CN112808261A - Preparation method of nest-shaped niobium oxide - Google Patents
Preparation method of nest-shaped niobium oxide Download PDFInfo
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- CN112808261A CN112808261A CN202110171210.7A CN202110171210A CN112808261A CN 112808261 A CN112808261 A CN 112808261A CN 202110171210 A CN202110171210 A CN 202110171210A CN 112808261 A CN112808261 A CN 112808261A
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- niobium oxide
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- distilled water
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- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 229910000484 niobium oxide Inorganic materials 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 230000001699 photocatalysis Effects 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000012153 distilled water Substances 0.000 claims abstract description 18
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 18
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 18
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 15
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 150000002821 niobium Chemical class 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 16
- XNHGKSMNCCTMFO-UHFFFAOYSA-D niobium(5+);oxalate Chemical group [Nb+5].[Nb+5].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O XNHGKSMNCCTMFO-UHFFFAOYSA-D 0.000 claims description 8
- 238000007146 photocatalysis Methods 0.000 claims description 8
- 235000005770 birds nest Nutrition 0.000 claims description 4
- 235000005765 wild carrot Nutrition 0.000 claims description 4
- 244000000626 Daucus carota Species 0.000 claims 2
- 230000036632 reaction speed Effects 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 28
- 239000000047 product Substances 0.000 description 17
- 239000010955 niobium Substances 0.000 description 16
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 11
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 6
- 229960000907 methylthioninium chloride Drugs 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 239000002073 nanorod Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- 230000000593 degrading effect Effects 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000010842 industrial wastewater Substances 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 238000013032 photocatalytic reaction Methods 0.000 description 2
- 238000000985 reflectance spectrum Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000009827 uniform distribution Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 231100001234 toxic pollutant Toxicity 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/20—Vanadium, niobium or tantalum
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract
The invention discloses a preparation method of nest-shaped niobium oxide, which comprises the following steps: (1) adding soluble niobium salt into distilled water, and uniformly stirring at 50-70 ℃ to obtain a solution a; (2) dispersing polyvinylpyrrolidone in distilled water, and uniformly stirring to obtain a solution b; (3) dropwise adding the solution b into the solution a, uniformly stirring, and transferring to a hydrothermal reaction kettle; (4) and (3) carrying out high-temperature reaction on the hydrothermal reaction kettle for 10-13h, taking out, cooling to room temperature, drying in an oven, taking out, and grinding to obtain the product. Through the control of raw materials, reaction speed, temperature and drying temperature, the finally prepared product has high purity, high utilization rate of visible light and high photocatalytic efficiency.
Description
Technical Field
The invention relates to the technical field of photocatalytic materials, in particular to a preparation method of nest-shaped niobium oxide.
Background
Niobium oxide is a semiconductor transition metal oxide, has excellent photoelectric properties, and is widely applied in the fields of catalysts, microelectronics, sensors, electrochromism, solar cells and the like. With the stricter requirements of the industrial environmental protection aspect in China at present, the application research of niobium oxide in the field of photocatalysis is more and more, the photocatalysis mechanism is that under the action of light, after transition of valence electrons of niobium oxide, holes are generated in situ, and part of electrons and holes are distributed on the surface of a crystal to form active reaction sites, so that the photocatalysis reaction is initiated, organic toxic pollutants can be oxidatively decomposed, the efficiency is high, the energy consumption is low, and the research value in the aspect of treating industrial wastewater is very high. Since niobium oxide has a band gap width of 3.4 to 4.0eV, absorption of light energy is mainly in the ultraviolet wavelength range, and utilization of light energy is relatively low. In the prior art, research on niobium oxide focuses on two aspects, the light energy utilization rate is improved, in addition, the photocatalytic efficiency is improved, and the specific experimental thought is as follows: on one hand, the band gap width is changed by doping other elements, so that the threshold value of the reaction to light energy is reduced; on the other hand, the light energy utilization rate of the niobium oxide is changed by changing the appearance of the niobium oxide and by band gap overlapping, complementation and the like; the photocatalysis efficiency is greatly influenced in the aspects of specific surface area, transmission rate, active reaction sites and the like while the morphology is changed.
