CN105381813A - Preparation method of carbon and nitrogen doped niobium (V) pentoxide nano sheet and application of nano sheet as photocatalyst - Google Patents
Preparation method of carbon and nitrogen doped niobium (V) pentoxide nano sheet and application of nano sheet as photocatalyst Download PDFInfo
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Abstract
The invention discloses a preparation method of a carbon and nitrogen doped niobium (V) pentoxide nano sheet and an application of the nano sheet as a photocatalyst. The preparation method comprises the following steps: weighing soluble niobium salt at a room temperature, adding anhydrous ethanol to form an ethanol solution of niobium salt, dropwise adding an organic ammonium hydroxide solution into the ethanol solution of niobium salt, wherein in the initial phase, white turbidity appears, keeping on adding the organic ammonium hydroxide solution until the white turbidity disappears so as to form a clear and transparent solution; transferring the obtained solution to a hydrothermal reactor, wherein the solution accounts for 50 to 70% of the volume of the hydrothermal reactor, carrying out hydrothermal reactions at a temperature of 100 to 280 DEG C, after reactions, naturally cooling the reactor to the room temperature, washing and drying the reaction product to obtain white powder; and burning the white powder for 2 to 12 hours at a temperature of 400 to 1200 under the protection of nitrogen gas so as to obtain the carbon and nitrogen doped niobium (V) pentoxide nano sheet. The invention also discloses an application of the carbon and nitrogen doped niobium (V) pentoxide nano sheet as a photocatalyst. The photocatalyst can be applied to benzyl alcohol oxidation to prepare benzaldehyde.
Description
Technical field
Nano material of the present invention and catalytic field, the particularly preparation method of the niobium pentoxide nano sheet of a kind of doping carbon, nitrogen and the application as photochemical catalyst thereof.
Background technology
Two-dimension nano materials is as Graphene, molybdenum bisuphide (MoS
2) nano thin-film, TiO
2nano thin-film, ZnO nano sheet etc. owing to having the abundant catalytic reaction activity site in large specific area and layer structure material edge, and are widely used in the photocatalysis field such as photocatalytic degradation of dye, photocatalysis conversion of methane, photolysis water hydrogen and photocatalysis synthesis of organic substance.In semiconductor catalyst, Nb
2o
5although belong to broad stopband oxide (3.2 ~ 4.0eV), Nb
2o
5there is the advantage such as acid and alkali-resistance, resistance to photoetch, in photosensitive dye battery, photocatalysis synthesis, photocatalysis degradation organic contaminant etc., receive the attention of researcher.
Existing nano-powder (CN101700910 in patent, a kind of preparation method of spherical nanoscale niobium pentaoxide powder), nano-hollow ball (CN101746826B mono-kind prepares the method for niobium pentoxide hollow nanosphere) and nano wire (method of a CN103253708B acetate solvate hot preparation pentoxide nanowire by use) report, but niobium pentoxide nano sheet report also fewer.In general, niobium pentoxide nano sheet is all utilize the method for chemical stripping to synthesize, as CN101570402B.First at high temperature form the base metal niobate of stratiform, then use concentrated acid ion-exchange, peel off with cationic chemical intercalations such as TBuAs more further, thus form nanometer sheet.This method step is many, and combined coefficient is low.Another method is exactly the mode (namely mode) from top to bottom of bottom-up, adds protective agent, thus forms nanometer sheet.Report in patent CN104852015A, add in the mixed solution of water and ethylenediamine at solubility niobium salt (acetic acid niobium, fluoridize niobium, niobium chloride, iodate niobium and bromination niobium), hydro-thermal method defines niobium pentoxide nano sheet.KeizoNakagawa reports ethanol niobium and is dissolved in triethanolamine, adds ammoniacal liquor and keeps pH=12.8, be then transferred in hydrothermal reaction kettle by this suspension, react 24 hours, can obtain mono-layer oxidized niobium nanometer sheet at 160 DEG C.
This patent take columbium pentachloride as niobium source, and with the hydroxide of organic ammonium for precipitating reagent and template, synthesized 2 ~ 10 layers of nano lamellar thing, interlayer exists organoammonium ions.Calcine completely cut off the condition of air at high temperature under, obtain a kind of ultra-thin dopant carbon, nitrogen niobium pentoxide nano sheet and as light-catalysed application.
