CN105289684A - Method for preparing porous flake-like graphite phase carbon nitride on large scale, and application thereof - Google Patents
Method for preparing porous flake-like graphite phase carbon nitride on large scale, and application thereof Download PDFInfo
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- CN105289684A CN105289684A CN201510632498.8A CN201510632498A CN105289684A CN 105289684 A CN105289684 A CN 105289684A CN 201510632498 A CN201510632498 A CN 201510632498A CN 105289684 A CN105289684 A CN 105289684A
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- carbon nitride
- phase carbon
- porous flake
- graphite phase
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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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention discloses a method for preparing porous flake-like graphite phase carbon nitride with efficient visible light photocatalytic degradation activity of pollutants on a large scale, and belongs to the technical field of polymeric materials and photocatalysis. A thermopolymerization method is adopted, and urea is taken as raw materials and is subjected to certain processing through a direct calcination method in an aluminum reactor to obtain efficient porous flake-like graphite phase carbon nitride photocatalyst. The yield and an input raw material amount have a good linear relationship, and mass preparation can be simply realized. The obtained graphite phase carbon nitride is flake like, has a large specific surface area and favorable visible light absorption capability and especially has efficient visible light photocatalytic degradation capability of organic pollutants. The technology of the invention can be used for the purification processing of organic maters in industrial wastewater and municipal domestic wastewater.
Description
Technical field
The invention belongs to polymeric material technical field and photocatalysis technology field, be specifically related to a kind of porous flake graphite phase carbon nitride method that preparation in enormous quantities has efficient visible light photocatalytic pollutant degradation activity.
Background technology
At present, along with industrial expansion, incident environmental problem also highlights day by day, and the phenomenons such as water pollutions, atmosphere pollution, noxious waste pollution emerge in an endless stream, and how to process the problem of environmental pollution faced now and attract attention all the more.Water is as Source of life, and be that the mankind depend on for existence one of most base substance, how administering water pollution problems is the focus that people pay close attention to naturally.Conventional sewage disposal technology is as physical absorption, Coagulation Method, By Bubble-floating Method etc., organic pollutants has been transferred to solid phase by these methods, but do not reach the object of real degradation of contaminant, cause secondary pollution also with the problem that adsorbent, coagulant regeneration etc. are new.Photocatalysis technology, as a kind of emerging pollutant treatment technology, is paid attention to widely in academia.The feature of this technology is, by the light absorbing energy of semiconductor light-catalyst, produce electronics and hole, these electronics and hole or participate in the degradation reaction of pollutant directly, or generate living radical by redox reaction and indirectly realize the degraded of pollutant.The degraded of this method thoroughly, and can utilize solar energy as energy source, non-secondary pollution and energy-conserving and environment-protective, and application prospect is vast.But current photocatalysis technology applies to actual pollution plot and is faced with some problems in addition, such as: in photochemical catalyst itself and preparation process thereof, whether can cause secondary pollution; Whether can realize batch synthesis at lower cost, and keep efficient photocatalytic activity etc.Although traditional P25 photochemical catalyst is nontoxic and achieve and commercially produce, titanium dioxide limits by the energy gap of himself, is confined to absorb ultraviolet light, and account for the visible ray of larger proportion in sunshine under, photocatalysis effect is unsatisfactory.Graphite phase carbon nitride is as a kind of two-dimensional polymer semi-conducting material, and energy gap is about 2.7eV, effectively can absorb visible ray, and synthetic method is simple, and cheaper starting materials is easy to get, and itself is nontoxic, is a kind of ideal catalysis material.But the block g-C that the employing of report at present obtains with the direct thermal polymerization of presoma (as: melamine, cyanamid dimerization etc.) that carbon nitrogen element is composition
3n
4, its specific area is little, and photo-generate electron-hole recombination rate is high, and photocatalysis performance is poor.Using urea as presoma, owing to producing complicated phase transformation disturbance in urea thermal decomposition process, porous g-C can be obtained
3n
4, specific area increases, and photocatalysis performance strengthens.Due to g-C
3n
4be a kind of two dimensional surface molecular structure material, utilize the two-dimensional nature of himself, synthesizing flaky structure g-C
3n
4photo-generate electron-hole will be contributed to be separated, improve photocatalytic activity.But, at present about g-C
3n
4synthesis be also in laboratory small lot preparation research, about preparation in enormous quantities there is the porous flake g-C of high efficiency photocatalysis activity
3n
4also do not appear in the newspapers.
Summary of the invention
Preparation in enormous quantities is the object of the present invention is to provide to have the porous flake graphite phase carbon nitride method of efficient visible light photocatalytic pollutant degradation activity.The inventive method is simple, and controllability is good.
