CN108686698A - A kind of interlayer adulterates the class graphene carbon nitride photocatalyst and preparation method thereof of seven water potassium phosphates - Google Patents
A kind of interlayer adulterates the class graphene carbon nitride photocatalyst and preparation method thereof of seven water potassium phosphates Download PDFInfo
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- CN108686698A CN108686698A CN201810480620.8A CN201810480620A CN108686698A CN 108686698 A CN108686698 A CN 108686698A CN 201810480620 A CN201810480620 A CN 201810480620A CN 108686698 A CN108686698 A CN 108686698A
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- carbon nitride
- interlayer
- class graphene
- water potassium
- potassium phosphates
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- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 title claims abstract description 281
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 155
- 229910001868 water Inorganic materials 0.000 title claims abstract description 148
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 144
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 137
- 235000011009 potassium phosphates Nutrition 0.000 title claims abstract description 137
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 112
- 239000011229 interlayer Substances 0.000 title claims abstract description 107
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 106
- 238000002360 preparation method Methods 0.000 title claims abstract description 42
- 239000003054 catalyst Substances 0.000 claims abstract description 53
- 238000000034 method Methods 0.000 claims abstract description 31
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000004202 carbamide Substances 0.000 claims abstract description 19
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims description 44
- 229910000160 potassium phosphate Inorganic materials 0.000 claims description 29
- 238000001953 recrystallisation Methods 0.000 claims description 7
- 230000005855 radiation Effects 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 11
- 239000010410 layer Substances 0.000 abstract description 8
- 238000007146 photocatalysis Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 7
- 238000010276 construction Methods 0.000 abstract description 6
- 229910019142 PO4 Inorganic materials 0.000 abstract description 5
- 230000031700 light absorption Effects 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 3
- 230000015556 catabolic process Effects 0.000 description 31
- 238000006731 degradation reaction Methods 0.000 description 31
- -1 alkene carbon nitride Chemical class 0.000 description 14
- 230000008569 process Effects 0.000 description 14
- 238000007792 addition Methods 0.000 description 13
- 238000012360 testing method Methods 0.000 description 12
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 11
- 239000004575 stone Substances 0.000 description 11
- 239000003643 water by type Substances 0.000 description 11
- 238000012512 characterization method Methods 0.000 description 10
- 238000004458 analytical method Methods 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 238000012986 modification Methods 0.000 description 6
- 230000004048 modification Effects 0.000 description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 5
- 229910052700 potassium Inorganic materials 0.000 description 5
- 239000011591 potassium Substances 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- DJFBJKSMACBYBD-UHFFFAOYSA-N phosphane;hydrate Chemical compound O.P DJFBJKSMACBYBD-UHFFFAOYSA-N 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000011031 large-scale manufacturing process Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 150000003254 radicals Chemical class 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 description 2
- 238000003916 acid precipitation Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000010183 spectrum analysis Methods 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- JIHQDMXYYFUGFV-UHFFFAOYSA-N 1,3,5-triazine Chemical compound C1=NC=NC=N1 JIHQDMXYYFUGFV-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- IOVCWXUNBOPUCH-UHFFFAOYSA-N Nitrous acid Chemical compound ON=O IOVCWXUNBOPUCH-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000003044 adaptive effect Effects 0.000 description 1
- 239000000809 air pollutant Substances 0.000 description 1
- 231100001243 air pollutant Toxicity 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012719 thermal polymerization Methods 0.000 description 1
Classifications
-
- B01J35/39—
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
Abstract
This application discloses the class graphene carbon nitride photocatalysts and preparation method thereof that a kind of interlayer adulterates seven water potassium phosphates, the method includes deionized water to be added in crucible, urea and seven water potassium phosphates are then added, obtain photochemical catalyst presoma;The photochemical catalyst is recrystallized, recrystallized product is obtained;The recrystallized product is heat-treated in Muffle furnace, obtains the class graphene carbon nitride photocatalyst that interlayer adulterates seven water potassium phosphates.Interlayer that preparation method shown in the embodiment of the present application is prepared adulterates the class graphene carbon nitride photocatalyst of seven water potassium phosphates, by by K+And PO4 3-It is entrained between class graphene carbon nitride layer, it can speed up the separation of class graphene carbonitride light induced electron and hole in this way, fault of construction is introduced in class graphene carbonitride, promotes the promotion of efficiency of light absorption, and then improves the activity of class graphene carbonitride visible light photocatalysis.
Description
Technical field
This application involves the class graphene carbonitride light that catalyst field more particularly to a kind of interlayer adulterate seven water potassium phosphates
Catalyst and preparation method thereof.
