CN103112894B - 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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- CN103112894B CN103112894B CN201310047220.5A CN201310047220A CN103112894B CN 103112894 B CN103112894 B CN 103112894B CN 201310047220 A CN201310047220 A CN 201310047220A CN 103112894 B CN103112894 B CN 103112894B
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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, 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 needs further to be improved, how to utilize the visible light part degradable organic pollutant of sun power, the catalyzer under visible ray with higher catalytic activity, has become one of focus in photochemical catalysis research field.
Bismuth based compound using 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, can effectively be oxidized organic pollutant, therefore there is very strong environmental applications ability and form the emphasis into people's research.
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 good performance and application potential as a kind of advanced person's function powder material in the application of the aspects such as electronic ceramics powder body material, electrolyte, photoelectric material, high temperature superconducting materia, catalystic material.Have been reported the experimental study containing nitrite waste water, sulphite waste water and dyeing waste water by bismuthous oxide bismuth trioxide photocatalysis treatment, but do not have at present report on processing tetracycline wastewater.
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 and is had a strong impact on, be deemed to be a kind of typical micro-Organic Pollutants of environment.The removal of the antibiotic substance taking tsiklomitsin as representative, had become a scientific research difficult problem urgently 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, dissolve in 40mL deionized water, ultrasonic and use magnetic agitation 1 hour to form mixing solutions;
B) take 0.70g～0.75g NaOH, add 40mL deionized water, ultrasonicly make it dispersed, form sodium hydroxide clear solution;
C), by the sodium hydroxide clear solution of step B gained, under magnetic agitation, dropwise join in the mixing solutions of steps A gained;
D) solution of step C gained is transferred in the quartzy container that capacity is 100mL, is placed in the reactor that microwave power is 800W, be warming up to 80 DEG C～100 DEG C, continue 10min～20min, naturally cooling, collects product;
E), by the product centrifugation of step D gained, wash respectively three times with deionized water and dehydrated alcohol;
F) by centrifugal step e gained product at 80 DEG C of air drying 12h, 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 (Bi prepared by method of the present invention
2o
3) nanotube, its structure is determined in x-ray diffraction pattern, there is no the peak of other materials 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 the bismuthous oxide bismuth trioxide (Bi being prepared by microwave assisting method
2o
3) nanotube length is about 20 μ m～40 μ m, thickness of pipe is about 300nm.
Applicant is to the bismuthous oxide bismuth trioxide (Bi obtaining
2o
3) valence state of element of nanotube analyzes, 163.7eV, these two strong peaks of 158.34eV 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 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 the photodegradative application containing tetracycline wastewater through experiment showed, of applicant, as follows to the degradation experiment of tsiklomitsin under xenon source irradiates:
Photocatalytic activity is evaluated: in GHX-2 type photochemical reaction instrument (purchased from Science and Technology City Science and Technology Ltd. of Yangzhou University), carry out, be that 10mg/L tsiklomitsin simulated wastewater 100mL adds in photochemical catalysis instrument reactor by 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 darkroom, after reaching reaction adsorption equilibrium, start sampling, then open aerating apparatus and open xenon source, it is to keep catalyzer in suspending or afloat that aeration passes into air object, in Xenon light shining process, at interval of 10min sampling, gets supernatant liquid at tsiklomitsin maximum absorption wavelength λ max=357nm place after centrifugation, use TU-1800 ultraviolet-visible pectrophotometer place working sample absorbancy, and pass through formula: DC=[(A
o-A
i)/A
o] × 100% calculates photodegradation rate, wherein A
othe absorbancy of tetracycline when reaching adsorption equilibrium, A
ithe absorbancy of tetracycline of measuring for timing sampling.
Bismuthous oxide bismuth trioxide (the Bi that the present invention is prepared
2o
3) nanotube, in the time that xenon lamp irradiates to reaching 83.64% containing the degradation rate of tetracycline wastewater when the 60min.
The present invention adopts liquid phase method under low temperature to react the bismuthous oxide bismuth trioxide (Bi for preparing the relative homogeneous of pattern through microwave-assisted
2o
3) nanotube, there is the advantages such as chemical stability is good, nontoxic.Its technique is simple, favorable reproducibility, and raw materials is mineral compound, cheap and easy to get, cost is low, meet environmental friendliness requirement, due to the method do not need high temperature, calcining and so on pre-treatment, synthesis temperature is lower, the reaction times is shorter, thereby reduce energy consumption and reaction cost, be convenient to batch production.Simultaneously due to bismuthous oxide bismuth trioxide (Bi
2o
3) tsiklomitsin is had to stronger photocatalytic degradation ability, in practical application, also there is feasibility.