Anhell et al, in "niobium pentoxide nanorod synthesis and photocatalytic performance", disclose: activating the obtained niobic acid (Nb) with hydrofluoric acid and ammonia water in acetic acid solvent2O5·nH2O) is taken as a precursor, a nano-wire-shaped niobium oxide is synthesized by solvothermal synthesis, and a sample is roasted for 1h at the temperature of 400 ℃ to prepare Nb2O5Nano meterA rod. XRD, SEM and TEM analysis show that the prepared Nb is2O5The nano-rod has a hexagonal crystal phase structure and a single crystal form, and grows along the c-axis [ 001 ] direction in a crystallization way. The calcined Nb was tested using methylene blue and rhodamine B as examples2O5The photocatalytic activity of the nano-rods is discovered to be Nb under the irradiation of ultraviolet light2O5The nano-rod has higher photocatalysis effect on two organic dyes. The research is to improve the photocatalytic performance of the niobium oxide by changing the shape of the niobium oxide.
Chinese patent document (application No. 2007101707946) discloses a method for synthesizing vermicular mesoporous niobium oxide. The invention takes amphiphilic block polymer surfactant as a structure directing agent to be dissolved in alcohol solvent, adds niobium source and inorganic salt aqueous solution as a structure promoter, forms colloid after stirring for a period of time at room temperature, heats and volatilizes at low temperature to remove the solvent, and is prepared by drying and high-temperature roasting. The mesoporous niobium oxide material synthesized by the method belongs to a worm-like mesoporous structure, has the characteristics of high specific surface, uniform pore size distribution and the like, is solid medium-strong acid with water resistance, and has wide application in the field of catalysis.
The research focuses on changing the shape of the niobium oxide by changing the synthesis process thereof, so as to improve the function of the niobium oxide in photocatalysis, and the improvement effect on the light energy utilization rate is limited.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for preparing a bird nest-shaped niobium oxide, which is simple in preparation process, high in purity of the prepared bird nest-shaped niobium oxide, 2.62eV in forbidden band width, high in utilization rate of visible light, and high in catalytic efficiency.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of nest-shaped niobium oxide comprises the following steps:
(1) adding soluble niobium salt into distilled water, and uniformly stirring at 50-70 ℃ to obtain a solution a;
(2) dispersing polyvinylpyrrolidone in distilled water, and uniformly stirring to obtain a solution b;
(3) dropwise adding the solution b into the solution a, uniformly stirring, and transferring to a hydrothermal reaction kettle;
(4) and (3) carrying out high-temperature reaction on the hydrothermal reaction kettle for 10-13h, taking out, cooling to room temperature, drying in an oven, taking out, and grinding to obtain the product.
Further, the niobium salt is niobium oxalate.
Further, the weight ratio of the niobium salt to the distilled water in the step (1) is 1: 24-26.
Further, the weight ratio of the polyvinylpyrrolidone to the distilled water in the step (2) is 0.1-0.9: 10.
further, the drying temperature of the oven is 80 ℃, and the drying time is 24 hours.
Further, the high temperature in the step (4) is 170-190 ℃.
A nest-shaped niobium oxide prepared by the preparation method of nest-shaped niobium oxide.
Application of the nest-shaped niobium oxide prepared by the preparation method of the nest-shaped niobium oxide in photocatalysis.
The invention has the beneficial effects that:
1. the invention discloses a preparation method of nest-shaped niobium oxide, which is characterized in that the purity of the finally prepared product is high, the utilization rate of visible light is high, the specific surface area is large, and the photocatalytic efficiency is high by controlling the raw materials, the reaction speed, the temperature and the drying temperature.
2. The preparation method takes soluble niobium salt (niobium oxalate) and polyvinylpyrrolidone as raw materials, wherein the polyvinylpyrrolidone can slowly nucleate the product after being slowly added into the niobium oxalate, the product is formed, the stabilizer is used, and after high-temperature reaction and drying, the nest-shaped niobium oxide is formed.
3. The prepared nest-shaped niobium oxide has very high purity through IR and XRD pattern analysis; SEM microscopic characterization can see that Nb has a bird nest structure2O5The product has very regular appearance and uniform distribution of internal pore channels, thereby greatly increasing the product ratioSurface area.
4. As can be seen from the ultraviolet and visible diffuse reflection light absorption spectrogram, the nest-shaped niobium oxide prepared by the preparation process has the forbidden band width of 2.62eV, can absorb all ultraviolet light and visible light within the wavelength range of 200-800 nm, and has the utilization rate of the visible light far higher than that of the prior art.
5. The photocatalytic performance of the product prepared by the method is detected, and the method can degrade 82% of MO and conventional Nb when the reaction is carried out for 25min2O5Only 30% of MO can be degraded; the rate constant for degrading MO was 0.05811min-1Is conventional Nb2O5（0.00979 min-1) 5.94 times of (B), shows Nb2O5The reaction speed of degrading MO by PVP is faster, and the reaction efficiency is higher.
