CN105688965A - Preparation method of mesoporous niobium pentoxide/nitrogen-doped graphene efficient composite photocatalyst - Google Patents
Preparation method of mesoporous niobium pentoxide/nitrogen-doped graphene efficient composite photocatalyst Download PDFInfo
- Publication number
- CN105688965A CN105688965A CN201610018709.3A CN201610018709A CN105688965A CN 105688965 A CN105688965 A CN 105688965A CN 201610018709 A CN201610018709 A CN 201610018709A CN 105688965 A CN105688965 A CN 105688965A
- Authority
- CN
- China
- Prior art keywords
- preparation
- solution
- nitrogen
- ngr
- graphene oxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 56
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 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 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 24
- 239000002131 composite material Substances 0.000 title claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 36
- 238000000034 method Methods 0.000 claims description 19
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 12
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 12
- 239000006185 dispersion Substances 0.000 claims description 12
- 229960004756 ethanol Drugs 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000013019 agitation Methods 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 239000004202 carbamide Substances 0.000 claims description 6
- 235000013877 carbamide Nutrition 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 238000003760 magnetic stirring Methods 0.000 claims description 6
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 6
- 229910052753 mercury Inorganic materials 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 230000000802 nitrating effect Effects 0.000 claims description 6
- YHBDIEWMOMLKOO-UHFFFAOYSA-I pentachloroniobium Chemical compound Cl[Nb](Cl)(Cl)(Cl)Cl YHBDIEWMOMLKOO-UHFFFAOYSA-I 0.000 claims description 6
- 238000007540 photo-reduction reaction Methods 0.000 claims description 6
- 229950000845 politef Drugs 0.000 claims description 6
- 238000003980 solgel method Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 238000002372 labelling Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 4
- 230000001699 photocatalysis Effects 0.000 abstract description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 2
- 239000001257 hydrogen Substances 0.000 abstract description 2
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract 1
- -1 niobium pentoxide compound Chemical class 0.000 abstract 1
- 229910052755 nonmetal Inorganic materials 0.000 abstract 1
- 238000011084 recovery Methods 0.000 abstract 1
- 230000027756 respiratory electron transport chain Effects 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 125000004433 nitrogen atom Chemical group N* 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 150000001721 carbon Chemical group 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003863 metallic catalyst Substances 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/39—
Abstract
The invention discloses a preparation method of a mesoporous niobium pentoxide/nitrogen-doped graphene efficient composite photocatalyst.The preparation method comprises the first step of preparing a nitrogen-doped graphene oxide solution, the second step of preparing mesoporous niobium pentoxide and the third step of preparing the mesoporous niobium pentoxide/nitrogen-doped graphene efficient composite photocatalyst.The interface bonding of graphene and the mesoporous niobium pentoxide is improved and electron transfer performance is enhanced by modifying the graphene oxide through non-metal nitrogen, and therefore the photocatalytic efficiency of the graphene/mesoporous niobium pentoxide compound is improved.The mesoporous niobium pentoxide/nitrogen-doped graphene photocatalyst can rapidly and effectively decompose water for hydrogen production, and is high in recovery rate, free of secondary pollution and environmentally friendly.
