CN103112894A - Bismuth trioxide nanotubes prepared by microwave-assisted liquid-phase process and application thereof - Google Patents
Bismuth trioxide nanotubes prepared by microwave-assisted liquid-phase process and application thereof Download PDFInfo
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Abstract
The invention relates to a method for preparing bismuth trioxide (Bi2O3) nanotubes by a microwave-assisted liquid-phase process and application of the bismuth trioxide (Bi2O3) nanotubes in photodegradating tetracycline-containing wastewater. The preparation method comprises the following steps: magnetically stirring proper amounts of Bi(NO3)3.5H2O and Na2SO4 to form a mixed solution, carrying out ultrasonic dispersion on NaOH and deionized water to form a sodium hydroxide transparent solution, and dropwisely adding the sodium hydroxide transparent solution into the Bi(NO3)3.5H2O/Na2SO4 mixed solution; and continuously heating in a reactor with the microwave power of 800W to obtain the product, centrifuging, washing and drying to obtain the bismuth trioxide (Bi2O3) nanotubes with uniform appearance. The invention has the advantages of simple technique and reproducibility; and the raw materials are cheap and accessible inorganic compounds, are low in cost, do not need pretreatment of high temperature and calcining, and have the advantages of low synthesis temperature and short reaction time, thereby lowering the energy consumption and reaction cost and facilitating the mass production. Since the bismuth trioxide (Bi2O3) has strong photocatalytic degradation capacity for tetracycline, the invention is feasible in practical application.
Description
Technical field
The invention belongs to inorganic nano material and environmentally conscious materials preparing technical field, relate to bismuthous oxide bismuth trioxide nanotube preparation method, relate in particular to a kind of microwave-assisted Liquid preparation methods bismuthous oxide bismuth trioxide nanotube and application thereof.
Background technology
In recent decades, the based semiconductor photocatalysis degradation organic contaminant for many existence and potential environmental problem provide feasible solution, has now become one of focus of people's research.What use was more at present is that catalytic activity is high, good stability and nontoxic titanium dioxide; But because of its greater band gap (3.2eV), can only absorb the UV-light that only accounts for sun power 4%, therefore its catalytic performance remains further to be improved, how to utilize the visible light part degradable organic pollutant of sun power, namely have the catalyzer of higher catalytic activity under visible light, become one of focus in the photochemical catalysis research field.
With the bismuth based compound of bismuthous oxide bismuth trioxide as matrix, owing to having multiple crystalline state, performance is abundant, becomes the focus that people pay close attention to.Bismuthous oxide bismuth trioxide is as one of most important bismuth based compound, its light absorbing ability is stronger, has well visible light-responded photocatalysis characteristic, and simultaneous oxidation is very capable, the oxidation organic pollutant, therefore have very strong environmental applications ability and form the emphasis of studying into people effectively.
The band-gap energy of bismuthous oxide bismuth trioxide is 2.8eV, and its absorbing wavelength is longer, can realize the utilization to sunlight.Bismuthous oxide bismuth trioxide has all shown performance and application potential preferably as a kind of advanced person's the application of function powder material at aspects such as electronic ceramics powder body material, electrolyte, photoelectric material, high temperature superconducting materia, catalystic materials.Have been reported the experimental study that contains nitrite waste water, sulphite waste water and dyeing waste water with the bismuthous oxide bismuth trioxide photocatalysis treatment, but on the processing tetracycline wastewater, report is not arranged at present.
At present tetracycline antibiotic use and abuse makes most microbiotic fully absorb without animal or human's body, directly excrete and enter water body, environmental system is caused have a strong impact on, be deemed to be the little Organic Pollutants of a kind of typical environment.The removal of the antibiotic substance take tsiklomitsin as representative had become a scientific research difficult problem that needs to be resolved hurrily already.
Summary of the invention
One object of the present invention is, provides a kind of technique simple, the microwave-assisted Liquid preparation methods bismuthous oxide bismuth trioxide (Bi that synthesis temperature is lower, the reaction times is shorter
2O
3) method of nanotube.