The porous flake graphite phase carbon nitride preparation method with efficient visible light photocatalytic pollutant degradation activity provided by the present invention, concrete steps are as follows:
Raw materials is directly put into a clean reactor, be placed in Muffle furnace and be heated to specified temp with certain heating rate, calcine some hours, then naturally cool.After cool to room temperature, reactor is taken out, obtain g-C
3n
4powder.The powder obtained is scattered in specific solvent with certain proportion, then through ultrasonic process, heats rapid draing under vacuum, obtain desired porous flake g-C
3n
4.
Wherein, raw materials used is urea.
Described reactor is semi-enclosed aluminum or ceramic reactor, and neglecting greatly of reactor adds material quantity and determine, and retains the reaction compartment of 30% ~ 80%.
Described heating ramp rate is 0.5 ~ 4 DEG C/min, and calcining heat is 560 ~ 640 DEG C, and calcination time is 1 ~ 4 hour.
Described dispersion solvent for use is ethanol, water or isopropyl alcohol, g-C
3n
4be 1g:20 ~ 100mL with solvent ratios, sonication treatment time is 20 ~ 90 minutes, and baking temperature is 50 ~ 100 DEG C, and dry vacuum is-0.1 ~-0.7MPa.
The method of photocatalytic degradation water pollutant provided by the present invention, concrete steps are as follows:
Target degradation product is dissolved in the aqueous solution, be mixed with certain density target degradation product solution, the porous flake graphite phase carbon nitride of preparation in step 2 is joined in degradation product solution, stirs, make target degradation product reach adsorption-desorption balance in photocatalyst surface.Afterwards, illumination is carried out to solution, sample analysis in Fixed Time Interval, observe the change in concentration of target degradation product in solution.
Wherein, described target degradation product comprises dyestuff, phenols, medicine, organic acid, and concentration is 10
-6~ 10
-3mol/L.
Described absorption mixing time is 10 ~ 60min.
Described light source is visible ray, simulated solar irradiation, sunshine.
Compared with prior art, the present invention has the following advantages:
1) method provided by the present invention is towards production in enormous quantities, simple to operation, and controllability is strong, is applicable to industrial applications.
2) g-C provided by the present invention
3n
4in porous flake, specific area is comparatively large, and photo-generate electron-hole is effectively separated, and photocatalysis degradation organic contaminant ability is strong.
Accompanying drawing explanation
Fig. 1, embodiment 1 (1) small batch preparation experiment output porous flake g-C
3n
4the linear regression graph of amount and urea input amount corresponding relation.
Preparation experiment output porous flake g-C in enormous quantities in Fig. 2, embodiment 1 (2)
3n
4the linear regression graph of amount and urea input amount corresponding relation.
The porous flake g-C that Fig. 3, embodiment 1 (2) obtain
3n
4scanning electron microscope (SEM) photograph.
Porous flake g-C in Fig. 4, embodiment 2
3n
4the degradation curve of photocatalytic degradation rhodamine B.
Ultraviolet-visible absorption spectroscopy figure in Fig. 5, embodiment 2 in rhodamine B degradation process.
Detailed description of the invention
Below in conjunction with accompanying drawing and example, the invention will be further described, but the present invention is not limited to following examples.
Embodiment 1
1) small lot prepares porous flake g-C
3n
4: in little volume reactor, get the urea (M of different quality
0=2.5g, 6.25g, 12.5g, 18g, 25g, 35g, 45g), with 3 DEG C per minute firing rate be warmed up to 600 DEG C, calcine 2 hours, Temperature fall is to room temperature.By the powder dispersion that obtains in ethanol in proper amount, ultrasonic process 30 minutes, 70 DEG C, rapid draing under-0.1MPa vacuum condition, obtains desired porous flake g-C
3n
4(take corresponding weight M
1).
2) porous flake g-C is prepared in enormous quantities
3n
4: in large volume reactor, expand preparative-scale, increase urea input amount (M
0=100g, 300g, 500g, 750g, 1000g), with 3 DEG C per minute firing rate be warmed up to 600 DEG C, calcine 2 hours, Temperature fall is to room temperature.By the powder dispersion that obtains in ethanol in proper amount, ultrasonic process 30 minutes, 70 DEG C, rapid draing under-0.1MPa vacuum condition, obtains desired porous flake g-C
3n
4(take corresponding weight M
1)
As Fig. 1, when prepared by small lot, to M
0-M
1scatter diagram carry out linear regression analysis, the linearly dependent coefficient R wherein obtained
2reach 0.99, show in small lot preparation process, the porous flake g-C that the method obtains
3n
4amount and raw material input amount be proportional, this proportional relation can be used for amplify produce, control output.
