CN108671956A - A kind of preparation method of ion filled graphite phase carbon nitride nanometer sheet - Google Patents
A kind of preparation method of ion filled graphite phase carbon nitride nanometer sheet Download PDFInfo
- Publication number
- CN108671956A CN108671956A CN201810550204.0A CN201810550204A CN108671956A CN 108671956 A CN108671956 A CN 108671956A CN 201810550204 A CN201810550204 A CN 201810550204A CN 108671956 A CN108671956 A CN 108671956A
- Authority
- CN
- China
- Prior art keywords
- nanometer sheet
- preparation
- carbon nitride
- phase carbon
- graphite phase
- 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.)
- Granted
Links
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 15
- 239000010439 graphite Substances 0.000 title claims abstract description 15
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 25
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 13
- 238000001354 calcination Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000007789 sealing Methods 0.000 claims abstract description 4
- 239000006185 dispersion Substances 0.000 claims abstract description 3
- 150000002500 ions Chemical class 0.000 claims description 32
- 239000000843 powder Substances 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 11
- 239000007787 solid Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 229920000877 Melamine resin Polymers 0.000 claims description 3
- 238000005352 clarification Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 239000008236 heating water Substances 0.000 claims description 3
- 238000013021 overheating Methods 0.000 claims description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- 238000013019 agitation Methods 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical group NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 12
- 238000000034 method Methods 0.000 abstract description 9
- 238000011049 filling Methods 0.000 abstract description 4
- 230000001681 protective effect Effects 0.000 abstract description 3
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000007539 photo-oxidation reaction Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 abstract 1
- 238000012805 post-processing Methods 0.000 abstract 1
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 51
- 230000000694 effects Effects 0.000 description 10
- 238000007146 photocatalysis Methods 0.000 description 9
- 230000003197 catalytic effect Effects 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 8
- 230000003647 oxidation Effects 0.000 description 8
- 238000007254 oxidation reaction Methods 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 6
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- LZDSILRDTDCIQT-UHFFFAOYSA-N dinitrogen trioxide Chemical compound [O-][N+](=O)N=O LZDSILRDTDCIQT-UHFFFAOYSA-N 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 238000004868 gas analysis Methods 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 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
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 1
- 206010014561 Emphysema Diseases 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 208000007443 Neurasthenia Diseases 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 206010033799 Paralysis Diseases 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 206010003549 asthenia Diseases 0.000 description 1
- 206010006451 bronchitis Diseases 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000008040 ionic compounds Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 150000007974 melamines Chemical class 0.000 description 1
- 229920005588 metal-containing polymer Polymers 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- RJIWZDNTCBHXAL-UHFFFAOYSA-N nitroxoline Chemical compound C1=CN=C2C(O)=CC=C([N+]([O-])=O)C2=C1 RJIWZDNTCBHXAL-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000012956 testing procedure Methods 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
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Biomedical Technology (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Catalysts (AREA)
Abstract
The present invention provides a kind of preparation method of ion filled graphite phase carbon nitride nanometer sheet, which is broadly divided into three steps：(1) preparation of predecessor is calcined, including the dissolving dispersion of nitrogen source, nitrogen source are combined the drying for generating predecessor and predecessor with hydrogen chloride；(2) the sealing calcining of predecessor；(3) post-processing of calcined product.The preparation method have many advantages, such as raw material it is cheap and easy to get, it is simple for process, environmentally protective, be easy to industrialized production.The ion filling g C prepared by the method for the invention3N4Nanometer sheet, compared to common g C3N4Energy bandgaps are lower, and photogenerated charge significantly improves separative efficiency, show preferable photooxidation removal NO performances under visible light, and by being used for multiple times, can still keep original photocatalytic activity, have extraordinary stability.
Description
Technical field
The invention belongs to photocatalysis nano materials to prepare and environmental contaminants processing technology field, and in particular to a kind of ion
Filled graphite phase carbon nitride (g-C3N4) nanometer sheet preparation method and application.
