CN104525202A - Preparation method of alpha-Fe2O3 mesoporous nanorod/nitrogen-doped graphene composite - Google Patents
Preparation method of alpha-Fe2O3 mesoporous nanorod/nitrogen-doped graphene composite Download PDFInfo
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- CN104525202A CN104525202A CN201510036209.8A CN201510036209A CN104525202A CN 104525202 A CN104525202 A CN 104525202A CN 201510036209 A CN201510036209 A CN 201510036209A CN 104525202 A CN104525202 A CN 104525202A
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Abstract
The invention discloses a preparation method of an alpha-Fe2O3 mesoporous nanorod/nitrogen-doped graphene composite and relates to a preparation method of an alpha-Fe2O3/graphene composite, aiming at solving the problem that the in-situ growth of an alpha-Fe2O3 mesoporous nanorod in nitrogen-doped graphene cannot be achieved and meanwhile the uniformity property of the alpha-Fe2O3 mesoporous nanorod cannot be guaranteed at present. The preparation method comprises the following steps: I. adding an alkali source and an inorganic iron solution to a pore forming agent water solution; II. adding graphene oxide to the mixed liquid of the step I, ultrasonically treating and stirring; and III. pouring a suspension obtained from the step II to a hydrothermal reaction kettle and reacting, cooling, centrifuging, washing and drying. The preparation method has the advantages that the composite functional material disclosed by the invention is high in removal rate on sulfamethoxazole, and the average grain size of the alpha-Fe2O3 mesoporous nanorod is just 4-10nm; and the preparation method is mild in reaction condition, simple in equipment, low in reagent cost, safe and non-toxic and suitable for large-scale production.
Description
Technical field
The present invention relates to a kind of α-Fe
2o
3the preparation method of/graphene composite material.
Background technology
α-Fe
2o
3as the n-type semiconductor that a kind of physics, chemical stability are good, there is suitable band gap width (2.0 ~ 2.2eV), compared with Strong oxdiative ability, higher electric capacity (~ 1000mAhg
-1), the plurality of advantages such as cheap, safety non-toxic, be widely used in the numerous areas such as photocatalysis, battery electrode material.Graphene, as a kind of novel two-dimension nano materials, because of the monoatomic layer crystal structure of its uniqueness, and has physico-chemical property (the high carrier mobility speed 2 × 10 of many excellences
5cmV
-1s
-1, superelevation specific area 2630m
2/ g etc.), and cause the extensive concern in the fields such as physics, chemistry, material.In recent years, round α-Fe
2o
3the preparation of/Graphene composite functional material, researcher expands large quantifier elimination, successfully prepares many α-Fe
2o
3/ graphene composite material, and be widely used in the numerous areas such as photocatalytic water, lithium ion battery, desalinization.But still there is following problem in above-mentioned preparation method: (1) growth in situ α-Fe on graphene film
2o
3be all compacting body, lack the loose structure being conducive to chemical reaction and material mass transfer; (2) α-Fe in prepared composite
2o
3and non-homogeneous dispersion, reunite comparatively serious.
Recently, researcher finds, introduces heteroatom (such as nitrogen, phosphorus, boron etc.), can not only improve the photoelectrochemical behaviour of Graphene further, can also strengthen α-Fe in the lattice of Graphene
2o
3with the synergy of Graphene.Therefore, by α-Fe
2o
3meso-porous nano rod is organically combined with nitrogen-doped graphene, greatly will improve the physical and chemical performance of composite.But, how to allow α-Fe
2o
3while meso-porous nano rod original position is born in nitrogen-doped graphene, and guaranteeing its uniform characteristic, is preparation high-performance high stability α-Fe
2o
3the key of meso-porous nano rod/nitrogen-doped graphene composite functional material.
Summary of the invention
The present invention cannot allow α-Fe at present in order to solve
2o
3meso-porous nano rod growth in situ guarantees α-Fe while nitrogen-doped graphene
2o
3the technical problem of meso-porous nano rod uniform properties, and a kind of α-Fe is provided
2o
3the preparation method of meso-porous nano rod/nitrogen-doped graphene composite.
