CN103272639B - Copolymerization modified graphite-phase carbon nitride nanosheet visible-light-driven photocatalyst - Google Patents
Copolymerization modified graphite-phase carbon nitride nanosheet visible-light-driven photocatalyst Download PDFInfo
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- CN103272639B CN103272639B CN201310230575.8A CN201310230575A CN103272639B CN 103272639 B CN103272639 B CN 103272639B CN 201310230575 A CN201310230575 A CN 201310230575A CN 103272639 B CN103272639 B CN 103272639B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention discloses a copolymerization modified graphite-phase carbon nitride nanosheet visible-light-driven photocatalyst as well as a preparation method and an application thereof, and belongs to the technical field of material preparation and photocatalysis. The graphite-phase carbon nitride nanosheet visible-light-driven photocatalyst which adopts a nanosheet structure and synthesized with a copolymerization method is formed by taking urea and different small organic molecule monomers as precursors through the high-temperature copolymerization action. The prepared graphite-phase carbon nitride has a lower-dimension nanosheet microstructure and a proper band gap; compared with conventional bulk-phase carbon nitride, the graphite-phase carbon nitride effectively increases the specific surface area, enhances the utilization rate of sunlight, and has efficient photocatalysis hydrogen production performance in visible light. According to the copolymerization modified graphite-phase carbon nitride nanosheet visible-light-driven photocatalyst, the synthetic process is simple, the cost is low, the catalytic efficiency is high, the actual production requirements are met, and the photocatalyst has broad application prospects in the field of photocatalysis.
Description
Technical field
The invention belongs to material preparation and light-catalysed technical field, be specifically related to graphite-phase carbon nitride nanosheet visible-light-driven photocatalyst of a kind of combined polymerization modification and its preparation method and application.
Background technology
An important issue of current energy and environment utilizes solar energy simulating nature photosynthesis to carry out decomposition water exactly and produces the clean energy resourcies such as hydrogen.Photocatalysis technology is then a kind of potential desirable solution route.But the aspects such as solar energy utilization ratio is low, photochemical catalyst easy in inactivation, use cost height constrain the application of photochemical catalyst in industrial production.Therefore efficient, stable, the nontoxic material of preparation is the core challenge in this field as visible light catalyst.
In recent years, a kind of nonmetal polymer semiconductor---graphite phase carbon nitride (g-C
3n
4), be used to the decomposition of visible light catalytic water to realize the conversion (Nat. Mater. 2009,8,76-80) of solar energy to chemical energy.Although g-C
3n
4make some progress in photocatalysis field, but still there is its very important defect: exciton binding energy that is as little in specific area, that produce photo-generated carrier is high, quantum efficiency is low and energy gap is comparatively large and effectively can not utilize sunshine etc.On the one hand, by layer stripping (Adv. Mater. 2013,25,2452-2456; Adv. Funct. Mater. 2012,22,4763-4770), the nanoscale twins g-C of the hetero atom regulation and control thermal polymerization means synthesizing high specific surface areas such as (J. Mater. Chem. 2012,22,8083-8091)
3n
4, effectively strengthen effect of mass transmitting and more Adsorption be provided.But the quantum size effect of low dimension material makes band gap broaden, limit absorption and the utilization of visible ray.On the other hand, the people such as king proposes to adopt combined polymerization means modification g-C
3n
4photochemical catalyst, react with the thermal polycondensation that the organic compound containing carboxyl, amino or cyano group participates in cyanamid dimerization for polymerization single polymerization monomer for organic molecule monomer, improve visible absorption performance and improve object (the Angew. Chem. Int. Ed. 2012 such as photo-generated carrier separative efficiency, 5,3183-3187).But the industrial chemicals adopting this cheapness of urea is carbon nitride precursor, and combined polymerization means are incorporated into nanoscale twins g-C
3n
4research work, have not been reported.Therefore, we utilize urea for raw material, by copolymerization to nanoscale twins g-C
3n
4conjugated structure regulate and control, while enhancing catalyst surface mass transport process, reduce semiconductor band gap width, promote that photo-generated carrier is separated and migration, improve solar energy utilization ratio, have wide practical use in photocatalysis field.Experiment proves, the graphite-phase carbon nitride nanosheet visible-light-driven photocatalyst of combined polymerization modification is a kind of photochemical catalyst of efficient visible photocatalysis aquatic products hydrogen.