Background technology
Nitrogen oxides (NOx) it is nitrogen and the general name of compound that oxygen element is formed, including nitric oxide (NO), two
Nitrogen oxide (NO2), nitrogen trioxide (N2O3) etc. variforms, be one of the major pollutants in air.Human activity discharge
NOxIn, NO accounts for 90% or more.NOxIt can cause many body illnesses such as bronchitis, pulmonary emphysema, neurasthenia and paralysis, can also
Cause the environmental pollutions such as acid rain, photochemical fog, depletion of the ozone layer, greenhouse effects, city haze.According to Environment Protect in China portion
The data of announcement, the in recent years NO in ChinaxDischarge capacity increases year by year, the problem of thus bringing getting worse, this is also to NOxPurification
More stringent requirements are proposed for the development of technology.
Photocatalitic Technique of Semiconductor is a kind of emerging Green Chemical Technology of fast development in recent years, it can utilize the sun
Free radical and the hole of high activity can be generated come the pollutant in environment of degrading, achieve the purpose that repairing environment pollutes.With tradition
Environmental pollution recovery technique compare, photocatalysis technology it is adaptable it is strong, reaction condition is mild, reaction product is nontoxic secondary makees
The advantages that with, energy conservation and environmental protection.The core of photocatalysis technology is that preparing the high light of of low cost, function admirable, stability urges
Agent.
2009, Wang Xinchen et al. reported a kind of no metal-containing polymer photochemical catalyst graphite phase carbon nitride (g- for the first time
C3N4).They have found g-C3N4Under the irradiation of visible light hydrogen and oxygen can be generated by decomposing water.Since then, g-
C3N4Because its excellent chemical stability, low cost, it is nontoxic, preparation process is simple the features such as rapidly become in photocatalysis field most
Popular one of research topic.However, common g-C3N4There is itself specific surface areas smaller, photogenerated charge is to easily compound etc.
Disadvantage causes its photocatalytic activity relatively low.By g-C3N4It is designed to that two-dimensional nano chip architecture is overcome above two defect effective
Method.g-C3N4The specific surface area of nanometer sheet is than block-like common g-C3N4It is much bigger, and nanometer chip architecture can significantly contract
Short photogenerated charge is to the migration distance from ontology to surface, to inhibit photogenerated charge a large amount of compound in the body.Therefore,
Pattern variation from bulk to nanometer sheet can significantly improve g-C3N4Photocatalytic activity.Even so, g-C3N4Nanometer sheet is still
So there are some inherent shortcomings, such as the increase of energy bandgaps and the surface recombination of photogenerated charge pair.Due to nanometer chip architecture
Quantum limitation effect leads to g-C3N4Nanometer sheet energy bandgaps increase, and adverse effect is produced in terms of spectral response and light excitation,
And the surface recombination of photogenerated charge pair can limit the availability of follow-up light-catalyzed reaction.Due to both intrinsic defects, g-C3N4
Practical application of the nanometer sheet in solar energy conversion is very limited.Therefore, it is necessary to develop the graphite that a kind of photocatalytic activity is stablized
Phase carbon nitride.
