CN103420414A - Solvothermal preparation method of bismuth trioxide microspheres and application thereof - Google Patents
Solvothermal preparation method of bismuth trioxide microspheres and application thereof Download PDFInfo
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- CN103420414A CN103420414A CN2013103469399A CN201310346939A CN103420414A CN 103420414 A CN103420414 A CN 103420414A CN 2013103469399 A CN2013103469399 A CN 2013103469399A CN 201310346939 A CN201310346939 A CN 201310346939A CN 103420414 A CN103420414 A CN 103420414A
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Abstract
The invention belongs to the technical field of preparation of inorganic nanomaterials and environmental materials, and relates to a solvothermal preparation method of bismuth trioxide microspheres and application thereof. The solvothermal preparation method of the bismuth trioxide microspheres adopts the technical steps as follows: dissolving soluble bismuth salt into ethylene glycol and dissolving soluble indium salt and urea into ethanol respectively; performing ultrasonic agitation and uniformly mixing, and obtaining a precursor through solvothermal reaction; centrifugally washing and drying the precursor, and roasting the precursor at high temperature to prepare the bismuth trioxide microspheres. The bismuth oxide (Bi2O3) microspheres with relatively uniform morphology are prepared at a low temperature through the solvothermal reaction by a liquid-phase method, the morphology thereof is a microspherical structure, and the diameter thereof is about 1-2 microns. When the bismuth trioxide microspheres prepared according to the solvothermal preparation method method can be applied to optical degradation of tetracycline-containing wastewater, and have the advantages of high chemical stability and the like. The solvothermal preparation method is simple in process and high in repeatability; used raw materials meet environment-friendly requirements; and by the solvothermal preparation method, mass production can be facilitated.
Description
Technical field
The invention belongs to inorganic nano material and environmentally conscious materials preparing technical field, relate to the preparation method of bismuthous oxide bismuth trioxide micron ball, relate in particular to a kind of solvent-thermal method and prepare bismuthous oxide bismuth trioxide micron ball and application thereof.
Background technology
At present microbiotic is widely used in the control of the diseases such as mankind's infection control disease and poultry, domestic animal, crop, but because still there are technological difficulties in antibiotic screening and the aspects such as production, strain improvement, thereby the problem such as residual antibiotic content height in waste water occurs, environment has been caused to great pollution.The removal of the antibiotic substance that the tsiklomitsin of therefore take is representative, become a scientific research difficult problem urgently to be resolved hurrily.
Bismuthous oxide bismuth trioxide is the important p-type semiconductor material of a class, mainly contains α, β, γ and tetra-kinds of crystal formations of δ, the crystal formation difference, and its application is also different.The band gap width of bismuthous oxide bismuth trioxide is 2.7～2.8eV, and absorbing wavelength is longer.Bismuthous oxide bismuth trioxide is widely used at aspects such as mineral dye, optical material, electronic material, superconducting material and catalyzer, and its application and development prospect is very wide.
Summary of the invention
One object of the present invention is to adopt low temperature liquid polymerization process through solvent thermal reaction, discloses a kind of technique simple, well behaved bismuthous oxide bismuth trioxide (Bi
2O
3) preparation method of micron ball.
A kind of solvent-thermal method prepares the bismuthous oxide bismuth trioxide micron ball, its technical scheme is respectively soluble bismuth salt to be dissolved in to ethylene glycol, solubility indium salt and urea are dissolved in dehydrated alcohol, after ultrasonic agitation mixes, obtain precursor through solvent thermal reaction, the precursor centrifuge washing is dried and is prepared from by high-temperature roasting.
