CN105148973B - A kind of preparation method of the electron beam irradiation modified class graphite phase carbon nitride as visible light catalyst - Google Patents
A kind of preparation method of the electron beam irradiation modified class graphite phase carbon nitride as visible light catalyst Download PDFInfo
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Abstract
The present invention relates to a kind of method of electron beam irradiation modified class graphite phase carbon nitride.Class graphite phase carbon nitride is produced using existing known technology method first, and class graphite phase carbon nitride, alcohol, alkali and water are made into suspension by a certain percentage.Then above-mentioned suspension is placed in electron beam generating apparatus, is subjected to the electron beam irradiation of doses, irradiation dose is 200 ~ 1200 kGy.By being centrifugally separating to obtain solid, and scrubbed and drying process, electron beam irradiation modified class graphite phase carbon nitride is produced.The modified material of gained of the invention, has excellent visible light photocatalysis performance, can effectively solve the problems such as environmental pollution.Meanwhile modification is not required to enter other dopants, and technique is simple, easy to operate, is easy to mass produce.
Description
Technical field
The present invention relates to the method for modifying of a species graphite phase carbon nitride, particularly a kind of electron beam irradiation modified class graphite
The method of phase carbon nitride.
Background technology
Recently, a kind of non-metal optical catalyst, class graphite phase carbon nitride, the extensive concern of people is caused.Due to its tool
There is the features such as suitable energy gap, high-specific surface area and excellent chemical stability, and attempted to be used for sunshine by scholars
The numerous areas such as energy conversion, light compositing, electro-catalysis and bio-imaging.Photocatalysis technology is a kind of environmentally friendly catalysis technique,
It has the characteristics that clean energy resource utilization, low energy consumption, reaction condition gentle, non-secondary pollution, easy to operate, is that current environment is controlled
Reason, the study hotspot in energy regeneration field.
However, simple class graphite phase carbon nitride, because the probability of recombination of higher photo-generate electron-hole pair be present in it,
So directly photocatalysis efficiency is not too much high.In order to overcome this shortcoming and inferior position, many measures and means are obtained for application
And development, such as noble-metal-supported（Such as silver, palladium, gold）, it is metal-doped（Such as iron, zinc, erbium）, nonmetal doping（Such as boron, sulphur, fluorine）、
It is carrier loaded（Such as graphene, CNT, mesoporous silicon oxide）And semiconductors coupling（Such as silver orthophosphate, molybdenum sulfide, bismuth tungstate）
The methods of.But, in these means, the overwhelming majority inevitably needs to introduce other materials and material.
Therefore, develop a kind of technique to be simple and convenient to operate, and the method for modifying of other dopants need not be introduced, be to grind
Study carefully of great value creation in class graphite phase carbon nitride visible light photocatalysis field.
The content of the invention
It is an object of the invention to provide a kind of electron beam irradiation modified class graphite-phase nitridation as visible light catalyst
The preparation method of carbon.
In order to achieve the above object, the present invention uses following technical scheme.
A kind of preparation method of the electron beam irradiation modified class graphite phase carbon nitride as visible light catalyst of the present invention, its
It is characterized by following process and step：
A. class graphite phase carbon nitride is prepared by existing known technology；
B. class graphite phase carbon nitride, alcohol, alkali and water are made into suspension by a certain percentage；Selected alcohol is isopropanol or second
The alcohols such as alcohol or the tert-butyl alcohol；Selected alkali is concentrated ammonia liquor or sodium hydroxide or sodium carbonate；Its mass ratio is as follows：Class graphite-phase nitrogen
Change carbon:Isopropanol:Concentrated ammonia liquor:Water=(10 ~ 200) mg: (2~5 )g : (50~100) mg : 30 g；Wherein ammonia
Concentration >=25% of water；
C. the suspension obtained by step b is subjected to electron beam irradiation, irradiation dose is 200 ~ 1200 kGy；By centrifugation
Isolated solid, and wash, dry, produce electron beam irradiation modified class graphite phase carbon nitride.
It is characteristic of the invention that：Using electron beam irradiation, class graphite phase carbon nitride surface texture is set to produce certain change,
It can improve its energy gap, promote efficiently separating for light induced electron and hole, and strengthen the absorbability of visible regime.Together
When, other dopants need not be introduced in modifying process, make modifying process more green.
In addition, by the present invention in that electron beam is modified the nitridation of class graphite-phase as radiation source caused by electron accelerator
Carbon.It is pollution-free in radiative process, and technique is simple, it is easy to operate, it is possible to achieve industrialized production.Electron accelerator is closed then
Electron beam disappears immediately, therefore the inventive method security is good, pollution-free, is advantageous to environmental protection.
Brief description of the drawings
Fig. 1 is the XRD spectra of the embodiment of the present invention and gained class graphite phase carbon nitride in comparative example.
Fig. 2 is the DRS spectrum of the embodiment of the present invention and gained class graphite phase carbon nitride in comparative example.
Fig. 3 is the PL spectrum of the embodiment of the present invention and gained class graphite phase carbon nitride in comparative example.
Fig. 4 is the Photocatalytic Activity for Degradation curve of the embodiment of the present invention and gained class graphite phase carbon nitride in comparative example
Figure.
Embodiment
Embodiment
The process and step of the present embodiment are as described below：
A. class graphite phase carbon nitride is produced by existing known technology first：4.0 g urea are taken to add 25 mL earthenwares with cover
Crucible, and being put into Muffle furnace, 80 °C of dryings 24 hours, 550 °C of thermal polymerizations 3 hours are then heated to, it is then naturally cold
But to room temperature.The yellow solid obtained by water and dilute nitric acid solution clean is multiple, is finally dried overnight under 60 °C.