Another object of the present invention is to provide prepared bismuthous oxide bismuth trioxide (Bi
2O
3) nanotube is to containing the photodegradative application of tetracycline wastewater.
In order to realize above-mentioned task, the present invention takes following technical solution:
A kind of microwave-assisted Liquid preparation methods bismuthous oxide bismuth trioxide (Bi
2O
3) method of nanotube, it is characterized in that, carry out according to following step:
A) take the Bi (NO of 0.95g～1.00g
3)
35H
2The Na of O and 0.45g～0.50g
2SO
4, to dissolve in the 40mL deionized water, ultrasonic and use magnetic agitation formed mixing solutions in 1 hour;
B) take 0.70g～0.75g NaOH, add the 40mL deionized water, ultrasonic its Uniform Dispersion that makes forms the sodium hydroxide clear solution;
C) with the sodium hydroxide clear solution of step B gained, dropwise join under magnetic agitation in the mixing solutions of steps A gained;
D) solution of step C gained is transferred in the container of quartz that capacity is 100mL, is placed in the reactor that microwave power is 800W, be warming up to 80 ℃～100 ℃, continue 10min～20min, naturally cooling is collected product;
E) with the product centrifugation of step D gained, wash respectively three times with deionized water and dehydrated alcohol;
F) with the centrifugal product of step e gained at 80 ℃ of air drying 12h, namely obtain the bismuthous oxide bismuth trioxide (Bi of pattern homogeneous
2O
3) nanotube.
Bi (NO in above-mentioned steps A
3)
35H
2O, Na
2SO
4Be analytical pure with NaOH.
Bismuthous oxide bismuth trioxide (the Bi of method preparation of the present invention
2O
3) nanotube, its structure is determined there is no the peak of other materials in x-ray diffraction pattern by x-ray diffractometer, this collection of illustrative plates shows, by the prepared bismuthous oxide bismuth trioxide (Bi of microwave assisting method
2O
3) be pure phase bismuthous oxide bismuth trioxide (Bi
2O
3), itself and standard bismuthous oxide bismuth trioxide (Bi
2O
3) card (41-1449) matches.
Field emission scanning electron microscope (SEM) is tested and is shown, at room temperature, and by the bismuthous oxide bismuth trioxide (Bi of microwave assisting method preparation
2O
3) nanotube length is about 20 μ m～40 μ m, thickness of pipe is about 300nm.
Bismuthous oxide bismuth trioxide (the Bi of applicant to obtaining
2O
3) valence state of element of nanotube analyzes, 163.7eV, 158.34eV these two strong peaks are correspondences and Bi respectively
2O
3In Bi4f5/2 and Bi4f7/2,530.93eV is corresponding to Bi
2O
3In O1s, near and the not appearance of other small peak main peak shows that there is not oxidized phenomenon on the surface of product.Therefore bismuthous oxide bismuth trioxide (the Bi for preparing by the present invention
2O
3) nanotube is more stable.
Bismuthous oxide bismuth trioxide (Bi obtained above
2O
3) nanotube, can be used in containing the photodegradative application of tetracycline wastewater through experiment showed, of applicant, as follows to the degradation experiment of tsiklomitsin under the xenon source irradiation:
Photocatalytic activity is estimated: carry out in GHX-2 type photochemical reaction instrument (available from Science and Technology City Science and Technology Ltd. of Yangzhou University), be that 10mg/L tsiklomitsin simulated wastewater 100mL adds in photochemical catalysis instrument reactor with concentration, then add the bismuthous oxide bismuth trioxide (Bi of this microwave-assisted reaction
2O
3) photocatalyst 0.1g, use magnetic stirring apparatus reaction 30 minutes in the darkroom, begin sampling after reaching the reaction adsorption equilibrium, then open aerating apparatus and open xenon source, it is to keep catalyzer to be in to suspend or afloat that aeration passes into the air purpose, at interval of the 10min sampling, gets supernatant liquid after centrifugation at tsiklomitsin maximum absorption wavelength λ max=357nm place in the Xenon light shining process, use TU-1800 ultraviolet-visible pectrophotometer place working sample absorbancy, and pass through formula: DC=[(A
O-A
i)/A
O] * 100% is calculated photodegradation rate, wherein A
OThe absorbancy of tetracycline when reaching adsorption equilibrium, A
iThe absorbancy of the tetracycline of measuring for timing sampling.