Summary of the invention
In sum, in order to achieve the above object.The invention provides a kind of doping carbon, the preparation method of niobium pentoxide nano sheet of nitrogen and the application as photochemical catalyst thereof.
A preparation method for the niobium pentoxide nano sheet of doping carbon, nitrogen, comprises the steps:
Step one: at room temperature, takes the solubility niobium salt of 0.1 ~ 10 mass parts, adds the absolute ethyl alcohol of 10 ~ 70 parts by volume, forms settled solution for subsequent use;
Step 2: in settled solution prepared by step one, drip the organic ammonium hydroxides solution of 25%, control rate of addition, form white opacity during beginning, continues to drip organic ammonium hydroxides solution and disappears to white opacity, form clear solution for subsequent use;
Step 3: the clear solution of step 2 gained is transferred in hydrothermal reaction kettle, loadings be kettle long-pending 50% ~ 70%, hydrothermal temperature is 100 ~ 280 DEG C, reaction time is 8 ~ 96 hours, after reaction, reactor is down to room temperature naturally, washing, drying, obtains white powder;
Step 4: by step 3 gained white powder in nitrogen atmosphere, calcining 2 ~ 12 hours at 400 ~ 1200 DEG C, the niobium pentoxide nano sheet of a kind of doping carbon, nitrogen can be obtained.
Further, the solubility niobium salt in described step one is: the hydrogen fluoride lysate of ammonium niobium oxalate or columbium pentachloride or niobic acid.
Further, the organic ammonium hydroxides in described step 2 is: TMAH or tetraethyl ammonium hydroxide or TBAH.
The niobium pentoxide nano sheet of a kind of doping carbon, nitrogen is as the application of photochemical catalyst.
beneficial effect:
Doping carbon synthesized by the present invention, nitrogen niobium pentoxide nano sheet have good pattern, and nanometer sheet thickness is 0.3 ~ 10 nanometer, is of a size of 100 ~ 1000nm, and product specific area is large, has multistage microstructural; The method has simply, and reaction temperature is low, reproducible, the advantage that cost is low.Doping carbon synthesized by the present invention, nitrogen niobium pentoxide nano sheet as solid acid catalyst, can also can be applicable to photosensitive dye battery, in lithium ion battery.Having the invention still further relates to synthesized doping carbon, nitrogen niobium pentoxide nano sheet as photocatalyst applications is in the organic synthesis of benzaldehyde in photocatalysis benzyl alcohol oxidation.
Accompanying drawing explanation
The X-ray diffractogram of the niobium pentoxide nano sheet of Fig. 1 prepared by the present invention.
The scanning electron microscope (SEM) photograph of the niobium pentoxide nano sheet of Fig. 2 prepared by the present invention.
The transmission electron microscope picture of the niobium pentoxide nano sheet of Fig. 3 prepared by the present invention.
The AFM figure of the niobium pentoxide nano sheet of Fig. 4 prepared by the present invention.
The infrared spectrogram of the niobium pentoxide nano sheet of Fig. 5 prepared by the present invention.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is further illustrated:
embodiment 1
A preparation method for the niobium pentoxide nano sheet of doping carbon, nitrogen, comprises the steps:
At room temperature (10-40 DEG C), 3.24g columbium pentachloride is dissolved in 40ml absolute ethyl alcohol, ultrasonic 10 minutes, form the solution of clear, then the tetramethyl ammonium hydroxide solution that 25ml concentration is 25% will dropwise be added in ethanolic solution, control drop rate is 0.27ml/min, stirs 30 minutes, obtains a settled solution.What this solution is transferred to 100ml has in teflon-lined reactor, 240 DEG C of hydro-thermal reactions 24 hours, after cool to room temperature, with Filter paper filtering, with the distilled water washing of 2000 ~ 3000 milliliters, then uses absolute ethanol washing.By much filtrate at 100 DEG C dry 8 hours, obtain niobium pentoxide nano sheet.By the niobium pentoxide nano sheet of gained in nitrogen atmosphere, calcining 2 hours in Muffle furnace at 500 DEG C, the niobium pentoxide nano sheet of doping carbon, nitrogen just can be obtained.