Solvent-thermal method disclosed in this invention prepares bismuthous oxide bismuth trioxide (Bi
2O
3) preparation method of micron ball, be to carry out according to following step:
A, take soluble bismuth salt, ultrasonic agitation is dissolved in ethylene glycol, forms bismuth salt ethylene glycol solution, and described soluble bismuth salt is 0.1～1.0 mmol:5～30 mL with the molecular volume ratio of ethylene glycol;
B, take solubility indium salt and urea respectively, magnetic agitation is dissolved in dehydrated alcohol, form the mixed ethanol solution of indium salt and urea, described solubility indium salt: urea: the molecular volume ratio of dehydrated alcohol is 0.1～1.0 mmol:0.1～1.0 mmol:5～30 mL;
C, the described solution of step B is added in the solution of steps A, then magnetic agitation 30 min;
D, the mixed system of step C gained is transferred in the teflon-lined reactor, is warmed up to 100～180 ℃ of constant temperature 12～36 h, naturally cooling, obtain the solvent thermal product;
E, the solvent thermal product of step D gained is washed respectively three times with deionized water and dehydrated alcohol, after centrifugation, at 60～80 ℃ of air drying 6～12h, obtain precursor;
F, by the precursor of step e gained roasting 60～180min under 350～550 ℃ of air atmospheres of retort furnace, can obtain the bismuthous oxide bismuth trioxide (Bi of pattern homogeneous
2O
3) micron ball.
Soluble bismuth salt of the present invention is any one or several in Bismuth trinitrate, bismuth chloride, bismuth citrate and bismuth sulfate.
Solubility indium salt of the present invention is any one or several in indium nitrate, indium chloride and indium sulfate.
In reaction process of the present invention, solubility indium salt plays the pattern inducing action in the forming process of bismuth oxide, and urea has γ-ray emission in heat-processed, so can form spherical; Have impurity in the solvent thermal product and produce, by deionized water and washing with alcohol, can wash away the inorganic and organic impurity be dissolved in wherein, finally by x-ray diffraction pattern, determine whether pure phase of final product.
Bismuthous oxide bismuth trioxide (Bi in the present invention
2O
3) structure of micron ball determined there is no the peak of other materials in x-ray diffraction pattern by x-ray diffractometer, this collection of illustrative plates shows, the prepared bismuthous oxide bismuth trioxide (Bi by solvent-thermal method
2O
3) be pure phase bismuthous oxide bismuth trioxide (Bi
2O
3), itself and standard bismuthous oxide bismuth trioxide (Bi
2O
3) card (27-0050) matches.
Field emission scanning electron microscope (SEM) is tested and is shown, at room temperature, and the bismuthous oxide bismuth trioxide (Bi prepared by solvent-thermal method
2O
3) the micron ball diameter is about 1～2 μ m.
Another object of the present invention is by preparation-obtained bismuthous oxide bismuth trioxide (Bi according to the method described above
2O
3) micron ball is applied to the photodegradation containing tetracycline wastewater.
Photocatalytic activity is estimated:
In GHX-2 type photochemical reaction instrument (purchased from Science and Technology City Science and Technology Ltd. of Yangzhou University), carry out, be that 20 mg/L tsiklomitsin simulated wastewater 100 mL add in photochemical catalysis instrument reactor by concentration, then add the prepared bismuthous oxide bismuth trioxide (Bi of the embodiment of the present invention 1
2O
3) micron ball 0.1 g, use magnetic stirring apparatus reaction 30min in darkroom, start sampling after reaching the reaction adsorption equilibrium, then open aerating apparatus and open xenon source, it is to keep catalyzer in suspending or afloat that aeration passes into the air purpose, at interval of 10 min samplings, get supernatant liquid after centrifugation at tsiklomitsin maximum absorption wavelength λ in the Xenon light shining process
max=357 nm places, used TU-1800 ultraviolet-visible pectrophotometer place working sample absorbancy, and pass through formula: DC=[(A
0-A
i)/A
0] * 100% is calculated photodegradation rate, wherein A
0The 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 embodiment of the present invention 1 is prepared
2O
3) micron ball when visible ray illumination 1h to the degradation rate of tsiklomitsin up to 91.07%.
The present invention's reagent used is analytical pure, in reaction process, does not further purify.
Beneficial effect
Utilize the prepared bismuthous oxide bismuth trioxide (Bi of simple solvent thermal reaction
2O
3), pattern is spherical micrometer structure, this material has good chemical stability.Technique of the present invention is simple, and favorable reproducibility is cheap and easy to get, and cost is low, meets the environmental friendliness requirement, is convenient to batch production.Bismuthous oxide bismuth trioxide (the Bi that the present invention is made
2O
3) the micron ball photocatalyst, degradation efficiency is higher, during visible ray illumination 1h to the degradation rate of tsiklomitsin up to 91.07%.
