CN108821346A - A kind of three-dimensional flower-shaped nanostructure ferriferous oxide preparation method and applications - Google Patents
A kind of three-dimensional flower-shaped nanostructure ferriferous oxide preparation method and applications Download PDFInfo
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Abstract
The present invention discloses a kind of preparation method and applications of three-dimensional flower-shaped nanostructure iron oxide material.The method includes immersing in solution containing azo dyes or sodium chloride-containing solution to be soaked for a period of time by Fe-based amorphous/nanometer crystal alloy band that three-dimensional flower-shaped nanostructure ferriferous oxide can be obtained.The preparation method is simple, operation under low in cost, normal temperature and pressure, easy to industrialized production.The three-dimensional flower-shaped nanostructure ferriferous oxide being prepared is attached to Fe-based amorphous/nanometer crystal alloy strip face, generally macroscopic material, convenient for application.Fe-based amorphous/nanocrystalline band with three-dimensional flower-shaped nanostructure ferriferous oxide is put into solution containing heavy metal ion, it can heavy metal ion in quick adsorption solution, and band is easy to take out or separate from solution, using simplicity, therefore has good application value.
Description
Technical field
The present invention relates to Fe-based amorphous/nanocrystalline stripping and the three-dimensional flower-shaped nanometers for growing and adhering on its surface
The preparation method and application of structure ferriferous oxide.
Background technique
Three-dimensional flower-shaped nanostructure ferriferous oxide has big specific surface area because of its nanostructure, is containing heavy metal ion
There is good application prospect in the processing of sewage.Three-dimensional flower-shaped nanostructure ferriferous oxide generallys use hydrothermal/solvent thermal response
Metal salt solution is reacted with chemical reagent and generates metal oxide by synthesis.This method is long reaction time, and preparation process is complicated,
Reaction temperature>It 150 DEG C, not in room temperature range, need to additionally heat, increase its preparation cost.Research and development prepare three-dimensional flower-shaped nanometer
The new method of structure ferriferous oxide simplifies preparation step and reaction condition for reducing cost, and expanding its practical application has weight
The meaning wanted.
Heavy metal ion in water is mainly from various industrial wastewaters, excessive heavy metal ion exposure on human and ecology
Environment has significant damage.Excessive heavy metal ion will lead to aquatic organism death in water, influence the ecological balance and water system certainly
Detergent power.Furthermore the heavy metal ion in water can accumulate in animal and plant body, enter human body, an excessive huge sum of money by food chain
Organ damage or even carcinogenic, teratogenesis can be generated to human body by belonging to ion intake.Therefore the heavy metal ion in removal sewage has weight
The meaning wanted.Dyeing and printing sewage accounts for about the 20% of industrial wastewater, and main pollutant component is dyestuff, additionally often contains heavy metal ion
CrVI.The optimal processing result of sewage treatment is that pollutant can be changed into useful material further to be applied.Zero-valent Iron
During deoxidization, degradation azo dyes, iron oxide deposits are generated, if can make to precipitate ferriferous oxide presentation by process
Three-dimensional flower-shaped nanostructure, and the Cr in dyeing and printing sewage is adsorbed simultaneouslyVI, will have important practical value, one kind can be developed into
Prepare the new method of three-dimensional flower-shaped nanostructure ferriferous oxide.
Summary of the invention
The present invention is intended to provide a kind of simple new method is used to prepare three-dimensional flower-shaped nanostructure ferriferous oxide.
Steps are as follows for three-dimensional flower-shaped nanostructure ferriferous oxide preparation method of the invention：With Fe-based amorphous/nanocrystalline conjunction
Gold bar band be ferro element source, using azo dyes solution or sodium chloride solution as oxidant, at a certain temperature by it is Fe-based amorphous/
Nanometer crystal alloy band immerses in solution containing azo dyes or sodium chloride-containing solution, is kept for the regular hour, can be prepared one
The fine and close three-dimensional flower-shaped nanostructure ferriferous oxide of layer and uniform fold and the table for being attached to Fe-based amorphous/nanometer crystal alloy band
Face.Continue to impregnate, the three-dimensional flower-shaped nanostructure is changed into three-dimensional flower shape from petal-shaped.Consistency also gradually increases.
