CN103801354A - Graphite carbon nitride hollow sphere visible-light catalyst for post annealing treatment - Google Patents
Graphite carbon nitride hollow sphere visible-light catalyst for post annealing treatment Download PDFInfo
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- CN103801354A CN103801354A CN201410089581.0A CN201410089581A CN103801354A CN 103801354 A CN103801354 A CN 103801354A CN 201410089581 A CN201410089581 A CN 201410089581A CN 103801354 A CN103801354 A CN 103801354A
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- hollow ball
- graphite
- carbonitride
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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
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- 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 graphite carbon nitride hollow sphere visible-light catalyst for post annealing treatment, and a preparation method and application thereof, and belongs to the technical fields of material preparation and photocatalysis. Post annealing is taken as an important post-treatment technology, the defects caused by the carbon nitride hollow sphere in the preparation process can be removed, the crystallization quality is improved, and the performance of a sample is improved. The prepared graphite carbon nitride hollow sphere for post annealing modification still can keep the morphology of the hollow sphere and even particle size distribution after high-temperature treatment. Compared with the traditional phase carbon nitride, the specific surface area is effectively improved, so that the performance of decomposing water to produce hydrogen is improved. The graphite carbon nitride hollow sphere visible-light catalyst is simple in synthetic process, low in cost and high in catalytic efficiency, accords with the practical production requirements, and has a broad 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 graphite-phase carbonitride hollow ball visible light catalyst of a kind of after annealing processing and its preparation method and application.
Background technology
Hollow ball nanostructured is because its unique structure is in all very attractive of Science and Technology field.It is unique that these hollow ball nanostructureds have advantages of, as: the bearing capacity that density is low, specific area is large, good and high osmosis can etc., can be applicable to the application such as encapsulation of medicine and gene delivery, Chu Qing, catalysis and cosmetics and coating as a kind of multi-functional material.In recent years, TiO
2, SnO
2, CdS, CdTe, Cu
2the semiconductor hollow ball nanostructureds such as O are used as photochemical catalyst for decomposing aquatic products hydrogen field.But due to them, all to contain metallic element, solar energy utilization ratio low and only ultraviolet light is had correspondingly, and toxicity is large simultaneously, self is unstable, the problems such as photoetch easily occur has seriously restricted its application in industrial production.
At present, graphite-phase carbonitride semi-conducting polymer material is subject to scientist and researchers' extensive concern as a kind of not containing metal, efficient, stable, nontoxic visible light catalytic agent material.Researcher utilizes hard template method successfully to prepare hollow ball-shape carbonitride (Nature Communications 2012,3,1139).It not only has the unique advantage of hollow ball nanostructured, also has the advantage of carbon nitride material concurrently simultaneously.But this material polymerization synthetic by high temperature thermopolymerization method is incomplete, has a large amount of defects in material.These defects may become right complex centre, light induced electron-hole, thereby reduce the quantum efficiency of light-catalyzed reaction.
After annealing method is incorporated into the research work of carbonitride hollow ball, have not been reported.By after annealing method, the structure of carbonitride hollow ball is regulated and controled, can eliminate the defect introduced in Material growth process, improve crystalline quality and improve the performance (Journal of Catalysis 2008,255,59) of sample.Still keep the pattern of hollow ball through high temperature after annealing carbonitride hollow ball after treatment, increase specific area simultaneously, reduced semiconductor band gap width, promoted photo-generated carrier to separate and migration, improve solar energy utilization ratio, have wide practical use in photocatalysis field.The carbonitride hollow ball visible light catalyst that experiment showed, after annealing processing 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 graphite-phase carbonitride hollow ball visible light catalyst of a kind of after annealing processing and its preparation method and application.Photochemical catalyst prepared by the present invention still can keep its hollow ball pattern after after annealing is processed, greatly improve its specific area, thereby have more avtive spot, photo-generated carrier separation fast, transfer ability, can realize visible ray decomposition water efficiently and produce 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:
The graphite-phase carbonitride hollow ball visible light catalyst of after annealing processing is a semi-conducting polymer with hollow ball pattern, and chemical formula is C
3n
4, and be class graphite-phase, specific area is 80 ~ 280 m
2/ g, absorbs visible ray, and light absorption band edge is at 420 ~ 700 nm, and has the performance of good photochemical catalyzing hydrogen making, can be used as a kind of photochemical catalyst efficiently.