A kind of α-Fe of the present invention
2o
3the preparation method of meso-porous nano rod/nitrogen-doped graphene composite carries out according to the following steps:
One, join in deionized water by pore creating material, mix and blend 3min ~ 10min, obtains organic solution; The aqueous solution of alkali source and inorganic iron is joined in organic solution successively, stirs 5min ~ 10min, form uniform transparent mixed liquor; The quality of described pore creating material and the volume ratio of deionized water are 1g:(3.33mL ~ 30mL); Described alkali source and the mass ratio of pore creating material are 1:(3.33 ~ 30); The concentration of the aqueous solution of described inorganic iron is 0.05mol/L ~ 0.5mol/L; The volume of the aqueous solution of described inorganic iron and the mass ratio of pore creating material are 1mL:(0.2g ~ 1.8g);
Two, joined by graphene oxide in the uniform transparent mixed liquor that step one obtains, ultrasonic 0.3h ~ 2h, then stirs 2h ~ 4h, obtains stable suspension; The mass ratio of described graphene oxide and the pore creating material described in step one is 1:(28.6 ~ 257.1);
Three, after stable suspension step 2 obtained pours hydrothermal reaction kettle into, be react 5h ~ 36h under the condition of 100 DEG C ~ 200 DEG C in temperature, naturally cool to room temperature, carry out centrifugal, then spend deionized water 3 times, 2 times are washed again with ethanol, finally dry 12h under temperature is the condition of 50 DEG C, obtains α-Fe
2o
3meso-porous nano rod/nitrogen-doped graphene composite.
Graphene oxide in step 2 of the present invention is standby by traditional Hummers legal system.
Principle of the present invention:
In the present invention, iron ion is due to electrostatic interaction, can be adsorbed on the graphenic surface of N doping, nucleating growth; In addition, because pore creating material contains multiple hydroxyl, it can effectively be adsorbed on α-Fe
2o
3nanocrystalline surface; In course of reaction, because the pore-creating dosage added is very low, α-Fe cannot be covered in completely
2o
3nanocrystalline, can not effectively stop nanocrystalline reunion; Therefore, along with the carrying out of hydro-thermal reaction, α-Fe
2o
3nanocrystalline along one-dimensional square to assembling, and then define nanometer rods; Then adopt ethanol/deionized water, as extractant, by the pore creating material eccysis in nanometer rods, thus define mesoporous, finally obtain α-Fe
2o
3meso-porous nano rod/nitrogen-doped graphene composite.
α-Fe prepared by the present invention
2o
3meso-porous nano rod/nitrogen-doped graphene composite and zero-dimension nano Particle Phase ratio, monodimension nano stick can transmit photogenerated charge efficiently, and then the recombination probability of photogenerated charge is declined, and is conducive to the lifting of photocatalytic activity; Due to α-Fe
2o
3nanometer rods has meso-hole structure, which not only improves α-Fe
2o
3to incident light utilization rate, also substantially reduce the radial distance that photo-generated carrier arrives material surface simultaneously, be conducive to follow-up oxidative degradation, simultaneously this meso-hole structure, also help the mass transport process of chemical reaction, therefore can improve chemical reaction efficiency.
Advantage of the present invention:
One, the α-Fe for preparing of the present invention
2o
3meso-porous nano rod/nitrogen-doped graphene composite functional material, wherein α-Fe
2o
3the average grain diameter of meso-porous nano rod is only 4 ~ 10nm;
Two, the reaction condition of the inventive method is gentle, and the consersion unit adopted is simple, and required reagent is cheap, and safety non-toxic, be conducive to large-scale production;
Three, the α-Fe prepared by the present invention
2o
3the active Fe apparently higher than business of light Fenton of meso-porous nano rod/nitrogen-doped graphene composite
2o
3, to the clearance of Sulfamethoxazole up to 99.5%.