The X-ray diffractogram of the niobium pentoxide nano sheet of Fig. 1 prepared by the present invention, the diffraction maximum of niobium pentoxide nano sheet corresponds to the stratiform niobium oxide that ICSD is numbered #91098.And at N
2atmosphere 500 DEG C calcining is after 2 hours, and the diffraction maximum of the niobium pentoxide nano sheet of doping carbon, nitrogen corresponds to the monocline niobium pentaoxide that JCPDS label is 27-1311.
The scanning electron microscope (SEM) photograph of the niobium pentoxide nano sheet of Fig. 2 prepared by the present invention.As can be seen from the figure, synthesized nanometer sheet constitutes flower-shaped, does not have the impurity of other patterns.
The transmission electron microscope picture of the niobium pentoxide nano sheet of Fig. 3 prepared by the present invention.As can be seen from the figure synthesized nanometer sheet is very thin, and electronic diffraction is shown as the point diffraction of rule, and the nanometer sheet synthesized by explanation has mono-crystalline structures.
The AFM figure of the niobium pentoxide nano sheet of Fig. 4 prepared by the present invention.The thickness of nanometer sheet is about 2.8 nanometers as can be seen from Fig..
The infrared spectrogram of the niobium pentoxide nano sheet of Fig. 5 prepared by the present invention.1488cm in figure
-1the absworption peak at place is the stretching vibration peak of C-N key in quaternary ammonium salt, shows containing tetramethyl-ammonium radical ion between synthesized nanoscale twins, at N
2under atmosphere during roasting, carbon, nitrogen-doping can be entered in niobium oxide.
embodiment 2
A preparation method for the niobium pentoxide nano sheet of doping carbon, nitrogen, comprises the steps:
At room temperature (10-40 DEG C), 3.24g columbium pentachloride is dissolved in 40ml absolute ethyl alcohol, ultrasonic 10 minutes, form the solution of clear, then the tetraethyl ammonium hydroxide solution that 30ml concentration is 25% will dropwise be added in ethanolic solution, control drop rate is 0.27ml/min, stirs 30 minutes, obtains a settled solution.What this solution is transferred to 100ml has in teflon-lined reactor, 220 DEG C of hydro-thermal reactions 24 hours, after cool to room temperature, with Filter paper filtering, with the distilled water washing of 2000 ~ 3000 milliliters, then uses absolute ethanol washing.By much filtrate at 100 DEG C dry 8 hours, obtain niobium pentoxide nano sheet.By the niobium pentoxide nano sheet of gained in nitrogen atmosphere, calcining 2 hours in Muffle furnace at 400 DEG C, the niobium pentoxide nano sheet of doping carbon, nitrogen just can be obtained.
embodiment 3
A preparation method for the niobium pentoxide nano sheet of doping carbon, nitrogen, comprises the steps:
At room temperature (10-40 DEG C), 1.5g ammonium niobium oxalate is dissolved in 30ml absolute ethyl alcohol, ultrasonic 10 minutes, form the solution of clear, then the tetramethyl ammonium hydroxide solution that 35ml concentration is 25% will dropwise be added in ethanolic solution, control drop rate is 0.27ml/min, stirs 30 minutes, obtains a settled solution.What this solution is transferred to 100ml has in teflon-lined reactor, 250 DEG C of hydro-thermal reactions 24 hours, after cool to room temperature, with Filter paper filtering, with the distilled water washing of 2000 ~ 3000 milliliters, then uses absolute ethanol washing.By much filtrate at 100 DEG C dry 8 hours, obtain niobium pentoxide nano sheet.By the niobium pentoxide nano sheet of gained in nitrogen atmosphere, calcining 2 hours in Muffle furnace at 600 DEG C, the niobium pentoxide nano sheet of doping carbon, nitrogen just can be obtained.
embodiment 4
A preparation method for the niobium pentoxide nano sheet of doping carbon, nitrogen, comprises the steps:
At room temperature (10-40 DEG C), 1.5g ammonium niobium oxalate is dissolved in 20ml absolute ethyl alcohol, ultrasonic 10 minutes, form the solution of clear, then the TBAH solution that 35ml concentration is 25% will dropwise be added in ethanolic solution, control drop rate is 0.27ml/min, stirs 30 minutes, obtains a settled solution.What this solution is transferred to 100ml has in teflon-lined reactor, 220 DEG C of hydro-thermal reactions 24 hours, after cool to room temperature, with Filter paper filtering, with the distilled water washing of 2000 ~ 3000 milliliters, then uses absolute ethanol washing.By much filtrate at 100 DEG C dry 8 hours, obtain niobium pentoxide nano sheet.By the niobium pentoxide nano sheet of gained in nitrogen atmosphere, calcining 2 hours in Muffle furnace at 500 DEG C, the niobium pentoxide nano sheet of doping carbon, nitrogen just can be obtained.
