CN109107599A - A kind of 3D Gr/g-C3N4Composite material, preparation method and application - Google Patents
A kind of 3D Gr/g-C3N4Composite material, preparation method and application Download PDFInfo
- Publication number
- CN109107599A CN109107599A CN201811105799.5A CN201811105799A CN109107599A CN 109107599 A CN109107599 A CN 109107599A CN 201811105799 A CN201811105799 A CN 201811105799A CN 109107599 A CN109107599 A CN 109107599A
- Authority
- CN
- China
- Prior art keywords
- composite material
- preparation
- urea
- dry
- quartz ampoule
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000463 material Substances 0.000 title abstract description 11
- 239000002131 composite material Substances 0.000 claims abstract description 35
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims abstract description 21
- 230000001699 photocatalysis Effects 0.000 claims abstract description 17
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000004202 carbamide Substances 0.000 claims abstract description 14
- 239000002091 nanocage Substances 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 239000003708 ampul Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 14
- 239000010453 quartz Substances 0.000 claims description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 238000010531 catalytic reduction reaction Methods 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 6
- 239000007924 injection Substances 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 3
- 239000001095 magnesium carbonate Substances 0.000 claims description 3
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 239000004575 stone Substances 0.000 claims 1
- 230000009467 reduction Effects 0.000 abstract description 10
- 238000007146 photocatalysis Methods 0.000 abstract description 7
- 150000001875 compounds Chemical class 0.000 abstract description 4
- 238000002474 experimental method Methods 0.000 abstract description 3
- 208000007578 phototoxic dermatitis Diseases 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 abstract 1
- 238000011065 in-situ storage Methods 0.000 abstract 1
- 238000006068 polycondensation reaction Methods 0.000 abstract 1
- 238000010189 synthetic method Methods 0.000 abstract 1
- 238000006722 reduction reaction Methods 0.000 description 9
- 238000012986 modification Methods 0.000 description 7
- 230000004048 modification Effects 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 229910052770 Uranium Inorganic materials 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000005286 illumination Methods 0.000 description 5
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 5
- 238000002835 absorbance Methods 0.000 description 4
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 239000000356 contaminant Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 230000005622 photoelectricity Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 1
- 206010067125 Liver injury Diseases 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000005802 health problem Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 231100000234 hepatic damage Toxicity 0.000 description 1
- 230000008818 liver damage Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000011824 nuclear material Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- -1 s-triazine heterocyclic compound Chemical class 0.000 description 1
- 231100000241 scar Toxicity 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000010891 toxic waste Substances 0.000 description 1
- 239000002023 wood Substances 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
Classifications
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
- G21F9/06—Processing
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- General Engineering & Computer Science (AREA)
- High Energy & Nuclear Physics (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of 3D Gr/g-C3N4The preparation method of composite material, comprising the following steps: using benzene as predecessor, using MgO template in situ, so that product, in the surface MgO homoepitaxial, tiling is grown in the surface MgO, obtains nano cages；It is ultrasonically treated using urea as predecessor dispersion liquid with nano cages, 3D Gr/g-C is obtained by thermal polycondensation synthetic method3N4Composite material.The present invention also provides a kind of 3D Gr/g-C3N4The application of composite material.The present invention introduces 3D Gr by simple experiment, and by 3D Gr and g-C3N4It carries out compound, the transport efficiency of photogenerated charge is effectively improved by 3D Gr three-dimensional hollow structure, specific surface area 3D Gr big simultaneously improves the collection photosensitiveness and inside coordinability of material, further enhances the photocatalytic activity of material, and then can high efficiency photocatalysis reduction removal UO2 2+。
Description
Technical field
The invention belongs to technical field of chemical material preparation, and in particular to a kind of 3D Gr/g-C3N4Composite material, preparation side
Method and its application.
Background technique
With the fast development of nuclear industry, from the exploitation of uranium ore, the harm for the nuke rubbish that grinding and processing release is
It has been to be concerned by more and more people.Research has shown that Long Term Contact uranium will lead to serious health problem, such as serious liver damage
Wound, renal damage are even dead.Therefore, uranium pollution solution nuclear material resource gentle for protection environment is eliminated to be of great significance.
It is well known that uranium species are such as U (0), U (III), U (IV) and U (VI) with existing for several chemical states, wherein in ring
Main chemical state is soluble U (VI) and sl. sol. U (IV) in border.Thus, soluble U (VI) is reduced into insoluble U
It (IV) is a kind of one of important method removal reflection contact scar and reuse uranium resource.But most of restoring method are all
It is very expensive, and it is related to the chemicals of high consumption, also generate toxic waste.