Accompanying drawing explanation
Fig. 1 is that α-Fe is prepared in test one
2o
3the transmission electron microscope picture of meso-porous nano rod/nitrogen-doped graphene composite;
Fig. 2 is α-Fe prepared by test one
2o
3the transmission electron microscope picture of meso-porous nano rod/nitrogen-doped graphene composite;
Fig. 3 is α-Fe prepared by test one
2o
3the x-ray photoelectron spectroscopy figure of meso-porous nano rod/nitrogen-doped graphene composite, peak 1 is the 3p track absworption peak of Fe, and peak 2 is the 1s track absworption peak of C, peak 3 is the 1s track absworption peak of N, peak 4 is the 1s track absworption peak of O, and peak 5 is the 2p track absworption peak of Fe, and peak 6 is the 2s track absworption peak of Fe;
Fig. 4 is the design sketch of Sulfamethoxazole in neutral light Fenton degradation water, and curve 1 is the effect curve of test five, and curve 2 is the effect curve of test four, and curve 3 is the effect curve of test three, and curve 4 is the effect curve of test two.
Detailed description of the invention
Detailed description of the invention one: present embodiment is a kind of α-Fe
2o
3the preparation method of meso-porous nano rod/nitrogen-doped graphene composite, specifically carries out according to the following steps:
One, join in deionized water by pore creating material, mix and blend 3min ~ 10min, obtains organic solution; The aqueous solution of alkali source and inorganic iron is joined in organic solution successively, stirs 5min ~ 10min, form uniform transparent mixed liquor; The quality of described pore creating material and the volume ratio of deionized water are 1g:(3.33mL ~ 30mL); Described alkali source and the mass ratio of pore creating material are 1:(3.33 ~ 30); The concentration of the aqueous solution of described inorganic iron is 0.05mol/L ~ 0.5mol/L; The volume of the aqueous solution of described inorganic iron and the mass ratio of pore creating material are 1mL:(0.2g ~ 1.8g);
Two, joined by graphene oxide in the uniform transparent mixed liquor that step one obtains, ultrasonic 0.3h ~ 2h, then stirs 2h ~ 4h, obtains stable suspension; The mass ratio of described graphene oxide and the pore creating material described in step one is 1:(28.6 ~ 257.1);
Three, after stable suspension step 2 obtained pours hydrothermal reaction kettle into, be react 5h ~ 36h under the condition of 100 DEG C ~ 200 DEG C in temperature, naturally cool to room temperature, carry out centrifugal, then spend deionized water 3 times, 2 times are washed again with ethanol, finally dry 12h under temperature is the condition of 50 DEG C, obtains α-Fe
2o
3meso-porous nano rod/nitrogen-doped graphene composite.
The principle of present embodiment:
In present embodiment, iron ion is due to electrostatic interaction, can be adsorbed on the graphenic surface of N doping, nucleating growth; In addition, because pore creating material contains multiple hydroxyl, it can effectively be adsorbed on α-Fe
2o
3nanocrystalline surface; In course of reaction, because the pore-creating dosage added is very low, α-Fe cannot be covered in completely
2o
3nanocrystalline, can not effectively stop nanocrystalline reunion; Therefore, along with the carrying out of hydro-thermal reaction, α-Fe
2o
3nanocrystalline along one-dimensional square to assembling, and then define nanometer rods; Then adopt ethanol/deionized water, as extractant, by the pore creating material eccysis in nanometer rods, thus define mesoporous, finally obtain α-Fe
2o
3meso-porous nano rod/nitrogen-doped graphene composite.
α-Fe prepared by present embodiment
2o
3meso-porous nano rod/nitrogen-doped graphene composite and zero-dimension nano Particle Phase ratio, monodimension nano stick can transmit photogenerated charge efficiently, and then the recombination probability of photogenerated charge is declined, and is conducive to the lifting of photocatalytic activity; Due to α-Fe
2o
3nanometer rods has meso-hole structure, which not only improves α-Fe
2o
3to incident light utilization rate, also substantially reduce the radial distance that photo-generated carrier arrives material surface simultaneously, be conducive to follow-up oxidative degradation, simultaneously this meso-hole structure, also help the mass transport process of chemical reaction, therefore can improve chemical reaction efficiency.