For Fe-based amorphous/nanocrystalline band composition based on ferro element, ferro element atomic percent is 50%~85%.
In the method, the Fe-based amorphous/nanometer crystal alloy band ingredient range of choice is wide, can be Fe-Ni-Si-B-
Nb-Cu, Fe-Si-B, Fe-Si-B-Co, Fe-Si-B-P-C-Mo etc. be Fe-based amorphous/nanometer crystal alloy material.
The azo dyes is following but one of is not limited to following dyestuff, gold orange II, methyl orange, directly indigo plant 6 etc..
Gold orange II (C may be selected in the azo dyes16H11N2NaO4S), gold orange II initial concentration solution 25mg/L, initial pH
Value is neutral to alkalinity.
The initial concentration of the solution containing azo dyes is 25~100mg/L, and pH value is 6~10；The sodium chloride-containing is molten
The aqueous solution that liquid is 3~5%, pH value 6-10.
The solution temperature is 25~55 DEG C, and soaking time 40~60 minutes, can be obtained one in azo dyes solution
The fine and close three-dimensional flower-shaped nanostructure ferriferous oxide of layer；It is impregnated 60-3600 minutes in sodium chloride solution, can be obtained one layer of cause
Close three-dimensional floral leaf shape/petal-shaped or flower shape nanostructure ferriferous oxide.Different sodium chloride concentrations and different soaking times pair
There is influence in flower-like nanostructure ferriferous oxide pattern, can regulate and control.
The three-dimensional flower-shaped nanostructure ferriferous oxide of preparation is FeOOH alpha-feooh or α-(Fe, M) OOH, wherein M
For Ni or Co.
The alpha-feooh can be used for adsorbing the heavy metal ion in water.
The heavy metal ion is hexavalent chromium (CrVI)。
Application of the above method in adsorption aqueous solution heavy metal ion is to utilize three-dimensional flower-shaped nanostructure ferriferous oxide
It is attached to the characteristics of amorphous alloy/nanometer crystal alloy item takes and band is applied together, be put into togerther in solution.It is main special
Sign is but is not limited to：It can be by band：(1) curved heap is agglomerating, is placed in solution is easy in the net basket passed through, is put into solution and adsorbs weight
Metal ion；(2) glass tube and glass bar both ends can be fixed the strip to, allows one end to float in sewage with glass tube molten
It in liquid, and is completely immersed in solution under the action of the self weight of other end glass bar, is that band main body immerses in solution, and it can be with glass
Steel drift；(3) sewage can also be allowed to flow through from pipeline by the pockets of band of curved heap or regularly arranged band as in pipeline,
It is flowed through from multiple valve according to adsorption time, flow velocity design, Adsorption heavy metal ion, and available strainer or externally-applied magnetic field etc.
The three-dimensional flower-shaped nanostructure iron oxidation that the iron-based material that method will fall off adsorbed heavy metal ion falls off in whole or in part
Object is removed from solution.
Fe-based amorphous/nanometer crystal alloy band and azo dyes solution are immersed in solution by a certain percentage, such as：Proportion
For 2.5g：250mL, reaction time are only 30~50 minutes, and reaction temperature can be room temperature, such as 25 DEG C, can prepare flower-shaped receive
Rice structure ferriferous oxide.To contact band uniformly with solution, mechanical stirring can be applied, stirring rate is
180rpm.If immersing in sodium chloride solution, the aqueous solution that the sodium chloride solution is 3~5%, pH value 6-10.
The above method of the present invention can under normal temperature and pressure conditions mix Fe-based amorphous/nanocrystalline band with reagent, in short-term
Interior realization attachment is used to prepare three-dimensional flower-shaped nanostructure ferriferous oxide for a kind of completely new method.This method is preparation three
Dimension flower-like nanostructure ferriferous oxide provides a kind of easy method, and the flower-shaped oxide growth for preparing and is attached to iron-based
Amorphous/nanocrystalline strip face is carried, generally macroscopic material by Fe-based amorphous/nanocrystalline band, be convenient for practical application.
