CN103752334A - Graphite phase carbon nitride nanosheet visible-light-induced photocatalyst synthesized by promotion of ionic liquid - Google Patents
Graphite phase carbon nitride nanosheet visible-light-induced photocatalyst synthesized by promotion of ionic liquid Download PDFInfo
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- CN103752334A CN103752334A CN201410038958.XA CN201410038958A CN103752334A CN 103752334 A CN103752334 A CN 103752334A CN 201410038958 A CN201410038958 A CN 201410038958A CN 103752334 A CN103752334 A CN 103752334A
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Abstract
The invention discloses a preparation method and application of a graphite phase carbon nitride nanosheet visible-light-induced photocatalyst synthesized by promotion of ionic liquid and belongs to the technical field of material preparation and photocatalysis. A graphite phase carbon nitride nanosheet material is formed by using room-temperature ionic liquid of urea and dialkyl imidazolium tetrafluoroborate as a precursor through high-temperature co-polymerization. The graphite phase carbon nitride prepared by the preparation method has a low-dimensional nanosheet layer microstructure and a suitable forbidden bandwidth and shows more efficient photocatalytic hydrogen production performance than that of conventional body phase carbon nitride under the visible light. The graphite phase carbon nitride nanosheet visible-light-induced photocatalyst synthesized by promotion of the ionic liquid is simple in synthetic process, is low in cost, has high photocatalytic efficiency, accords with the actual production requirement and has a wide application prospect in the field of photocatalysis.
Description
Technical field
The invention belongs to material preparation and light-catalysed technical field, be specifically related to the preparation method and application that a kind of ionic liquid promotes synthetic graphite phase carbon nitride nanometer sheet visible light catalyst.
Background technology
Hydrogen is a kind of clean type energy transmission body, and photocatalysis Decomposition aquatic products hydrogen is a kind of method with the solution energy problem of high evaluation.The core of photocatalysis research is to find the photochemical catalyst of function admirable, so the exploitation of high efficiency photocatalyst is the core topic of photocatalysis research.Yet the photochemical catalyst of research exists the problems such as low, the easy inactivation of solar energy utilization ratio, use cost height mostly at present, has greatly restricted the application of photocatalysis in industrial production.Therefore the core challenge that exploitation is efficient, stable, nontoxic, cheap visible light catalyst is this field.
In recent years, Wang etc. are by the organic polymer semiconductor of the abnormal stable not containing metal composition of chemical constitution, graphite-phase carbonitride (g-C
3n
4), be incorporated into photocatalysis field and carry out photodissociation aquatic products hydrogen, produce oxygen, evoked people's very big interest, make the research of polymer semiconductor's photochemical catalyst enter a fast-developing period (Nat. Mater. 2009,8,76-80).Yet, g-C
3n
4intrinsic propesties due to its organic polymer, as photochemical catalyst, also there are some problems, exciton binding energy as little in specific area, that produce photo-generated carrier is high, light induced electron-hole-recombination is serious, quantum efficiency is low and energy gap compared with large and can not effectively utilize sunshine etc., seriously restrict it at the large-scale promotion application of the energy, surround lighting catalytic field.For a science difficult problem for these objective realities, researcher both domestic and external is around g-C
3n
4, carry out a large amount of research work.
Graphite-phase carbonitride (g-C
3n
4) kind, synthetic method and the preparation process of semi-conductive photocatalysis performance and predecessor be closely related.Because the kind of predecessor, preparation technology's improvement (calcining heat, temperature retention time) and preparation method's difference can effectively be optimized g-C
3n
4semiconductor energy band structure, nanostructured and surface topography, thus its photocatalysis performance significantly affected.