Drawings
FIG. 1 is an IR image of a product of the invention.
Figure 2 is the XRD pattern of the product.
Fig. 3 is an SEM image of the product.
FIG. 4 is a graph of the UV-visible diffuse reflectance spectrum of a product.
FIG. 5 is a diagram of the photocatalytic effect of the product.
FIG. 6 is a graph of the photocatalytic rate of the product.
Detailed Description
The invention is further described below with reference to the figures and examples.
Example 1
A preparation method of nest-shaped niobium oxide comprises the following steps:
(1) adding 1g of niobium oxalate into 25mL of distilled water, and stirring at 60 ℃ for 10min to obtain a solution a;
(2) 0.5 g of polyvinylpyrrolidone is taken to be dispersed in 10mL of distilled water and stirred for five minutes to be used as a solution b;
(3) dropwise adding the solution b into the solution a, stirring for 10min, and transferring to a 50mL hydrothermal reaction kettle;
(4) and (3) reacting the hydrothermal reaction kettle in an oven at 180 ℃ for 12 h, taking out, cooling to room temperature, drying in the oven at 80 ℃ for 24h, taking out a sample, and grinding for later use.
Example 2
A preparation method of nest-shaped niobium oxide comprises the following steps:
(1) adding 1g of niobium oxalate into 24mL of distilled water, and stirring at 50 ℃ for 10min to obtain a solution a;
(2) 0.1g of PVP (polyvinylpyrrolidone) is taken to be dispersed in 10mL of distilled water and stirred for five minutes to be used as a solution b;
(3) dropwise adding the solution b into the solution a, stirring for 10min, and transferring to a 50mL hydrothermal reaction kettle;
(4) and (3) reacting the hydrothermal reaction kettle in an oven at 170 ℃ for 13h, taking out, cooling to room temperature, drying in the oven at 80 ℃ for 24h, taking out a sample, and grinding for later use.
Example 3
A preparation method of nest-shaped niobium oxide comprises the following steps:
(1) adding 1g of niobium oxalate into 25mL of distilled water, and stirring at 60 ℃ for 10min to obtain a solution a;
(2) 0.9g of polyvinylpyrrolidone is taken to be dispersed in 10mL of distilled water and stirred for five minutes to be used as a solution b;
(3) dropwise adding the solution b into the solution a, stirring for 10min, and transferring to a 50mL hydrothermal reaction kettle;
(4) and (3) reacting the hydrothermal reaction kettle in an oven at 190 ℃ for 10h, taking out, cooling to room temperature, drying in the oven at 80 ℃ for 24h, taking out a sample, and grinding for later use.
Example 4
A preparation method of nest-shaped niobium oxide comprises the following steps:
(1) adding 1g of niobium oxalate into 26mL of distilled water, and stirring at 70 ℃ for 10min to obtain a solution a;
(2) 0.7g of polyvinylpyrrolidone is taken to be dispersed in 10mL of distilled water and stirred for five minutes to be used as a solution b;
(3) dropwise adding the solution b into the solution a, stirring for 10min, and transferring to a 50mL hydrothermal reaction kettle;
(4) and (3) reacting the hydrothermal reaction kettle in an oven at 180 ℃ for 10h, taking out, cooling to room temperature, drying in the oven at 80 ℃ for 24h, taking out a sample, and grinding for later use.
Product characterization and photocatalytic performance detection
1. Characterization of the product
The phase, microstructure and the like of the sample prepared in the embodiment 1 of the invention are detected and analyzed, wherein the Fourier transform infrared spectrum analysis result is shown in figure 1, and the X-ray diffractometer phase analysis result is shown in figure 2; the results of the SEM analysis are shown in FIG. 3; the ultraviolet-visible diffuse reflectance spectrum is shown in FIG. 4.
As can be seen from the infrared spectrum in fig. 1, and Nb2O5Compared with a standard product, the nest-shaped niobium oxide (Nb) prepared by the method2O5/PVP) at 520cm-1~820cm-1Has Nb-O bond and Nb-O-Nb bond stretching vibration peak, and the coupling is generated at 1500cm-1~2500cm-1The characteristic absorption peak between corresponds to the absorption of H2Bending vibration of O at 3400cm-1~3500cm-1The characteristic absorption peak between belongs to the sample adsorption H2The hydroxyl (-OH) group of O vibrates telescopically.
As can be seen from the X-ray diffraction pattern of fig. 2, Nb appeared at 2 Ɵ =23.022 °, 33.626 °, 46.483 °, 55.114 °2O5The characteristic diffraction peaks of (2) correspond to crystal planes of (101), (107), (200), and (208).