Photocatalysis technology is a kind of directly using the method for solar energy degradation environmental contaminants, at present in photo catalytic reduction depth
In-depth study has been obtained in terms of degree removal heavy metal contaminants, in efficient utilization, storage and the conversion solar energy energy
While, with easy to operate, reaction condition is mild, reaction speed is fast, does not have selectivity to organic pollutant, without secondary dirt
Dye, the advantages such as processing cost is low, have broad application prospects repairing ecological environment field.However, photocatalysis technology develops
Up to the present problems are encountered, such as low visible absorption efficiency, low quantum efficiency and low chemical stability.
In view of the above problems, on the one hand, it would be desirable to expand photochemical catalyst to the absorption bands of sunlight, exploitation is even red to visible light
The stabilization photocatalytic system of outer photoresponse is particularly important；On the other hand, in photocatalytic system, the separation of charge and light
The migration of raw carrier is Fast synchronization progress, but due to the loss of heat, photocatalyst surface defect and some external worlds
Factor will lead to low photo-generated carrier transport efficiency and photo-generate electron-hole to compound again, this is to cause quantum efficiency low
Standard want reason, therefore, photochemical catalyst is selected suitable method of modifying to improve the transport efficiency of light induced electron and reduces light
The recombination rate of raw electron-hole pair is to improve the research key point of photocatalysis quantum efficiency.
Class graphite type carbon nitride (g-C3N4) it is used as a kind of nonmetallic organic polymer semiconductor material, the relatively narrow (Eg of band gap
=2.70eV), to visible light-responded, pure g-C3N4About in -1.23V, this compares UO for the position of conduction band2 2+/U4+(0.267V)、UO2 2 +/UO2(0.411V) and U4O9/UO2The reduction potential of (0.267V) is negative, therefore g-C3N4It can be used as visible-light photocatalyst light
Catalysis reduction UO2 2+, while g-C3N4Chemical stability with higher, low cost, nontoxic, easy modification and there is higher photocatalysis
The advantages that performance, is now widely used in the research work in terms of photocatalysis degradation organic contaminant, but g-C3N4In the presence of
It can be seen that the problems such as light utilization efficiency is low, specific surface area is small, quantum efficiency is low, hinders its development.Therefore, to g-C3N4It is appropriate to carry out
Modification seem outstanding with the transport efficiency for improving the visible light activity of photochemical catalyst, visible light-responded range and photo-generated carrier
It is important.
Summary of the invention
The purpose of the present invention is intended to overcome the shortcomings of existing methods place, provides a kind of 3D Gr/g-C3N4Composite material,
Preparation method and applications.
The first purpose of the invention is to provide a kind of 3D Gr/g-C3N4The preparation method of composite material, specifically include with
Lower step:
Step 1, basic magnesium carbonate is laid in sealable quartz ampoule, then quartz ampoule is placed in tube furnace, then
N is passed through with the flow of 200L/h after quartz ampoule is vacuumized2To normal pressure, repetition vacuumizes and is passed through N2To operation 3 times of normal pressure,
Continue to be passed through N into quartz ampoule with the flow of 200L/h later2；
Step 2, tube furnace is warming up to 800 DEG C according to the heating rate of 10 DEG C/min, then at 800 DEG C, with 1mL/
The speed of 30min benzene injection predecessor into boiler tube, after continuous injection 30min, the N that will be continually fed into quartz ampoule2Flow tune
To 600L/h, it is simultaneously stopped syringe pump benzene predecessor, and stops heating, until tubular type in-furnace temperature stops after being down to 100 DEG C or less
Only it is passed through N2, obtain nano cages；
Nano cages are flowed back in hydrochloric acid solution and rinse 12h, are then washed to neutrality, re-dry obtains 3D Gr；
Step 3, urea is dissolved in deionized water, obtains urea liquid；Wherein, the ratio of the urea and deionized water
Example is 2g:15ml；
3D Gr obtained in step 2 is added in the urea liquid, 20min, ultrasonic disperse after stirring are stirred
30min, dry 5h, obtains drying sample after dry at 80 DEG C；Wherein, the mass ratio of the 3D Gr and urea is
1:2000；
Drying sample is placed in Muffle furnace, is kept the temperature after Muffle furnace is then risen to 540 DEG C with the heating rate of 5 DEG C/min
2h is down to room temperature naturally to get the 3D Gr/g-C powdered to light gray after heat preservation3N4Composite material.