The accompanying drawing explanation
Fig. 1 embodiment 1 makes bismuthous oxide bismuth trioxide (Bi
2O
3) the X-ray diffraction analysis figure (XRD) of micron ball.
Fig. 2 embodiment 1 makes bismuthous oxide bismuth trioxide (Bi
2O
3) scanning electron microscope (SEM) photograph (SEM) of micron ball.
Fig. 3 embodiment 1 makes bismuthous oxide bismuth trioxide (Bi
2O
3) the photodegradation figure of micron ball.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail, so that those skilled in the art understand the present invention better, but the present invention is not limited to following examples.
Embodiment 1
A kind of bismuthous oxide bismuth trioxide (Bi
2O
3) preparation method of micron ball, be to carry out according to following step:
A, take the Bi (NO of 0.5 mmoL
3)
35H
2O, ultrasonic agitation is dissolved in 5 mL ethylene glycol solutions, forms bismuth nitrate solution;
B, take 0.1 mmoL In (NO respectively
3)
34.5H
2O and 0.1mmoL urea, magnetic agitation is dissolved in 5 mL ethanol solutions it, forms the mixing solutions of indium nitrate and urea;
C, the described solution of step B is added in the solution of steps A, then magnetic agitation 30 min;
D, the mixed system of step C gained is transferred in the teflon-lined reactor, is warmed up to constant temperature 24 h at 180 ℃ of temperature, naturally cooling, obtain the solvent thermal product;
E, by the solvent thermal product centrifugation of step D gained, with deionized water and dehydrated alcohol, wash respectively three times, the product after centrifugation, at 60 ℃ of air drying 6h, obtains precursor;
F, by the precursor of step e gained roasting 120min under 350 ℃ of air atmospheres of retort furnace, can obtain the bismuthous oxide bismuth trioxide (Bi of pattern homogeneous
2O
3) micron ball.
Bismuthous oxide bismuth trioxide (Bi
2O
3) micron ball degradation experiment step to tsiklomitsin under visible light source irradiates is as follows:
Photocatalytic activity is estimated: in GHX-2 type photochemical reaction instrument (purchased from Science and Technology City Science and Technology Ltd. of Yangzhou University), carry out, be that 20 mg/L tsiklomitsin simulated wastewater 100 mL add in photochemical catalysis instrument reactor by concentration, then add the bismuthous oxide bismuth trioxide (Bi of this solvent thermal reaction
2O
3) photocatalyst 0.1 g, use magnetic stirring apparatus reaction 30min in darkroom, start sampling after reaching the reaction adsorption equilibrium, then open aerating apparatus and open xenon source, it is to keep catalyzer in suspending or afloat that aeration passes into the air purpose, in the Xenon light shining process, at interval of 10 min, sample, get supernatant liquid after centrifugation at tsiklomitsin maximum absorption wavelength λ max=357 nm place, use TU-1800 ultraviolet-visible pectrophotometer place working sample absorbancy, and pass through formula: DC=[(A
0-A
i)/A
0] * 100% is calculated photodegradation rate, wherein A
0The 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 micron ball is shown in accompanying drawing 1, the product morphology analysis is shown in accompanying drawing 2, photocatalysis effect is shown in accompanying drawing 3.
In accompanying drawing 1 position of each diffraction peak and relative intensity all with JCPDS(JCPDS) card (27-0050) matches, and there is no other diffraction peak of mix in XRD figure spectrum, the bismuthous oxide bismuth trioxide (Bi prepared under the solvent thermal condition of the present invention's proposition is described
2O
3) phase of micron ball is pure.
In accompanying drawing 2, field emission scanning electron microscope (SEM) is tested and is shown, at room temperature, and the bismuthous oxide bismuth trioxide (Bi prepared by solvent-thermal method
2O
3) the micron ball diameter is about 1～2 μ m.
In accompanying drawing 3, photocatalysis effect figure demonstrates prepared bismuthous oxide bismuth trioxide (Bi
2O
3) micron ball degradation rate to tsiklomitsin under visible light source reaches 91.07%.