As can be seen by combining the infrared spectrogram of FIG. 1 and the X-ray diffraction pattern of FIG. 2, the sample prepared by the preparation process of the present application is Nb2O5And the purity is very high.
As is apparent from the SEM image of FIG. 3, a large number of Nb in birdcage structure2O5The product has very regular appearance, uniform distribution of internal pore channels, greatly increased specific surface area, unique structure for nest-shaped niobium oxide (Nb)2O5PVP) and the photocatalytic performance.
FIG. 4 is a graph of diffuse reflection spectrum of ultraviolet and visible light, from which it can be seen that the width of the energy gap of the bird-nest-shaped niobium oxide prepared by the present application is 2.62eV, and the bird-nest-shaped niobium oxide has absorption in the wavelength range of 200-800 nm, i.e. all ultraviolet light and visible light can be absorbed, which illustrates the bird-nest prepared by the preparation process of the present applicationNiobium (Nb) oxide2O5PVP) has higher utilization rate of the solar spectral energy.
2. Photocatalytic Performance detection
Using methylene blue (MO) solution to simulate industrial wastewater, 100mg of the photocatalyst, i.e., bird's nest-shaped niobium oxide (Nb) oxide in the method of example 1, was weighed out during photocatalytic reaction using a 300W xenon lamp as a light source, i.e., CEL-HXF300, a source of Mikan Kagaku, Beijing2O5/PVP) was added to 100mL of 50mg/L methylene blue solution and stirred in the dark for 1h to reach equilibrium between adsorption and desorption of the dye and the photocatalyst. In the degradation process, the distance between the visible light liquid level and the light source is kept at 20cm, and magnetic stirring is carried out. Approximately 3mL of methylene blue solution was removed at intervals. Centrifuging for 5min at 3000r/min, and collecting the supernatant to determine its absorbance. Degradation rate of methylene blue by C/C0Is represented by the formula (I) in which C0-absorbance of the initial solution; c-absorbance of the solution at different degradation reaction times, the results are shown in FIGS. 5 and 6.
As can be seen from FIG. 5, the bird's nest-shaped niobium oxide (Nb) prepared by the present application proceeded for 25min when the photocatalytic reaction proceeded2O5/PVP) degrades 82% of MO compared to conventional Nb2O5Only 30% of MO can be degraded; as can be seen from FIG. 6, the nest-like niobium oxide (Nb)2O5/PVP) rate constant for degradation of MO was 0.05811min-1Is conventional Nb2O5（0.00979min-1) 5.94 times of (B), shows Nb2O5The reaction speed of degrading MO by PVP is higher, the reaction efficiency is higher, and the application cost can be saved.
Finally, the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting, and other modifications or equivalent substitutions made by the technical solutions of the present invention by those of ordinary skill in the art should be covered within the scope of the claims of the present invention as long as they do not depart from the spirit and scope of the technical solutions of the present invention.
Claims (8)
1. A preparation method of nest-shaped niobium oxide is characterized by comprising the following steps: the method comprises the following steps:
(1) adding soluble niobium salt into distilled water, and uniformly stirring at 50-70 ℃ to obtain a solution a;
(2) dispersing polyvinylpyrrolidone in distilled water, and uniformly stirring to obtain a solution b;
(3) dropwise adding the solution b into the solution a, uniformly stirring, and transferring to a hydrothermal reaction kettle;
(4) and (3) carrying out high-temperature reaction on the hydrothermal reaction kettle for 10-13h, taking out, cooling to room temperature, drying in an oven, taking out, and grinding to obtain the product.
2. The method for preparing bird nest-shaped niobium oxide according to claim 1, characterized in that: the niobium salt is niobium oxalate.
3. The method for preparing bird nest-shaped niobium oxide according to claim 1, characterized in that: in the step (1), the weight ratio of the niobium salt to the distilled water is 1: 24-26.
4. The method for preparing bird nest-shaped niobium oxide according to claim 1, characterized in that: in the step (2), the weight ratio of the polyvinylpyrrolidone to the distilled water is 0.1-0.9: 10.
5. the method for preparing bird nest-shaped niobium oxide according to claim 1, characterized in that: the drying temperature of the oven is 80 ℃, and the drying time is 24 hours.
6. The method for preparing bird nest-shaped niobium oxide according to claim 1, characterized in that: the high temperature in the step (4) is 170-190 ℃.
7. A bird's nest of niobium oxide made by the method of claim 1.
8. Use of the bird's nest of niobium oxide prepared by the method of claim 1 in photocatalysis.
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