Background technology
With the progress of mankind's science and technology civilization, industry has obtained developing on a large scale, and the nitrogen oxides that coal combustion generates is
Cause one of the typical air pollutant of city fog and acid rain.Nitrogen oxides is as photochemical fog, acid rain, depletion of the ozone layer
Pollutant, nitrogen oxides has become countries in the world atmosphere pollution urgently to be resolved hurrily.It can be seen that the photocatalysis method of optical drive
It has all been shown in environmental pollution purification and solar energy conversion aspect as a kind of environmental-friendly green technology good
Application prospect.It can be seen that the photocatalysis method of optical drive can make nitrogen oxides that oxidation reaction occur under photochemical catalyst effect, generate
Water (H2O), nitrate, nitrous acid etc. and reach innoxious, to environment purification.
Catalysis material plays important role in the photocatalytic process.Organic photochemical catalyst class graphene carbonitride
(g-C3N4), it is conjugated photochemical catalyst as a kind of low cost, the layering without metal, due to its attractive electron energy band
Structure, physical and chemical stability and controllable molecular structure, water decomposition under visible light illumination, organic pollution drop
Solution, organic catalysis and elctro-catalyst etc. are widely used.
However, class graphene carbonitride (g-C3N4) be covalently made of the weak of three s-triazine repetitive units and interlayer, it is interior
Chemical reaction caused by source property graphene sp2 array hybridizations is slow, and the carrier random migration for making light generate triggers low charge
Separative efficiency limits the large-scale application of carbonitride to keep photocatalysis performance undesirable.
Invention content
This application provides class graphene carbon nitride photocatalyst and its preparation sides that a kind of interlayer adulterates seven water potassium phosphates
Method adulterates the class graphene carbon nitride photocatalyst of seven water potassium phosphates by preparing interlayer, by K+And PO4 3-It is entrained in class stone
Between black alkene carbon nitride layer, the separation of class graphene carbonitride light induced electron and hole is can speed up, in class graphene carbonitride
Fault of construction is introduced, promotes the promotion of efficiency of light absorption, and then improve the activity of class graphene carbonitride visible light photocatalysis.
First aspect shows that a kind of interlayer adulterates the class graphene carbonitride of seven water potassium phosphates according to an embodiment of the present application
The preparation method of photochemical catalyst, the method includes:
Step S101, deionized water is added in crucible, urea and seven water potassium phosphates is then added, obtain photochemical catalyst
Presoma;
Step S102, the photochemical catalyst is recrystallized, obtains recrystallized product;
Step S103, the recrystallized product is heat-treated in Muffle furnace, obtains interlayer and adulterates seven water potassium phosphates
Class graphene carbon nitride photocatalyst.
Selectable, the quality of the seven water potassium phosphate is 0.018-0.110g.
Selectable, the quality of the seven water potassium phosphate is 0.073g.
Selectable, the temperature of the recrystallization is 60-80 DEG C.
Selectable, the temperature of the recrystallization is 60 DEG C.
Selectable, the temperature of the heat treatment is 550-575 DEG C.
Selectable, the temperature of the heat treatment is 550 DEG C.
Selectable, the time of the heat treatment is 2-4h.
The application second aspect shows that a kind of interlayer adulterates the class graphene carbon nitride photocatalyst of seven water potassium phosphates, described
Interlayer adulterate seven water potassium phosphates class graphene carbon nitride photocatalyst be to the removal rate of NO under conditions of radiation of visible light
27.41%-35.81%.
By above technical scheme it is found that this application discloses the class graphene carbonitrides that a kind of interlayer adulterates seven water potassium phosphates
Then urea and seven water phosphorus are added the method includes deionized water to be added in crucible in photochemical catalyst and preparation method thereof
Sour potassium obtains photochemical catalyst presoma;The photochemical catalyst is recrystallized, recrystallized product is obtained;By the recrystallized product
It is heat-treated in Muffle furnace, obtains the class graphene carbon nitride photocatalyst that interlayer adulterates seven water potassium phosphates.The application is real
The class graphene carbon nitride photocatalyst that the interlayer that the preparation method exemplified prepares adulterates seven water potassium phosphates is applied, by by K+
And PO4 3-It is entrained between class graphene carbon nitride layer, can speed up class graphene carbonitride light induced electron and point in hole in this way
From, introduce fault of construction in class graphene carbonitride, promote the promotion of efficiency of light absorption, and then improve class graphene nitridation
The activity of carbon visible light photocatalysis.Interlayer provided by the invention adulterates the class graphene carbon nitride photocatalyst item of seven water potassium phosphates
Part is mild, prepares simply, is suitable for large-scale production.