Description
Technical field
The present invention relates to semiconductor light-catalyst preparation field, the preparation method being specifically related to a kind of mesoporous niobium pentaoxide/nitrogen-doped graphene high-efficiency composite photocatalyst。
Background technology
Under the severe challenge of global energy crisis and environmental pollution; photocatalysis technology is as emerging, efficient, energy-conservation Modern Green green technology, it is possible to directly utilize solar photolysis water hydrogen to produce clean energy resource or degradable organic pollutant and to become newly wishing of following new and high technology。
N-type semiconductor niobium pentaoxide (Nb in recent years2O5), it is widely used by self excellent catalytic performance, stable in properties, safety, purification, the advantage such as controlledly synthesis of durable, pattern。And nanometer Nb2O5Energy gap be 3.4eV, the ultraviolet light (λ < 365nm) of occupied sunlight 3～5% can only be excited and can optionally be exposed high activity or particular energy crystal face simultaneously, increased substantially the utilization rate of catalysis activity, stability, selectivity and solar energy。Research finds that ordered mesopore structure has the feature such as good crystalline structure and higher specific surface area, light-catalyzed reaction can reduce the photo-generate electron-hole probability to compound, it is also beneficial to the photogenerated charge fast transfer on its surface, and then improves its photocatalysis performance。
Nitrogen-doped graphene is by Graphene sp2The carbon atom of hydridization introduces nitrogen-atoms formed；Owing to the entrance of nitrogen-atoms changes the kinetic activity approach of Graphene, the nitrogen-atoms namely adulterated can affect the electronegativity of carbon atom in Graphene so that the carbon atom around nitrogen-atoms, with positive charge, causes that graphenic surface produces high " active site "；These high " active sites " can directly participate in redox reaction, improves photocatalysis usefulness。Synthesizing at present in the process of quasiconductor/nitrogen catalyst, the nitrogen content mixed is wayward and easily causes loss；So nitrogen-doped graphene has not only been assembled all advantages of graphen catalyst but also has been improve the utilization rate of nitrogen。It addition, compared with precious metals pt/C (platinum/carbon) catalyst, nitrogen-doped graphene has high catalytic activity and electrochemical stability as non-metallic catalyst；Therefore, it is widely believed that nitrogen-doped graphene is one of noble metal catalyst ideal substitution material。Prior art not yet openly has the synthetic method of the mesoporous niobium pentaoxide/nitrogen-doped graphene photocatalyst of bigger serface and orderly pore passage structure。
Summary of the invention
Goal of the invention: in order to solve the deficiencies in the prior art, the invention provides the preparation method under a kind of effective visible ray with the mesoporous niobium pentaoxide/nitrogen-doped graphene of high catalytic activity。
Technical scheme: the preparation method of a kind of mesoporous niobium pentaoxide/nitrogen-doped graphene high-efficiency composite photocatalyst, comprises the following steps:
1) preparation of N doping graphene oxide solution, represents with NGO solution
Solid state heat reaction method is adopted to prepare N doping graphene oxide。The carbamide of the graphene oxide of 0.5-1.0g and 1.5-3.0g is placed in tube furnace through being fully ground。With roasting 2h after argon emptying furnace air, repeatedly washing the impurity removing sample surfaces with the hydrochloric acid of 1mol, under 60 DEG C of conditions of constant temperature, dry 12h, obtains N doping graphene oxide。3.5-7mg N doping graphene oxide powder is dissolved in 10-20mL distilled water ultrasonic 48 hours, ultimately forms the dispersion of taupe。Natural subsidence is disgorging (being approximately 2.5-5.0mg) after 24 hours。25-50mL ethanol is added in dispersion ultrasonic 1h simultaneously, ultimately forms stable NGO solution。
2) preparation of mesoporous niobium pentaoxide, uses m-Nb2O5Represent