Brief description of the 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 example preferably, 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, dissolve in 40mL deionized water, ultrasonic and use magnetic agitation 1 hour to form mixing solutions;
B, take the NaOH of 0.70g, add 40mL deionized water, ultrasonicly make it dispersed, form sodium hydroxide clear solution;
C, by the sodium hydroxide clear solution of step B gained, under magnetic agitation, dropwise join in the mixing solutions of steps A gained;
D, the solution of step C gained is transferred in the quartzy container that capacity is 100mL, is placed in microwave reactor, microwave power is 800W, is warming up to 80 DEG C, continues 10min, and naturally cooling is collected product;
E, by the product centrifugation of step D gained, wash respectively three times with deionized water and dehydrated alcohol;
F, by centrifugal step e gained product at 80 DEG C of air drying 12h, 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, dissolve in 40mL deionized water, ultrasonic and use magnetic agitation 1 hour to form mixing solutions;
B, take the NaOH of 0.75g, add 40mL deionized water, ultrasonicly make it dispersed, form sodium hydroxide clear solution;
C, by the sodium hydroxide clear solution of step B gained, under magnetic agitation, dropwise join in the mixing solutions of steps A gained;
D, the solution of step C gained is transferred in the quartzy container that capacity is 100mL, is placed in microwave reactor, microwave power is 800W, is warming up to 100 DEG C, continues 20min, and naturally cooling is collected product;
E, by the product centrifugation of step D gained, wash respectively three times with deionized water and dehydrated alcohol;
F, by centrifugal step e gained product at 80 DEG C of air drying 12h, 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, dissolve in 40mL deionized water, ultrasonic and use magnetic agitation 1 hour to form mixing solutions;
B, take the NaOH of 0.75g, add 40mL deionized water, ultrasonicly make it dispersed, form sodium hydroxide clear solution;
C, by the sodium hydroxide clear solution of step B gained, under magnetic agitation, dropwise join in the mixing solutions of steps A gained;
D, the solution of step C gained is transferred in the quartzy container that capacity is 100mL, is placed in microwave reactor, microwave power is 800W, is warming up to 100 DEG C, continues 20min, and naturally cooling is collected product;
E, by the product centrifugation of step D gained, wash respectively three times with deionized water and dehydrated alcohol;
F, by centrifugal step e gained product at 80 DEG C of air drying 12h, 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, dissolve in 40mL deionized water, ultrasonic and use magnetic agitation 1 hour to form mixing solutions;
B, take the NaOH of 0.75g, add 40mL deionized water, ultrasonicly make it dispersed, form sodium hydroxide clear solution;
C, by the sodium hydroxide clear solution of step B gained, under magnetic agitation, dropwise join in the mixing solutions of steps A gained;
D, the solution of step C gained is transferred in the quartzy container that capacity is 100mL, is placed in microwave reactor, microwave power is 800W, is warming up to 80 DEG C, continues 10min, and naturally cooling is collected product;
E, by the product centrifugation of step D gained, wash respectively three times with deionized water and dehydrated alcohol;
F, by centrifugal step e gained product at 80 DEG C of air drying 12h, 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, dissolve in 40mL deionized water, ultrasonic and use magnetic agitation 1 hour to form mixing solutions;
B, take the NaOH of 0.73g, add 40mL deionized water, ultrasonicly make it dispersed, form sodium hydroxide clear solution;
C, by the sodium hydroxide clear solution of step B gained, under magnetic agitation, dropwise join in the mixing solutions of steps A gained;
D, the solution of step C gained is transferred in the quartzy container that capacity is 100mL, is placed in microwave reactor, microwave power is 800W, is warming up to 90 DEG C, continues 15min, and naturally cooling is collected product;
E, by the product centrifugation of step D gained, wash respectively three times with deionized water and dehydrated alcohol;
F, by centrifugal step e gained product at 80 DEG C of air drying 12h, 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, dissolve in 40mL deionized water, ultrasonic and use magnetic agitation 1 hour to form mixing solutions;
B, take the NaOH of 0.72g, add 40mL deionized water, ultrasonicly make it dispersed, form sodium hydroxide clear solution;
C, by the sodium hydroxide clear solution of step B gained, under magnetic agitation, dropwise join in the mixing solutions of steps A gained;
D, the solution of step C gained is transferred in the quartzy container that capacity is 100mL, is placed in microwave reactor, be warming up to 100 DEG C, power is 800W, continues after 15min, and naturally cooling, collects product;
E, by the product centrifugation of step D gained, wash respectively three times with deionized water and dehydrated alcohol;
F, by centrifugal step e gained product at 80 DEG C of air drying 12h, obtain the bismuthous oxide bismuth trioxide (Bi of pattern homogeneous
2o
3) nanotube.