Preferably, the concentration of hydrochloric acid solution is 6mol/L in the step 2.
Preferably, step 2 drying temperature is 60 DEG C, drying time 12h.
Preferably, ultrasonic power is 120W in the step 3.
A second object of the present invention is to provide a kind of 3D Gr/g-C3N4Composite material.
Third object of the present invention is to provide a kind of above-mentioned 3D Gr/g-C3N4Composite material is removed in photo catalytic reduction
UO2 2+In application.
Compared with the conventional method, the beneficial effects of the present invention are:
The present invention introduces three-dimensional carbon material (3D Gr) by green, easy experimental method, and by 3D Gr and g-C3N4Into
Row is compound, and the transport efficiency of photogenerated charge, while the ratio table that 3D Gr is big are effectively improved by the three-dimensional hollow structure of 3D Gr
Area improves the collection photosensitiveness and inside coordinability of material, further enhances the photocatalytic activity of material, and then can
Enough high efficiency photocatalysis reduction removal UO2 2+。
Detailed description of the invention
Fig. 1 is the 3D Gr/g-C that embodiment 1 is prepared3N4The scanning electron microscope (SEM) photograph of composite material, that CN is represented in figure is g-
C3N4；
Fig. 2 is the 3D Gr/g-C that embodiment 1 is prepared3N4The X-ray diffractogram of composite material；
Fig. 3 is the 3D Gr/g-C that embodiment 1 is prepared3N4The Raman spectrogram of composite material, that CN is represented in figure is g-
C3N4, that CN/3D Gr is represented is 3D Gr/g-C3N4；
Fig. 4 is the 3D Gr/g-C that embodiment 1 is prepared3N4The photoelectricity flow graph of composite material, that CN is represented in figure is g-
C3N4, that CN/3D Gr is represented is 3D Gr/g-C3N4；
Fig. 5 is 3D Gr/g-C in embodiment 23N4The photo catalytic reduction UO of composite material2 2+Effect picture, CN is represented in figure
It is g-C3N4, that CN/3D Gr is represented is 3D Gr/g-C3N4。
Specific embodiment
Methods of this invention will be better understood in order to enable art processes personnel, and scheme is practiced, below with reference to specific
The invention will be further described for embodiment and attached drawing, but illustrated embodiment is not as a limitation of the invention.
Experimental method and detection method described in following each embodiments are unless otherwise specified conventional method；The examination
Agent and material can be commercially available on the market unless otherwise specified.
Embodiment 1
A kind of 3D Gr/g-C3N4The preparation method of composite material, specifically includes the following steps:
Step 1,2g basic magnesium carbonate is laid in sealable quartz ampoule, then quartz ampoule is placed in tube furnace, so
N is passed through with the flow of 200L/h after quartz ampoule is vacuumized afterwards2To normal pressure, repetition vacuumizes and is passed through N2To the operation 3 of normal pressure
It is secondary, continue to be passed through N into quartz ampoule with the flow of 200L/h later2；
Step 2, start tube furnace, tube furnace is warming up to 800 DEG C according to the heating rate of 10 DEG C/min, then open note
Penetrate pump, at 800 DEG C, with the speed of 1mL/30min into boiler tube benzene injection predecessor, after continuous injection 30min, will persistently lead to
Enter the N in quartz ampoule2Flow is adjusted to 600L/h, is simultaneously stopped syringe pump benzene predecessor, and stop heating, until temperature in tube furnace
Degree stops being passed through N after being down to 100 DEG C or less2, obtain nano cages；
Nano cages are flowed back in the hydrochloric acid of 6mol/L and rinse 12h, neutrality is then washed to, places into baking oven in 80
It is taken out after DEG C dry 12h, obtains 3D Gr；
Step 3,2g urea is dissolved in 15ml deionized water, obtains urea liquid；
3D Gr obtained in 1mg step 1 is added in above-mentioned urea liquid, 20min is stirred, it is ultrasonic after stirring
Disperse 30min, then be placed in 80 DEG C of baking ovens dry 5h, obtains drying sample after dry；
Dry sample is placed in crucible, then crucible is placed in Muffle furnace, then by Muffle furnace with the heating of 5 DEG C/min
Rate keeps the temperature 2h after rising to 540 DEG C, room temperature is down to after heat preservation naturally to get the 3D Gr/g-C powdered to light gray3N4
Composite material.