The method of preparing the graphite-phase carbonitride hollow ball visible light catalyst of after annealing processing as above is, after using hard template method by high temperature thermal condensation, remove template, then by the graphite-phase carbonitride hollow ball after annealing 5h under air atmosphere different temperatures obtaining.Described preparation method comprises the following steps: (1) synthetic different-grain diameter size and the thick silica spheres (St ber silica sol) of different shells.(2) 3 g cyanamides are dissolved in the aqueous solution of 15.5 g silica spheres colloidal sols, ultrasonic, and 80 ℃ add thermal agitation, centrifugal, dry, and obtain white powder, and in air or nitrogen atmosphere, in 550 ℃ of insulation 4 h, heating rate is 2.3 ℃/min, obtains yellow powder.(3) join 8 mol/L NH
4hF
2in solution, stir 48 h, filter, washing, then stir 48 h, and filter, washing, 80 ℃ of vacuum drying, obtain carbonitride hollow ball.(4) by hollow ball carbonitride after annealing 5h at 300-550 ℃ in air atmosphere.
The graphite-phase carbonitride hollow ball visible light catalyst of described combined polymerization modification is applied to decomposition water hydrogen making under visible ray.
Remarkable advantage of the present invention is:
(1) the present invention is incorporated into the means of after annealing the modification of hollow ball carbonitride first, can eliminate defect, raising crystalline quality that carbonitride hollow ball is introduced in preparation process, has increased its specific area simultaneously.
(2) the graphite-phase carbonitride hollow ball of the synthetic after annealing processing of the present invention, not containing metal, has the advantages such as cheapness, environmental protection, stable, light weight.
(3) the graphite-phase carbonitride hollow ball of the synthetic after annealing processing of the present invention, the method for post processing is comparatively simple, has good Modulatory character and universality.
(4) the graphite-phase carbonitride hollow ball that the synthetic post processing of this method is annealed by the control to the after annealing time, can be realized the regulation and control of the structure and activity to carbonitride hollow ball in last handling process.
(5) the present invention is applied to photochemical catalyzing by the graphite-phase carbonitride hollow ball of after annealing processing first, finds that after annealing processing is conducive to improve the Photocatalyzed Hydrogen Production performance of carbonitride, and has good activity stability.In light-catalyzed reaction system, it can carry out separating treatment easily, and 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 transmission electron microscope (TEM) figure of the graphite-phase carbonitride hollow ball of the after annealing processing of embodiment 1-4 gained.
Fig. 2 is the Fourier transform infrared FT-IR spectrogram of the graphite-phase carbonitride hollow ball of the after annealing processing of embodiment 4 gained.
Fig. 3 is the X-ray powder diffraction XRD figure of the graphite-phase carbonitride hollow ball of the after annealing processing of embodiment 4 gained.
Fig. 4 is the UV-vis DRS DRS figure of the graphite-phase carbonitride hollow ball of the after annealing processing of embodiment 4 gained.
Fig. 5 is the performance comparison diagram that the graphite-phase carbonitride hollow ball of after annealing processing of embodiment 4 gained and the carbonitride hollow ball of the non-modified of comparative example 1 gained carry out 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
3g cyanamide is dissolved in the aqueous solution of 15.5 g silica spheres colloidal sols, ultrasonic, 80 ℃ add thermal agitation, centrifugal, dry, and obtain white powder, and in air or nitrogen atmosphere, in 550 ℃ of insulation 4 h, heating rate is 2.3 ℃/min, obtains yellow powder.Join 8 mol/L NH
4hF
2in solution, stir 48 h, filter, washing, then stir 48 h, and filter, washing, 80 ℃ of vacuum drying, obtain carbonitride hollow ball.After annealing 5h at 300 ℃ in air atmosphere.
3g cyanamide is dissolved in the aqueous solution of 15.5 g silica spheres colloidal sols, ultrasonic, 80 ℃ add thermal agitation, centrifugal, dry, and obtain white powder, and in air or nitrogen atmosphere, in 550 ℃ of insulation 4 h, heating rate is 2.3 ℃/min, obtains yellow powder.Join 8 mol/L NH
4hF
2in solution, stir 48 h, filter, washing, then stir 48 h, and filter, washing, 80 ℃ of vacuum drying, obtain carbonitride hollow ball.After annealing 5h at 400 ℃ in air atmosphere.