Sol-gel process is adopted to prepare m-Nb2O5。The F127 weighing 0.5-2.0 weight portion is dissolved in 10-40.0 weight portion dehydrated alcohol and processes 30min with the magnetic stirring apparatus of 500-1000rpm rotating speed, after F127 is completely dissolved, add 2.75-11.00mmol Columbium pentachloride. strong agitation 10min, the color from light yellow of solution becomes colorless transparent, is added dropwise over the CaCl of 0.5mol/L2Solution 0.25-1.0mL, and continue stirring 10min after prepare Nb2O5Colloidal sol, is then transferred to colloidal sol in the autoclave that 100mL politef is liner, reacts 5-8 days at constant temperature 60-70 DEG C, takes out sample and also dries, and naturally is down to room temperature, prepared m-Nb after after 450 DEG C of roasting 5h2O5。
3) preparation of mesoporous niobium pentaoxide/nitrating reduced graphene high-efficiency composite photocatalyst, uses m-Nb2O5/ NGR represents
Photoreduction met hod is adopted to prepare m-Nb2O5/ NGR complex。First by m-Nb2O5Mix homogeneously with NGO solution (0.5mg/ml), add 40ml ethanol, ultrasonic half an hour stirs 6-8h in 500W mercury lamp when and reduces, and is then dried under 60 DEG C of conditions by gained solution, finally repeatedly obtains sample m-Nb by dehydrated alcohol eccentric cleaning2O5/ NGR powder。The mass percent of NGR can be regulated by the NGO solution of addition different quality。The complex m-Nb of preparation2O5/ NGR-x carrys out labelling, and x represents the mass percent of NGR。
The present invention is beneficial effect compared with prior art:
1, the mesoporous niobium pentaoxide/nitrogen-doped graphene photocatalyst with bigger serface and orderly pore passage structure has successfully been synthesized。
2, solve the difficult problem that niobium pentaoxide activity itself is low, it is possible to effectively expand the photoresponse scope of niobium pentaoxide, improve photocatalyst catalysis activity under visible light conditions, expand the suitable application area of niobium pentaoxide photocatalyst further。
3, this composite photocatalyst can decomposition water, catalyst recyclable regenerative, non-secondary pollution quickly and efficiently, be the photocatalyst of a kind of green。
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be described in detail。
Specific embodiment 1:
The preparation method of a kind of mesoporous niobium pentaoxide/nitrogen-doped graphene high-efficiency composite photocatalyst, comprises the following steps:
1) preparation of N doping graphene oxide solution, represents with NGO solution
Solid state heat reaction method is adopted to prepare N doping graphene oxide。The carbamide of the graphene oxide of 0.5-1.0g and 1.5-3.0g is placed in tube furnace through being fully ground。With roasting 2h after argon emptying furnace air, repeatedly washing the impurity removing sample surfaces with the hydrochloric acid of 1mol, under 60 DEG C of conditions of constant temperature, dry 12h, obtains N doping graphene oxide。3.5-7mg N doping graphene oxide powder is dissolved in 10-20mL distilled water ultrasonic 48 hours, ultimately forms the dispersion of taupe。Natural subsidence is disgorging (being approximately 2.5-5.0mg) after 24 hours。25-50mL ethanol is added in dispersion ultrasonic 1h simultaneously, ultimately forms stable NGO solution。
2) preparation of mesoporous niobium pentaoxide, uses m-Nb2O5Represent
Sol-gel process is adopted to prepare m-Nb2O5。The F127 weighing 0.5-2.0 weight portion is dissolved in 10-40.0 weight portion dehydrated alcohol and processes 30min with the magnetic stirring apparatus of 500-1000rpm rotating speed, after F127 is completely dissolved, add 2.75-11.00mmol Columbium pentachloride. strong agitation 10min, the color from light yellow of solution becomes colorless transparent, is added dropwise over the CaCl of 0.5mol/L2Solution 0.25-1.0mL, and continue stirring 10min after prepare Nb2O5Colloidal sol, is then transferred to colloidal sol in the autoclave that 100mL politef is liner, reacts 5-8 days at constant temperature 60-70 DEG C, takes out sample and also dries, and naturally is down to room temperature, prepared m-Nb after after 450 DEG C of roasting 5h2O5。
3) preparation of mesoporous niobium pentaoxide/nitrating reduced graphene high-efficiency composite photocatalyst, uses m-Nb2O5/ NGR represents