The 3D Gr/g-C that embodiment 1 is prepared3N4The performance of composite material is detected, specific as shown in Figs 1-4,
In, Fig. 1 is the 3D Gr/g-C that embodiment 1 is prepared3N4The scanning electron microscope (SEM) photograph of composite material, that CN is represented in figure is g-C3N4,
The 3D Gr structure of caged and the g-C of stratiform as seen from Figure 13N4Structure, and 3D Gr and g-C3N4Between combine closely,
Intuitively reflect the feasibility of material preparation；
Fig. 2 is the 3D Gr/g-C that embodiment 1 is prepared3N4The X-ray diffractogram of composite material, as seen from Figure 2 3D
The X-ray diffractogram of Gr only has the broad peak near 26 °, this belongs to (002) crystal face of graphene, and in g-C3N4X-ray spread out
It penetrates in figure and shows as 13.1 ° and 27.5 ° of two characteristic peaks, respectively correspond g-C3N4(100) s-triazine heterocyclic compound in the layer of crystal face
The pi-conjugated system of object and g-C3N4(002) the Regularia graphite layers accumulation of crystal face, and 3D Gr/g-C3N4Composite material
(002) reduction has had occurred centainly in crystallographic plane diffraction peak intensity, this may be since the addition of 3D Gr results in g-C3N4It is endless
Full polymerization, while also further illustrating the successful preparation of sample；
Fig. 3 is the 3D Gr/g-C that embodiment 1 is prepared3N4The Raman spectrogram of composite material, that CN is represented in figure is g-
C3N4, that CN/3D Gr is represented is 3D Gr/g-C3N4, Raman spectrum is commonly used for characterizing carbon material graphitic carbon (peak G) and defect
The relative amount at (peak D), from figure 3, it can be seen that 3D Gr/g-C3N4Composite material is relative to g-C3N4There is apparent graphitic carbon
Peak and defect peak, it was demonstrated that 3D Gr and g-C3N4It has carried out successful compound；
Fig. 4 is the 3D Gr/g-C that embodiment 1 is prepared3N4The photoelectricity flow graph of composite material, that CN is represented in figure is g-
C3N4, that CN/3D Gr is represented is 3D Gr/g-C3N4, can see in Fig. 4 photoelectric current characterization, 3D Gr/g-C3N4Composite wood
Material is relative to g-C3N4There is higher photo-current intensity, it was demonstrated that in During Illumination, 3D Gr/g-C3N4Composite inner
There is more efficient electron transfer efficiency, this is conducive to the progress of light reaction system.
Embodiment 2
The 3D Gr/g-C that 50mg embodiment 1 is prepared3N4Composite material is added to 50mL UO2 2+In (10ppm) solution,
5ml methanol is added, then magnetic agitation 2h obtains reduction system to reach absorption-desorption balance under no light condition；
Use the xenon lamp of 350W as light source, filtering off ultraviolet light with wavelength X >=400nm optical filter will restore before irradiation
Reaction system nitrogen is bubbled 60min and removes oxygen, to ensure that reaction system is in oxygen free condition；Every illumination 10min is used
Arsenazo III spectrophotometry analyzes UO by UVmini-1240 under the absorbing wavelength of 650nm2 2+Absorbance, illumination
Total time is 100min.
UO is converted by the absorbance intensity of different irradiation times2 2+Reduction rate, calculated with following formula: UO2 2+Reduction
Rate: C/C0=(A0-At)/A0× 100%, wherein A0And AtIt respectively represents when the time is 0 (after unglazed absorption) and the time is t
UO2 2+Absorbance.
Effect in order to further illustrate the present invention also utilizes g-C in experimentation3N4, CdS/rGO (cadmium sulfide/oxidation
Graphene) absorbance intensity under the conditions of same illumination is converted into UO2 2+Reduction rate as a comparison；After illumination 100min,
g-C3N4、CdS/rGO、3D Gr/g-C3N4To UO2 2+Reduction rate be respectively 32.2%, 82.7% and 90.2%, be specifically shown in figure
5, Fig. 5 be 3D Gr/g-C in embodiment 23N4The photo catalytic reduction UO of composite material2 2+Effect picture, that CN is represented in figure is g-
C3N4, that CN/3D Gr is represented is 3D Gr/g-C3N4, in contrast to g-C3N and CdS/rGO, 3D Gr/g-C3N4Composite material exhibits
Best photo catalytic reduction UO out2 2+Performance.
It should be noted that the present invention describes preferred embodiment, but method personnel in the art once know
Basic creative concept, then additional changes and modifications may be made to these embodiments.So appended claims are intended to explain
Being includes preferred embodiment and all change and modification for falling into the scope of the invention.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by the method personnel of this field
Mind and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent processes
Within be also intended to include these modifications and variations.