Ionic liquid is comprised of the anion of large cation and weak coordination, has special physicochemical properties, such as fixedness, incombustibility and heat endurance etc.This functional material is widely used as solvent, not long ago, is also used as the material that soft template is synthesized various nanostructureds.Had report, ionic liquid promotes two paracyanogen ammonia thermal polymerizations to prepare the nitride porous material with carbon element of Heteroatom doping, and effective Visible Light Induced Photocatalytic dyestuff.Yet adopting this cheap industrial chemicals of urea is carbonitride presoma, ionic liquid is incorporated into and in reaction system, promotes g-C
3n
4the synthetic research work of nanometer sheet, have not been reported.Therefore, we utilize urea for raw material, and ionic liquid, as soft template and doping auxiliary agent, successfully makes graphite-phase nitrogenize carbon back nanometer sheet visible light catalyst.Experiment showed, that ionic liquid promotes that synthetic graphite-phase azotized carbon nano sheet visible light catalyst is the photochemical catalyst that a kind of efficient visible ray decomposes aquatic products hydrogen.
Summary of the invention
The object of the present invention is to provide a kind of ionic liquid to promote the preparation method and application of synthetic graphite phase carbon nitride nanometer sheet visible light catalyst.The photochemical catalyst of the porous nano chip architecture of Heteroatom doping prepared by the present invention, can not only accelerate the migration of photo-generated carrier and can promote mass transport process, realizes the aquatic products of visible ray photodissociation efficiently hydrogen.Technique of the present invention is simple, with low cost, and catalytic efficiency is high, and realistic Production requirement, has broad application prospects in photocatalysis field.
For achieving the above object, the present invention adopts following technical scheme:
Graphite-phase azotized carbon nano sheet visible light catalyst is the semiconductive organic polymer with the porous nano lamella structure of Heteroatom doping, and specific area is 60 ~ 100 m
2/ g, absorbs visible ray, and has the performance of good photochemical catalyzing hydrogen making, can be used as a kind of efficient photochemical catalyst.
Prepare as mentioned above the method for graphite-phase carbonitride visible light catalyst and be that to take urea and ionic liquid be predecessor, by high temperature thermal condensation, obtain graphite-phase azotized carbon nano sheet.Described preparation method comprises the following steps: the urea that (1) is 100:1 ~ 15 by mass ratio and different ionic liquids (ionic liquid at room temperature that dialkylimidazolium cation and tetrafluoro boric acid anion form) are dissolved in water, stirring at room 2 ~ 12h, evaporate to dryness, grinds; (2) by pressed powder 500 ~ 600 ℃ of heat treatment 1 ~ 4h in Muffle furnace, make graphite-phase azotized carbon nano sheet photochemical catalyst.
Described graphite-phase azotized carbon nano sheet catalyst is applied to decomposition water hydrogen making under visible ray.
Remarkable advantage of the present invention is:
(1) the present invention first using ionic liquid as soft template and adulterant be incorporated in the modification of nanoscale twins carbonitride, increased specific area, promote the transport efficiency of mass transport process and photo-generated carrier simultaneously.
(2) synthetic graphite phase carbon nitride nanometer sheet of the present invention, its advantage is that preparation technology is simple, and energy consumption is low, and catalyst is stable, nontoxic, be easy to reclaim, reusable edible, realistic need of production.
(3) synthetic graphite phase carbon nitride nanometer sheet of the present invention, the ionic liquid wherein with modifying function is selectively in extensive range, has good Modulatory character and universality.
(4) the present invention promotes ionic liquid synthetic graphite-phase azotized carbon nano sheet to be applied to photocatalysis hydrogen making first, finds that it has efficient visible ray photodissociation aquatic products hydrogen performance.In light-catalyzed reaction system, can carry out easily separating treatment, photochemical catalyst renewable is strong, and recycling rate of waterused is high, has very high practical value and application prospect widely.
Accompanying drawing explanation
Fig. 1 is the X-ray powder diffraction XRD figure that the ionic liquid of embodiment 2 gained promotes synthetic graphite-phase azotized carbon nano sheet a.