Description of the drawings
In order to illustrate more clearly of the technical solution of the application, letter will be made to attached drawing needed in the embodiment below
Singly introduce, it should be apparent that, for those of ordinary skills, without having to pay creative labor,
Other drawings may also be obtained based on these drawings.
Fig. 1 is the preparation method for the class graphene carbon nitride photocatalyst that a kind of interlayer of the application adulterates seven water potassium phosphates
Flow chart;
Fig. 2 be the embodiment of the present invention 1,2,3,4,5 prepare four kinds of different qualities than interlayer adulterate seven water potassium phosphates
The XRD diagram of class graphene carbon nitride photocatalyst and pure phase class graphene carbon nitride photocatalyst, (XRD diagram X-ray
The abbreviation of diffraction, i.e. X-ray diffraction);
Fig. 3 is the K for the class graphene carbon nitride photocatalyst that interlayer prepared by the embodiment of the present application 3 adulterates seven water potassium phosphates
The high-resolution XPS figures of 2p, (XPS is the abbreviation of X-ray photoelectron spectroscop, i.e. x-ray photoelectron energy
Spectrum analysis);
Fig. 4 is the class graphene carbon nitride photocatalyst that interlayer prepared by the embodiment of the present application 3,5 adulterates seven water potassium phosphates
Scheme with the SURVERY of the XPS of pure phase class graphene carbon nitride photocatalyst;
Fig. 5 is the class graphene carbon nitride photocatalyst that interlayer prepared by the embodiment of the present application 3 adulterates seven water potassium phosphates
SEM schemes, (SEM figures are the abbreviation of scanning electron microscope, i.e. scanning electron microscope);
Fig. 6 is the SEM figures of pure phase class graphene carbon nitride photocatalyst prepared by the embodiment of the present application 5;
Fig. 7 is the class graphene carbon nitride photocatalyst that interlayer prepared by the embodiment of the present application 3 adulterates seven water potassium phosphates
TEM schemes, (TEM figures are the abbreviation of transmission electron microscope, i.e. transmission electron microscope);
Fig. 8 is the TEM figures of pure phase class graphene carbon nitride photocatalyst prepared by the embodiment of the present application 5;
Fig. 9 is the class graphene carbon nitride photocatalyst that interlayer prepared by the embodiment of the present application 3,5 adulterates seven water potassium phosphates
Scheme with the PL of pure phase class graphene carbon nitride photocatalyst, (abbreviation that PL figures are Photoluminescence, i.e. fluorescence Spectra);
Figure 10 is the class that interlayer prepared by the embodiment of the present application 1,2,3,4,5,6,7,8,9,10,11 adulterates seven water potassium phosphates
The N of graphene carbon nitride photocatalyst and pure phase class graphene carbon nitride photocatalyst2Adsorption-desorption figure;
Figure 11 is the class that interlayer prepared by the embodiment of the present application 1,2,3,4,5,6,7,8,9,10,11 adulterates seven water potassium phosphates
Graphene carbon nitride photocatalyst and the BET-BJH of pure phase class graphene carbon nitride photocatalyst scheme, (BET-BJH The
The abbreviation of specific surface area andpore size analyzer, i.e. specific surface area and pore analysis);
Figure 12 is the class that interlayer prepared by the embodiment of the present application 1,2,3,4,5,6,7,8,9,10,11 adulterates seven water potassium phosphates
Degradation of the graphene carbon nitride photocatalyst with pure phase class graphene carbon nitride photocatalyst under visible light conditions to NO degradations
Efficiency comparative schemes;
Figure 13 is the class graphene carbon nitride photocatalyst that interlayer prepared by the embodiment of the present application 3,5 adulterates seven water potassium phosphates
It detects and schemes with the living radical (superoxide anion) of pure phase class graphene carbon nitride photocatalyst;
Figure 14 is the class graphene carbon nitride photocatalyst that interlayer prepared by the embodiment of the present application 3,5 adulterates seven water potassium phosphates
It detects and schemes with the living radical (hydroxyl) of pure phase class graphene carbon nitride photocatalyst.