Claims (6)
1. a kind of 3D Gr/g-C3N4The preparation method of composite material, which is characterized in that specifically includes the following steps:
Step 1, basic magnesium carbonate is laid in sealable quartz ampoule, then quartz ampoule is placed in tube furnace, then by stone
English pipe with the flow of 200L/h is passed through N after vacuumizing2To normal pressure, repetition vacuumizes and is passed through N2To operation 3 times of normal pressure, later
Continue to be passed through N into quartz ampoule with the flow of 200L/h2；
Step 2, tube furnace is warming up to 800 DEG C according to the heating rate of 10 DEG C/min, then at 800 DEG C, with 1mL/30min
Speed into boiler tube benzene injection predecessor, after continuous injection 30min, the N that will be continually fed into quartz ampoule2Flow is adjusted to
600L/h is simultaneously stopped syringe pump benzene predecessor, and stops heating, until tubular type in-furnace temperature stops after being down to 100 DEG C or less
It is passed through N2, obtain nano cages；
Nano cages are flowed back in hydrochloric acid solution and rinse 12h, are then washed to neutrality, re-dry obtains 3D Gr；
Step 3, urea is dissolved in deionized water, obtains urea liquid；Wherein, the ratio of the urea and deionized water is
2g:15ml；
3D Gr obtained in step 2 is added in the urea liquid, 20min, ultrasonic disperse 30min after stirring are stirred,
Dry 5h, obtains drying sample after dry at 80 DEG C；Wherein, the mass ratio of the 3D Gr and urea is 1:2000；
Drying sample is placed in Muffle furnace, keeps the temperature 2h after Muffle furnace is then risen to 540 DEG C with the heating rate of 5 DEG C/min,
Naturally room temperature is down to after heat preservation to get the 3D Gr/g-C powdered to light gray3N4Composite material.
2. 3D Gr/g-C according to claim 13N4The preparation method of composite material, which is characterized in that in the step 2
The concentration of hydrochloric acid solution is 6mol/L.
3. 3D Gr/g-C according to claim 13N4The preparation method of composite material, which is characterized in that the step 2 is dry
Dry temperature is 60 DEG C, drying time 12h.
4. 3D Gr/g-C according to claim 13N4The preparation method of composite material, which is characterized in that in the step 3
Ultrasonic power is 120W.
5. the 3D Gr/g-C that one kind is prepared method according to claim 13N4Composite material.
6. the 3D Gr/g-C that one kind is prepared method according to claim 13N4Composite material removes UO in photo catalytic reduction2 2 +In application.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811105799.5A CN109107599A (en) | 2018-09-21 | 2018-09-21 | A kind of 3D Gr/g-C3N4Composite material, preparation method and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811105799.5A CN109107599A (en) | 2018-09-21 | 2018-09-21 | A kind of 3D Gr/g-C3N4Composite material, preparation method and application |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109107599A true CN109107599A (en) | 2019-01-01 |
Family
ID=64856097
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811105799.5A Pending CN109107599A (en) | 2018-09-21 | 2018-09-21 | A kind of 3D Gr/g-C3N4Composite material, preparation method and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109107599A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110479344A (en) * | 2019-08-26 | 2019-11-22 | 河海大学 | A kind of g-C3N4/ CNCs composite photocatalyst material and preparation method thereof |
| CN111018041A (en) * | 2019-12-19 | 2020-04-17 | 南华大学 | Preparation method and application of polypyrrole graphite phase carbon nitride composite material for treating uranium-containing wastewater through photocatalytic reduction |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101284663A (en) * | 2008-04-14 | 2008-10-15 | 南京大学 | Method for mass preparing hollow nano cages in high quality |
| CN106040213A (en) * | 2016-05-26 | 2016-10-26 | 河海大学 | TiO2/CNCs composite photocatalyst and preparation method and application thereof |
| CN106634102A (en) * | 2016-12-29 | 2017-05-10 | 佛山市高明绿化纳新材料有限公司 | Graphite phase carbon nitride/graphene oxide heterojunction-epoxy acrylate composite material as well as preparation method and application thereof |
| CN107537544A (en) * | 2017-09-19 | 2018-01-05 | 江苏理工学院 | A kind of g C3N4- CNTs heterojunction photocatalysts and preparation method thereof |
-
2018
