CN110142055A - Enhance the microwave irradiation method of graphite phase carbon nitride photocatalysis performance - Google Patents
Enhance the microwave irradiation method of graphite phase carbon nitride photocatalysis performance Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 108
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 107
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 65
- 239000010439 graphite Substances 0.000 title claims abstract description 65
- 238000000034 method Methods 0.000 title claims abstract description 29
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 16
- 238000007146 photocatalysis Methods 0.000 title claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 80
- 235000019441 ethanol Nutrition 0.000 claims abstract description 31
- 239000002243 precursor Substances 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 230000002708 enhancing effect Effects 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 230000015556 catabolic process Effects 0.000 claims description 14
- 238000006731 degradation reaction Methods 0.000 claims description 14
- 239000000975 dye Substances 0.000 claims description 14
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 9
- 239000004202 carbamide Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 4
- 229920000877 Melamine resin Polymers 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims 1
- 238000004321 preservation Methods 0.000 claims 1
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 230000005855 radiation Effects 0.000 abstract description 2
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 21
- 229940043267 rhodamine b Drugs 0.000 description 21
- 238000012360 testing method Methods 0.000 description 12
- 238000002835 absorbance Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- 239000010431 corundum Substances 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 239000004575 stone Substances 0.000 description 3
- -1 carbon nitrides Chemical class 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910014033 C-OH Inorganic materials 0.000 description 1
- 229910014570 C—OH Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229910052571 earthenware Inorganic materials 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000003863 metallic catalyst Substances 0.000 description 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen(.) Chemical compound [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/344—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
- B01J37/346—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy of microwave energy
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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Abstract
The invention discloses a kind of microwave irradiation methods for enhancing graphite phase carbon nitride photocatalysis performance, the following steps are included: graphite phase carbon nitride is evenly spread in ethyl alcohol, obtain precursor ethanol mixture, by the precursor ethanol mixture microwave irradiation N minutes in micro-wave oven, obtain modified graphite phase carbon nitride, wherein, N=1~5, the power of microwave irradiation are 800~1000W；The ratio of the quality of the graphite phase carbon nitride and the volume of the ethyl alcohol is 5:(1~4).Microwave irradiation method of the invention can simply, efficiently improve the catalytic efficiency of graphite phase carbon nitride, achieve the effect that fast decoupled organic pollutant under radiation of visible light, and simple process, preparation process are pollution-free, it is significant to the Photocatalytic Performance Study of carbon nitride material.
Description
Technical field
The invention belongs to catalysis material preparation and applied technical fields, and in particular to a kind of enhancing graphite phase carbon nitride light is urged
Change the microwave irradiation method of performance.
Background technique
Modern society, environmental pollution increasingly become a very important problem, especially water pollution, live to people
Cause very big harm.Traditionally many measures, such as emerging inorganic non-metallic are taken in order to handle contaminated water
Catalysis, wherein graphite phase carbon nitride has the advantages that efficient, succinct, there is outstanding pollutant drop under the irradiation of visible light
Solution ability.The stratiform packed structures of graphite phase carbon nitride are similar to graphite, and electronic band structure makes it have outstanding catalysis
Performance, including photocatalysis degradation organic contaminant and photolysis water hydrogen.In order to by the catalytic performance of graphite phase carbon nitride into one
Step improves, and the method being modified to it is also varied, including the common methods such as compound, doped metal ion, also changes including form
The methods of become, be surface-treated.Although graphite phase carbon nitride is inorganic non-metallic catalyst of good performance at this stage, but it is urged
Change the space that efficiency still has promotion.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of enhancing graphite phase carbon nitride photocatalysis performances
Microwave irradiation method, which can simply, efficiently improve the catalytic efficiency of graphite phase carbon nitride.
It is a further object of the present invention to provide a kind of modified graphite phase carbon nitrides.
It is a further object of the present invention to provide a kind of microwave irradiation methods in enhancing graphite phase carbon nitride photocatalysis performance
Application.