Invention content
In view of the problems of the existing technology, the present invention is the technical solution for solving problems of the prior art and using
It is as follows：
A kind of preparation method of ion filled graphite phase carbon nitride nanometer sheet, which is characterized in that include the following steps：
The solid powder for analyzing purity nitrogen source is added in the deionized water of 80 DEG C of heating water baths by step 1, while magnetic force stirs
Acceleration dissolving is mixed, is to stop heating and stirring, and natural cooling after nitrogen source is completely dissolved dispersion after solution clarification；
Step 2, when the clear solution that step 1 obtains is cooled to and begins with white crystal and be precipitated, open stirring and to molten
Concentrated hydrochloric acid is slowly added in liquid dropwise, obtains mixed solution；
It is dry to be then transferred to 120 DEG C of air blast by step 3, the 80 DEG C of continuous heating 30min of mixed solution for obtaining step 2
It is to calcine predecessor that the white crystal obtained for 24 hours is dried in dry case；
Step 4 is packed into after carefully grinding the predecessor that step 3 obtains in the small-sized calcining tube of sealing, with 20 DEG C/min
Persistently overheating to 520 DEG C of heating rate, and constant temperature is calcined 4h, and faint yellow solid powder is obtained after cooling；
After step 5, the pale yellow powder regrinding for obtaining step 4, alcohol and deionized water washes clean are used successively,
And 50 DEG C of low temperature dryings, obtained faint yellow solid powder are ion filled graphite phase carbon nitride (g-C3N4) nanometer sheet.
Nitrogen source is melamine (C in the step 16N6H6) or urea (CO (NH2)2), the nitrogen source and deionization of addition
The mass ratio of water is 1:50~1:500.
The mass fraction for the concentrated hydrochloric acid being added in the step 2 is 37%.
The quality for the nitrogen source being added in the volume (in terms of mL) for the concentrated hydrochloric acid being added in the step 2 and step 1 (in terms of g)
Numeric ratio be 1:1~1:2.
The volume ratio for the concentrated hydrochloric acid being added in the middle-size and small-size calcining tube of step 4 and step 2 is 25:1~100:1.
G-C is filled using the ion that the method for the present invention is prepared3N4Nanometer sheet photochemical catalytic oxidation removes the step in NO
For：
Take ion filling g-C prepared by 100mg3N4Nanometer sheet powder is placed in the culture dish of radius 20cm, and appropriate second is added
Alcohol ultrasonic disperse is then placed in vacuum drying oven and is dried under the conditions of 80 DEG C.Culture dish is then placed in NOXPhotocatalysis experimental provision
Quartz glass reactor in, fixed lamp source face culture dish pours the mixing of the NO and air of stable ratio into reactor
Gas, and open NOx gas analysis detecting systems.After dark adsorption reaction 10min, opens lamp source and carry out photochemical catalytic oxidation removal NO
Reaction.
The invention has the advantages that：
The preparation method of a kind of ion filled graphite phase carbon nitride nanometer sheet provided by the invention, based in calcining predecessor
HCl pairs with the protective effects of the N-H keys of its chemical combination, make to be lost the ability for participating in thermal polycondensation reaction by the N-H of chemical combination, and those
The N-H keys that do not protect remain able to participate in thermal polycondensation reaction, and then a large amount of hole is produced around these protected N-H keys
It is raw；Again because predecessor is calcined in seal pipe, NH3With HCl when the respective release stage most starts, seal pipe can be discharged into
In inner space, but as the NH in space in pipe3When reaching a certain concentration with HCl, the NH of release3It can be because pressure acts on HCl
And stay between lattice and react, generate ionic compound NH4Cl is filled in the cavity being introduced into.This method has raw material honest and clean
Valence is easy to get, is simple for process, is environmentally protective, being easy to the advantages that industrialized production.
Ion prepared according to the methods of the invention fills g-C3N4Nanometer sheet, compared to common g-C3N4, because fill from
Sub- NH4 +And Cl-Presence, eliminate the influence of system part quantum size effect, reduce energy bandgaps；It has been formed simultaneously interior
Build electric field so that photogenerated charge greatly improves separative efficiency, therefore, shows preferable photooxidation removal under visible light
NO performances, also, the catalyst can still keep original photocatalytic activity, have extraordinary steady by being used for multiple times
It is qualitative.