embodiment 5
The niobium pentoxide nano sheet of a kind of doping carbon, nitrogen is as the application of photochemical catalyst:
Get the phenmethylol aqueous solution 10mL of 10mmol/L, add the catalyst 50mg after calcining, together put into the jacketed reactor with temperature-adjustable, be placed on by reactor on electromagnetic mixing apparatus together with little magneton, arranging rotating speed is 30r/min, dark treatment half an hour.Connect oxygen, open low temperature thermostat bath, the temperature of whole experiment is controlled at 25 DEG C.Again mixed solution is transferred to illumination under xenon lamp, light-catalyzed reaction 2 ~ 24 hours.Then take off reactor, use syringe draw samples, with the membrane filtration with 0.2 micron of filter opening.By the concentration of the solution after filtration with phenmethylol and benzaldehyde in solution after gas chromatograph test reaction, calculate the conversion ratio of phenmethylol and the selective of benzaldehyde.As in table one, niobium pentoxide nano sheet photocatalysis benzyl alcohol oxidation is the catalytic activity of benzaldehyde.Table one shows the catalytic activity that synthesized niobium oxide nanometer sheet has photochemical catalytic oxidation phenmethylol, and carbon, after N doping, catalytic activity significantly improves.Under UV-irradiation, the conversion ratio of phenmethylol is 51.3%.
Table one niobium pentaoxide nanometer sheet photocatalysis benzyl alcohol oxidation is the catalytic activity of benzaldehyde
Nb
2o
5-NS is niobium pentoxide nano sheet, Nb
2o
5-NS-C-N is the niobium pentoxide nano sheet of doping carbon, nitrogen.Reaction condition is: phenmethylol 10mmol/L, 10ml, catalyst quality 50mg, light application time 2h.
Although above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, all belong to the scope of protection of present invention.
Claims (4)
1. a preparation method for the niobium pentoxide nano sheet of doping carbon, nitrogen, is characterized in that, comprise the following steps:
Step one: at room temperature, takes the solubility niobium salt of 0.1 ~ 10 mass parts, adds the absolute ethyl alcohol of 10 ~ 70 parts by volume, forms settled solution for subsequent use;
Step 2: in settled solution prepared by step one, drip the organic ammonium hydroxides solution of 25%, control rate of addition, form white opacity during beginning, continues to drip organic ammonium hydroxides solution and disappears to white opacity, form clear solution for subsequent use;
Step 3: the clear solution of step 2 gained is transferred in hydrothermal reaction kettle, loadings be kettle long-pending 50% ~ 70%, hydrothermal temperature is 100 ~ 280 DEG C, reaction time is 8 ~ 96 hours, after reaction, reactor is down to room temperature naturally, washing, drying, obtains white powder;
Step 4: by step 3 gained white powder in nitrogen atmosphere, calcining 2 ~ 12 hours at 400 ~ 1200 DEG C, the niobium pentoxide nano sheet of a kind of ultra-thin dopant carbon, nitrogen can be obtained.
2. the preparation method of the niobium pentoxide nano sheet of a kind of doping carbon according to claim 1, nitrogen, is characterized in that, the solubility niobium salt in described step one is: the hydrogen fluoride lysate of ammonium niobium oxalate or columbium pentachloride or niobic acid.
3. the preparation method of the niobium pentoxide nano sheet of a kind of doping carbon according to claim 1, nitrogen, is characterized in that, the organic ammonium hydroxides in described step 2 is: TMAH or tetraethyl ammonium hydroxide or TBAH.
4. the niobium pentoxide nano sheet of a doping carbon, nitrogen is as the application of photochemical catalyst.