Bismuthous oxide bismuth trioxide (Bi prepared by above-described embodiment
2o
3) nanotube, as follows to the degradation experiment step of tsiklomitsin under xenon source irradiates:
Photocatalytic activity is evaluated: in GHX-2 type photochemical reaction instrument (purchased from Science and Technology City Science and Technology Ltd. of Yangzhou University), carry out, be that 10mg/L tsiklomitsin simulated wastewater 100mL adds in photochemical catalysis instrument reactor by 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 darkroom, after reaching reaction adsorption equilibrium, start sampling, then open aerating apparatus and open xenon source, it is to keep catalyzer in suspending or afloat that aeration passes into air object, in Xenon light shining process, at interval of 10min sampling, gets supernatant liquid at tsiklomitsin maximum absorption wavelength λ max=357nm place after centrifugation, use TU-1800 ultraviolet-visible pectrophotometer place working sample absorbancy, and pass through formula: DC=[(A
o-A
i)/A
o] × 100% calculates photodegradation rate, wherein A
othe absorbancy of tetracycline when reaching adsorption equilibrium, A
ithe absorbancy of tetracycline of measuring for timing sampling.
Bismuthous oxide bismuth trioxide (Bi
2o
3) the XRD figure spectrum of nanotube is shown in accompanying drawing 1, product morphology analysis is shown in accompanying drawing 2, and accompanying drawing 3 is shown in the analysis of surface-element valence state, and photocatalysis effect is shown in accompanying drawing 4.
In Fig. 1 the position of each diffraction peak and relative intensity all with JCPDS(JCPDS) card (41-1449) matches, and in XRD figure spectrum, there is no other diffraction peak of mixing, 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, so show that there is not oxidized phenomenon on the surface of product.Bismuthous oxide bismuth trioxide (the Bi 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 in the time that xenon lamp irradiates.
Claims (3)
1. a microwave-assisted Liquid preparation methods bismuthous oxide bismuth trioxide (Bi
2o
3) method of nanotube, it is characterized in that this bismuthous oxide bismuth trioxide (Bi making
2o
3) nanotube is for to containing the photodegradation of tetracycline wastewater, described bismuthous oxide bismuth trioxide (Bi
2o
3) nanotube carries 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, dissolve in 40mL deionized water, ultrasonic and use magnetic agitation 1 hour to form mixing solutions;
B) take 0.70g～0.75g NaOH, add 40mL deionized water, ultrasonicly make it dispersed, form sodium hydroxide clear solution;
C), by the sodium hydroxide clear solution of step B gained, under magnetic agitation, dropwise join in the mixing solutions of steps A gained;
D) solution of step C gained is transferred in the quartzy container that capacity is 100mL, is placed in the reactor that microwave power is 800W, be warming up to 80 DEG C～100 DEG C, continue 10min～20min, naturally cooling, collects product;
E), by the product centrifugation of step D gained, wash respectively three times with deionized water and dehydrated alcohol;
F) by centrifugal step e gained product at 80 DEG C of air drying 12h, obtain the bismuthous oxide bismuth trioxide (Bi of pattern homogeneous
2o
3) nanotube, bismuthous oxide bismuth trioxide (Bi
2o
3) nanotube length is 20 μ m～40 μ m, thickness of pipe is 300nm.
2. the method for claim 1, is characterized in that, the Bi (NO in described steps A
3)
35H
2o and Na
2sO
4be analytical pure.
3. method as claimed in claim 1, is characterized in that described bismuthous oxide bismuth trioxide (Bi
2o
3) nanotube is for to containing the photodegradation of tetracycline wastewater, under xenon source irradiates, carries out, specific as follows:
Photocatalytic activity is evaluated: in GHX-2 type photochemical reaction instrument, carrying out, is that 10mg/L tsiklomitsin simulated wastewater 100mL adds in photochemical catalysis instrument reactor by concentration, then adds the bismuthous oxide bismuth trioxide (Bi of this microwave-assisted reaction
2o
3) photocatalyst 0.1g, use magnetic stirring apparatus reaction 30 minutes in darkroom, after reaching reaction adsorption equilibrium, start sampling, then open aerating apparatus and open xenon source, it is to keep catalyzer in suspending or afloat that aeration passes into air object, in Xenon light shining process, sample at interval of 10min, after centrifugation, get supernatant liquid at tsiklomitsin maximum absorption wavelength λ max=357nm place, use TU-1800 ultraviolet-visible pectrophotometer place working sample absorbancy, and pass through formula: DC=[(A
0-A
i)/A
0] × 100% calculates photodegradation rate, wherein A
0the absorbancy of tetracycline when reaching adsorption equilibrium, A
ithe absorbancy of tetracycline of measuring for timing sampling.
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| CN103420414B (en) * | 2013-08-12 | 2015-02-04 | 江苏大学 | Solvothermal preparation method of bismuth trioxide microspheres and application thereof |
| 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 |
| 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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| 锶掺杂氧化铋可见光催化降解水中四环素研究;丁士元等;《持久性有机污染物论坛暨第七届有机污染物全国学术研讨会论文集》;20120517;第273-274页 * |
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