Description of the drawings
Fig. 1 is that ion prepared by the embodiment of the present invention 1 fills g-C3N4The transmission electron microscope photo of nanometer sheet；
Fig. 2 is that ion prepared by the embodiment of the present invention 1 fills g-C3N4Nanometer sheet and common g-C3N4XRD powder diffractions
Compose comparison diagram；
Fig. 3 is that ion prepared by the embodiment of the present invention 1 fills g-C3N4Nanometer sheet and common g-C3N4Energy bandgaps comparison
Figure；
Fig. 4 is that ion prepared by the embodiment of the present invention 1 fills g-C3N4Nanometer sheet and common g-C3N4Fluorescence spectrum comparison
Figure；
Fig. 5 is that ion prepared by the embodiment of the present invention 1 fills g-C3N4Nanometer sheet and common g-C3N4Photochemical catalytic oxidation go
Except the effect contrast figure of NO；
Fig. 6 is that ion prepared by the embodiment of the present invention 1 fills g-C3N4Nanometer sheet photochemical catalytic oxidation removes the loop test of NO
Figure.
Specific implementation mode
Below with reference to the embodiments and with reference to the accompanying drawing the technical solutions of the present invention will be further described,
Embodiment 1
A, by 2g analysis pure melamines (C3N6H6) solid powder be added to 100mL 80 DEG C of heating water baths deionization
In water, while magnetic agitation accelerates dissolving, stops heating and stirring, and natural cooling after solution clarification；
B, when the obtained clear solutions of step a, which are cooled to, begins with white crystal precipitation, stirring is opened and into solution
It is slowly added to the concentrated hydrochloric acid (HCl) that 1mL mass fractions are 37% dropwise, obtains mixed solution；
C, 80 DEG C of continuous heating 30min of mixed solution for obtaining step b, then place it in 120 DEG C of forced air drying
It is dried in case for 24 hours, obtains white crystal；
D, it is put into the 100mL calcining tubes of sealing after carefully grinding the white crystal that step c is obtained, with 20 DEG C/min's
Persistently overheating to 520 DEG C of heating rate, and constant temperature is calcined 4h at 520 DEG C, and faint yellow solid powder is obtained after cooling；
F, after the pale yellow powder regrinding obtained step d, alcohol and deionized water washes clean, and 50 are used successively
DEG C low temperature drying, obtained faint yellow solid powder are ion filling g-C3N4Nanometer sheet.
G-C is filled to the ion made from embodiment 13N4Nanometer sheet and common g-C3N4A series of test experiments are carried out, are tied
Fruit is as follows：
Attached drawing 1 is that ion prepared by embodiment 1 fills g-C3N4The transmission electron microscope photo of nanometer sheet, it can be seen that
The sample of preparation is in nanoscale flake structure, because pore space structure does not occur in the filling effect surface of ion.
Attached drawing 2 is that ion prepared by embodiment 1 fills g-C3N4Nanometer sheet and common g-C3N4XRD powder diffraction spectrums pair
Than figure, it can be seen that the sample of preparation not only has g-C3N4Base peak, while also have ammonium chloride (NH4Cl base peak).
Attached drawing 3 is that ion prepared by embodiment 1 fills g-C3N4Nanometer sheet and common g-C3N4Energy bandgaps comparison diagram,
It can be seen that the sample prepared compares common g-C3N4Band-gap energy smaller, improve its absorbability to visible light so that
Electronics is easier to be excited.
Attached drawing 4 is that ion prepared by embodiment 1 fills g-C3N4Nanometer sheet and common g-C3N4Fluorescence spectrum comparison diagram,
It can be seen that the sample prepared compares common g-C3N4Fluorescence intensity it is lower, illustrate its photogenerated charge separative efficiency higher.
G-C is filled to ion prepared by embodiment 13N4Nanometer sheet and common g-C3N4The effect of photocatalysis removal NO is carried out
Fruit is tested, and testing procedure is as follows：It takes 100mg photocatalyst powders to be placed in the culture dish of radius 20cm, it is super that ethanol in proper amount is added
Sound disperses, and is then placed in vacuum drying oven and is dried under the conditions of 80 DEG C.Culture dish is then placed in NOXThe stone of photocatalysis experimental provision
In English glass reactor, fixed lamp source face culture dish pours the NO of stable ratio and the mixed gas of air into reactor,
And open NOx gas analysis detecting systems.After dark adsorption reaction 10min, opens lamp source and carry out photochemical catalytic oxidation removal NO reactions.