Photoreduction met hod is adopted to prepare m-Nb2O5/ NGR complex。First by m-Nb2O5Mix homogeneously with NGO solution (0.5mg/ml), add 40ml ethanol, ultrasonic half an hour stirs 6-8h in 500W mercury lamp when and reduces, and is then dried under 60 DEG C of conditions by gained solution, finally repeatedly obtains sample m-Nb by dehydrated alcohol eccentric cleaning2O5/NGR-2。
Specific embodiment 2:
The preparation method of a kind of mesoporous niobium pentaoxide/nitrogen-doped graphene high-efficiency composite photocatalyst, comprises the following steps:
1) preparation of N doping graphene oxide solution, represents with NGO solution
Solid state heat reaction method is adopted to prepare N doping graphene oxide。The carbamide of the graphene oxide of 0.5-1.0g and 1.5-3.0g is placed in tube furnace through being fully ground。With roasting 2h after argon emptying furnace air, repeatedly washing the impurity removing sample surfaces with the hydrochloric acid of 1mol, under 60 DEG C of conditions of constant temperature, dry 12h, obtains N doping graphene oxide。3.5-7mg N doping graphene oxide powder is dissolved in 10-20mL distilled water ultrasonic 48 hours, ultimately forms the dispersion of taupe。Natural subsidence is disgorging (being approximately 2.5-5.0mg) after 24 hours。25-50mL ethanol is added in dispersion ultrasonic 1h simultaneously, ultimately forms stable NGO solution。
2) preparation of mesoporous niobium pentaoxide, uses m-Nb2O5Represent
Sol-gel process is adopted to prepare m-Nb2O5。The F127 weighing 0.5-2.0 weight portion is dissolved in 10-40.0 weight portion dehydrated alcohol and processes 30min with the magnetic stirring apparatus of 500-1000rpm rotating speed, after F127 is completely dissolved, add 2.75-11.00mmol Columbium pentachloride. strong agitation 10min, the color from light yellow of solution becomes colorless transparent, is added dropwise over the CaCl of 0.5mol/L2Solution 0.25-1.0mL, and continue stirring 10min after prepare Nb2O5Colloidal sol, is then transferred to colloidal sol in the autoclave that 100mL politef is liner, reacts 5-8 days at constant temperature 60-70 DEG C, takes out sample and also dries, and naturally is down to room temperature, prepared m-Nb after after 450 DEG C of roasting 5h2O5。
3) preparation of mesoporous niobium pentaoxide/nitrating reduced graphene high-efficiency composite photocatalyst, uses m-Nb2O5/ NGR represents
Photoreduction met hod is adopted to prepare m-Nb2O5/ NGR complex。First by m-Nb2O5Mix homogeneously with NGO solution (0.5mg/ml), add 40ml ethanol, ultrasonic half an hour stirs 6-8h in 500W mercury lamp when and reduces, and is then dried under 60 DEG C of conditions by gained solution, finally repeatedly obtains sample m-Nb by dehydrated alcohol eccentric cleaning2O5/NGR-3。
Specific embodiment 3:
The preparation method of a kind of mesoporous niobium pentaoxide/nitrogen-doped graphene high-efficiency composite photocatalyst, comprises the following steps:
1) preparation of N doping graphene oxide solution, represents with NGO solution
Solid state heat reaction method is adopted to prepare N doping graphene oxide。The carbamide of the graphene oxide of 0.5-1.0g and 1.5-3.0g is placed in tube furnace through being fully ground。With roasting 2h after argon emptying furnace air, repeatedly washing the impurity removing sample surfaces with the hydrochloric acid of 1mol, under 60 DEG C of conditions of constant temperature, dry 12h, obtains N doping graphene oxide。3.5-7mg N doping graphene oxide powder is dissolved in 10-20mL distilled water ultrasonic 48 hours, ultimately forms the dispersion of taupe。Natural subsidence is disgorging (being approximately 2.5-5.0mg) after 24 hours。25-50mL ethanol is added in dispersion ultrasonic 1h simultaneously, ultimately forms stable NGO solution。
2) preparation of mesoporous niobium pentaoxide, uses m-Nb2O5Represent
Sol-gel process is adopted to prepare m-Nb2O5。The F127 weighing 0.5-2.0 weight portion is dissolved in 10-40.0 weight portion dehydrated alcohol and processes 30min with the magnetic stirring apparatus of 500-1000rpm rotating speed, after F127 is completely dissolved, add 2.75-11.00mmol Columbium pentachloride. strong agitation 10min, the color from light yellow of solution becomes colorless transparent, is added dropwise over the CaCl of 0.5mol/L2Solution 0.25-1.0mL, and continue stirring 10min after prepare Nb2O5Colloidal sol, is then transferred to colloidal sol in the autoclave that 100mL politef is liner, reacts 5-8 days at constant temperature 60-70 DEG C, takes out sample and also dries, and naturally is down to room temperature, prepared m-Nb after after 450 DEG C of roasting 5h2O5。