Another object of the present invention provides the application of prepared three-dimensional flower-shaped nanostructure ferriferous oxide.
Application provided by the invention is the heavy metal ion in three-dimensional flower-shaped nanostructure ferriferous oxide absorption water, selection
Heavy metal ion is Cr common in dyeing and printing sewageVI。
It is raw material that the present invention, which selects the easy iron based nano crystal band of preparation process, is oxidant with azo dyes solution,
The two sides that one layer of three-dimensional flower-shaped nanostructure ferriferous oxide is attached to band is prepared, the three-dimensional flower-shaped nanostructure iron oxidation
Object is to CrVIWith suction-operated.
Detailed description of the invention
Fig. 1 is (Fe73.5Si13.5B9Nb3Cu1)91.5Ni8.5Fe-based amorphous alloy (Fe-AR), iron-base nanometer crystal alloy (Fe-
MNR), iron-base nanometer crystal alloy adheres to three-dimensional flower-shaped nanostructure ferriferous oxide (Fe-MNRs+3D-FNs) and iron based nano crystal closes
Gold adheres to three-dimensional flower-shaped nanostructure ferriferous oxide and adsorbs CrVI(Fe-MNRs+3D-FNs+Cr afterwardsVI) band XRD spectrum.
Fig. 2 is that iron based nano crystal band is immersed in the surface topography differentiation of different time in gold orange II solution (wherein (a)
1min,(b)5min,(c)10min,(d)20min,(e)50min,(f)50min.(a)-(e):Amplification factor is identical, is (f)
(e) low power picture).
Fig. 3 is the XRD spectrum of three-dimensional flower-shaped nanostructure ferriferous oxide.
Fig. 4 is Fe-MNR+3D-FNs adsorption-desorption isothermal.
Fig. 5 is Fe81Si4B14Cu1AMORPHOUS ALLOY RIBBONS XRD spectrum.
Fig. 6 is three-dimensional flower-shaped nanostructure ferriferous oxide SEM spectrum.
Fig. 7 is that ferrum-based amorphous alloy strip is immersed in the surface topography differentiation of different time in sodium-chloride water solution (in (c)
The scale bar of display figure (a)-(c)) (a) 10 hours, (b) 20 hours, (c) 60 hours, (d) figure (c) partial enlargement (60 is small
When).
Fig. 8 is Fe-MNRs and Fe-MNRs+3D-FNs to CrVIThe adsorption rate curve of ion (initial concentration 10mg/L).
Fig. 9 is Fe-MNRs+3D-FNs+CrVISurface EDS map.
Specific embodiment
The present invention is specifically described below by drawings and examples, but the present invention is not limited thereto.
Fe-based amorphous/nanometer crystal alloy band is immersed in solution containing azo dyes or sodium chloride solution, reaction temperature is
25~55 DEG C, after impregnating 20-3600 minutes, it can be obtained one layer of three-dimensional floral leaf shape/petal-shaped for being attached to alloy strip surface
Or flower shape nanostructure ferriferous oxide.There are shadows to flower-like nanostructure ferriferous oxide for different solutions and different soaking times
It rings, can regulate and control.
Embodiment 1
Iron based nano crystal band is soaked in solution containing azo dyes, three-dimensional flower-shaped nanostructure ferriferous oxide is prepared.
By (Fe73.5Si13.5B9Nb3Cu1)91.5Ni8.5Ferrum-based amorphous alloy strip under protection of argon gas, 800 DEG C of isothermal annealings
5-30 minutes.(Fe before and after isothermal annealing73.5Si13.5B9Nb3Cu1)91.5Ni8.5The X-ray diffracting spectrum of band as shown in Figure 1,
Only one diffusing scattering peak of preceding article band is made annealing treatment, shows it for amorphous structure；The band obtained after isothermal annealing has point
Sharp diffraction maximum, i.e. annealing band are crystal alloy band, and Crystallization Phases are α-Fe phase, Fe2B phase and Fe16Nb6Si7Phase.Crystal grain
Having a size of nanometer tens-several hundred nanoscales.