The lamp source of use does not use optical filter.
G-C is also filled to ion using identical step3N4The cycle that nanometer sheet has carried out photochemical catalytic oxidation removal NO is surveyed
Examination, has recycled altogether 4 times.In addition to the 1st time needs to disperse photocatalyst powder in culture dish, latter 3 times first by reactor
Interior remaining mixed gas discharge, pours new mixed gas, then directly carries out secretly absorption and light-catalyzed reaction.
Attached drawing 5 is that ion prepared by embodiment 1 fills g-C3N4Nanometer sheet and common g-C3N4Photochemical catalytic oxidation remove NO
Effect contrast figure.As seen from the figure, when being irradiated without light, the two is to NO all without adsorption capacity；After opening lamp source irradiation, pass through
50 minutes, ion fill g-C3N4Nanometer sheet is about common g-C to the photocatalysis removal ability of NO3N43 times.
Attached drawing 6 is that ion prepared by embodiment 1 fills g-C3N4Nanometer sheet photochemical catalytic oxidation removes the loop test figure of NO.
It is recycled by 4 times, nanometer sheet still remains the photocatalysis removal ability of preferable NO.
Protection scope of the present invention is not limited to the above embodiments, it is clear that those skilled in the art can be to this hair
It is bright to carry out various changes and deformation without departing from scope and spirit of the present invention.If these changes and deformation belong to power of the present invention
In the range of profit requirement and its equivalent technologies, then including the intent of the present invention also includes these changes and deforms.
Claims (5)
1. a kind of preparation method of ion filled graphite phase carbon nitride nanometer sheet, which is characterized in that include the following steps：
The solid powder for analyzing purity nitrogen source is added in the deionized water of 80 DEG C of heating water baths by step 1, while magnetic agitation adds
Instant solution is to stop heating and stirring, and natural cooling after nitrogen source is completely dissolved dispersion after solution clarification；
Step 2, when the clear solution that step 1 obtains be cooled to begin with white crystal be precipitated when, open stirring and into solution
It is slowly added to concentrated hydrochloric acid dropwise, obtains mixed solution；
Step 3, the 80 DEG C of continuous heating 30min of mixed solution for obtaining step 2, are then transferred to 120 DEG C of air dry oven
For 24 hours, obtained white crystal is to calcine predecessor for middle drying；
Step 4 is packed into after carefully grinding the predecessor that step 3 obtains in the small-sized calcining tube of sealing, with the liter of 20 DEG C/min
Persistently overheating to 520 DEG C of warm rate, and constant temperature is calcined 4h, and faint yellow solid powder is obtained after cooling；
After step 5, the pale yellow powder regrinding for obtaining step 4, alcohol and deionized water washes clean, and 50 are used successively
DEG C low temperature drying, obtained faint yellow solid powder is ion filled graphite phase carbon nitride nanometer sheet.
2. a kind of preparation method of ion filled graphite phase carbon nitride nanometer sheet as described in claim 1, it is characterised in that：Institute
It is melamine or urea to state nitrogen source in step 1.
3. a kind of preparation method of ion filled graphite phase carbon nitride nanometer sheet as described in claim 1, it is characterised in that：Institute
The mass ratio of the nitrogen source and deionized water of stating step 1 addition is 1:50~1:500.
4. a kind of preparation method of ion filled graphite phase carbon nitride nanometer sheet as described in claim 1, it is characterised in that：Institute
The mass fraction for stating the concentrated hydrochloric acid being added in step 2 is 37%, the volume (in terms of mL) and step of the concentrated hydrochloric acid being added in step 2
The numeric ratio of the quality (in terms of g) for the nitrogen source being added in 1 is 1:1~1:2.