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Cited By (9)
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| CN107055613A (en) * | 2017-02-27 | 2017-08-18 | 湖南工业大学 | One kind is without substrate niobium pentoxide nano chip arrays negative material and its preparation method and application |
| CN108097250A (en) * | 2017-11-09 | 2018-06-01 | 浙江裕文环保科技有限公司 | Can the infrared shortwave of efficient absorption Thief zone nanometer infrared excitation matchmaker, its preparation method and its application in air purification |
| CN109046421A (en) * | 2018-07-24 | 2018-12-21 | 山东科技大学 | It is a kind of to prepare C, N co-doped nano pipe/stick catalysis material method using quaternary ammonium base |
| CN110935482A (en) * | 2019-11-20 | 2020-03-31 | 华南农业大学 | Semiconductor NbNO nanosheet and preparation method and application thereof |
| CN111153437A (en) * | 2019-12-25 | 2020-05-15 | 苏州机数芯微科技有限公司 | Blue niobium pentoxide and preparation method and application thereof |
| CN111470535A (en) * | 2020-04-17 | 2020-07-31 | 扬州大学 | Niobium pentoxide yolk structure nano material with controllable core volume and preparation method thereof |
| CN112337457A (en) * | 2020-11-11 | 2021-02-09 | 郑州轻工业大学 | Mo-doped HNb3O8Preparation method and application of nanosheet |
| CN112661675A (en) * | 2021-01-07 | 2021-04-16 | 中国科学院青岛生物能源与过程研究所 | Synthetic method of alpha-carbonyl sulfonate and catalyst used by same |
| CN113851332A (en) * | 2021-08-26 | 2021-12-28 | 合肥工业大学 | Niobium oxynitride with adjustable nitrogen-oxygen atom ratio and preparation method and energy storage application thereof |
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| CN107055613A (en) * | 2017-02-27 | 2017-08-18 | 湖南工业大学 | One kind is without substrate niobium pentoxide nano chip arrays negative material and its preparation method and application |
| CN108097250A (en) * | 2017-11-09 | 2018-06-01 | 浙江裕文环保科技有限公司 | Can the infrared shortwave of efficient absorption Thief zone nanometer infrared excitation matchmaker, its preparation method and its application in air purification |
| CN108097250B (en) * | 2017-11-09 | 2019-11-19 | 浙江裕文环保科技有限公司 | Can the infrared shortwave of efficient absorption Thief zone nanometer infrared excitation matchmaker, preparation method, and its application in air cleaning |
| CN109046421A (en) * | 2018-07-24 | 2018-12-21 | 山东科技大学 | It is a kind of to prepare C, N co-doped nano pipe/stick catalysis material method using quaternary ammonium base |
| CN110935482A (en) * | 2019-11-20 | 2020-03-31 | 华南农业大学 | Semiconductor NbNO nanosheet and preparation method and application thereof |
| CN111153437B (en) * | 2019-12-25 | 2022-03-18 | 苏州机数芯微科技有限公司 | Blue niobium pentoxide and preparation method and application thereof |
| CN111153437A (en) * | 2019-12-25 | 2020-05-15 | 苏州机数芯微科技有限公司 | Blue niobium pentoxide and preparation method and application thereof |
| CN111470535A (en) * | 2020-04-17 | 2020-07-31 | 扬州大学 | Niobium pentoxide yolk structure nano material with controllable core volume and preparation method thereof |
| CN112337457A (en) * | 2020-11-11 | 2021-02-09 | 郑州轻工业大学 | Mo-doped HNb3O8Preparation method and application of nanosheet |
| CN112337457B (en) * | 2020-11-11 | 2023-02-03 | 郑州轻工业大学 | Mo-doped HNb 3 O 8 Preparation method and application of nanosheet |
| CN112661675A (en) * | 2021-01-07 | 2021-04-16 | 中国科学院青岛生物能源与过程研究所 | Synthetic method of alpha-carbonyl sulfonate and catalyst used by same |
| CN112661675B (en) * | 2021-01-07 | 2022-10-21 | 中国科学院青岛生物能源与过程研究所 | Synthetic method of alpha-carbonyl sulfonate and catalyst used by same |
| CN113851332A (en) * | 2021-08-26 | 2021-12-28 | 合肥工业大学 | Niobium oxynitride with adjustable nitrogen-oxygen atom ratio and preparation method and energy storage application thereof |
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