Bismuthous oxide bismuth trioxide (the Bi that the present invention is prepared
2O
3) nanotube, when xenon lamp shines, the degradation rate that contains tetracycline wastewater is reached 83.64% when the 60min.
The present invention adopts liquid phase method under low temperature to prepare the bismuthous oxide bismuth trioxide (Bi of the relative homogeneous of pattern through the microwave-assisted reaction
2O
3) nanotube, have the advantages such as chemical stability is good, nontoxic.Its technique is simple, favorable reproducibility, and raw materials is mineral compound, and is cheap and easy to get, and cost is low, meet the environmental friendliness requirement, do not need the pre-treatment of high temperature, calcining and so on due to the method, synthesis temperature is lower, and the reaction times is shorter, thereby reduced energy consumption and reaction cost, be convenient to batch production.Simultaneously due to bismuthous oxide bismuth trioxide (Bi
2O
3) tsiklomitsin is had stronger photocatalytic degradation ability, also have feasibility in practical application.
Description of drawings
Fig. 1 is bismuthous oxide bismuth trioxide (Bi
2O
3) the X-ray diffraction analysis figure (XRD) of nanotube.
Fig. 2 is bismuthous oxide bismuth trioxide (Bi
2O
3) scanning electron microscope (SEM) photograph (SEM) of nanotube.
Fig. 3 is bismuthous oxide bismuth trioxide (Bi
2O
3) nanotube XPS collection of illustrative plates at room temperature.
Fig. 4 is bismuthous oxide bismuth trioxide (Bi
2O
3) the photodegradation figure of nanotube.
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Embodiment
Following embodiment is better example, so that those skilled in the art understand the present invention better, but the present invention is not limited to following examples.
Embodiment 1:
The present embodiment provides a kind of microwave-assisted Liquid preparation methods bismuthous oxide bismuth trioxide (Bi
2O
3) method of nanotube, carry out according to following step:
A, take the Bi (NO of 0.95g
3)
35H
2The Na of O and 0.45g
2SO
4, to dissolve in the 40mL deionized water, ultrasonic and use magnetic agitation formed mixing solutions in 1 hour;
B, take the NaOH of 0.70g, add the 40mL deionized water, ultrasonic its Uniform Dispersion that makes forms the sodium hydroxide clear solution;
C, with the sodium hydroxide clear solution of step B gained, dropwise join under magnetic agitation in the mixing solutions of steps A gained;
D, the solution of step C gained is transferred in the container of quartz that capacity is 100mL, is placed in microwave reactor, microwave power is 800W, is warming up to 80 ℃, continues 10min, and naturally cooling is collected product;
E, with the product centrifugation of step D gained, wash respectively three times with deionized water and dehydrated alcohol;
F, with the centrifugal product of step e gained at 80 ℃ of air drying 12h, namely obtain the bismuthous oxide bismuth trioxide (Bi of pattern homogeneous
2O
3) nanotube.
Embodiment 2:
The present embodiment provides a kind of microwave-assisted Liquid preparation methods bismuthous oxide bismuth trioxide (Bi
2O
3) method of nanotube, carry out according to following step:
A, take the Bi (NO of 1.00g
3)
35H
2The Na of O and 0.50g
2SO
4, to dissolve in the 40mL deionized water, ultrasonic and use magnetic agitation formed mixing solutions in 1 hour;
B, take the NaOH of 0.75g, add the 40mL deionized water, ultrasonic its Uniform Dispersion that makes forms the sodium hydroxide clear solution;
C, with the sodium hydroxide clear solution of step B gained, dropwise join under magnetic agitation in the mixing solutions of steps A gained;
D, the solution of step C gained is transferred in the container of quartz that capacity is 100mL, is placed in microwave reactor, microwave power is 800W, is warming up to 100 ℃, continues 20min, and naturally cooling is collected product;
E, with the product centrifugation of step D gained, wash respectively three times with deionized water and dehydrated alcohol;
F, with the centrifugal product of step e gained at 80 ℃ of air drying 12h, namely obtain the bismuthous oxide bismuth trioxide (Bi of pattern homogeneous
2O
3) nanotube.