5. a kind of preparation method of ion filled graphite phase carbon nitride nanometer sheet as described in claim 1, it is characterised in that：Institute
The volume ratio for stating the concentrated hydrochloric acid being added in the middle-size and small-size calcining tube of step 4 and step 2 is 25:1~100:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810550204.0A CN108671956B (en) | 2018-05-31 | 2018-05-31 | Preparation method of ion-filled graphite-phase carbon nitride nanosheet |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810550204.0A CN108671956B (en) | 2018-05-31 | 2018-05-31 | Preparation method of ion-filled graphite-phase carbon nitride nanosheet |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108671956A true CN108671956A (en) | 2018-10-19 |
| CN108671956B CN108671956B (en) | 2021-04-02 |
Family
ID=63809473
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810550204.0A Active CN108671956B (en) | 2018-05-31 | 2018-05-31 | Preparation method of ion-filled graphite-phase carbon nitride nanosheet |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108671956B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109692698A (en) * | 2018-12-29 | 2019-04-30 | 陕西师范大学 | A kind of Bi/Ti of catalytic reduction of NOx3C2Nano-sheet photochemical catalyst and preparation method thereof |
| CN110252409A (en) * | 2019-07-15 | 2019-09-20 | 常熟理工学院 | One kind is for removing nitric oxide production photochemical catalyst and preparation method thereof |
| CN111646437A (en) * | 2020-07-07 | 2020-09-11 | 安阳工学院 | Method for preparing white graphite phase carbon nitride by closed self-pressurization strategy |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5023308A (en) * | 1988-07-12 | 1991-06-11 | Central Glass Company, Limited | Aminotriazine polymers and method of preparing same |
| CN105271141A (en) * | 2015-11-19 | 2016-01-27 | 南京工程学院 | Method for preparing porous graphite-phase carbon nitride material |
| CN105642329A (en) * | 2016-01-01 | 2016-06-08 | 三峡大学 | Loaded graphite phase carbonized nitrogen composite material as well as preparation method and application thereof |
| US20170173571A1 (en) * | 2015-12-17 | 2017-06-22 | Soochow University | Composite material used for catalyzing and degrading nitrogen oxide and preparation method and application thereof |
| CN106938198A (en) * | 2016-01-04 | 2017-07-11 | 中国科学院化学研究所 | A kind of graphite phase carbon nitride porous microsphere and preparation method thereof |
-
2018
- 2018-05-31 CN CN201810550204.0A patent/CN108671956B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5023308A (en) * | 1988-07-12 | 1991-06-11 | Central Glass Company, Limited | Aminotriazine polymers and method of preparing same |
| CN105271141A (en) * | 2015-11-19 | 2016-01-27 | 南京工程学院 | Method for preparing porous graphite-phase carbon nitride material |
| US20170173571A1 (en) * | 2015-12-17 | 2017-06-22 | Soochow University | Composite material used for catalyzing and degrading nitrogen oxide and preparation method and application thereof |
| CN105642329A (en) * | 2016-01-01 | 2016-06-08 | 三峡大学 | Loaded graphite phase carbonized nitrogen composite material as well as preparation method and application thereof |
| CN106938198A (en) * | 2016-01-04 | 2017-07-11 | 中国科学院化学研究所 | A kind of graphite phase carbon nitride porous microsphere and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| GUOHUI DONG ET AL.: ""Facile synthesis of porous graphene-like carbon nitride (C6N9H3) with excellent photocatalytic activity for NO removal"", 《APPLIED CATALYSIS B: ENVIRONMENTAL》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109692698A (en) * | 2018-12-29 | 2019-04-30 | 陕西师范大学 | A kind of Bi/Ti of catalytic reduction of NOx3C2Nano-sheet photochemical catalyst and preparation method thereof |