Embodiment 2
A kind of bismuthous oxide bismuth trioxide (Bi
2O
3) preparation method of micron ball, be to carry out according to following step:
A, take the Bi (NO of 5.0 mmoL
3)
35H
2O, ultrasonic agitation is dissolved in 30 mL ethylene glycol solutions, forms bismuth nitrate solution;
B, take 1.0 mmoL In (NO respectively
3)
34.5H
2O and 1.0mmoL urea, magnetic agitation is dissolved in 30 mL ethanol solutions it, forms the mixing solutions of indium nitrate and urea;
C, the described solution of step B is added in the solution of steps A, then magnetic agitation 30 min;
D, the mixed system of step C gained is transferred in the teflon-lined reactor, is warmed up to constant temperature 24 h at 100 ℃ of temperature, naturally cooling, obtain the solvent thermal product;
E, by the solvent thermal product centrifugation of step D gained, with deionized water and dehydrated alcohol, wash respectively three times, the product after centrifugation, at 60 ℃ of air drying 6h, obtains precursor;
F, by the precursor of step e gained roasting 120min under 550 ℃ of air atmospheres of retort furnace, can obtain the bismuthous oxide bismuth trioxide (Bi of pattern homogeneous
2O
3) micron ball.
Embodiment 3
A kind of bismuthous oxide bismuth trioxide (Bi
2O
3) preparation method of micron ball, be to carry out according to following step:
A, take the Bi (NO of 0.5 mmoL
3)
35H
2O, ultrasonic agitation is dissolved in 5 mL ethylene glycol solutions, forms bismuth nitrate solution;
B, take 0.1 mmoL In (NO respectively
3)
34.5H
2O and 1.0mmoL urea, magnetic agitation is dissolved in 30 mL ethanol solutions it, forms the mixing solutions of indium nitrate and urea;
C, the described solution of step B is added in the solution of steps A, then magnetic agitation 30 min;
D, the mixed system of step C gained is transferred in the teflon-lined reactor, is warmed up to constant temperature 24 h at 120 ℃ of temperature, naturally cooling, obtain the solvent thermal product;
E, by the solvent thermal product centrifugation of step D gained, with deionized water and dehydrated alcohol, wash respectively three times, the product after centrifugation, at 60 ℃ of air drying 6h, obtains precursor;
F, by the precursor of step e gained roasting 120min under 550 ℃ of air atmospheres of retort furnace, can obtain the bismuthous oxide bismuth trioxide (Bi of pattern homogeneous
2O
3) micron ball.
Embodiment 4
A kind of bismuthous oxide bismuth trioxide (Bi
2O
3) preparation method of micron ball, be to carry out according to following step:
A, take the Bi (NO of 5.0 mmoL
3)
35H
2O, ultrasonic agitation is dissolved in 30 mL ethylene glycol solutions, forms bismuth nitrate solution;
B, take 1.0 mmoL In (NO respectively
3)
34.5H
2O and 0.1mmoL urea, magnetic agitation is dissolved in 5 mL ethanol solutions it, forms the mixing solutions of indium nitrate and urea;
C, the described solution of step B is added in the solution of steps A, then magnetic agitation 30 min;
D, the mixed system of step C gained is transferred in the teflon-lined reactor, is warmed up to constant temperature 24 h at 140 ℃ of temperature, naturally cooling, obtain the solvent thermal product;
E, by the solvent thermal product centrifugation of step D gained, with deionized water and dehydrated alcohol, wash respectively three times, the product after centrifugation, at 60 ℃ of air drying 6h, obtains precursor;
F, by the precursor of step e gained roasting 180min under 350 ℃ of air atmospheres of retort furnace, can obtain the bismuthous oxide bismuth trioxide (Bi of pattern homogeneous
2O
3) micron ball.
Embodiment 5
A kind of bismuthous oxide bismuth trioxide (Bi
2O
3) preparation method of micron ball, be to carry out according to following step:
A, take the Bi (NO of 1.0 mmoL
3)
35H
2O, ultrasonic agitation is dissolved in 10 mL ethylene glycol solutions, forms bismuth nitrate solution;
B, take 0.5 mmoL In (NO respectively
3)
34.5H
2O and 0.8mmoL urea, magnetic agitation is dissolved in 25 mL ethanol solutions it, forms the mixing solutions of indium nitrate and urea;
C, the described solution of step B is added in the solution of steps A, then magnetic agitation 30 min;
D, the mixed system of step C gained is transferred in the teflon-lined reactor, is warmed up to constant temperature 24 h at 160 ℃ of temperature, naturally cooling, obtain the solvent thermal product;
E, by the solvent thermal product centrifugation of step D gained, with deionized water and dehydrated alcohol, wash respectively three times, the product after centrifugation, at 60 ℃ of air drying 6h, obtains precursor;
F, by the precursor of step e gained roasting 120min under 400 ℃ of air atmospheres of retort furnace, can obtain the bismuthous oxide bismuth trioxide (Bi of pattern homogeneous
2O
3) micron ball.