0.2500g gold orange II powder is weighed with Libra, is dissolved in 100mL deionized water, obtains initial concentration 2.5g/L's
Gold orange II mother solution；The 2.5g/L gold orange II mother solution that 2.5mL is taken with liquid-transfering gun prepares aimed concn 25mg/ with 250mL measuring bottle
L gold orange II solution；Matched gold orange II solution ph is measured, is needed to adjust gold with the hydrochloric acid or sodium hydroxide of 1mol/L according to experiment
The pH value of orange II solution is to 6 ± 0.05；Prepared gold orange II solution is poured into 500mL beaker, beaker is put into water-bath
Heat preservation is to 25 DEG C；(the Fe of preparation is weighed with Libra73.5Si13.5B9Nb3Cu1)91.5Ni8.5Nanocrystalline band 2.5g, band is added
In the gold orange II solution of water-bath beaker, 50min is impregnated, in soaking process, mechanical stirring is applied to solution, stirring rate is about
180rpm.Different soaking time bands are taken, its surface topography is observed, three-dimensional flower-shaped nanostructure ferriferous oxide is characterized and grew
Journey.As shown in Fig. 2, three-dimensional flower-shaped nanostructure is first in strip face forming core, subsequent long slabbing petal, after petal quantity increase
It is self-assembled into three-dimensional flower-shaped structure, the time extends, and flower-like structure petal quantity increases size and increases, and finally grows up at 50 minutes
The complete flower-like structure that diameter is about 2~3 microns.
The powder of three-dimensional flower-shaped nanostructure is collected, XRD test is carried out.As shown in figure 3, these three-dimensional flower-shaped nanostructures
Product is α-FeO (OH).
Specific surface area and the hole that three-dimensional flower-shaped nanostructure ferriferous oxide band is adhered on surface are measured by N2 adsorption-desorption
Diameter distribution, as shown in figure 4, its specific surface area is 9m2/g。
Embodiment 2
Fe-based amorphous alloy is soaked in azo dyes solution, is stirred and prepares three-dimensional flower-shaped nanostructure iron oxidation
Object.
0.2500g gold orange II powder is weighed with Libra, is dissolved in 100mL deionized water, obtains initial concentration 2.5g/L's
Gold orange II mother solution；The 2.5g/L gold orange II mother solution that 2.5mL is taken with liquid-transfering gun prepares aimed concn 25mg/ with 250mL measuring bottle
L gold orange II solution；Matched gold orange II solution ph is measured, is needed to adjust gold with the hydrochloric acid or sodium hydroxide of 1mol/L according to experiment
The pH value of orange II solution is to 10 ± 0.05；Prepared gold orange II solution is poured into 500mL beaker, beaker is put into water-bath
Heat preservation is to 25 DEG C；Fe is weighed with Libra81Si4B14Cu1AMORPHOUS ALLOY RIBBONS 2.5g (the XRD diffracting spectrum of the ferrous alloy band
As shown in figure 5, showing it with amorphous structure), band is added in the gold orange II solution of water-bath beaker, in soaking process,
Mechanical stirring, stirring rate 180rpm are applied to solution.Different soaking time bands are taken, its surface topography, characterization three are observed
Tie up flower-like nanostructure ferriferous oxide growth course.As shown in fig. 6, when impregnating 50min, Fe81Si4B14Cu1AMORPHOUS ALLOY RIBBONS
One layer of fine and close three-dimensional flower-shaped nanostructure ferriferous oxide is successfully adhered on surface.
Embodiment 3
Fe-based amorphous alloy is soaked in sodium chloride solution, three-dimensional flower-shaped nanostructure ferriferous oxide is prepared.