| CN110252409A (en) * | 2019-07-15 | 2019-09-20 | 常熟理工学院 | One kind is for removing nitric oxide production photochemical catalyst and preparation method thereof |
| CN110252409B (en) * | 2019-07-15 | 2021-12-31 | 常熟理工学院 | Photocatalyst for removing nitric oxide and preparation method thereof |
| CN111646437A (en) * | 2020-07-07 | 2020-09-11 | 安阳工学院 | Method for preparing white graphite phase carbon nitride by closed self-pressurization strategy |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108671956B (en) | 2021-04-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103657619B (en) | The preparation method of the titanium dioxide nanosheet photocatalytic material that a kind of size is controlled | |
| CN109482179A (en) | The preparation of TiO2/ graphene/nano silver composite photo-catalyst and its degradation of PARA FORMALDEHYDE PRILLS(91,95) | |
| Dara et al. | Green sol–gel auto combustion synthesis and characterization of double perovskite Tb 2 ZnMnO 6 nanoparticles and a brief study of photocatalytic activity | |
| CN102060330B (en) | Method for synthetizing bismuth molybdate octahedral nanoparticle by microwave radiation heating | |
| CN107159295A (en) | A kind of inverse opal materials derived of visible light photocatalytic degradation of organic pollutants and preparation method thereof | |
| CN106622293B (en) | A kind of H-TiO2/CdS/Cu2-xThe preparation method of S nanobelt | |
| CN108671956A (en) | A kind of preparation method of ion filled graphite phase carbon nitride nanometer sheet | |
| CN109433229A (en) | A kind of preparation method of CdS/CoO nano-heterogeneous structure | |
| Yang et al. | rGO/Fe-doped g-C3N4 visible-light driven photocatalyst with improved NO removal performance | |
| CN108298591B (en) | synthesis method and application of hexagonal iron titanate nanosheet material | |
| CN103521237A (en) | Method for preparing Fe3O4/SiO2/Bi2WO6 magnetic microsphere photocatalyst | |
| CN106362768B (en) | A kind of honeycomb ceramic plate loads TiO2The preparation technology of the immobilized photochemical catalysts of-NCP | |
| CN106944096A (en) | A kind of preparation method of efficient Emission in Cubic CdS nano-crystalline photocatalysis materials | |
| CN112028119B (en) | Anatase TiO with co-exposed {101}, {100} and {111} -crystal faces 2 Nanocrystal | |
| CN105032471B (en) | A kind of visible light-responded nano-TiO2The preparation of/Zeolite composite materials | |
| Xue et al. | Construction of Cu 2+-doped CeO 2 nanocrystals hierarchical hollow structure and its enhanced photocatalytic performance | |
| CN114471707B (en) | Hydrogel sphere containing catalyst, preparation method thereof and application thereof in photocatalytic treatment of organic pollutants | |
| Wang et al. | Photocatalytic activity of N-doped TiO2 to vehicle exhaust in road tunnel | |
| CN113198458B (en) | Bismuth-chromium composite oxide semiconductor photocatalyst and preparation method and application thereof | |
| CN104828865A (en) | A preparing method of black single brookite phase titanium dioxide | |
| Ding et al. | One-step synthesis of spherical NaTaO3 and graphene spherical NaTaO3 nanoparticles with enhanced photocatalytic activity for NO purification | |
| CN113797910B (en) | Defect-containing nano microspherical perovskite catalyst and preparation method and application thereof | |
| Dong et al. | Synthesis of β-FeOOH/TiO2/SiO2 by melting phase separation-hydrothermal method to improve photocatalytic performance | |
| CN112973664A (en) | Aurivillius type lead-containing layered perovskite catalyst, and preparation method and application thereof | |
| CN112973692A (en) | Preparation method of fullerene doped titanium dioxide composite photocatalyst |
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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |