when control stirring rate is 120r/min, stirs
A length of 60min, it is 250g/L ferro-aluminum base mother liquor that iron-content is obtained after stirring, for use；
S2, it takes a certain amount of graphene that the suspension for obtaining graphene concentration in deionized water as 250g/L is added, will hang
The pH value of supernatant liquid is adjusted to 3 or so, and the suspension for being then 3 or so to pH value carries out obtaining carbon-based point after ultrasonic wave disperses 60min
Dispersion liquid, for use；
S3, the sodium citrate, ascorbic acid and sodium sulfite that are 2.5:1:1.5 by molar ratio are added in deionized water and obtain
Reducing solution, solvent and Solute mass ratio are 1:100 in reducing solution；After the pH value of reducing solution is adjusted to 3 or so
Sodium borohydride is added to it and obtains reproducibility group mother liquor, for use；Wherein, sodium borohydride concentration is in reproducibility group mother liquor
4g/L；Reproducibility group mother liquor need to charcoal ferro-aluminum composite material prepare before 20min preparation；
S4, ferro-aluminum base mother liquor and carbon-based dispersion liquid are mixed to get ferro-aluminum carbon mixed liquor with the mass ratio of 5:1, to ferro-aluminum carbon
Mixed liquor is stirred, and controlling stirring rate is 120r/min, and control a length of 90min when stirring is stood after stirring
It is obtained by filtration after ferro-aluminum carbon mixed liquor 90min and carries ferro-aluminum carbon carrier；
S5, load ferro-aluminum carbon carrier being placed in pallet 4, pallet 4 is placed in reaction kettle 1, and reaction kettle 1 is equipped with filter 9,
The preferred G4 sand core filter of filter 9, pallet 4 is interior to be equipped with multiple graphite rods 6, and graphite rod 6 is connect with power cathode, carries ferro-aluminum
Carbon carrier is contacted with graphite rod 6；Then reproducibility group mother liquor is slowly sprayed by 5 Xiang Zaitie carbon carrier of spray head, sprays process
In the detection (detecting using conductivity measuring instrument 5) of conductivity is carried out to the load iron carbon carrier in pallet 4, overflow in pallet 4
Reproducibility group mother liquor flows into 1 bottom of reaction kettle and is collected into again through the filtering of filter 9 equipped with the storage of reproducibility group mother liquor
It is recycled in tank 2, the reproducibility group mother liquor in reproducibility group mother liquor hold tank 2 carries out oxidation-reduction potential detection at this time
(pH meter 8 detects reproducibility base for (oxidation-reduction potential of the detection reproducibility group mother liquor of oxidation reduction potential determination instrument 7) and pH value
Group mother liquor pH value) detection, when the oxidation-reduction potential of reproducibility group mother liquor be higher than 65mV when, add to reproducibility group mother liquor
Add sodium borohydride that oxidation-reduction potential is made to be reduced to 65mV or 65mV or less；Pass through the pH of detection reproducibility group mother liquor simultaneously
Value control (pH value of addition dust technology, dilute sulfuric acid control reproducibility group mother liquor) reproducibility group mother liquor pH is within the scope of 3-4；
When the conductivity for carrying ferro-aluminum carbon carrier reaches 0.85 × 102When μ s/cm or more, stop to load ferro-aluminum carbon carrier sprinkling
Reproducibility group mother liquor, at this time by the load ferro-aluminum carbon carrier in pallet 4 collect it is dry after obtain charcoal ferro-aluminum composite material,
Obtained charcoal in ferro-aluminum composite material the mass ratio of iron and carbon be 1:3, charcoal in ferro-aluminum composite material carbon load have
Ferrous 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
In conjunction with Fig. 1, Fig. 2 to charcoal provided by the invention the preparation method of ferro-aluminum composite material be described in detail:
A kind of charcoal ferro-aluminum composite material preparation method the following steps are included:
S1, take certain ferrous nitrate, aluminum nitrate that deionized water is added, then to added with ferrous nitrate, aluminum nitrate
Deionized water is heated and is stirred, and the temperature for controlling deionized water is 423K, when control stirring rate is 80r/min, stirs
A length of 50min obtains the ferro-aluminum base mother liquor that alferric amount is 150g/L, for use after stirring；
S2, take a certain amount of carbon nanotube that the suspension for obtaining carbon nanotube concentration in deionized water as 100g/L is added,
The pH value of suspension is adjusted to 3 or so, the suspension for being then 3 or so to pH value carries out obtaining carbon after ultrasonic wave disperses 50min
Base dispersion liquid, for use；
S3, the sodium citrate, ascorbic acid and sodium sulfite that are 2.5:1:1.5 by molar ratio are added in deionized water and obtain
Reducing solution, solvent and Solute mass ratio are 1:100 in reducing solution；After the pH value of reducing solution is adjusted to 3 or so
Sodium borohydride is added to it and obtains reproducibility group mother liquor, for use；Wherein, sodium borohydride concentration is in reproducibility group mother liquor
4g/L；Reproducibility group mother liquor need to charcoal ferro-aluminum composite material prepare before 20min preparation；