Embodiment 3:
The present embodiment provides a kind of microwave-assisted Liquid preparation methods bismuthous oxide bismuth trioxide (Bi
2O
3) method of nanotube, carry out according to following step:
A, take the Bi (NO of 0.95g
3)
35H
2The Na of O and 0.45g
2SO
4, to dissolve in the 40mL deionized water, ultrasonic and use magnetic agitation formed mixing solutions in 1 hour;
B, take the NaOH of 0.75g, add the 40mL deionized water, ultrasonic its Uniform Dispersion that makes forms the sodium hydroxide clear solution;
C, with the sodium hydroxide clear solution of step B gained, dropwise join under magnetic agitation in the mixing solutions of steps A gained;
D, the solution of step C gained is transferred in the container of quartz that capacity is 100mL, is placed in microwave reactor, microwave power is 800W, is warming up to 100 ℃, continues 20min, and naturally cooling is collected product;
E, with the product centrifugation of step D gained, wash respectively three times with deionized water and dehydrated alcohol;
F, with the centrifugal product of step e gained at 80 ℃ of air drying 12h, namely obtain the bismuthous oxide bismuth trioxide (Bi of pattern homogeneous
2O
3) nanotube.
Embodiment 4:
The present embodiment provides a kind of microwave-assisted Liquid preparation methods bismuthous oxide bismuth trioxide (Bi
2O
3) method of nanotube, carry out according to following step:
A, take the Bi (NO of 1.00g
3)
35H
2The Na of O and 0.50g
2SO
4, to dissolve in the 40mL deionized water, ultrasonic and use magnetic agitation formed mixing solutions in 1 hour;
B, take the NaOH of 0.75g, add the 40mL deionized water, ultrasonic its Uniform Dispersion that makes forms the sodium hydroxide clear solution;
C, with the sodium hydroxide clear solution of step B gained, dropwise join under magnetic agitation in the mixing solutions of steps A gained;
D, the solution of step C gained is transferred in the container of quartz that capacity is 100mL, is placed in microwave reactor, microwave power is 800W, is warming up to 80 ℃, continues 10min, and naturally cooling is collected product;
E, with the product centrifugation of step D gained, wash respectively three times with deionized water and dehydrated alcohol;
F, with the centrifugal product of step e gained at 80 ℃ of air drying 12h, namely obtain the bismuthous oxide bismuth trioxide (Bi of pattern homogeneous
2O
3) nanotube.
Embodiment 5:
The present embodiment provides a kind of microwave-assisted Liquid preparation methods bismuthous oxide bismuth trioxide (Bi
2O
3) method of nanotube, carry out according to following step:
A, take the Bi (NO of 0.97g
3)
35H
2The Na of O and 0.48g
2SO
4, to dissolve in the 40mL deionized water, ultrasonic and use magnetic agitation formed mixing solutions in 1 hour;
B, take the NaOH of 0.73g, add the 40mL deionized water, ultrasonic its Uniform Dispersion that makes forms the sodium hydroxide clear solution;
C, with the sodium hydroxide clear solution of step B gained, dropwise join under magnetic agitation in the mixing solutions of steps A gained;
D, the solution of step C gained is transferred in the container of quartz that capacity is 100mL, is placed in microwave reactor, microwave power is 800W, is warming up to 90 ℃, continues 15min, and naturally cooling is collected product;
E, with the product centrifugation of step D gained, wash respectively three times with deionized water and dehydrated alcohol;
F, with the centrifugal product of step e gained at 80 ℃ of air drying 12h, namely obtain the bismuthous oxide bismuth trioxide (Bi of pattern homogeneous
2O
3) nanotube.