3) preparation of mesoporous niobium pentaoxide/nitrating reduced graphene high-efficiency composite photocatalyst, uses m-Nb2O5/ NGR represents
Photoreduction met hod is adopted to prepare m-Nb2O5/ NGR complex。First by m-Nb2O5Mix homogeneously with NGO solution (0.5mg/ml), add 40ml ethanol, ultrasonic half an hour stirs 6-8h in 500W mercury lamp when and reduces, and is then dried under 60 DEG C of conditions by gained solution, finally repeatedly obtains sample m-Nb by dehydrated alcohol eccentric cleaning2O5/NGR-4。
Specific embodiment 4:
The preparation method of a kind of mesoporous niobium pentaoxide/nitrogen-doped graphene high-efficiency composite photocatalyst, comprises the following steps:
1) preparation of N doping graphene oxide solution, represents with NGO solution
Solid state heat reaction method is adopted to prepare N doping graphene oxide。The carbamide of the graphene oxide of 0.5-1.0g and 1.5-3.0g is placed in tube furnace through being fully ground。With roasting 2h after argon emptying furnace air, repeatedly washing the impurity removing sample surfaces with the hydrochloric acid of 1mol, under 60 DEG C of conditions of constant temperature, dry 12h, obtains N doping graphene oxide。3.5-7mg N doping graphene oxide powder is dissolved in 10-20mL distilled water ultrasonic 48 hours, ultimately forms the dispersion of taupe。Natural subsidence is disgorging (being approximately 2.5-5.0mg) after 24 hours。25-50mL ethanol is added in dispersion ultrasonic 1h simultaneously, ultimately forms stable NGO solution。
2) preparation of mesoporous niobium pentaoxide, uses m-Nb2O5Represent
Sol-gel process is adopted to prepare m-Nb2O5。The F127 weighing 0.5-2.0 weight portion is dissolved in 10-40.0 weight portion dehydrated alcohol and processes 30min with the magnetic stirring apparatus of 500-1000rpm rotating speed, after F127 is completely dissolved, add 2.75-11.00mmol Columbium pentachloride. strong agitation 10min, the color from light yellow of solution becomes colorless transparent, is added dropwise over the CaCl of 0.5mol/L2Solution 0.25-1.0mL, and continue stirring 10min after prepare Nb2O5Colloidal sol, is then transferred to colloidal sol in the autoclave that 100mL politef is liner, reacts 5-8 days at constant temperature 60-70 DEG C, takes out sample and also dries, and naturally is down to room temperature, prepared m-Nb after after 450 DEG C of roasting 5h2O5。
3) preparation of mesoporous niobium pentaoxide/nitrating reduced graphene high-efficiency composite photocatalyst, uses m-Nb2O5/ NGR represents
Photoreduction met hod is adopted to prepare m-Nb2O5/ NGR complex。First by m-Nb2O5Mix homogeneously with NGO solution (0.5mg/ml), add 40ml ethanol, ultrasonic half an hour stirs 6-8h in 500W mercury lamp when and reduces, and is then dried under 60 DEG C of conditions by gained solution, finally repeatedly obtains sample m-Nb by dehydrated alcohol eccentric cleaning2O5/NGR-5。
Claims (1)
1. the preparation method of mesoporous niobium pentaoxide/nitrogen-doped graphene high-efficiency composite photocatalyst, it is characterised in that: comprise the following steps:
1) preparation of N doping graphene oxide solution, represents with NGO solution
Adopt solid state heat reaction method to prepare N doping graphene oxide, the carbamide of the graphene oxide of 0.5-1.0g and 1.5-3.0g is placed in tube furnace through being fully ground。With roasting 2h after argon emptying furnace air, repeatedly washing the impurity removing sample surfaces with the hydrochloric acid of 1mol, under 60 DEG C of conditions of constant temperature, dry 12h, obtains N doping graphene oxide。3.5-7mg N doping graphene oxide powder is dissolved in 10-20mL distilled water ultrasonic 48 hours, ultimately form the dispersion of taupe, natural subsidence is disgorging (being approximately 2.5-5.0mg) after 24 hours, 25-50mL ethanol is added in dispersion ultrasonic 1h simultaneously, ultimately forms stable NGO solution；