S4, ferro-aluminum base mother liquor and carbon-based dispersion liquid are mixed to get ferro-aluminum carbon mixed liquor with the mass ratio of 2:1, to ferro-aluminum carbon
Mixed liquor is stirred, and controlling stirring rate is 70r/min, and control a length of 70min when stirring stands aluminium after stirring
It is obtained by filtration after iron carbon mixed liquor 90min and carries ferro-aluminum carbon carrier；
S5, load ferro-aluminum carbon carrier being placed in pallet 4, pallet 4 is placed in reaction kettle 1, and reaction kettle 1 is equipped with filter 9,
The preferred G4 sand core filter of filter 9, pallet 4 is interior to be equipped with multiple graphite rods 6, and graphite rod 6 is connect with power cathode, carries ferro-aluminum
Carbon carrier is contacted with graphite rod 6；Then reproducibility group mother liquor is slowly sprayed to ferro-aluminum carbon carrier is carried by spray head 5, sprayed
The detection (detecting using conductivity measuring instrument 5) of conductivity is carried out in journey to the load ferro-aluminum carbon carrier in pallet 4, is overflow in pallet 4
Reproducibility group mother liquor out flows into 1 bottom of reaction kettle and is collected into again through the filtering of filter 9 equipped with reproducibility group mother liquor
It is recycled in holding vessel 2, the reproducibility group mother liquor in reproducibility group mother liquor hold tank 2 carries out oxidation-reduction potential at this time
Detection (oxidation-reduction potential of the detection reproducibility group mother liquor of oxidation reduction potential determination instrument 7) and pH value (the detection reduction of pH meter 8
Property group mother liquor pH value) detection, it is female to reproducibility group when the oxidation-reduction potential of reproducibility group mother liquor is higher than 65mV
Liquid addition sodium borohydride makes oxidation-reduction potential be reduced to 65mV or 65mV or less；Pass through detection reproducibility group mother liquor simultaneously
PH value control (pH value of addition dust technology, dilute sulfuric acid control reproducibility group mother liquor) reproducibility group mother liquor pH is in 3-4 model
In enclosing；
When the conductivity for carrying ferro-aluminum carbon carrier reaches 0.95 × 102When μ s/cm or more, stop to load ferro-aluminum carbon carrier sprinkling
Reproducibility group mother liquor, at this time by the load ferro-aluminum carbon carrier in pallet 4 collect it is dry after obtain charcoal ferro-aluminum composite material,
Obtained charcoal in ferro-aluminum composite material the mass ratio of iron and carbon be 1:5, charcoal in ferro-aluminum composite material carbon load have
Ferrous iron, Zero-valent Iron, zeroth order aluminium, sulfydryl, carboxyl and hydroxyl etc., Zero-valent Iron uniform deposition is on carbon.
Charcoal provided by the invention the preparation method of ferro-aluminum composite material there is process control, without secondary pollution excellent
Point.
Although the preferred embodiment of the embodiment of the present invention has been described, once a person skilled in the art knows bases
This creative concept, then additional changes and modifications can be made to these embodiments.So the following claims are intended to be interpreted as
Including preferred embodiment and fall into all change and modification of range of embodiment of the invention.
Claims (10)
1. a kind of preparation method of Sheng Wutan ferro-aluminum composite material, which is characterized in that the preparation method uses controllable stacking cladding
Device obtains Sheng Wutan ferro-aluminum composite material, and the controllable stacking coating unit includes the homogeneous plating with graphitiferous tooth bed
Reaction bed, reproducibility group mother liquor hold tank and spray head, reaction bed conductivity sensor and controller, connecting tube and circulating pump,
The electroplating reaction bed is connect with the reproducibility group mother liquor hold tank, the reproducibility group mother liquor hold tank and the spray
Head connection；Pallet is equipped in the reaction kettle, the pallet is equipped with conductivity measuring instrument, and the preparation method includes following step
It is rapid:
S1, it 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
Carbon-based dispersion liquid is obtained after carrying out ultrasonic wave dispersion；
S3, it the reducing agent containing group is dissolved in deionized water obtains reproducibility radical solution, by the reproducibility radical solution
PH value obtains reproducibility group mother liquor after being adjusted to 3-4, and the reproducibility group mother liquor is configured in using preceding 20min；It is described
Reducing agent is rich in carboxyl, hydroxyl and sulfydryl；
S4, ferro-aluminum carbon mixed liquor is obtained after the ferro-aluminum base mother liquor and the carbon-based dispersion liquid are mixed, to the ferro-aluminum
Carbon mixed liquor, which is obtained by filtration, 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 spray head
It states reproducibility group mother liquor and detects the conductivity for carrying ferro-aluminum carbon carrier using the conductivity measuring instrument, when the load aluminium
When the 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 dry, obtain the charcoal ferro-aluminum composite material.