Wherein, CN-1/6KP is that interlayer prepared by the preparation method shown in embodiment 1 adulterates the class graphite of seven water potassium phosphates
Alkene carbon nitride photocatalyst;CN-1/3KP is the class that interlayer prepared by the preparation method shown in embodiment 2 adulterates seven water potassium phosphates
Graphene carbon nitride photocatalyst;CN-2/3KP is that interlayer prepared by the preparation method shown in embodiment 3 adulterates seven water potassium phosphates
Class graphene carbon nitride photocatalyst;CN-KP is that interlayer prepared by the preparation method shown in embodiment 4 adulterates seven water potassium phosphates
Class graphene carbon nitride photocatalyst;CN is the carbon nitride photocatalyst of pure phase prepared by the preparation method shown in embodiment 5;
CN-2/3KP-70 is the class graphene carbonitride light that interlayer prepared by the preparation method shown in embodiment 6 adulterates seven water potassium phosphates
Catalyst;CN-2/3KP-80 is the class graphene nitrogen that interlayer prepared by the preparation method shown in embodiment 7 adulterates seven water potassium phosphates
Change carbon photochemical catalyst;CN-2/3KP-565 is the class that interlayer prepared by the preparation method shown in embodiment 8 adulterates seven water potassium phosphates
Graphene carbon nitride photocatalyst;CN-2/3KP-575 is that interlayer prepared by the preparation method shown in embodiment 9 adulterates seven water phosphorus
The class graphene carbon nitride photocatalyst of sour potassium;CN-2/3KP-3 is interlayer doping prepared by the preparation method shown in embodiment 10
The class graphene carbon nitride photocatalyst of seven water potassium phosphates;CN-2/3KP-4 is layer prepared by the preparation method shown in embodiment 11
Between adulterate the class graphene carbon nitride photocatalysts of seven water potassium phosphates.
Specific implementation mode
With reference to the attached drawing in the application, technical solutions in the embodiments of the present application is clearly and completely described,
Obviously, described embodiment is only a part of the embodiment of the application, instead of all the embodiments.Based in the application
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts,
It shall fall within the protection scope of the present invention.
Attached drawing 1 is please referred to, is the class graphene carbon nitride photocatalyst that a kind of interlayer of the application adulterates seven water potassium phosphates
The flow chart of preparation method.Seven water potassium phosphate doped graphite ene-type carbon nitride photocatalysts shown in the embodiment of the present application and its system
Preparation Method includes the following steps:
Step S101, deionized water is added in crucible, urea and seven water potassium phosphates is then added, obtain photochemical catalyst
Presoma;
Step S102, the photochemical catalyst is recrystallized, obtains recrystallized product;
Step S103, the recrystallized product is heat-treated in Muffle furnace, the heating rate of the Muffle furnace is
15 DEG C/min, obtain the class graphene carbon nitride photocatalyst that interlayer adulterates seven water potassium phosphates.
Selectable, the quality of the seven water potassium phosphate is 0.018-0.110g.
Selectable, the quality of the seven water potassium phosphate is 0.073g.
Selectable, the temperature of the recrystallization is 60-80 DEG C.
Selectable, the temperature of the recrystallization is 60 DEG C.
Selectable, the temperature of the heat treatment is 550-575 DEG C.
Selectable, the temperature of the heat treatment is 550 DEG C.
Selectable, the time of the heat treatment is 2-4h.
The quality of the seven water potassium phosphate is 0.073g, and the temperature of the recrystallization is 60 DEG C, the temperature of the heat treatment
When being 550 DEG C, prepared interlayer adulterates the class graphene carbon nitride photocatalysts of seven water potassium phosphates to the degradation rate of NO most
It is high.
By above technical scheme it is found that this application discloses the class graphene carbonitrides that a kind of interlayer adulterates seven water potassium phosphates
Then urea and seven water phosphoric acid are added the method includes deionized water to be added in crucible in the preparation method of photochemical catalyst
Potassium obtains photochemical catalyst presoma;The photochemical catalyst is recrystallized, recrystallized product is obtained;The recrystallized product is existed
It is heat-treated in Muffle furnace, obtains the class graphene carbon nitride photocatalyst that interlayer adulterates seven water potassium phosphates.The application is implemented
Interlayer that the preparation method exemplified is prepared adulterates the class graphene carbon nitride photocatalyst of seven water potassium phosphates, by by K+With
PO4 3-It is entrained between class graphene carbon nitride layer, can speed up the separation of class graphene carbonitride light induced electron and hole in this way,
Fault of construction is introduced in class graphene carbonitride, promotes the promotion of efficiency of light absorption, and then improves class graphene carbonitride
The activity of visible light photocatalysis.Interlayer provided by the invention adulterates the class graphene carbon nitride photocatalyst condition of seven water potassium phosphates
Mildly, it prepares simply, is suitable for large-scale production.
Experiment is it is found that adulterate the class graphene nitrogen of seven water potassium phosphates by interlayer prepared by above-mentioned preparation method by analysis
Change carbon photochemical catalyst, catalytic activity is higher than the catalytic activity of pure phase class graphene carbonitride, the method system shown in the application
Standby interlayer adulterates the cost of the class graphene carbon nitride photocatalyst of seven water potassium phosphates in practical applications and significantly reduces.