- 2018-09-21 CN CN201811105799.5A patent/CN109107599A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101284663A (en) * | 2008-04-14 | 2008-10-15 | 南京大学 | Method for mass preparing hollow nano cages in high quality |
| CN106040213A (en) * | 2016-05-26 | 2016-10-26 | 河海大学 | TiO2/CNCs composite photocatalyst and preparation method and application thereof |
| CN106634102A (en) * | 2016-12-29 | 2017-05-10 | 佛山市高明绿化纳新材料有限公司 | Graphite phase carbon nitride/graphene oxide heterojunction-epoxy acrylate composite material as well as preparation method and application thereof |
| CN107537544A (en) * | 2017-09-19 | 2018-01-05 | 江苏理工学院 | A kind of g C3N4- CNTs heterojunction photocatalysts and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 尹竞等: ""g-C3N4/石墨烯复合材料的制备及光催化活性的研究"", 《中国环境科技》 * |
| 陈荣跃等: ""光催化还原去除六价铀污染非金属光催化材料制备与性能研究"", 《中国优秀硕士学位论文全文数据库工程科技I辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110479344A (en) * | 2019-08-26 | 2019-11-22 | 河海大学 | A kind of g-C3N4/ CNCs composite photocatalyst material and preparation method thereof |
| CN111018041A (en) * | 2019-12-19 | 2020-04-17 | 南华大学 | Preparation method and application of polypyrrole graphite phase carbon nitride composite material for treating uranium-containing wastewater through photocatalytic reduction |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110038607B (en) | Titanium carbide nanosheet/layered indium sulfide heterojunction and application thereof in degradation and removal of water pollutants | |
| CN109603880B (en) | Hollow tubular carbon nitride photocatalyst and preparation method and application thereof | |
| CN103736513B (en) | A kind of TiO 2(B) g-C 3n 4the preparation method of composite nano plate photochemical catalyst | |
| CN107088434B (en) | A kind of g-C3N4-Cu2The preparation method and applications of O catalyst | |
| CN105032468A (en) | Cu2O-TiO2/g-C3N4 ternary complex and preparation and application method thereof | |
| CN103191766A (en) | CdS/g-C3N4 composite visible light catalyst, preparation method and application | |
| CN104014291B (en) | A kind of fluorescence disk reactor applying Ag/BiOBr visible light catalytic film | |
| CN103191725B (en) | BiVO4/Bi2WO6 composite semiconductor material as well as hydrothermal preparation method and application thereof | |
| CN107570174A (en) | A kind of preparation method and application of efficient stable nickel foam base optic catalytic material | |
| CN103990485A (en) | Carbon nitride nano particle modified pucherite composite photocatalyst and preparation method thereof | |
| CN110841670B (en) | Zero-dimensional black phosphorus quantum dot/one-dimensional tubular carbon nitride composite photocatalyst and preparation method thereof | |
| CN109967074A (en) | A kind of preparation method and application of the titanium dioxide optical catalyst of silver load | |
| CN106622293B (en) | A kind of H-TiO2/CdS/Cu2-xThe preparation method of S nanobelt | |
| CN106563477A (en) | Ternary composite visible light photocatalyst, preparation method and application thereof | |
| CN109107599A (en) | A kind of 3D Gr/g-C3N4Composite material, preparation method and application | |
| CN106944074A (en) | A kind of visible-light response type composite photo-catalyst and its preparation method and application | |
| CN108043429A (en) | A kind of preparation method of composite nano Tb/BiOCl materials | |
| CN109665560A (en) | A kind of carbon, BiOCl of full spectral absorption of N doping and its preparation method and application | |
| CN108479749A (en) | A kind of synthetic method of metal ion mixing vanadate nanocatalyst | |
| CN114849752A (en) | Hexagonal boron nitride/flower ring-shaped graphite type carbon nitride heterojunction composite photocatalyst and preparation method and application thereof | |
| CN113289669B (en) | Preparation method of beaded carbon nanofiber loaded titanium oxide photocatalyst | |
| CN106000370A (en) | Preparation method of photoinduced Ti<3+> self-doped TiO2 photocatalyst | |
| CN103506104B (en) | Carbon-doped TiO2 visible light-responding catalytic film on glass carrier and preparation method thereof | |
| CN106076422B (en) | A kind of sepiolite supported porphyrin sensitization Bi2WO6The preparation method of visible light catalyst | |
| CN102380368A (en) | Bi2MoO6:Ln<3+> catalyst and its preparation method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190101 |
|
| RJ01 | Rejection of invention patent application after publication |