The present invention is achieved by the following technical solutions:
A kind of microwave irradiation method enhancing graphite phase carbon nitride photocatalysis performance, comprising the following steps:
Graphite phase carbon nitride is evenly spread in ethyl alcohol, precursor ethanol mixture is obtained, by the precursor ethanol
Mixture obtains modified graphite phase carbon nitride microwave irradiation N minutes in micro-wave oven, wherein N=1~5, microwave
The power of irradiation is 800~1000W；The ratio of the quality of the graphite phase carbon nitride and the volume of the ethyl alcohol is 5:(1~4).
In the above-mentioned technical solutions, the micro-wave oven is household microwave oven.
In the above-mentioned technical solutions, the unit of the quality is g, and the unit of the volume is L.
In the above-mentioned technical solutions, as the N > 1, N minutes of the microwave irradiation is divided into n times interruption and is carried out, often
Microwave irradiation suspends after 1 minute, is further continued for carrying out after the precursor ethanol mixture cools to 20~25 DEG C of room temperature with the furnace
Microwave irradiation, until whole microwave irradiation times reach N minutes.
In the above-mentioned technical solutions, the graphite phase carbon nitride the preparation method comprises the following steps: under air environment, by melamine
Amine, urea, dicyanodiamine or thiocarbamide are warming up to 550~600 DEG C from 20~25 DEG C of room temperature and keep the temperature 2~3 hours, obtain the graphite
Phase carbon nitride, wherein the rate of heating is 2~10 DEG C/min.
The modified graphite phase carbon nitride that above-mentioned microwave irradiation method obtains.
Application of the above-mentioned microwave irradiation method in enhancing graphite phase carbon nitride photocatalysis performance.
Application of the above-mentioned modified graphite phase carbon nitride in shortening the photocatalysis time.
In the above-mentioned technical solutions, by the modified graphite phase carbon nitride be added into dye solution and by visible light into
Row irradiation, degrades after 10min, the surplus ratio of dyestuff is less than 20% in the dye solution；It is described when degradation is to 15min
Dyestuff is degradable.
In the above-mentioned technical solutions, the dyestuff is rhodamine B, the quality and the dye of the modified graphite phase carbon nitride
The ratio for expecting the concentration of solution is 0.1:20, and the unit of the quality is g, and the unit of the concentration is mg/L.
Compared to now possessing technology, microwave irradiation method of the invention can simply, efficiently improve graphite phase carbon nitride
Catalytic efficiency, achieve the effect that fast decoupled organic pollutant under radiation of visible light, and simple process, preparation process are without dirt
Dye, it is significant to the Photocatalytic Performance Study of carbon nitride material.
Detailed description of the invention
Fig. 1 is the XRD diffracting spectrum of graphite phase carbon nitride and modified graphite phase carbon nitride；
Fig. 2 is the FTIR spectrum of graphite phase carbon nitride and modified graphite phase carbon nitride；
Fig. 3 is the BET map of graphite phase carbon nitride and modified graphite phase carbon nitride；
Fig. 4 is the SEM and TEM of graphite phase carbon nitride and modified graphite phase carbon nitride；
Fig. 5 is the light degradation rhodamine B performance map of graphite phase carbon nitride and modified graphite phase carbon nitride.
Specific embodiment
In order to enable those skilled in the art to better understand the present invention/scheme of the invention, it is with reference to the accompanying drawing and specific real
It applies example and further illustrates technical solution of the present invention.
In a specific embodiment of the invention, urea CO (NH2)2It buys from Hengshan Mountain chemical industry, rhodamine B (RhB)
C28H37ClN2O3It buys from Tianjin good fortune morning chemical reagent factory, ethyl alcohol C2H6O is bought from Hengshan Mountain chemical industry, and the purity of mentioned reagent is equal
It is pure to analyze.