Present embodiment advantage:
One, the α-Fe for preparing of present embodiment
2o
3meso-porous nano rod/nitrogen-doped graphene composite functional material, wherein α-Fe
2o
3the average grain diameter of meso-porous nano rod is only 4 ~ 10nm;
Two, the reaction condition of present embodiment method is gentle, and the consersion unit adopted is simple, and required reagent is cheap, and safety non-toxic, be conducive to large-scale production;
Three, the α-Fe prepared by present embodiment
2o
3the active Fe apparently higher than business of light Fenton of meso-porous nano rod/nitrogen-doped graphene composite
2o
3, to the clearance of Sulfamethoxazole up to 99.5%.
Detailed description of the invention two: present embodiment and detailed description of the invention one unlike: the pore creating material described in step one is glycerine, sucrose, glucose or hydroxylated cellulose.Other is identical with detailed description of the invention one.
Detailed description of the invention three: one of present embodiment and detailed description of the invention one to two unlike: the alkali source described in step one is urea, ammoniacal liquor or ammonium acetate.Other is identical with one of detailed description of the invention one to two.
Detailed description of the invention four: one of present embodiment and detailed description of the invention one to three unlike: the inorganic iron described in step one is ferric trichloride, ferrous chloride, ferrous sulfate or ferric nitrate.Other is identical with one of detailed description of the invention one to three.
Detailed description of the invention five: one of present embodiment and detailed description of the invention one to four unlike: the mass ratio of the described alkali source described in step one and pore creating material is 1:(10 ~ 20).Other is identical with one of detailed description of the invention one to four.
Detailed description of the invention six: one of present embodiment and detailed description of the invention one to five unlike: the volume of the aqueous solution of the described inorganic iron described in step one and the mass ratio of pore creating material are 1mL:(0.6g ~ 1.5g).Other is identical with one of detailed description of the invention one to five.
Detailed description of the invention seven: one of present embodiment and detailed description of the invention one to six are 1:(50 ~ 150 unlike the mass ratio of the pore creating material described in: the graphene oxide described in step 2 and step one).Other is identical with one of detailed description of the invention one to six.
Detailed description of the invention eight: one of present embodiment and detailed description of the invention one to seven unlike: after stable suspension step 2 obtained described in step 3 pours hydrothermal reaction kettle into, be react 24h under the condition of 150 DEG C in temperature, naturally cool to room temperature.Other is identical with one of detailed description of the invention one to seven.
Adopt following verification experimental verification effect of the present invention:
Test one: this test is a kind of α-Fe
2o
3the preparation method of meso-porous nano rod/nitrogen-doped graphene composite, specifically carries out according to the following steps:
One, join in deionized water by pore creating material, mix and blend 3min, obtains organic solution; The aqueous solution of alkali source and inorganic iron is joined in organic solution successively, stirs 5min, form uniform transparent mixed liquor; The quality of described pore creating material and the volume ratio of deionized water are 1g:6mL; Described alkali source and the mass ratio of pore creating material are 1:16.67; The concentration of the aqueous solution of described inorganic iron is 0.2mol/L; The volume of the aqueous solution of described inorganic iron and the mass ratio of pore creating material are 1mL:1g;
Two, joined by graphene oxide in the uniform transparent mixed liquor that step one obtains, ultrasonic 1h, then stirs 2h, obtains stable suspension; The mass ratio of described graphene oxide and the pore creating material described in step one is 1:142.9;
Three, after stable suspension step 2 obtained pours hydrothermal reaction kettle into, be react 24h under the condition of 150 DEG C in temperature, naturally cool to room temperature, carry out centrifugal, then spend deionized water 3 times, 2 times are washed again with ethanol, finally dry 12h under temperature is the condition of 50 DEG C, obtains α-Fe
2o
3meso-porous nano rod/nitrogen-doped graphene composite.
Pore creating material described in step one is glycerine; Alkali source described in step one is urea; Inorganic iron described in step one is ferric trichloride.