B. class graphite phase carbon nitride, 30 g water, 3 g isopropanols and the mixing of 60 mg concentrated ammonia liquors of the above-mentioned synthesis of 60 mg are taken
It is sealed in after uniformly in a Polythene Bag.This bag is placed in progress room temperature radiation treatment under electron accelerator.Irradiation dose is set
It is set to 800 kGy.
C. the suspension after upper step is irradiated produces electron beam irradiation modified after the centrifugation, washing, drying of routine
Class graphite phase carbon nitride.
The sample of gained is characterized, its partial results is as shown in drawings.Modified class graphite phase carbon nitride it is grand
See darker more yellow, illustrate that it has stronger visible absorption ability.
Comparative example：
With embodiment a steps, difference is without b and step c, that is, to obtain not the preparation process and step of this comparative example
Primitive class graphite phase carbon nitride through electron beam irradiation modified processing.
The every instrument test and photocatalysis performance of embodiment product are tested
20 mg photochemical catalysts are taken to add 50 mL（20 mg·L-1）Rhodamine B solution.Then it is transferred in a quartz ampoule,
The dark bubbling of 90 minutes is carried out, reaches adsorption equilibrium.Under bubbling state, coordinate the ultraviolet filters of 420 nm using 350 W xenon lamps
Mating plate is light source, carries out circulating type visible ray light and excites.At the interval of light-catalyzed reaction, a small amount of solution is taken out, by 0.22
μm filtering with microporous membrane obtains clear solution.Using the absorbance at spectrophotometer detection characteristic peak 550 nm, so as to analyze
Light-catalysed efficiency.
Referring to accompanying drawing, Fig. 1 is the X-ray diffraction of the embodiment of the present invention and gained class graphite phase carbon nitride in comparative example
（XRD）Spectrogram.XRD analysis：Using the thing of Rigaku Co., Ltd. D/max-2550 types X-ray diffractometer analysis resulting materials
Phase and crystallinity.It is can be seen that by the contrast of spectrogram after electron beam irradiation modified processing, the diffraction peak intensity of material is slightly
Weaken, illustrate that electron beam irradiation generates certain destruction to its surface micro-structure.
Fig. 2 is the diffusing reflection spectrum of the embodiment of the present invention and gained class graphite phase carbon nitride in comparative example（DRS）Spectrum.
DRS is analyzed：Using HIT's U-3010 types are ultraviolet and the light absorbs energy of visible spectrophotometer analysis resulting materials
Power.Be can be seen that by the contrast of spectrogram after electron beam irradiation modified processing, material for visible ray absorbability significantly
Increase.
Fig. 3 is the luminescence generated by light of the embodiment of the present invention and gained class graphite phase carbon nitride in comparative example（PL）Spectrum.PL points
Analysis：Using the photoluminescence property of HIT F-7000 types sepectrophotofluorometer analysis resulting materials.Pass through spectrogram
Contrast can be seen that after electron beam irradiation modified processing, the photoluminescence property of material significantly weakens, imply that photoproduction electricity
Son and the raising of hole separative efficiency.
Fig. 4 is that gained class graphite phase carbon nitride is as photochemical catalyst in the embodiment of the present invention and comparative example, in visible striation
The degradation curve of rhodamine B degradation under part, it can be seen that after electron beam irradiation modified processing, can under visible light conditions
With about 4.5 times of photocatalysis efficiency of lifting.
Claims (1)
- A kind of 1. preparation method of the electron beam irradiation modified class graphite phase carbon nitride as visible light catalyst, it is characterised in that This method concretely comprises the following steps：A. class graphite phase carbon nitride is prepared by existing known technology；B. class graphite phase carbon nitride, alcohol, alkali and water are made into suspension by a certain percentage；Selected alcohol is isopropanol；Selected Alkali is concentrated ammonia liquor or sodium hydroxide or sodium carbonate；Its mass ratio is as follows：Class graphite phase carbon nitride:Isopropanol:Concentrated ammonia liquor: Water=(10 ~ 200) mg: (2~5 )g : (50~100) mg : 30 g；Wherein concentration >=25% of ammoniacal liquor；C. the suspension obtained by step b is subjected to electron beam irradiation, irradiation dose is 200 ~ 1200 kGy；By centrifugation Solid is obtained, and washs, dry, produces electron beam irradiation modified class graphite phase carbon nitride.
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| CN105565427B (en) * | 2015-12-17 | 2018-05-25 | 南京工业大学 | A kind of light degradation reactor based on graphite phase carbon nitride film and preparation method thereof |
| CN107824156B (en) * | 2017-10-31 | 2020-02-18 | 南京大学昆山创新研究院 | Gas-assisted renewable sol/gel type decolorizing agent and preparation method and application thereof |
| CN110142055B (en) * | 2018-02-11 | 2022-04-12 | 天津理工大学 | Microwave irradiation method for enhancing photocatalytic performance of graphite-phase carbon nitride |
| CN112090423A (en) * | 2020-09-27 | 2020-12-18 | 湖北科技学院 | Enhancement of Bi based on electron beam radiation2WO6Method for photocatalytic performance |
| CN113680358B (en) * | 2021-07-13 | 2023-09-12 | 湖南农业大学 | Silver phosphate/boron carbide composite photocatalyst and preparation method and application thereof |
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Effective date of registration: 20201224 Address after: 201499 Building 1, No. 5601 Yanqian Road, Fengxian District, Shanghai Patentee after: Shanghai qiaoyue environmental technology partnership (L.P.) Address before: No.99 SHANGDA Road, Baoshan District, Shanghai 200444 Patentee before: Shanghai University |
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