Summary of the invention
The object of the present invention is to provide graphite-phase carbon nitride nanosheet visible-light-driven photocatalyst of a kind of combined polymerization modification and its preparation method and application.Photochemical catalyst prepared by the present invention has the nano-lamellar structure of high-specific surface area, narrow band gap width, photo-generated carrier separation fast, transfer ability, can realize visible ray photocatalytic water efficiently and produce hydrogen.Present invention process is simple, and with low cost, 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:
A kind of graphite-phase carbon nitride nanosheet visible-light-driven photocatalyst of combined polymerization modification is the semi-conducting polymer chemical formula with nano-lamellar structure is C
3n
4, and be class graphite-phase, specific area is 60 ~ 300 m
2/ g, absorb visible ray, light absorption band edge at 430 ~ 700 nm, and has the performance of good photochemical catalyzing hydrogen making, can be used as a kind of photochemical catalyst efficiently.
The method preparing the graphite-phase carbon nitride nanosheet visible-light-driven photocatalyst of combined polymerization modification as above be with urea and organic molecule monomer for predecessor, by high-temperature hot condensation, namely obtain the graphite phase carbon nitride nanometer sheet of combined polymerization modification.Described preparation method comprises the following steps: mass ratio is that (organic compound namely containing carboxyl, amino or cyano group is polymerization single polymerization monomer for the urea of 10000:1 ~ 500 and organic molecule monomer by (1), as barbiturates, 2-anthranilo nitrile, 2-aminothiophene-3-formonitrile HCN, diaminomaleonitrile etc.) be dissolved in water, stirring at room temperature 5 ~ 48h, evaporate to dryness, grinding; (2) by pressed powder 450 ~ 700 DEG C of heat treatment 1 ~ 10h in Muffle furnace, the graphite phase carbon nitride nanometer sheet of obtained combined polymerization modification.
The graphite-phase carbon nitride nanosheet visible-light-driven photocatalyst of described combined polymerization modification is applied to decomposition water hydrogen making under visible ray.
Remarkable advantage of the present invention is:
(1) means of combined polymerization are incorporated into the modification of nanoscale twins carbonitride by the present invention first, increase specific area and reduce band gap width, and photo-generated carrier separation simultaneously, transport efficiency are improved.
(2) the graphite phase carbon nitride nanometer sheet of the combined polymerization modification of the present invention's synthesis, its advantage is low in raw material price, and preparation technology is simple, energy consumption is low, catalyst stabilization, nontoxic, be easy to reclaim, reusable edible, realistic need of production, is conducive to large-scale popularization.
(3) the graphite phase carbon nitride nanometer sheet of the combined polymerization modification of the present invention's synthesis, the organic molecule monomer selectivity wherein with modifying function is in extensive range, has good Modulatory character and universality.
(4) the graphite phase carbon nitride nanometer sheet of combined polymerization modification is applied to photocatalysis hydrogen making by the present invention first, finds that it has efficient visible ray photocatalytic water H2-producing capacity.Can carry out separating treatment easily in light-catalyzed reaction system, 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 Fourier transform infrared FT-IR spectrogram of the graphite phase carbon nitride nanometer sheet a of the combined polymerization modification of embodiment 3 gained.
Fig. 2 is that the X-ray powder diffraction XRD of the graphite phase carbon nitride nanometer sheet a of the combined polymerization modification of embodiment 3 gained schemes.
Fig. 3 is the atomic force microscope figure of the graphite phase carbon nitride nanometer sheet a of the combined polymerization modification of embodiment 3 gained.
Fig. 4 is that the UV-vis DRS DRS of the graphite phase carbon nitride nanometer sheet a of the combined polymerization modification of embodiment 3 gained schemes.
Fig. 5 is the Performance comparision figure that the graphite phase carbon nitride nanometer sheet a of the combined polymerization modification of embodiment 3 gained and traditional body phase carbon nitride b carry out visible light catalytic decomposition water hydrogen making.