36.27g sodium chloride is weighed with Libra, is dissolved in 1000mL deionized water, the chlorine of initial concentration 3.5wt.% is obtained
Change sodium water solution；Fe is weighed with Libra78Si9B13Band is added in sodium-chloride water solution Fe-based amorphous band 0.2g, impregnates
60-3600 minutes.Different soaking time bands are taken, its surface topography is observed, it is raw to characterize three-dimensional flower-shaped nanostructure ferriferous oxide
Growth process.As shown in fig. 7, three-dimensional flower-shaped nanostructure is first in strip face forming core, at 600 minutes, in strip surface shape
At one layer of fine and close three-dimensional flower foliation structure (Fig. 7 (a))；At 1200 minutes, one layer of fine and close three were formed in strip surface
Tie up petal design, including part flower structure (Fig. 7 (b))；Extending at any time, flower-like structure petal quantity increases size and increases,
After 3600 minutes (Fig. 7 (c), (d)), one layer of fine and close three-dimensional petal/flower structure, three-dimensional flower knot have been formed in strip surface
The diameter of structure is about 2~10 microns.
Embodiment 4
Three-dimensional flower nanostructure iron oxidation is applied to adsorbing hexavalent chromium ions (CrVI)。
0.2500g high chromic acid content first powder is weighed with Libra, is dissolved in 100mL deionized water, obtains initial concentration 2.5g/L
CrVIMother solution；The 2.5g/L Cr of 1mL is taken with liquid-transfering gunVIMother solution prepares aimed concn 10mg/L with 250mL measuring bottle
CrVISolution；Matched azo dyes gold orange II solution ph is measured, needs to adjust gold orange II with the hydrochloric acid of 1mol/L according to experiment molten
The pH value of liquid is to 3 ± 0.05；By prepared CrVISolution pours into 500mL beaker, and beaker is put into water-bath and is kept the temperature to 25
℃；The gold orange II solution that water-bath beaker is added in three-dimensional flower-shaped nanostructure ferriferous oxide iron based nano crystal band is adhered on surface
In, mechanical stirring, stirring rate 180rpm are applied to solution；Different soaking time solution are taken, keep solution aobvious with 1-5 carbonohydrazides
Color, with measurement of ultraviolet-visible spectrophotometer concentration.
As shown in figure 8, three-dimensional flower-shaped nanostructure ferriferous oxide iron based nano crystal band (Fe-MNRs+3D- is adhered on surface
FNs) there is fine Adsorption effect to hexavalent chromium, the Cr after adsorption treatment 50 minutes, in solutionVIIt substantially inhales
Attached removal.And original iron based nano crystal band (Fe-MNRs) in 60 minutes to CrVIAdsorption effect it is not significant.Fig. 8's
The result shows that three-dimensional flower-shaped nanostructure ferriferous oxide iron based nano crystal band (Fe-MNRs+3D-FNs) is adhered to Cr in surfaceVI
With significant Adsorption effect.
Adhere to (Fe-MNRs after three-dimensional flower-shaped nanostructure ferriferous oxide iron based nano crystal band adsorbs with EDS characterization surface
+3D-FNs+CrVI) surface power spectrum, as shown in figure 9, detecting CrVIShow three-dimensional flower-shaped nanostructure ferriferous oxide to CrVI
With suction-operated
Technical solution of the present invention is described in detail in above-described embodiment.It is apparent that the present invention is not limited being retouched
The embodiment stated.Based on the embodiments of the present invention, those skilled in the art can also make a variety of variations accordingly, but appoint
What is equal with the present invention or similar variation shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of three-dimensional flower-shaped nanostructure ferriferous oxide preparation method that can be used for adsorbing heavy metal ion, which is characterized in that
Include the following steps：
1) Fe-based amorphous/nanometer crystal alloy band is soaked in solution containing azo dyes or sodium chloride-containing solution, generates attachment
In the three-dimensional flower-shaped nanostructure ferriferous oxide of the alloy surface；
2) continue to impregnate, the three-dimensional flower-shaped nanostructure is changed into three-dimensional flower shape from petal-shaped, and consistency also gradually increases.
2. according to claim 1 the method, it is characterised in that：Fe-based amorphous/nanocrystalline band, which is formed with ferro element, is
Main, ferro element atomic percent is 50%~85%.