Fig. 2 is the Fourier transform infrared FT-IR spectrogram that the ionic liquid of embodiment 2 gained promotes synthetic graphite-phase azotized carbon nano sheet a.
Fig. 3 is the transmission electron microscope TEM figure that the ionic liquid of embodiment 2 gained promotes synthetic graphite-phase azotized carbon nano sheet a.
Fig. 4 is the atomic force microscope figure that the ionic liquid of embodiment 2 gained promotes synthetic graphite-phase azotized carbon nano sheet a.
Fig. 5 is the x-ray photoelectron power spectrum XPS figure that the ionic liquid of embodiment 5 gained promotes synthetic graphite-phase azotized carbon nano sheet a.
Fig. 6 is the UV-vis DRS DRS figure that the ionic liquid of embodiment 2 gained promotes synthetic graphite-phase azotized carbon nano sheet a.
Fig. 7 is that the ionic liquid of embodiment 2 gained promotes synthetic graphite-phase azotized carbon nano sheet a and traditional body phase carbon nitride b to carry out the performance comparison diagram of visible light catalytic decomposition water hydrogen making.
The specific embodiment
Be below several embodiments of the present invention, further illustrate the present invention, but the present invention is not limited only to this.
embodiment 1
The urea that is 50:1 by mass ratio and 1-ethyl-3-methylimidazole tetrafluoroborate (EmimBF
4) be dissolved in water, stirring at room 12h, evaporate to dryness, grinds.By pressed powder 550 ℃ of heat treatment 2h in Muffle furnace, make ionic liquid and promote synthetic graphite-phase azotized carbon nano sheet.
embodiment 2
The urea that is 45:1 by mass ratio and 1-butyl-3-methyl imidazolium tetrafluoroborate (BmimBF
4) be dissolved in water, stirring at room 12h, evaporate to dryness, grinds.By pressed powder 550 ℃ of heat treatment 2h in Muffle furnace, make ionic liquid and promote synthetic graphite-phase azotized carbon nano sheet.
embodiment 3
The urea that is 40:1 by mass ratio and 1-hexyl-3-methyl imidazolium tetrafluoroborate (HmimBF
4) be dissolved in water, stirring at room 12h, evaporate to dryness, grinds.By pressed powder 550 ℃ of heat treatment 2h in Muffle furnace, make ionic liquid and promote synthetic graphite-phase azotized carbon nano sheet.
embodiment 4
The urea that is 35:1 by mass ratio and 1-octyl group-3-methyl imidazolium tetrafluoroborate (OmimBF
4) be dissolved in water, stirring at room 12h, evaporate to dryness, grinds.By pressed powder 550 ℃ of heat treatment 2h in Muffle furnace, make ionic liquid and promote synthetic graphite-phase azotized carbon nano sheet.
embodiment 5
The urea that is 9:1 by mass ratio and 1-butyl-3-methyl imidazolium tetrafluoroborate (BmimBF
4) be dissolved in water, stirring at room 12h, evaporate to dryness, grinds.By pressed powder 550 ℃ of heat treatment 2h in Muffle furnace, make ionic liquid and promote synthetic graphite-phase azotized carbon nano sheet.
Performance test
Fig. 1 is the X-ray powder diffraction XRD figure that the ionic liquid of embodiment 2 gained promotes synthetic graphite-phase azotized carbon nano sheet a.From figure, can find 13.0
owith 27.5
othere are two XRD diffraction maximums that significantly belong to graphite-phase carbonitride (100) and (002) crystal face in place, confirms that the product of preparation is graphite-phase carbonitride.
Fig. 2 is the Fourier transform infrared FT-IR spectrogram that the ionic liquid of embodiment 2 gained promotes synthetic graphite-phase azotized carbon nano sheet a.As can be seen from the figure gained sample has the characteristic peak of graphite-phase carbon nitride material, i.e. 800 cm
-1with 1200 ~ 1600 cm
-1interval, they correspond respectively to the breathing vibration of seven piperazine rings and the stretching vibration of armaticity CN heterocycle.