Micro-wave oven is household microwave oven, and concrete model is the KD21C, AN (B) of beauty；
The test equipment and model of XRD are as follows: x-ray powder diffraction instrument, RINT Ultima- III, Japanese Rigaku are public
Department；
The test equipment and model of SEM are as follows: scanning electron microscope, S-4800, Japanese Hitachi company；
The test equipment and model of TEM are as follows: high-resolution-ration transmission electric-lens instrument, JEM-6700F, Japanese Hitachi company；
The test equipment and model of FTIR spectrum are as follows: Fourier infrared spectrograph, WQE-410, Bruker company, the U.S.；
The test equipment and model of BET map are as follows: Full-automatic physical chemical adsorption instrument, AUTOSORB-1, U.S. Kang Ta
Company；
The test equipment and model of light degradation rhodamine B performance map are as follows: ultraviolet-uisible spectrophotometer, TU-1901, north
Jing Puxi all purpose instrument Co., Ltd；The test method of light degradation rhodamine B performance map is as follows: configuration concentration 20mg/
The rhodamine B solution of L takes 100ml rhodamine B solution as simulating pollution object, takes sample to be tested (graphite phase carbon nitride and modification
Graphite phase carbon nitride) it 0.1g and is put into simulating pollution object, it carries out shading dark treatment (beaker is wrapped with tinfoil), by magnetic
Power stirs 40min, reach first sampling after adsorption equilibrium it is primary (sampling about 7ml upper solution, at this time 0) irradiation time is set as,
Start to test, i.e., is irradiated (while magnetic agitation) by visible light (>=420nm), illumination 30min terminates, wherein every
5min sampling is primary, and 7 samples (1 time including 6 times in test process and before testing) will be taken to be centrifuged respectively, take upper layer clear
Clear its ultravioletvisible absorption all-wave scanning spectra of liquid testing, data are the absorbance of rhodamine B at 554nm.With testing
In 6 samples taken in journey the absorbance of (remaining) rhodamine B respectively with rhodamine B in 1 samples taken before test
Absorbance (i.e. initial soln) compare, the as surplus ratio of dyestuff.
Rhodamine B or methyl orange can be used in graphite phase carbon nitride and the organic pollutant of modified graphite phase carbon nitride degradation
To simulate.
Embodiment 1
A kind of microwave irradiation method enhancing graphite phase carbon nitride photocatalysis performance, comprising the following steps:
The graphite phase carbon nitride of pale yellow powder shape is evenly spread in ethyl alcohol, precursor ethanol mixture is obtained, it will
Precursor ethanol mixture microwave irradiation 4 minutes in micro-wave oven, obtain modified graphite phase carbon nitride, wherein 4 minutes
Microwave irradiation, which is divided into 4 interruptions, to carry out, and every microwave irradiation suspends after 1 minute, cools to room with the furnace to precursor ethanol mixture
It is further continued for carrying out microwave irradiation after 20~25 DEG C of temperature, until whole microwave irradiation times reach 4 minutes；The power of microwave irradiation is
800W；The quality of graphite phase carbon nitride is 0.5g, and the volume of ethyl alcohol is 200mL.
Wherein, graphite phase carbon nitride the preparation method comprises the following steps: the urea as presoma is fitted into corundum crucible, in air
Under environment, crucible is placed in Muffle furnace, so that urea is warming up to 550 DEG C from 20~25 DEG C of room temperature and keeps the temperature 3 hours, obtain graphite-phase
Carbonitride, wherein the rate of heating is 10 DEG C/min.
Fig. 1 is that the XRD diffracting spectrum of graphite phase carbon nitride and modified graphite phase carbon nitride changes as seen from the figure in embodiment 1
Property graphite phase carbon nitride be carbonitride, wherein MT-g-C3N4For modified graphite phase carbon nitride, g-C3N4For graphite phase carbon nitride.
Fig. 2 is the FTIR spectrum of graphite phase carbon nitride and modified graphite phase carbon nitride in embodiment 1, wherein MT-g-C3N4
For modified graphite phase carbon nitride, g-C3N4For graphite phase carbon nitride.As seen from the figure, the modified graphite phase nitrogen after microwave treatment
The absorbance for changing-OH group of carbon improves, and the graphite phase carbon nitride the adsorbed hydroxyl content after showing microwave treatment increases.
Fig. 3 is the BET map of graphite phase carbon nitride and modified graphite phase carbon nitride in embodiment 1, wherein MT-g-C3N4For
Modified graphite phase carbon nitride, g-C3N4For graphite phase carbon nitride.As seen from the figure, the modified graphite after microwave treatment mutually nitrogenizes
The specific surface area and porosity of carbon is all promoted, and specific surface area is by 66.7m2/ g (graphite phase carbon nitride) is promoted to 72.5m2/g
(modified graphite phase carbon nitride).