By the class graphene carbon nitride photocatalyst for adulterating seven water potassium phosphates to the interlayer prepared by the embodiment of the present application
It is characterized, it can be seen that the class graphene carbon nitride photocatalyst that interlayer adulterates seven water potassium phosphates has following characteristic:
(1) the class graphene carbon nitride photocatalyst that seven water potassium phosphates are adulterated to interlayer carries out XRD diagram spectrum analysis (such as Fig. 2
It is shown), it was demonstrated that carbon nitride layer spacing increases.
(2) the class graphene carbon nitride photocatalyst that seven water potassium phosphates are adulterated to interlayer carries out the XPS atlas analysis of K 2p
(as shown in Figure 3), it was demonstrated that K+It is successfully doped into class graphene carbonitride.
(3) the class graphene carbon nitride photocatalyst that seven water potassium phosphates are adulterated to interlayer carries out XPS analysis (such as Fig. 4 institutes
Show), it was demonstrated that there are carbon, nitrogen and oxygen elements in the class graphene carbon nitride photocatalyst of interlayer seven water potassium phosphates of doping.
(4) the class graphene carbon nitride photocatalyst that seven water potassium phosphates are adulterated to interlayer carries out sem analysis (such as Fig. 5, Fig. 6
It is shown), it is observed that seven water potassium phosphate additions, which are the interlayer of 0.073g, adulterates the class graphene carbonitride of seven water potassium phosphates
Photochemical catalyst is that two-dimensional nano is laminar structured.
(5) the class graphene carbon nitride photocatalyst that seven water potassium phosphates are adulterated to interlayer carries out tem analysis (such as Fig. 7, Fig. 8
It is shown), it is observed that seven water potassium phosphate additions, which are the interlayer of 0.073g, adulterates the class graphene carbonitride of seven water potassium phosphates
Photochemical catalyst is that two-dimensional nano is laminar structured, and seven water potassium phosphates adulterate class graphene carbonitride not to the body construction of carbonitride
It damages.
(6) the class graphene carbon nitride photocatalyst that seven water potassium phosphates are adulterated to interlayer carries out PL test analysis (such as Fig. 9 institutes
Show), it was demonstrated that seven water potassium phosphates doping class graphene carbonitride makes PL strength reductions, promotes light induced electron and point in hole
From.
(7) interlayer is adulterated seven water potassium phosphates class graphene carbon nitride photocatalyst carry out BET-JH analyses (such as Figure 10,
Shown in Figure 11), reflect its specific surface area and the relevant information of aperture structure, while also demonstrating mesoporous presence.
The class graphene carbonitride light of seven water potassium phosphates is adulterated to interlayer provided by the embodiments of the present application by degrading NO
The catalytic performance of catalyst is tested.Test process is as follows:
(1) the class graphene carbon nitride photocatalyst that interlayer prepared by 0.2g embodiments is adulterated to seven water potassium phosphates is placed in NO
In continuous flow reactor;
(2) under dark condition, when NO concentration reaches balance, it is the halogen tungsten lamp of 150W as visible light to use power
Source, and with the edge filter filtering ultraviolet light of 420nm, the photochemical catalyst is shone when NO concentration reaches balance
It penetrates.
(3) condition of above-mentioned catalytic performance test process is:Relative humidity 60%, oxygen content 21%, NO air-flows
Flow is 2.4L/min, and the initial concentration of NO is 530ppb.
The class graphene carbon nitride photocatalyst that interlayer provided by the embodiments of the present application adulterates seven water potassium phosphates degrades to NO
Degradation it is as follows:
(1) the class graphene carbon nitride photocatalyst that interlayer adulterates seven water potassium phosphates is 27.41%- to the degradation rate of NO
The calculation formula of 35.81% (as shown in figure 12), degradation rate is η (%)=(1-C/C0) × 100%, C0For the initial concentration of NO,
C is the instantaneous concentration of NO after illumination 30min.
(2) compared to the class graphene carbonitride of pure phase, the interlayer that seven water potassium phosphate additions are 0.073g adulterates seven water
Class graphene carbon nitride photocatalyst (CN-2/3KP) principal degradation free radical of potassium phosphate removes superoxide anion (O2 -) go back outside
There is hydroxyl radical free radical (OH) (as shown in Figure 13, Figure 14), so that its photocatalytic activity greatly improves.
Embodiment 1:
(1) 10g urea and seven water potassium phosphates of 0.018g are added in the 50mL crucibles containing 20mL deionized waters, keeps it mixed
It closes, photochemical catalyst presoma is obtained after being uniformly dispersed;
(2) the photochemical catalyst presoma is recrystallized under the conditions of 60 DEG C in an oven, obtains recrystallized product;
(3) by the recrystallized product in Muffle furnace with the heating rate of 15 DEG C/min, temperature be increased to 550 DEG C it is laggard
Row heat treatment 2h obtains the class stone that the interlayer that seven water potassium phosphate additions are 0.018g adulterates seven water potassium phosphates after heat treatment
Black alkene carbon nitride photocatalyst (CN-1/6KP).