3g cyanamide is dissolved in the aqueous solution of 15.5 g silica spheres colloidal sols, ultrasonic, 80 ℃ add thermal agitation, centrifugal, dry, and obtain white powder, and in air or nitrogen atmosphere, in 550 ℃ of insulation 4 h, heating rate is 2.3 ℃/min, obtains yellow powder.Join 8 mol/L NH
4hF
2in solution, stir 48 h, filter, washing, then stir 48 h, and filter, washing, 80 ℃ of vacuum drying, obtain carbonitride hollow ball.After annealing 5h at 500 ℃ in air atmosphere.
embodiment 4
3g cyanamide is dissolved in the aqueous solution of 15.5 g silica spheres colloidal sols, ultrasonic, 80 ℃ add thermal agitation, centrifugal, dry, and obtain white powder, and in air or nitrogen atmosphere, in 550 ℃ of insulation 4 h, heating rate is 2.3 ℃/min, obtains yellow powder.Join 8 mol/L NH
4hF
2in solution, stir 48 h, filter, washing, then stir 48 h, filter washing.80 ℃ of vacuum drying, obtain carbonitride hollow ball.After annealing 5h at 550 ℃ in air atmosphere.
comparative example 1
3g cyanamide is dissolved in the aqueous solution of 15.5 g silica spheres colloidal sols, ultrasonic, 80 ℃ add thermal agitation, centrifugal, dry, and obtain white powder, and in air or nitrogen atmosphere, in 550 ℃ of insulation 4 h, heating rate is 2.3 ℃/min, obtains yellow powder.Join 8 mol/L NH
4hF
2in solution, stir 48 h, filter, washing, then stir 48 h, filter washing.80 ℃ of vacuum drying, obtain carbonitride hollow ball.
performance test
Fig. 1 is transmission electron microscope (TEM) figure of the graphite-phase carbonitride hollow ball through after annealing processing of embodiment 1-4 and comparative example 1 gained.From finding figure that graphite-phase carbonitride hollow ball still has uniform hollow ball pattern after high-temperature process, particle diameter is in 270 nm left and right, about thick 60 nm of shell.(a), (b) undressed carbonitride hollow ball; (c) 300 ℃ of after annealings of carbonitride hollow ball; (d) 400 ℃ of after annealings of carbonitride hollow ball; (e) 500 ℃ of after annealings of carbonitride hollow ball; (f) 550 ℃ of after annealings of carbonitride hollow ball.
Fig. 2 is the Fourier transform infrared FT-IR spectrogram of the graphite-phase carbonitride hollow ball through 550 ℃ of after annealing processing of embodiment 4 gained.As can be seen from the figure hollow ball carbonitride still keeps the structure of graphite-phase carbonitride after high-temperature heat treatment.At 2180 cm
-1locate the degree of polymerization that the not disappearance of polymerization itrile group shows to have improved through after annealing processing sample.
Fig. 3 is the X-ray powder diffraction XRD figure of the graphite-phase carbonitride hollow ball through 550 ℃ of after annealing processing of embodiment 4 gained.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 not destroy after high temperature after annealing is processed the structure of graphite-phase carbonitride hollow ball.
Fig. 4 is the UV-vis DRS DRS figure of the graphite-phase carbonitride hollow ball through 550 ℃ of after annealing processing of embodiment 4 gained.From figure, can find that its light absorption of product of preparation widens 550 nm, confirm that after annealing processing is expanded the pi-conjugated structure of carbonitride hollow ball, thereby increased its light abstraction width.
Fig. 5 is the performance comparison diagram of the graphite-phase carbonitride hollow ball (HCNS550) through 550 ℃ of after annealing processing of embodiment 4 gained and untreated carbonitride hollow ball (HCNS) the photochemical catalyzing hydrogen making of comparative example 1 gained.20mg catalyst and reaction reagent are (containing the 100mL triethanolamine aqueous solution of 10 vol. %, original position photo-reduction H
2ptCl
6, i.e. 3 wt.% Pt) react in upper photograph in formula reactor.From figure, can find product (xenon lamp 300W under visible ray of preparation, filter plate λ > 420 nm) hydrogen-producing speed reach 351 μ mol/h, improved 2 times compared with carbonitride hollow ball (168 μ mol/h) without after annealing processing.
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 (6)
1. a graphite-phase carbonitride hollow ball visible light catalyst for after annealing processing, is characterized in that: chemical formula is C
3n
4, and be class graphite-phase, be a kind of polymer semiconductor.