Fig. 3 is the transmission electron microscope TEM figure that the ionic liquid of embodiment 2 gained promotes synthetic graphite-phase azotized carbon nano sheet a.The product of preparation is nanoporous flake structure as we can see from the figure.
Fig. 4 is the atomic force microscope figure that the ionic liquid of embodiment 2 gained promotes synthetic graphite-phase azotized carbon nano sheet a.The product that can find preparation from figure has nanoscale twins pattern, the general 2 ~ 5nm of lamellar spacing.
Fig. 5 is the x-ray photoelectron power spectrum XPS figure that the ionic liquid of embodiment 5 gained promotes synthetic graphite-phase azotized carbon nano sheet a.As can be seen from the figure gained sample comprises boron, fluorine hetero atom, and from their combination can be able to know boron, fluorine atom successfully mix carbonitride matrix.
Fig. 6 is the UV-vis DRS DRS figure that the ionic liquid of embodiment 2 gained promotes synthetic graphite-phase azotized carbon nano sheet a.From figure, can find that gained sample has obvious and precipitous absorption band edge in 440 nm left and right, corresponding energy gap is 2.82 eV.
Fig. 7 is the performance comparison diagram that the ionic liquid of embodiment 2 gained promotes synthetic graphite-phase azotized carbon nano sheet a and body phase carbon nitride b photochemical catalyzing hydrogen making.50mg catalyst, 10 vol. % triethanolamines (hole sacrifice agent), 3 wt. % Pt(co-catalysts), in the water of 100 milliliters, in upper photograph in formula reactor, react.The product hydrogen-producing speed of (xenon lamp 300W, filter plate λ > 420 nm) under visible ray that can find preparation from figure reaches 130 μ mol/h, compares and has improved 3.7 times with body phase carbon nitride (35 μ mol/h).
The foregoing is only preferred embodiment of the present invention, all equalizations of doing according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (4)
1. ionic liquid promotes a method for synthetic graphite phase carbon nitride nanometer sheet visible light catalyst, it is characterized in that: the diversity of ionic liquid, synthetic photochemical catalyst has the porous nano chip architecture of Heteroatom doping and visible light-responded.
2. ionic liquid according to claim 1 promotes the method for synthetic graphite phase carbon nitride nanometer sheet visible light catalyst, it is characterized in that: comprise the following steps:
(1) urea that is 100:1 ~ 15 by mass ratio and ion liquid dissolving in water, stirring at room 2 ~ 12h, evaporate to dryness, grinds to obtain pressed powder;
(2) by the pressed powder of step (1) 500 ~ 600 ℃ of heat treatment 1 ~ 4h in Muffle furnace, make graphite-phase azotized carbon nano sheet visible light catalyst.
3. ionic liquid according to claim 2 promotes the method for synthetic graphite phase carbon nitride nanometer sheet visible light catalyst, it is characterized in that: described ionic liquid is the ionic liquid at room temperature that dialkylimidazolium cation and tetrafluoro boric acid anion form.
4. an application for the graphite-phase azotized carbon nano sheet visible light catalyst that the method for claim 1 makes, is characterized in that: described graphite-phase azotized carbon nano sheet is applied to visible light catalytic decomposition water hydrogen making.
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Cited By (13)
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| CN104475153A (en) * | 2014-12-05 | 2015-04-01 | 复旦大学 | Functional-ionic-liquid-modified graphite C3N3 catalytic material, and preparation method and application thereof |
| CN105214708A (en) * | 2015-10-14 | 2016-01-06 | 黑龙江大学 | A kind of titanium dioxide-boron modification carbon nitride photocatalyst and preparation method thereof |
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| CN104475153A (en) * | 2014-12-05 | 2015-04-01 | 复旦大学 | Functional-ionic-liquid-modified graphite C3N3 catalytic material, and preparation method and application thereof |
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