The class graphene carbon nitride photocatalyst (CN-1/ of seven water potassium phosphates is adulterated to interlayer prepared by the embodiment of the present application 1
6KP) characterized by XRD, XPS, SEM, TEM, PL, BET-BJH, ESR.
Interlayer prepared by the embodiment of the present application 1 adulterates the class graphene carbon nitride photocatalyst (CN-1/ of seven water potassium phosphates
6KP) (CN-1/6KP) degrades with its determining photocatalytic activity to NO, and detailed process is:In relative humidity 60%, oxygen contains
Amount be that the flow of 21%, NO air-flows is 2.4L/min, and 0.2g embodiments 1 is under conditions of 530ppb, are made by the initial concentration of NO
The class graphene carbon nitride photocatalyst (CN-1/6KP) that standby interlayer adulterates seven water potassium phosphates is placed in NO continuous flow reactors,
It is the halogen tungsten lamp of 150W as visible light source to use power, and with the edge filter filtering ultraviolet light of 420nm, when NO concentration
The class graphene carbon nitride photocatalyst (CN-1/6KP) for adulterating seven water potassium phosphates when reaching balance to the interlayer is irradiated,
The interlayer that the embodiment of the present application preparation is calculated adulterates the class graphene carbon nitride photocatalyst (CN-1/ of seven water potassium phosphates
It is 6KP) 27.41% to the degradation rate of NO.
Embodiment 2:
(1) 10g urea and seven water potassium phosphates of 0.037g are added in the 50mL crucibles containing 20mL deionized waters, keeps it mixed
It closes, photochemical catalyst presoma is obtained after being uniformly dispersed;
(2) the photochemical catalyst presoma is recrystallized under the conditions of 60 DEG C in an oven, obtains recrystallized product;
(3) by the recrystallized product in Muffle furnace with the heating rate of 15 DEG C/min, temperature be increased to 550 DEG C it is laggard
Row heat treatment 2h obtains the class stone that the interlayer that seven water potassium phosphate additions are 0.037g adulterates seven water potassium phosphates after heat treatment
Black alkene carbon nitride photocatalyst (CN-1/3KP).
The class graphene carbon nitride photocatalyst (CN-1/ of seven water potassium phosphates is adulterated to interlayer prepared by the embodiment of the present application 2
Characterization 3KP) and to the degradation test process of NO with embodiment 1.The interlayer doping seven of the preparation of the embodiment of the present application 2 is calculated
The class graphene carbon nitride photocatalyst (CN-1/3KP) of water potassium phosphate is 34.46% to the degradation rate of NO.
Embodiment 3:
(1) 10g urea and seven water potassium phosphates of 0.073g are added in the 50mL crucibles containing 20mL deionized waters, keeps it mixed
It closes, photochemical catalyst presoma is obtained after being uniformly dispersed;
(2) the photochemical catalyst presoma is recrystallized under the conditions of 60 DEG C in an oven, obtains recrystallized product;
(3) by the recrystallized product in Muffle furnace with the heating rate of 15 DEG C/min, temperature be increased to 550 DEG C it is laggard
Row heat treatment 2h obtains the class stone that the interlayer that seven water potassium phosphate additions are 0.073g adulterates seven water potassium phosphates after heat treatment
Black alkene carbon nitride photocatalyst (CN-2/3KP).
The class graphene carbon nitride photocatalyst (CN-2/ of seven water potassium phosphates is adulterated to interlayer prepared by the embodiment of the present application 3
Characterization 3KP) and to the degradation test process of NO with embodiment 1.The interlayer doping seven of the preparation of the embodiment of the present application 3 is calculated
The class graphene carbon nitride photocatalyst (CN-2/3KP) of water potassium phosphate is 35.81% to the degradation rate of NO.
Embodiment 4:
(1) 10g urea and seven water potassium phosphates of 0.110g are added in the 50mL crucibles containing 20mL deionized waters, keeps it mixed
It closes, photochemical catalyst presoma is obtained after being uniformly dispersed;
(2) the photochemical catalyst presoma is recrystallized under the conditions of 60 DEG C in an oven, obtains recrystallized product;
(3) by the recrystallized product in Muffle furnace with the heating rate of 15 DEG C/min, temperature be increased to 550 DEG C it is laggard
Row heat treatment 2h obtains the class stone that the interlayer that seven water potassium phosphate additions are 0.110g adulterates seven water potassium phosphates after heat treatment
Black alkene carbon nitride photocatalyst (CN-KP).