2) preparation of mesoporous niobium pentaoxide, uses m-Nb2O5Represent
Sol-gel process is adopted to prepare m-Nb2O5The F127 weighing 0.5-2.0 weight portion is dissolved in 10-40.0 weight portion dehydrated alcohol and processes 30min with the magnetic stirring apparatus of 500-1000rpm rotating speed, after F127 is completely dissolved, add 2.75-11.00mmol Columbium pentachloride. strong agitation 10min, the color from light yellow of solution becomes colorless transparent, is added dropwise over the CaCl of 0.5mol/L2Solution 0.25-1.0mL, and continue stirring 10min after prepare Nb2O5Colloidal sol, is then transferred to colloidal sol in the autoclave that 100mL politef is liner, reacts 5-8 days at constant temperature 60-70 DEG C, takes out sample and also dries, and naturally is down to room temperature, prepared m-Nb after after 450 DEG C of roasting 5h2O5；
3) preparation of mesoporous niobium pentaoxide/nitrating reduced graphene high-efficiency composite photocatalyst, uses m-Nb2O5/ NGR represents
Photoreduction met hod is adopted to prepare m-Nb2O5/ NGR complex, by m-Nb2O5Mix homogeneously with NGO solution (0.1-0.5mg/ml), add 40ml ethanol, ultrasonic half an hour stirs 6-8h in 500W mercury lamp when and reduces, more repeatedly obtains sample m-Nb by dehydrated alcohol eccentric cleaning after being dried under 60 DEG C of conditions by gained solution2O5/ NGR powder, the mass percent of NGR can be regulated by the NGO solution of addition different quality, the complex m-Nb of preparation2O5/ NGR-x carrys out labelling, and x represents the mass percent of NGR。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610018709.3A CN105688965B (en) | 2016-01-12 | 2016-01-12 | Mesoporous niobium pentaoxide/nitrogen-doped graphene high-efficiency composite photocatalyst preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610018709.3A CN105688965B (en) | 2016-01-12 | 2016-01-12 | Mesoporous niobium pentaoxide/nitrogen-doped graphene high-efficiency composite photocatalyst preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105688965A true CN105688965A (en) | 2016-06-22 |
| CN105688965B CN105688965B (en) | 2019-02-12 |
Family
ID=56226351
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610018709.3A Expired - Fee Related CN105688965B (en) | 2016-01-12 | 2016-01-12 | Mesoporous niobium pentaoxide/nitrogen-doped graphene high-efficiency composite photocatalyst preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105688965B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107149931A (en) * | 2017-04-17 | 2017-09-12 | 天津理工大学 | The preparation method of Zinc oxide quantum dot potassium niobate photochemical catalyst and the purposes of the catalyst |
| CN107626338A (en) * | 2017-10-11 | 2018-01-26 | 南通科技职业学院 | The preparation method of the mesoporous niobium pentaoxide of molybdenum sulfide Nanoparticle Modified/nitrogen-doped graphene composite photo-catalyst |
| CN109167002A (en) * | 2018-08-15 | 2019-01-08 | 合肥国轩高科动力能源有限公司 | A kind of preparation method of lithium-sulfur cell composite diaphragm |
| CN109980210A (en) * | 2019-04-19 | 2019-07-05 | 陕西科技大学 | A kind of niobium pentaoxide three-dimensional doped graphene composite material and preparation method and application |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103084198A (en) * | 2013-02-01 | 2013-05-08 | 南通职业大学 | Preparation method of efficient photocatalyst nitrogen doped meso-porous niobium pentoxide |
| CN103521252A (en) * | 2013-10-30 | 2014-01-22 | 苏州大学 | Photocatalyst of N-doped graphene compound semiconductor nano particles and preparation method thereof |
| CN103638922A (en) * | 2013-12-13 | 2014-03-19 | 南通职业大学 | Preparation method of mesoporous tungsten trioxide/reduction-oxidation graphene composite photocatalyst |
-
2016
- 2016-01-12 CN CN201610018709.3A patent/CN105688965B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103084198A (en) * | 2013-02-01 | 2013-05-08 | 南通职业大学 | Preparation method of efficient photocatalyst nitrogen doped meso-porous niobium pentoxide |
| CN103521252A (en) * | 2013-10-30 | 2014-01-22 | 苏州大学 | Photocatalyst of N-doped graphene compound semiconductor nano particles and preparation method thereof |
| CN103638922A (en) * | 2013-12-13 | 2014-03-19 | 南通职业大学 | Preparation method of mesoporous tungsten trioxide/reduction-oxidation graphene composite photocatalyst |