As Fig. 2, reaction unit is expanded, increase raw material input amount, to M
0-M
1scatter diagram carry out linear regression analysis, the linearly dependent coefficient R wherein obtained
2still keep 0.99, prove that this linear relationship also meets in a large amount of preparation process, what output was controlled prepares porous flake g-C in enormous quantities
3n
4can be realized by the method.
Fig. 3 is the porous flake g-C prepared in enormous quantities
3n
4scanning electron microscope (SEM) photograph, obvious sheet-like morphology, is of value to the separation of photo-generate electron-hole as we can see from the figure, and centre is mingled with complicated duct, is conducive to the mass transfer in photocatalytic degradation course of reaction, effectively strengthens photocatalysis efficiency.
Embodiment 2
Compound concentration is 2.5 × 10
-5the rhodamine B solution of mol/L, use the porous flake graphite phase carbon nitride of preparation in embodiment 1 (1) and (2) respectively, getting 10mg joins in 60mL degradation product solution, stirring 30min makes target degradation product reach adsorption-desorption balance in photocatalyst surface, and period every 10min sample analysis once.Afterwards, illumination (300W xenon lamp, visible ray, wavelength 420nm< λ <780nm) is carried out to solution, interval 5min sample analysis, observe the change in concentration of target degradation product in solution.
As Fig. 4, the porous flake g-C that preparation in enormous quantities is prepared with small lot can be found out
3n
4photocatalytic activity is more or less the same, and can be decomposed completely by rhodamine B rapidly in 25min.
Rhodamine B shown in Fig. 5 is degraded process medium ultraviolet visible absorption spectra, and can see the carrying out along with photocatalysis experiment, all absworption peaks are all on a declining curve, and final rhodamine B is thoroughly degraded.
Claims (10)
1. preparation in enormous quantities has a porous flake graphite phase carbon nitride method for efficient visible light photocatalytic pollutant degradation activity, it is characterized in that, adds thermal response by raw material is placed in reactor, then through certain process, obtains porous flake g-C
3n
4, the material quantity of its output and input has good linear relationship, and has the activity of efficient Degradation of Organo-pollutants in Water with Photo-catalysis under visible light.
2. the preparation method in enormous quantities of a kind of porous flake graphite phase carbon nitride according to claim 1, is characterized in that, comprise following content:
Raw materials is directly put into a clean reactor, be placed in Muffle furnace and be heated to specified temp with certain heating rate, calcine some hours, then naturally cool.After cool to room temperature, reactor is taken out, obtain g-C
3n
4powder.The powder obtained is scattered in specific solvent with certain proportion, then through ultrasonic process, heats rapid draing under vacuum, obtain desired porous flake g-C
3n
4.
3. Photocatalyst according to claim 1, is characterized in that, comprises the following steps:
Target degradation product is dissolved in the aqueous solution, be mixed with certain density target degradation product solution, the porous flake graphite phase carbon nitride of preparation in step 2 is joined in degradation product solution, stirs, make target degradation product reach adsorption-desorption balance in photocatalyst surface.Afterwards, illumination is carried out to solution, sample analysis in Fixed Time Interval, observe the change in concentration of target degradation product in solution.
4. method according to claim 2, is characterized in that, raw materials used is urea.
5. method according to claim 2, is characterized in that, described reactor is semi-enclosed aluminum or ceramic reactor, and neglecting greatly of reactor adds material quantity and determine, and retains the reaction compartment of 30% ~ 80%.
6. method according to claim 2, is characterized in that, heating ramp rate is 0.5 ~ 4 DEG C/min, and calcining heat is 560 ~ 640 DEG C, and calcination time is 1 ~ 4 hour.
7. method according to claim 2, is characterized in that, dispersion solvent for use is ethanol, water or isopropyl alcohol, g-C
3n
4be 1g:20 ~ 100mL with solvent ratios, sonication treatment time is 10 ~ 100 minutes, and baking temperature is 50 ~ 200 DEG C, and dry vacuum is-0.1 ~-0.5MPa.
8. method according to claim 3, it is characterized in that described target degradation product comprises dyestuff, phenols, concentration is≤10
-2mol/L.
9. method according to claim 3, is characterized in that described absorption mixing time is 10 ~ 100min.
10. method according to claim 3, is characterized in that, described light source is visible ray, simulated solar irradiation, sunshine.
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Application publication date: 20160203 |
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| RJ01 | Rejection of invention patent application after publication |