Embodiment 6
A kind of bismuthous oxide bismuth trioxide (Bi
2O
3) preparation method of micron ball, be to carry out according to following step:
A, take the Bi (NO of 3.0 mmoL
3)
35H
2O, ultrasonic agitation is dissolved in the 25mL ethylene glycol solution, forms bismuth nitrate solution;
B, take 0.2 mmoL In (NO respectively
3)
34.5H
2O and 0.5mmoL urea, magnetic agitation is dissolved in 10 mL ethanol solutions it, forms the mixing solutions of indium nitrate and urea;
C, the described solution of step B is added in the solution of steps A, then magnetic agitation 30 min;
D, the mixed system of step C gained is transferred in the teflon-lined reactor, is warmed up to constant temperature 24 h at 180 ℃ of temperature, naturally cooling, obtain the solvent thermal product;
E, by the solvent thermal product centrifugation of step D gained, with deionized water and dehydrated alcohol, wash respectively three times, the product after centrifugation, at 60 ℃ of air drying 6h, obtains precursor;
F, by the precursor of step e gained roasting 180min under 400 ℃ of air atmospheres of retort furnace, can obtain the bismuthous oxide bismuth trioxide (Bi of pattern homogeneous
2O
3) micron ball.
Embodiment 7
A kind of bismuthous oxide bismuth trioxide (Bi
2O
3) preparation method of micron ball, be to carry out according to following step:
A, take the BiCl of 1.0 mmoL
3, ultrasonic agitation is dissolved in the 15mL ethylene glycol solution, forms bismuth chloride solution;
B, take 0.2 mmoL InCl respectively
34H
2O and 0.8 mmoL urea, magnetic agitation is dissolved in 25 mL second anhydrous alcohol solutions it, forms the mixing solutions of indium chloride and urea;
C, the described solution of step B is added in the solution of steps A, then magnetic agitation 30 min;
D, the mixed system of step C gained is transferred in the teflon-lined reactor, is warmed up to constant temperature 12 h at 160 ℃ of temperature, naturally cooling, obtain the solvent thermal product;
E, by the solvent thermal product centrifugation of step D gained, with deionized water and dehydrated alcohol, wash respectively three times, the product after centrifugation, at 80 ℃ of air drying 12h, obtains precursor;
F, by the precursor of step e gained roasting 180min under 450 ℃ of air atmospheres of retort furnace, can obtain the bismuthous oxide bismuth trioxide (Bi of pattern homogeneous
2O
3) micron ball.
Embodiment 8
A kind of bismuthous oxide bismuth trioxide (Bi
2O
3) preparation method of micron ball, be to carry out according to following step:
A, take 2.0 mmoL C
6H
5BiO
7, ultrasonic agitation is dissolved in the 10mL ethylene glycol solution, forms bismuth citrate solution;
B, take 0.2 mmoL In respectively
2(SO
4)
34H
2O and 0.8 mmoL urea, magnetic agitation is dissolved in 20 mL ethanol solutions it, forms the mixing solutions of indium nitrate and urea;
C, the described solution of step B is added in the solution of steps A, then magnetic agitation 30 min;
D, the mixed system of step C gained is transferred in the teflon-lined reactor, is warmed up to constant temperature 24 h at 120 ℃ of temperature, naturally cooling, obtain the solvent thermal product;
E, by the solvent thermal product centrifugation of step D gained, with deionized water and dehydrated alcohol, wash respectively three times, the product after centrifugation, at 70 ℃ of air drying 10h, obtains precursor;
F, by the precursor of step e gained roasting 120min under 450 ℃ of air atmospheres of retort furnace, can obtain the bismuthous oxide bismuth trioxide (Bi of pattern homogeneous
2O
3) micron ball.