Fig. 1 is α-Fe prepared by test one
2o
3the transmission electron microscope picture of meso-porous nano rod/nitrogen-doped graphene composite, Fig. 2 is α-Fe prepared by test one
2o
3the transmission electron microscope picture of meso-porous nano rod/nitrogen-doped graphene composite, as shown in Figure 1, the α-Fe of this test preparation
2o
3meso-porous nano rod/nitrogen-doped graphene composites pattern is two-dimensional sheet structure, α-Fe
2o
3what meso-porous nano rod was even and intensive is dispersed on nitrogen-doped graphene; As shown in Figure 2, the hyperfine α-Fe of this test preparation
2o
3meso-porous nano rod length is in the scope of 30 ~ 70nm, and average aspect ratio is 4.5, and its mesopore size is 4 ~ 10nm.。
Fig. 3 is α-Fe prepared by test one
2o
3the x-ray photoelectron spectroscopy figure of meso-porous nano rod/nitrogen-doped graphene composite, peak 1 is the 3p track absworption peak of Fe, peak 2 is the 1s track absworption peak of C, peak 3 is the 1s track absworption peak of N, peak 4 is the 1s track absworption peak of O, and peak 5 is the 2p track absworption peak of Fe, and peak 6 is the 2s track absworption peak of Fe, this collection of illustrative plates obviously can find the absworption peak of C, O, N and Fe element, illustrate that composite prepared by test one is α-Fe
2o
3meso-porous nano rod/nitrogen-doped graphene composite.
Test two: this test is the effect test of rhodamine B in light Fenton degradation water:
The light source that this test adopts is the xenon lamp of 300W, and configures the edge filter of 400nm, and concrete steps are: by the aqueous solution of 50mL Sulfamethoxazole at (C
0=30mg/L) dark place stirs after 30min, and the pH of solution is adjusted to 3.0 by NaOH or the HCl solution then adopted, and opens xenon lamp, carries out photochemical reaction, and in test solution, the concentration of Sulfamethoxazole is along with the change in reaction time.
Test three: this test is the effect test of rhodamine B in light Fenton degradation water:
The light source that this test adopts is the xenon lamp of 300W, and configures the edge filter of 400nm, and concrete steps are: by the aqueous solution of 50mL Sulfamethoxazole at (C
0=30mg/L) dark place stirs after 30min, and the pH of solution is adjusted to 3.0 by NaOH or the HCl solution then adopted, then adds the H that 0.5mL mass concentration is 3%
2o
2the aqueous solution, opens xenon lamp, carries out photochemical reaction, and in test solution, the concentration of Sulfamethoxazole is along with the change in reaction time.
Test four: this test is the effect test of rhodamine B in light Fenton degradation water:
The light source that this test adopts is the xenon lamp of 300W, and configures the edge filter of 400nm, and concrete steps are: by 10mg business Fe
2o
3join the aqueous solution (C of 50mL Sulfamethoxazole
0=30mg/L) in, after in the dark stirring 30min, the pH of solution is adjusted to 3.0 by NaOH or the HCl solution then adopted, then adds the H that 0.5mL mass concentration is 3%
2o
2the aqueous solution, opens xenon lamp, carries out photochemical reaction, and in test solution, the concentration of Sulfamethoxazole is along with the change in reaction time.
Test five: this test is the effect test of rhodamine B in light Fenton degradation water:
The light source that this test adopts is the xenon lamp of 300W, and configures the edge filter of 400nm, and concrete steps are: by the α-Fe of 10mg test one preparation
2o
3meso-porous nano rod/nitrogen-doped graphene composite joins the aqueous solution (C of 50mL Sulfamethoxazole
0=30mg/L) in, after in the dark stirring 30min, the pH of solution is adjusted to 3.0 by NaOH or the HCl solution then adopted, then adds the H that 0.5mL mass concentration is 3%
2o
2the aqueous solution, opens xenon lamp, carries out photochemical reaction, and in test solution, the concentration of Sulfamethoxazole is along with the change in reaction time.
Fig. 4 is the design sketch of Sulfamethoxazole in neutral light Fenton degradation water, curve 1 is the effect curve of test five, and curve 2 is the effect curve of test four, and curve 3 is the effect curve of test three, curve 4 is the effect curve of test two, tests the α-Fe of a preparation as seen from Figure 4
2o
3meso-porous nano rod/nitrogen-doped graphene composite is as the active Fe apparently higher than business of heterogeneous fenton catalyst time Fenton
2o
3with independent hydrogen peroxide 15%, the clearance of its Sulfamethoxazole is up to 99.5%.