2. charcoal according to claim 1 ferro-aluminum composite material preparation method, which is characterized in that the homogeneous electricity
Plating reaction bed is equipped with the graphite tooth plate for mutually uniformly contacting with the load ferro-aluminum carbon carrier, the graphite truss plate connection power supply yin
Pole is can provide electronics to the load ferro-aluminum carbon carrier.
3. charcoal according to claim 1 ferro-aluminum composite material preparation method, which is characterized in that the reproducibility
Oxidation-reduction potential monitor is equipped in group mother liquor hold tank, the preparation method includes: to use institute in the step S5
The oxidation-reduction potential that oxidation-reduction potential monitor detects the reproducibility group mother liquor is stated, when the reproducibility group mother liquor
Oxidation-reduction potential when being higher than 65mV, Xiang Suoshu reproducibility group mother liquor adds citric acid and sodium borohydride weak solution so that institute
The oxidation-reduction potential for stating reproducibility group mother liquor is reduced to 65mV or 65mV or less.
4. charcoal according to claim 3 ferro-aluminum composite material preparation method, which is characterized in that the reproducibility
PH meter is equipped in group mother liquor hold tank, the preparation method includes: in the step S5, using described in pH meter detection
The pH value of reproducibility group mother liquor, when the reproducibility group mother liquor pH value is higher than 4, the addition of Xiang Suoshu reproducibility group mother liquor
Diluted acid is so that the reproducibility group mother liquor pH value is 3-4.
5. charcoal according to claim 3 ferro-aluminum composite material preparation method, which is characterized in that the reaction kettle
Bottom is provided with the filter for filtering the reproducibility group mother liquor overflowed from the pallet, and the filter was used for
Filter reproducibility group mother liquor is simultaneously drained in group mother liquor hold tank.
6. charcoal according to claim 1 ferro-aluminum composite material preparation method, which is characterized in that the predetermined value
For 0.85 × 102 μ of μ s/cm-0.95 × 102 s/cm.
7. charcoal according to claim 1 ferro-aluminum composite material preparation method, which is characterized in that in the step
Further include following steps in S1: heating and stirring being carried out to the deionized water added with the ferro-aluminum source, and are gone described in control
The temperature of ionized water is 413K-433K, a length of 30min-60min when control stirring rate is 60r/min-120r/min, stirs,
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
When stirring rate be 60r/min-120r/min, stirring when a length of 60min-90min.
8. charcoal according to claim 1 ferro-aluminum composite material preparation method, which is characterized in that the ferro-aluminum base
In mother liquor the total concentration of ferro-aluminum be 150g/L-250g/L, in the carbon-based dispersion liquid concentration of carbon be 100g/L-250g/L, institute
Stating ferro-aluminum base mother liquor and the mass ratio with the carbon-based dispersion liquid in ferro-aluminum carbon mixed liquor is 2:1-5:1.
9. charcoal according to claim 1 ferro-aluminum composite material preparation method, which is characterized in that in the step
In S3, the reducing agent contains sodium citrate, ascorbic acid, sodium sulfite and sodium borohydride, the sodium citrate, described anti-bad
Hematic acid and the sodium sulfite molar ratio are 2.0-3.0:0.5-1.5:1.0-2.0, the sodium citrate, the ascorbic acid and
The mixture of the sodium sulfite three and the mass ratio of the deionized water are 1:100-2:100, and the sodium borohydride is in institute
Stating the concentration in reproducibility group mother liquor is 3g/L-5g/L.
10. charcoal according to claim 1 to 9 ferro-aluminum composite material preparation method, which is characterized in that
The ferro-aluminum source is the mixture of silicon source and source of iron, and source of aluminium is aluminum sulfate, in aluminum nitrate, aluminium chloride, polyaluminium sulfate
One or more, the source of iron is one of ferrous nitrate, ferrous sulfate heptahydrate, bodied ferric sulfate, potassium ferrate or a variety of,
The carbon source is one of charcoal, carbon nanotube, graphene, graphene oxide, lamellar graphite powder or a variety of.
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