Embodiment 9
A kind of bismuthous oxide bismuth trioxide (Bi
2O
3) preparation method of micron ball, be to carry out according to following step:
A, take the Bi of 1.5 mmoL
2(SO
4)
3, ultrasonic agitation is dissolved in the 25mL ethylene glycol solution, forms bismuth sulfate solution;
B, take 0.2 mmoLInCl respectively
34H
2O and 1.0 mmoL urea, magnetic agitation is dissolved in 10 mL ethanol solutions it, forms the mixing solutions of indium chloride and urea;
C, the described solution of step B is added in the solution of steps A, then magnetic agitation 30 min;
D, the mixed system of step C gained is transferred in the teflon-lined reactor, is warmed up to constant temperature 24 h at 160 ℃ of temperature, naturally cooling, obtain the solvent thermal product;
E, by the solvent thermal product centrifugation of step D gained, with deionized water and dehydrated alcohol, wash respectively three times, the product after centrifugation, at 60 ℃ of air drying 10h, obtains precursor;
F, by the precursor of step e gained roasting 180min under 400 ℃ of air atmospheres of retort furnace, can obtain the bismuthous oxide bismuth trioxide (Bi of pattern homogeneous
2O
3) micron ball.
A kind of bismuthous oxide bismuth trioxide (Bi
2O
3) preparation method of micron ball, be to carry out according to following step:
A, take respectively the Bi (NO of 0.25 mmoL
3)
35H
2O, and the BiCl of 0.25mmol
3, ultrasonic agitation is dissolved in 5 mL ethylene glycol solutions, forms the soluble bismuth salts solution;
B, take 0.05 mmoL In (NO respectively
3)
34.5H
2O, 0.05mmolIn
2(SO
4)
34H
2O and 0.1mmoL urea, magnetic agitation is dissolved in 5 mL ethanol solutions it, forms the mixing solutions of solubility indium salt and urea;
C, the described solution of step B is added in the solution of steps A, then magnetic agitation 30 min;
D, the mixed system of step C gained is transferred in the teflon-lined reactor, is warmed up to constant temperature 24 h at 180 ℃ of temperature, naturally cooling, obtain the solvent thermal product;
E, by the solvent thermal product centrifugation of step D gained, with deionized water and dehydrated alcohol, wash respectively three times, the product after centrifugation, at 60 ℃ of air drying 6h, obtains precursor;
F, by the precursor of step e gained roasting 120min under 350 ℃ of air atmospheres of retort furnace, can obtain the bismuthous oxide bismuth trioxide (Bi of pattern homogeneous
2O
3) micron ball.
Embodiment 11
A kind of bismuthous oxide bismuth trioxide (Bi
2O
3) preparation method of micron ball, be to carry out according to following step:
A, take the BiCl of 0.25mmol
3With 0.25mmol C
6H
5BiO
7, ultrasonic agitation is dissolved in 10 mL ethylene glycol solutions, forms the soluble bismuth salts solution;
B, take 0.25 mmoL In respectively
2(SO
4)
34H
2O, 0.25mmolInCl
34H
2O and 0.8mmoL urea, magnetic agitation is dissolved in 25 mL ethanol solutions it, forms the mixing solutions of solubility indium salt and urea;
C, the described solution of step B is added in the solution of steps A, then magnetic agitation 30 min;
D, the mixed system of step C gained is transferred in the teflon-lined reactor, is warmed up to constant temperature 24 h at 180 ℃ of temperature, naturally cooling, obtain the solvent thermal product;
E, by the solvent thermal product centrifugation of step D gained, with deionized water and dehydrated alcohol, wash respectively three times, the product after centrifugation, at 60 ℃ of air drying 6h, obtains precursor;
F, by the precursor of step e gained roasting 120min under 400 ℃ of air atmospheres of retort furnace, can obtain the bismuthous oxide bismuth trioxide (Bi of pattern homogeneous
2O
3) micron ball.
The foregoing is only embodiments of the invention; not thereby limit the scope of the claims of the present invention; every equivalent structure or conversion of equivalent flow process that utilizes specification sheets of the present invention to do, or directly or indirectly be used in other relevant technical fields, all in like manner be included in scope of patent protection of the present invention.