Claims (8)
1. a α-Fe
2o
3the preparation method of meso-porous nano rod/nitrogen-doped graphene composite, is characterized in that α-Fe
2o
3the preparation method of meso-porous nano rod/nitrogen-doped graphene composite carries out according to the following steps:
One, join in deionized water by pore creating material, mix and blend 3min ~ 10min, obtains organic solution; The aqueous solution of alkali source and inorganic iron is joined in organic solution successively, stirs 5min ~ 10min, form uniform transparent mixed liquor; The quality of described pore creating material and the volume ratio of deionized water are 1g:(3.33mL ~ 30mL); Described alkali source and the mass ratio of pore creating material are 1:(3.33 ~ 30); The concentration of the aqueous solution of described inorganic iron is 0.05mol/L ~ 0.5mol/L; The volume of the aqueous solution of described inorganic iron and the mass ratio of pore creating material are 1mL:(0.2g ~ 1.8g);
Two, joined by graphene oxide in the uniform transparent mixed liquor that step one obtains, ultrasonic 0.3h ~ 2h, then stirs 2h ~ 4h, obtains stable suspension; The mass ratio of described graphene oxide and the pore creating material described in step one is 1:(28.6 ~ 257.1);
Three, after stable suspension step 2 obtained pours hydrothermal reaction kettle into, be react 5h ~ 36h under the condition of 100 DEG C ~ 200 DEG C in temperature, naturally cool to room temperature, carry out centrifugal, then spend deionized water 3 times, 2 times are washed again with ethanol, finally dry 12h under temperature is the condition of 50 DEG C, obtains α-Fe
2o
3meso-porous nano rod/nitrogen-doped graphene composite.
2. a kind of α-Fe according to claim 1
2o
3the preparation method of meso-porous nano rod/nitrogen-doped graphene composite, is characterized in that the pore creating material described in step one is glycerine, sucrose, glucose or hydroxylated cellulose.
3. a kind of α-Fe according to claim 1
2o
3the preparation method of meso-porous nano rod/nitrogen-doped graphene composite, is characterized in that the alkali source described in step one is urea, ammoniacal liquor or ammonium acetate.
4. a kind of α-Fe according to claim 1
2o
3the preparation method of meso-porous nano rod/nitrogen-doped graphene composite, is characterized in that the inorganic iron described in step one is ferric trichloride, ferrous chloride, ferrous sulfate or ferric nitrate.
5. a kind of α-Fe according to claim 1
2o
3the preparation method of meso-porous nano rod/nitrogen-doped graphene composite, is characterized in that the mass ratio of the alkali source described in step one and pore creating material is 1:(10 ~ 20).
6. a kind of α-Fe according to claim 1
2o
3the preparation method of meso-porous nano rod/nitrogen-doped graphene composite, is characterized in that the volume of the aqueous solution of the inorganic iron described in step one and the mass ratio of pore creating material are 1mL:(0.6g ~ 1.5g).
7. a kind of α-Fe according to claim 1
2o
3the preparation method of meso-porous nano rod/nitrogen-doped graphene composite, is characterized in that the mass ratio of the pore creating material described in the graphene oxide described in step 2 and step one is 1:(50 ~ 150).
8. a kind of α-Fe according to claim 1
2o
3the preparation method of meso-porous nano rod/nitrogen-doped graphene composite, after it is characterized in that stable suspension step 2 obtained described in step 3 pours hydrothermal reaction kettle into, is react 24h under the condition of 150 DEG C in temperature, naturally cools to room temperature.
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| CN111073850A (en) * | 2020-03-24 | 2020-04-28 | 朗姿赛尔生物科技（广州）有限公司 | Culture medium for promoting mesenchymal stem cell differentiation |
| CN111073850B (en) * | 2020-03-24 | 2020-09-01 | 朗姿赛尔生物科技（广州）有限公司 | Culture medium for promoting mesenchymal stem cell differentiation |
| CN115739151A (en) * | 2022-11-04 | 2023-03-07 | 山西大学 | Preparation and application of nitrogen-doped graphene-supported magnetic nanoparticle material |
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