Fig. 4 is SEM the and TEM map of graphite phase carbon nitride and modified graphite phase carbon nitride in embodiment 1, wherein Fig. 4
It (a) is the SEM of graphite phase carbon nitride, Fig. 4 (b) is the SEM of modified graphite phase carbon nitride, and Fig. 4 (c) is graphite phase carbon nitride
TEM, Fig. 4 (d) are the TEM of modified graphite phase carbon nitride.As seen from the figure, modified graphite phase carbon nitride lamellar structure become thinner and
It is loose porous.
EDX elemental analysis shows g-C3N4The C/N molar ratio and O content of (C/N=1.40, O=1.40at%) are lower than MT-
g-C3N4(C/N=1.51, O=3.25at%), shows MT-g-C3N4Nitrogen is likely to form in (modified graphite phase carbon nitride) skeleton
Vacancy defect or microwave bombardment may cause C-NH2Conversion of the end group to C-OH group.
Embodiment 2
A kind of microwave irradiation method enhancing graphite phase carbon nitride photocatalysis performance, comprising the following steps:
The graphite phase carbon nitride of pale yellow powder shape is evenly spread in ethyl alcohol, precursor ethanol mixture is obtained, it will
Precursor ethanol mixture microwave irradiation 3 minutes in micro-wave oven, obtain modified graphite phase carbon nitride, wherein 3 minutes
Microwave irradiation, which is divided into 3 interruptions, to carry out, and every microwave irradiation suspends after 1 minute, cools to room with the furnace to precursor ethanol mixture
It is further continued for carrying out microwave irradiation after 20~25 DEG C of temperature, until whole microwave irradiation times reach 3 minutes；The power of microwave irradiation is
800W；The quality of graphite phase carbon nitride is 0.5g, and the volume of ethyl alcohol is 200mL.
Wherein, the preparation method of graphite phase carbon nitride is thermal polycondensation process, specifically: urea is fitted into corundum crucible,
Under air environment, crucible is placed in Muffle furnace, so that urea is warming up to 550 DEG C from 20~25 DEG C of room temperature and keeps the temperature 3 hours, obtain stone
Black phase carbon nitride, wherein the rate of heating is 10 DEG C/min.
Embodiment 3
A kind of microwave irradiation method enhancing graphite phase carbon nitride photocatalysis performance, comprising the following steps:
The graphite phase carbon nitride of pale yellow powder shape is evenly spread in ethyl alcohol, precursor ethanol mixture is obtained, it will
Precursor ethanol mixture microwave irradiation 5 minutes in micro-wave oven, obtain modified graphite phase carbon nitride, wherein 5 minutes
Microwave irradiation, which is divided into 5 interruptions, to carry out, and each microwave irradiation suspends after 1 minute, cools to the furnace to precursor ethanol mixture
It is further continued for carrying out microwave irradiation after 20~25 DEG C of room temperature, until whole microwave irradiation times reach 5 minutes；The power of microwave irradiation
For 800W；The quality of graphite phase carbon nitride is 0.5g, and the volume of ethyl alcohol is 200mL.
Wherein, graphite phase carbon nitride the preparation method comprises the following steps: urea is fitted into corundum crucible, under air environment, by earthenware
Crucible is placed in Muffle furnace, so that urea is warming up to 550 DEG C from 20~25 DEG C of room temperature and is kept the temperature 3 hours, obtains graphite phase carbon nitride,
In, the rate of heating is 10 DEG C/min.