3. according to claim 1 the method, it is characterised in that：Other than ferro element, Fe-based amorphous/nanocrystalline band is also
Include other amorphous formation elements：B, C, Si, P, Co, Ni, Cu, Nb, Mo are prepared into alloy strip by melt-quenching method.
4. according to claim 1 the method, it is characterised in that：The azo dyes is one of following dyestuff, gold orange II,
Methyl orange, directly indigo plant 6.
5. according to claim 1 the method, it is characterised in that：The initial concentration of the solution containing azo dyes be 25~
100mg/L, pH value are 6~10；The aqueous solution that the sodium chloride-containing solution is 3~5%, pH value 6-10.
6. according to claim 1 the method, it is characterised in that：The solution temperature is 25~55 DEG C, is contaminated described containing azo
Expect in solution soaking time 40~60 minutes, can be obtained three-dimensional flower-shaped nanostructure ferriferous oxide；It is molten in the sodium chloride-containing
It is impregnated 60-3600 minutes in liquid, can be obtained three-dimensional floral leaf shape/petal-shaped or flower shape nanostructure ferriferous oxide.
7. according to claim 1 the method, it is characterised in that：To contact band uniformly with solution, mechanical stirring can be applied,
Stirring rate is~180rpm.
8. according to claim 1 the method, it is characterised in that：The three-dimensional flower-shaped nanostructure ferriferous oxide of preparation is hydroxyl oxygen
Change iron alpha-feooh or α-(Fe, M) OOH, wherein M is Ni or Co；The alpha-feooh can be used for adsorbing the heavy metal ion in water.
9. according to claim 8 the method, it is characterised in that：The heavy metal ion is hexavalent chromium.
10. application of any the method for claim 1-9 in adsorption aqueous solution heavy metal ion, which is characterized in that
(1) the curved heap of band is agglomerating, be placed in containing in heavy metal ion solution, adsorb heavy metal ion；Or
(2) glass tube and glass bar both ends are fixed the strip to, allows one end with glass tube in dirty water float, and the other end exists
It is completely immersed in solution under the action of glass bar self weight, immerses band main body containing in heavy metal ion solution；Or
(3) by the pockets of band of curved heap or regularly arranged band as in the sewage conduct of flowing, making its Adsorption huge sum of money
Belong to ion, and three to be fallen off in whole or in part with the iron-based material for having adsorbed heavy metal ion that strainer or externally-applied magnetic field will fall off
Dimension flower-like nanostructure ferriferous oxide is removed from solution.
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| CN108821346B CN108821346B (en) | 2021-04-02 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103100309A (en) * | 2013-01-28 | 2013-05-15 | 西北农林科技大学 | Method for preparing porous stainless steel iron oxide film for removing heavy metal ion Cr (VI) in aqueous solution |
| CN105314726A (en) * | 2014-07-01 | 2016-02-10 | 中国科学院宁波材料技术与工程研究所 | Printing and dyeing wastewater treatment method |
| CN107326159A (en) * | 2017-06-20 | 2017-11-07 | 清华大学 | It is a kind of to be used for the iron-base nanometer crystal alloy methods for making and using same and device of the processing containing azo dye printing and dyeing wastewater |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103100309A (en) * | 2013-01-28 | 2013-05-15 | 西北农林科技大学 | Method for preparing porous stainless steel iron oxide film for removing heavy metal ion Cr (VI) in aqueous solution |
| CN105314726A (en) * | 2014-07-01 | 2016-02-10 | 中国科学院宁波材料技术与工程研究所 | Printing and dyeing wastewater treatment method |
| CN107326159A (en) * | 2017-06-20 | 2017-11-07 | 清华大学 | It is a kind of to be used for the iron-base nanometer crystal alloy methods for making and using same and device of the processing containing azo dye printing and dyeing wastewater |
Non-Patent Citations (1)
| Title |
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| SHUANGQIN CHEN等: "Unexpected high performance of Fe-based nanocrystallized ribbons for azo dye decomposition", 《J. MATER. CHEM. A》 * |
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