Detailed description of the invention
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
Be that urea and the barbiturates of 25:1 is dissolved in water by mass ratio, stirring at room temperature 48h, evaporate to dryness, grinding.By pressed powder 450 DEG C of heat treatment 10h in Muffle furnace, the graphite phase carbon nitride nanometer sheet of obtained combined polymerization modification.
embodiment 2
Be that urea and the 2-anthranilo nitrile of 100:1 is dissolved in water by mass ratio, stirring at room temperature 24h, evaporate to dryness, grinding.By pressed powder 500 DEG C of heat treatment 5h in Muffle furnace, the graphite phase carbon nitride nanometer sheet of obtained combined polymerization modification.
embodiment 3
Be that urea and the 2-aminothiophene-3-formonitrile HCN of 1000:1 is dissolved in water by mass ratio, stirring at room temperature 12h, evaporate to dryness, grinding.By pressed powder 550 DEG C of heat treatment 2h in Muffle furnace, the graphite phase carbon nitride nanometer sheet of obtained combined polymerization modification.
embodiment 4
Be that urea and the diaminomaleonitrile of 200:1 is dissolved in water by mass ratio, stirring at room temperature 6h, evaporate to dryness, grinding.By pressed powder 650 DEG C of heat treatment 4h in Muffle furnace, the graphite phase carbon nitride nanometer sheet of obtained combined polymerization modification.
Performance test
Fig. 1 is the Fourier transform infrared FT-IR spectrogram of the graphite phase carbon nitride nanometer sheet a of the combined polymerization modification of embodiment 3 gained.As can be seen from the figure at 800 cm
-1with 1200 ~ 1600 cm
-1interval, they correspond respectively to breathing vibration and the stretching vibration of armaticity CN heterocycle of piperazine ring, at 3200 cm
-1the interval NH that there is many non-bondings mainly due to nano lamellar carbonitride surface
2, caused by NH, confirm that the product of preparation is carbon nitride material.
Fig. 2 is that the X-ray powder diffraction XRD of the graphite phase carbon nitride nanometer sheet a of the combined polymerization modification of embodiment 3 gained schemes.Can find 13.0 from figure
owith 27.5
oplace's appearance two significantly belongs to the XRD diffraction maximum of graphite phase carbon nitride (100) and (002) crystal face, confirms that the product of preparation is graphite phase carbon nitride.
Fig. 3 is the atomic force microscope figure of the graphite phase carbon nitride nanometer sheet a of the combined polymerization modification of embodiment 3 gained.Can find that from figure the product prepared has nanoscale twins pattern, lamellar spacing 2 ~ 5nm, planar dimension 2 ~ 10 μm, containing irregular holes structure among lamella.
Fig. 4 is that the UV-vis DRS DRS of the graphite phase carbon nitride nanometer sheet a of the combined polymerization modification of embodiment 3 gained schemes.Can find that from figure 600nm is widened in its light absorption of product prepared, confirm that it belongs to semi-conducting material.
Fig. 5 is the graphite phase carbon nitride nanometer sheet a of the combined polymerization modification of embodiment 3 gained and the Performance comparision figure of body phase carbon nitride b photochemical catalyzing hydrogen making.50mg catalyst and reaction reagent (containing the 100mL triethanolamine aqueous solution of 10 vol. %, original position photo-reduction H
2ptCl
6, i.e. 3 wt. % Pt) react in upper illuminated reactor.Can find that from figure the hydrogen-producing speed of the product (xenon lamp 300W, filter plate λ > 420 nm) under visible light prepared reaches 740 μm of ol/h, improve 74 times compared with body phase carbon nitride (10 μm of ol/h).
The foregoing is only preferred embodiment of the present invention, all equalizations done 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 (1)
1. a preparation method for the graphite-phase carbon nitride nanosheet visible-light-driven photocatalyst of combined polymerization modification, is characterized in that: comprise the following steps:
(1) be that the urea of 10000:1 ~ 500 and organic molecule monomer are dissolved in water by mass ratio, stirring at room temperature 5 ~ 48h, evaporate to dryness, grinding; Described organic molecule monomer is 2-aminothiophene-3-formonitrile HCN;
(2) by the pressed powder of step (1) 450 ~ 700 DEG C of heat treatment 1 ~ 10h in Muffle furnace, the graphite phase carbon nitride nanometer sheet of obtained combined polymerization modification, chemical formula is C
3n
4, and be class graphite-phase, specific area is 60 ~ 300 m
2/ g, absorb visible ray, light absorption band edge is at 430 ~ 700 nm;
The graphite phase carbon nitride nanometer sheet of described combined polymerization modification is applied to visible light catalytic decomposition water hydrogen making.
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