Embodiment 6:
The present embodiment provides a kind of microwave-assisted Liquid preparation methods bismuthous oxide bismuth trioxide (Bi
2O
3) method of nanotube, carry out according to following step:
A, take the Bi (NO of 0.95g
3)
35H
2The Na of O and 0.45g
2SO
4, to dissolve in the 40mL deionized water, ultrasonic and use magnetic agitation formed mixing solutions in 1 hour;
B, take the NaOH of 0.72g, add the 40mL deionized water, ultrasonic its Uniform Dispersion that makes forms the sodium hydroxide clear solution;
C, with the sodium hydroxide clear solution of step B gained, dropwise join under magnetic agitation in the mixing solutions of steps A gained;
D, the solution of step C gained is transferred in the container of quartz that capacity is 100mL, is placed in microwave reactor, be warming up to 100 ℃, power is 800W, and after continuing 15min, naturally cooling is collected product;
E, with the product centrifugation of step D gained, wash respectively three times with deionized water and dehydrated alcohol;
F, with the centrifugal product of step e gained at 80 ℃ of air drying 12h, namely obtain the bismuthous oxide bismuth trioxide (Bi of pattern homogeneous
2O
3) nanotube.
Bismuthous oxide bismuth trioxide (the Bi of above-described embodiment preparation
2O
3) nanotube, the degradation experiment step to tsiklomitsin under the xenon source irradiation is as follows:
Photocatalytic activity is estimated: carry out in GHX-2 type photochemical reaction instrument (available from Science and Technology City Science and Technology Ltd. of Yangzhou University), be that 10mg/L tsiklomitsin simulated wastewater 100mL adds in photochemical catalysis instrument reactor with concentration, then add the bismuthous oxide bismuth trioxide (Bi of this microwave microwave-assisted reaction
2O
3) photocatalyst 0.1g, use magnetic stirring apparatus reaction 30 minutes in the darkroom, begin sampling after reaching the reaction adsorption equilibrium, then open aerating apparatus and open xenon source, it is to keep catalyzer to be in to suspend or afloat that aeration passes into the air purpose, at interval of the 10min sampling, gets supernatant liquid after centrifugation at tsiklomitsin maximum absorption wavelength λ max=357nm place in the Xenon light shining process, use TU-1800 ultraviolet-visible pectrophotometer place working sample absorbancy, and pass through formula: DC=[(A
O-A
i)/A
O] * 100% is calculated photodegradation rate, wherein A
OThe absorbancy of tetracycline when reaching adsorption equilibrium, A
iThe absorbancy of the tetracycline of measuring for timing sampling.
Bismuthous oxide bismuth trioxide (Bi
2O
3) the XRD figure spectrum of nanotube sees accompanying drawing 1, the product morphology analysis is seen accompanying drawing 2, and accompanying drawing 3 is seen in the analysis of surface-element valence state, and photocatalysis effect is seen accompanying drawing 4.
In Fig. 1 the position of each diffraction peak and relative intensity all with JCPDS(JCPDS) card (41-1449) matches, and there is no other diffraction peak of mixing in the XRD figure spectrum, and the bismuthous oxide bismuth trioxide (Bi that the present embodiment is prepared is described
2O
3) nanotube is pure.
In Fig. 2, field emission scanning electron microscope (SEM) is tested and is shown, at room temperature, and by the bismuthous oxide bismuth trioxide (Bi of microwave-assisted Liquid preparation methods
2O
3) nanotube length is about 20 μ m～40 μ m, thickness of pipe is about 300～600nm.
In Fig. 3, bismuthous oxide bismuth trioxide (Bi
2O
3) nanotube XPS collection of illustrative plates at room temperature.At 163.7eV, 158.34eV distinguishes correspondences and Bi in these two strong peaks as can be seen from Figure 3
2O
3In Bi4f5/2 and Bi4f7/2,530.93eV is corresponding to Bi
2O
3In O1s, near and the not appearance of other small peak main peak is so show that there is not oxidized phenomenon on the surface of product.Bismuthous oxide bismuth trioxide (the Bi for preparing by the present embodiment
2O
3) nanotube, more stable.