Claims (7)
1. solvent-thermal method prepares the bismuthous oxide bismuth trioxide micron ball, it is characterized in that, respectively soluble bismuth salt is dissolved in to ethylene glycol, solubility indium salt and urea are dissolved in dehydrated alcohol, after ultrasonic agitation mixes, obtain precursor through solvent thermal reaction, the precursor centrifuge washing is dried and is made and form by high-temperature roasting.
2. solvent-thermal method according to claim 1 prepares the bismuthous oxide bismuth trioxide micron ball, it is characterized in that, according to following step, carries out:
A, take soluble bismuth salt, ultrasonic agitation is dissolved in ethylene glycol, forms bismuth salt ethylene glycol solution, and described soluble bismuth salt is 0.1～1.0 mmol:5～30 mL with the molecular volume ratio of ethylene glycol;
B, take solubility indium salt and urea respectively, magnetic agitation is dissolved in dehydrated alcohol, form the mixed ethanol solution of indium salt and urea, described solubility indium salt: urea: the molecular volume ratio of dehydrated alcohol is 0.1～1.0 mmol:0.1～1.0 mmol:5～30 mL;
C, the described solution of step B is added in the solution of steps A, then magnetic agitation 30 min;
D, the mixed system of step C gained is transferred in the teflon-lined reactor, is warmed up to 100～180 ℃ of constant temperature 12～36 h, naturally cooling, obtain the solvent thermal product;
E, the solvent thermal product of step D gained is washed respectively three times with deionized water and dehydrated alcohol, after centrifugation, at 60～80 ℃ of air drying 6～12h, obtain precursor;
F, by the precursor of step e gained roasting 60～180min under 350～550 ℃ of air atmospheres of retort furnace, can obtain the bismuthous oxide bismuth trioxide micron ball of pattern homogeneous.
3. solvent-thermal method according to claim 1 and 2 prepares the bismuthous oxide bismuth trioxide micron ball, it is characterized in that, described soluble bismuth salt is any one or several in Bismuth trinitrate, bismuth chloride, bismuth citrate and bismuth sulfate.
4. solvent-thermal method according to claim 1 and 2 prepares the bismuthous oxide bismuth trioxide micron ball, it is characterized in that, described solubility indium salt is any one or several in indium nitrate, indium chloride and indium sulfate.
5. the bismuthous oxide bismuth trioxide micron ball prepared according to the described method of aforementioned arbitrary claim.
6. bismuthous oxide bismuth trioxide micron ball according to claim 5, is characterized in that, described bismuthous oxide bismuth trioxide micron ball is pure phase, the pattern homogeneous, and diameter is about 1～2 μ m.
7. be applied to the photodegradation containing tetracycline wastewater according to the described bismuthous oxide bismuth trioxide micron ball of claim 5 or 6.
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| CN104045107A (en) * | 2014-06-09 | 2014-09-17 | 江苏大学 | Preparation method for three-dimensional laminar six-pointed star indium oxide |
| CN104591264A (en) * | 2015-02-06 | 2015-05-06 | 西安工业大学 | Indium oxide nanosphere and preparation method thereof |
| CN105749918A (en) * | 2016-03-15 | 2016-07-13 | 江苏大学 | Preparation method and application of dual-electroconductivity C/Fe3O4/Bi2O3 complex photocatalyst |
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| GB2605671A (en) * | 2021-04-08 | 2022-10-12 | Qingdao Univ China | Porous bismuth oxide endow seaweed fabric for breath ammonia detection |
| GB2605671B (en) * | 2021-04-08 | 2023-11-29 | Qingdao Univ China | Porous Bismuth Oxide Endow Seaweed Fabric for Breath Ammonia Detection |
| CN113713752A (en) * | 2021-08-20 | 2021-11-30 | 西安交通大学 | Micron flower-like bismuth oxide material, preparation method thereof and application thereof in radioactive anion adsorption |
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| CN113699375A (en) * | 2021-09-01 | 2021-11-26 | 河北工程大学 | Additive solution for improving leaching rate of rare earth elements leached by microorganisms, preparation method and application |
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| CN114944288B (en) * | 2022-06-20 | 2023-04-25 | 江西科技师范大学 | Flower-like bismuth trioxide, preparation method and application thereof, and prepared electrode |
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