Fig. 5 is the light degradation rhodamine B performance map of graphite phase carbon nitride and modified graphite phase carbon nitride in Examples 1 to 3
(visible light source being replaced with the xenon lamp with 420nm edge filter, organic pollutant is rhodamine B), wherein curve 1 is absorption
Blank control is balanced, i.e., sample made from embodiment 1, not illumination, it was demonstrated that other curve dyestuffs disappear are added in rhodamine B solution
Failure fruit is generated by degradation, and non-adsorbed.Curve 2 is the light degradation rhodamine B performance map of graphite phase carbon nitride, and curve 3 is
The light degradation rhodamine B performance map for the modified graphite phase carbon nitride that embodiment 2 obtains, curve 4 are the modification stone that embodiment 1 obtains
The light degradation rhodamine B performance map of black phase carbon nitride, curve 5 are the light degradation for the modified graphite phase carbon nitride that embodiment 3 obtains
Rhodamine B performance map.As seen from the figure, compared to graphite phase carbon nitride, modified graphite phase carbon nitride the disposal efficiency is obviously improved,
And the disposal efficiency highest of the modified graphite phase carbon nitride by 4 minutes microwave irradiations, using modified stone made from embodiment 1
When black phase carbon nitride degradation 10min, the surplus ratio of dyestuff (rhodamine B) is less than 20% (before starting illumination in solution
The amount of the substance of rhodamine B), when 15min, is degradable.Other embodiments sample, degradable dyestuff at least want 20min, former
Beginning graphite phase carbon nitride is even more to need 30min that could complete to degrade.Microwave irradiation improves the separative efficiency of photo-generated carrier, promotees
The absorption of organic pollutant, respond on into surface.
Illustrative description is done to the present invention/invention above, it should which explanation is not departing from core of the invention
In the case of, any simple deformation, modification or other skilled in the art can not spend being equal for creative work to replace
It changes and each falls within the present invention/invention protection scope.
Claims (10)
1. a kind of microwave irradiation method for enhancing graphite phase carbon nitride photocatalysis performance, which comprises the following steps:
Graphite phase carbon nitride is evenly spread in ethyl alcohol, precursor ethanol mixture is obtained, the precursor ethanol is mixed
Object obtains modified graphite phase carbon nitride microwave irradiation N minutes in micro-wave oven, wherein N=1~5, microwave irradiation
Power be 800~1000W；The ratio of the quality of the graphite phase carbon nitride and the volume of the ethyl alcohol is 5:(1~4).
2. microwave irradiation method according to claim 1, which is characterized in that the preparation method of the graphite phase carbon nitride
Are as follows: under air environment, melamine, urea, dicyanodiamine or thiocarbamide are warming up to 550~600 DEG C from 20~25 DEG C of room temperature
Heat preservation 2~3 hours, obtains the graphite phase carbon nitride, wherein the rate of heating is 2~10 DEG C/min.
3. microwave irradiation method according to claim 2, which is characterized in that micro- by described N minutes as the N > 1
Amplitude is carried out according to n times interruption is divided into, and every microwave irradiation suspends after 1 minute, cools to the furnace to the precursor ethanol mixture
It is further continued for carrying out microwave irradiation after 20~25 DEG C of room temperature, until whole microwave irradiation times reach N minutes.
4. microwave irradiation method according to claim 3, which is characterized in that the unit of the quality is g, the volume
Unit is L.
5. microwave irradiation method according to claim 4, which is characterized in that the micro-wave oven is household microwave oven.
6. the modified graphite phase carbon nitride that microwave irradiation method as claimed in claim 1 or 2 obtains.
7. modified graphite phase carbon nitride according to claim 6, which is characterized in that as the N > 1, by described N minutes
Microwave irradiation, which is divided into n times interruption, to carry out, and every microwave irradiation suspends after 1 minute, to the precursor ethanol mixture furnace cooling
It is further continued for carrying out microwave irradiation after to 20~25 DEG C of room temperature, until whole microwave irradiation times reach N minutes.
8. modified graphite phase carbon nitride according to claim 7, which is characterized in that the suction of the modified graphite phase carbon nitride
The mean values of attached rate are 72.5m2/g。
9. microwave irradiation method is in enhancing graphite phase carbon nitride photocatalysis performance as described in any one of Claims 1 to 5
Application.
10. application as claimed in claim 9, which is characterized in that being added the modified graphite phase carbon nitride to dye solution
In and be irradiated by visible light, degrade after 10min, the surplus ratio of dyestuff is less than 20% in the dye solution；Work as degradation
When to 15min, the dyestuff is degradable.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810142188.1A CN110142055B (en) | 2018-02-11 | 2018-02-11 | Microwave irradiation method for enhancing photocatalytic performance of graphite-phase carbon nitride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810142188.1A CN110142055B (en) | 2018-02-11 | 2018-02-11 | Microwave irradiation method for enhancing photocatalytic performance of graphite-phase carbon nitride |
Publications (2)
| Publication Number | Publication Date |
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