In Fig. 4, photocatalysis effect figure demonstrates prepared bismuthous oxide bismuth trioxide (Bi
2O
3) nanotube reaches 83.64% to the degradation rate of tsiklomitsin when the 60min when xenon lamp shines.
Claims (3)
1. microwave-assisted Liquid preparation methods bismuthous oxide bismuth trioxide (Bi
2O
3) method of nanotube, it is characterized in that, carry out according to following step:
A) take the Bi (NO of 0.95g～1.00g
3)
35H
2The Na of O and 0.45g～0.50g
2SO
4, to dissolve in the 40mL deionized water, ultrasonic and use magnetic agitation formed mixing solutions in 1 hour;
B) take 0.70g～0.75g NaOH, add the 40mL deionized water, ultrasonic its Uniform Dispersion that makes forms the sodium hydroxide clear solution;
C) with the sodium hydroxide clear solution of step B gained, dropwise join under magnetic agitation in the mixing solutions of steps A gained;
D) solution of step C gained is transferred in the container of quartz that capacity is 100mL, is placed in the reactor that microwave power is 800W, be warming up to 80 ℃～100 ℃, continue 10min～20min, naturally cooling is collected product;
E) with the product centrifugation of step D gained, wash respectively three times with deionized water and dehydrated alcohol;
F) with the centrifugal product of step e gained at 80 ℃ of air drying 12h, namely obtain the bismuthous oxide bismuth trioxide (Bi of pattern homogeneous
2O
3) nanotube.
2. the method for claim 1, is characterized in that, the Bi (NO in described steps A
3)
35H
2O, Na
2SO
4Be analytical pure with NaOH.
3. bismuthous oxide bismuth trioxide (the Bi that obtains of the described method of claim 1
2O
3) nanotube is used for containing the photodegradative application of tetracycline wastewater.
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| CN107362805A (en) * | 2017-08-02 | 2017-11-21 | 江苏大学 | A kind of Preparation method and use of the magnetic oxygenated bismuth composite photo-catalyst based on biomass carbon |
| CN108579722A (en) * | 2018-06-15 | 2018-09-28 | 南阳师范学院 | One kind is for light-catalysed semiconductor nano material and preparation method thereof |
| CN110961158A (en) * | 2019-11-19 | 2020-04-07 | 江苏大学 | Environment response type PNIPAM/Bi2O3Preparation method and application thereof |
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| CN103420414A (en) * | 2013-08-12 | 2013-12-04 | 江苏大学 | Solvothermal preparation method of bismuth trioxide microspheres and application thereof |
| CN103420414B (en) * | 2013-08-12 | 2015-02-04 | 江苏大学 | Solvothermal preparation method of bismuth trioxide microspheres and application thereof |
| CN107362805A (en) * | 2017-08-02 | 2017-11-21 | 江苏大学 | A kind of Preparation method and use of the magnetic oxygenated bismuth composite photo-catalyst based on biomass carbon |
| CN107362805B (en) * | 2017-08-02 | 2020-02-21 | 江苏大学 | Preparation method and application of magnetic bismuth oxide composite photocatalyst based on biomass charcoal |
| CN108579722A (en) * | 2018-06-15 | 2018-09-28 | 南阳师范学院 | One kind is for light-catalysed semiconductor nano material and preparation method thereof |
| CN110961158A (en) * | 2019-11-19 | 2020-04-07 | 江苏大学 | Environment response type PNIPAM/Bi2O3Preparation method and application thereof |
| CN110961158B (en) * | 2019-11-19 | 2023-03-21 | 江苏大学 | Environment response type PNIPAM/Bi 2 O 3 Preparation method and application thereof |
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| CN103112894B (en) | 2014-09-10 |
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