The class graphene carbon nitride photocatalyst (CN- of seven water potassium phosphates is adulterated to interlayer prepared by the embodiment of the present application 4
KP characterization) and to the degradation test process of NO with embodiment 1.The interlayer doping seven of the preparation of the embodiment of the present application 4 is calculated
The class graphene carbon nitride photocatalyst (CN-KP) of water potassium phosphate is 28.17% to the degradation rate of NO.
Embodiment 5:
(1) 10g urea is added in the 50mL crucibles containing 20mL deionized waters, makes it dissolve and is placed in baking oven in 60
It is recrystallized under the conditions of DEG C, obtains recrystallized product;
(2) by the recrystallized product in Muffle furnace with the heating rate of 15 DEG C/min, temperature be increased to 550 DEG C it is laggard
Row heat treatment 2h, the product obtained after heat treatment is the class graphene carbon nitride photocatalyst (CN) of pure phase.
To the embodiment of the present application 5 prepare pure phase class graphene carbon nitride photocatalyst (CN) characterization and to the drop of NO
Test process is solved with embodiment 1.The class graphene carbon nitride photocatalyst (CN) of the preparation of the embodiment of the present application 5 is calculated to NO
Degradation rate be 23.92%.
Embodiment 6:
(1) 10g urea and seven water potassium phosphates of 0.073g are added in the 50mL crucibles containing 20mL deionized waters, keeps it mixed
It closes, photochemical catalyst presoma is obtained after being uniformly dispersed;
(2) the photochemical catalyst presoma is recrystallized under the conditions of 70 DEG C in an oven, obtains recrystallized product;
(3) by the recrystallized product in Muffle furnace with the heating rate of 15 DEG C/min, temperature be increased to 550 DEG C it is laggard
Row heat treatment 2h obtains the class stone that the interlayer that seven water potassium phosphate additions are 0.073g adulterates seven water potassium phosphates after heat treatment
Black alkene carbon nitride photocatalyst (CN-2/3KP-70).
The class graphene carbon nitride photocatalyst (CN-2/ of seven water potassium phosphates is adulterated to interlayer prepared by the embodiment of the present application 6
Characterization 3KP-70) and to the degradation test process of NO with embodiment 1.The interlayer that the preparation of the embodiment of the present application 6 is calculated is mixed
The class graphene carbon nitride photocatalyst (CN-2/3KP-70) of miscellaneous seven water potassium phosphate is 32.81% to the degradation rate of NO.
Embodiment 7:
(1) 10g urea and seven water potassium phosphates of 0.073g are added in the 50mL crucibles containing 20mL deionized waters, keeps it mixed
It closes, photochemical catalyst presoma is obtained after being uniformly dispersed;
(2) the photochemical catalyst presoma is recrystallized under the conditions of 80 DEG C in an oven, obtains recrystallized product;
(3) by the recrystallized product in Muffle furnace with the heating rate of 15 DEG C/min, temperature be increased to 550 DEG C it is laggard
Row heat treatment 2h obtains the class stone that the interlayer that seven water potassium phosphate additions are 0.073g adulterates seven water potassium phosphates after heat treatment
Black alkene carbon nitride photocatalyst (CN-2/3KP-80).
The class graphene carbon nitride photocatalyst (CN-2/ of seven water potassium phosphates is adulterated to interlayer prepared by the embodiment of the present application 7
Characterization 3KP-80) and to the degradation test process of NO with embodiment 1.The interlayer that the preparation of the embodiment of the present application 7 is calculated is mixed
The class graphene carbon nitride photocatalyst (CN-2/3KP-80) of miscellaneous seven water potassium phosphate is 32.10% to the degradation rate of NO.
Embodiment 8:
(1) 10g urea and seven water potassium phosphates of 0.073g are added in the 50mL crucibles containing 20mL deionized waters, keeps it mixed
It closes, photochemical catalyst presoma is obtained after being uniformly dispersed;
(2) the photochemical catalyst presoma is recrystallized under the conditions of 60 DEG C in an oven, obtains recrystallized product;
(3) by the recrystallized product in Muffle furnace with the heating rate of 15 DEG C/min, temperature be increased to 565 DEG C it is laggard
Row heat treatment 2h obtains the class stone that the interlayer that seven water potassium phosphate additions are 0.073g adulterates seven water potassium phosphates after heat treatment
Black alkene carbon nitride photocatalyst (CN-2/3KP-565).