2. the graphite-phase carbonitride hollow ball visible light catalyst of after annealing processing according to claim 1, is characterized in that: pattern and micro-nano structure that described graphite-phase carbonitride is hollow ball.
3. the graphite-phase carbonitride hollow ball visible light catalyst of after annealing processing according to claim 1, is characterized in that: the specific area of graphite-phase carbonitride hollow ball is 80 ~ 280 m
2/ g, particle size is 270-600nm, and the thick 30-100nm of shell absorbs visible ray, and light absorption band edge is at 420 ~ 700 nm.
4. a method of preparing the graphite-phase carbonitride hollow ball visible light catalyst of after annealing processing as claimed in claim 1, is characterized in that: the graphite-phase carbonitride hollow ball visible light catalyst that carbonitride hollow ball is carried out under air atmosphere to after annealing processing and obtain described after annealing processing.
5. the preparation method of the graphite-phase carbonitride hollow ball visible light catalyst of after annealing processing according to claim 1, is characterized in that: comprise the following steps:
(1) synthetic silica ball;
(2) 3 g cyanamides are dissolved in the aqueous solution of 15.5g silica spheres colloidal sol, ultrasonic, and 80 ℃ add thermal agitation, centrifugal, dry, and in air or nitrogen atmosphere, are heated to 550 ℃ of insulation 4 h take heating rate as 2.3 ℃/min;
(3) product of step (2) is joined to 8 mol/L NH
4hF
2in solution, stir 48 h, filter, washing, then stir 48 h, and filter, washing, 80 ℃ of vacuum drying, obtain carbonitride hollow ball;
(4) 300-550 ℃ of after annealing 5h under air atmosphere, the graphite-phase carbonitride hollow ball visible light catalyst of the after annealing processing described in obtaining.
6. the application of the graphite-phase carbonitride hollow ball visible light catalyst of after annealing processing according to claim 1, is characterized in that: described graphite-phase carbonitride hollow ball visible light catalyst is applied to photochemical catalyzing hydrogen making under visible ray.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104722325A (en) * | 2015-02-27 | 2015-06-24 | 清华大学 | Three-dimensional macro-scale porous graphite phase carbon nitride photocatalyst and preparation and application of photocatalyst |
| CN106744742A (en) * | 2016-11-11 | 2017-05-31 | 天津大学 | Many shell graphite phase carbon nitride hollow nano-spheres and its synthetic method and application |
| CN106938198A (en) * | 2016-01-04 | 2017-07-11 | 中国科学院化学研究所 | A kind of graphite phase carbon nitride porous microsphere and preparation method thereof |
| CN108584892A (en) * | 2018-04-26 | 2018-09-28 | 福州大学 | A kind of preparation method and applications of crystalline phase azotized carbon nano particle |
| CN111659451A (en) * | 2020-07-14 | 2020-09-15 | 中国科学院山西煤炭化学研究所 | Preparation method and application of nitrogen vacancy-containing few-layer porous carbon nitride photocatalyst |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104722325A (en) * | 2015-02-27 | 2015-06-24 | 清华大学 | Three-dimensional macro-scale porous graphite phase carbon nitride photocatalyst and preparation and application of photocatalyst |
| CN106938198A (en) * | 2016-01-04 | 2017-07-11 | 中国科学院化学研究所 | A kind of graphite phase carbon nitride porous microsphere and preparation method thereof |
| CN106938198B (en) * | 2016-01-04 | 2019-08-20 | 中国科学院化学研究所 | A kind of graphite phase carbon nitride porous microsphere and preparation method thereof |
| CN106744742A (en) * | 2016-11-11 | 2017-05-31 | 天津大学 | Many shell graphite phase carbon nitride hollow nano-spheres and its synthetic method and application |
| CN108584892A (en) * | 2018-04-26 | 2018-09-28 | 福州大学 | A kind of preparation method and applications of crystalline phase azotized carbon nano particle |
| CN111659451A (en) * | 2020-07-14 | 2020-09-15 | 中国科学院山西煤炭化学研究所 | Preparation method and application of nitrogen vacancy-containing few-layer porous carbon nitride photocatalyst |
| CN111659451B (en) * | 2020-07-14 | 2023-03-24 | 中国科学院山西煤炭化学研究所 | Preparation method and application of nitrogen vacancy-containing few-layer porous carbon nitride photocatalyst |
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