Non-Patent Citations (1)
| Title |
|---|
| 丁敏娟，等: "Nb2O5纳米棒/还原氧化石墨烯复合材料的制备及其光催化制氢性能", 《南通大学学报（自然科学版）》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107149931A (en) * | 2017-04-17 | 2017-09-12 | 天津理工大学 | The preparation method of Zinc oxide quantum dot potassium niobate photochemical catalyst and the purposes of the catalyst |
| CN107149931B (en) * | 2017-04-17 | 2019-11-05 | 天津理工大学 | Zinc oxide quantum dot-preparation method of potassium niobate photochemical catalyst and the purposes of the catalyst |
| CN107626338A (en) * | 2017-10-11 | 2018-01-26 | 南通科技职业学院 | The preparation method of the mesoporous niobium pentaoxide of molybdenum sulfide Nanoparticle Modified/nitrogen-doped graphene composite photo-catalyst |
| CN109167002A (en) * | 2018-08-15 | 2019-01-08 | 合肥国轩高科动力能源有限公司 | A kind of preparation method of lithium-sulfur cell composite diaphragm |
| CN109980210A (en) * | 2019-04-19 | 2019-07-05 | 陕西科技大学 | A kind of niobium pentaoxide three-dimensional doped graphene composite material and preparation method and application |
| CN109980210B (en) * | 2019-04-19 | 2021-01-29 | 陕西科技大学 | Niobium pentoxide three-dimensional doped graphene composite material and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105688965B (en) | 2019-02-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109289895B (en) | Porous reticular g-C3N4Supported TiO2Preparation method of composite nano material | |
| CN112495401B (en) | Mo-doped MoO3@ZnIn2S4Z-system photocatalyst and preparation method and application thereof | |
| CN105502286B (en) | A kind of porous nano NiFe2O4Preparation method | |
| CN105688972B (en) | Mesoporous-α-di-iron trioxide/nitrating reduced graphene high-efficiency composite photocatalyst preparation method | |
| CN111203231B (en) | Indium zinc sulfide/bismuth vanadate composite material and preparation method and application thereof | |
| WO2021008196A1 (en) | Catalyst for electrocatalytic carbon dioxide reduction and preparation method thereof | |
| CN105600828B (en) | A kind of porous nano CuFe2O4Preparation method | |
| CN110252346B (en) | MoS2/SnS2Preparation method and application of/r-GO composite photocatalyst | |
| CN105854881B (en) | The mesoporous cuprous oxide of visible light type/reduced graphene composite catalyst preparation method | |
| CN105688965A (en) | Preparation method of mesoporous niobium pentoxide/nitrogen-doped graphene efficient composite photocatalyst | |
| CN106512985B (en) | A kind of ZnO/WO3The synthetic method of heterojunction array | |
| CN105664950B (en) | A kind of porous nano ZnFe2O4Preparation method | |
| CN103861621B (en) | A kind of Bi 7o 9i 3/ Graphene composite visible light catalyst and preparation method thereof | |
| CN104056620A (en) | Visible-light catalyst and preparation method and application thereof | |
| CN112495421B (en) | Preparation method of nitrogen-doped carbon quantum dot modified nitrogen-rich graphite type carbon nitride photocatalyst | |
| CN102489318B (en) | Preparation method for porous nano p-CuS/n-CdS compound semiconductor photochemical catalyst | |
| CN114950502B (en) | Preparation method of nano rod-shaped red phosphorus photocatalyst with photocatalytic hydrogen evolution activity and stability | |
| CN105688966A (en) | Bismuth vanadate modified boron nitride nanosheet composite material and preparation method thereof | |
| CN113663705B (en) | Lanthanum vanadate/graphite phase carbon nitride composite material and preparation method and application thereof | |
| CN107376956B (en) | Zinc oxide/red phosphorus heterojunction composite photocatalyst and preparation method thereof | |
| CN110586149B (en) | Bismuth molybdate/titanium carbide heterojunction two-dimensional photocatalytic material and preparation method and application thereof | |
| CN103977785A (en) | Bi2Sn2O7-graphene composite visible-light-driven photocatalyst and preparation method thereof | |
| CN116173987A (en) | CdIn 2 S 4 /CeO 2 Heterojunction photocatalyst, preparation method and application thereof | |
| CN103977821A (en) | Cu3SnS4-graphene composite visible-light-driven photocatalyst and preparation method thereof | |
| CN114471586A (en) | Composite photocatalyst for treating organic pollutants in wastewater and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20190212 Termination date: 20200112 |