The class graphene carbon nitride photocatalyst (CN-2/ of seven water potassium phosphates is adulterated to interlayer prepared by the embodiment of the present application 8
Characterization 3KP-565) and to the degradation test process of NO with embodiment 1.The interlayer that the preparation of the embodiment of the present application 8 is calculated is mixed
The class graphene carbon nitride photocatalyst (CN-2/3KP-565) of miscellaneous seven water potassium phosphate is 35.16% to the degradation rate of NO.
Embodiment 9:
(1) 10g urea and seven water potassium phosphates of 0.073g are added in the 50mL crucibles containing 20mL deionized waters, keeps it mixed
It closes, photochemical catalyst presoma is obtained after being uniformly dispersed;
(2) the photochemical catalyst presoma is recrystallized under the conditions of 60 DEG C in an oven, obtains recrystallized product;
(3) by the recrystallized product in Muffle furnace with the heating rate of 15 DEG C/min, temperature be increased to 575 DEG C it is laggard
Row heat treatment 2h obtains the class stone that the interlayer that seven water potassium phosphate additions are 0.073g adulterates seven water potassium phosphates after heat treatment
Black alkene carbon nitride photocatalyst (CN-2/3KP-575).
The class graphene carbon nitride photocatalyst (CN-2/ of seven water potassium phosphates is adulterated to interlayer prepared by the embodiment of the present application 9
Characterization 3KP-575) and to the degradation test process of NO with embodiment 1.The interlayer that the preparation of the embodiment of the present application 9 is calculated is mixed
The class graphene carbon nitride photocatalyst (CN-2/3KP-575) of miscellaneous seven water potassium phosphate is 28.71% to the degradation rate of NO.
Embodiment 10:
(1) 10g urea and seven water potassium phosphates of 0.073g are added in the 50mL crucibles containing 20mL deionized waters, keeps it mixed
It closes, photochemical catalyst presoma is obtained after being uniformly dispersed;
(2) the photochemical catalyst presoma is recrystallized under the conditions of 60 DEG C in an oven, obtains recrystallized product;
(3) by the recrystallized product in Muffle furnace with the heating rate of 15 DEG C/min, temperature be increased to 550 DEG C it is laggard
Row heat treatment 3h obtains the class stone that the interlayer that seven water potassium phosphate additions are 0.073g adulterates seven water potassium phosphates after heat treatment
Black alkene carbon nitride photocatalyst (CN-2/3KP-3).
The class graphene carbon nitride photocatalyst (CN- of seven water potassium phosphates is adulterated to interlayer prepared by the embodiment of the present application 10
Characterization 2/3KP-3) and to the degradation test process of NO with embodiment 1.The interlayer of the preparation of the embodiment of the present application 10 is calculated
The class graphene carbon nitride photocatalyst (CN-2/3KP-3) for adulterating seven water potassium phosphates is 30.29% to the degradation rate of NO.
Embodiment 11:
(1) 10g urea and seven water potassium phosphates of 0.073g are added in the 50mL crucibles containing 20mL deionized waters, keeps it mixed
It closes, photochemical catalyst presoma is obtained after being uniformly dispersed;
(2) the photochemical catalyst presoma is recrystallized under the conditions of 60 DEG C in an oven, obtains recrystallized product;
(3) by the recrystallized product in Muffle furnace with the heating rate of 15 DEG C/min, temperature be increased to 550 DEG C it is laggard
Row heat treatment 4h obtains the class stone that the interlayer that seven water potassium phosphate additions are 0.073g adulterates seven water potassium phosphates after heat treatment
Black alkene carbon nitride photocatalyst (CN-2/3KP-4).
The class graphene carbon nitride photocatalyst (CN- of seven water potassium phosphates is adulterated to interlayer prepared by the embodiment of the present application 11
Characterization 2/3KP-4) and to the degradation test process of NO with embodiment 1.The interlayer of the preparation of the embodiment of the present application 11 is calculated
The class graphene carbon nitride photocatalyst (CN-2/3KP-4) for adulterating seven water potassium phosphates is 29.81% to the degradation rate of NO.
Table 1 is the degradation rate that each photochemical catalyst degrades to NO in above-described embodiment 1-11:
As it can be seen from table 1 adulterating seven water phosphorus by the interlayer that thermal polymerization urea and seven water potassium phosphates in situ are prepared
The class graphene carbon nitride photocatalyst of sour potassium is to the degradation of NO relative to pure phase class graphene carbon nitride photocatalyst to NO's
For degradation, the former degradation effect significantly improves.Preparation method mild condition provided by the invention, it is easy to operate, it is conducive to it
It mass produces, and also substantially increases the performance of photochemical catalyst by the modification of seven water potassium phosphates.
It is apparent to those skilled in the art although describing the application in a manner of specific embodiment
, in the case where not departing from spirit and scope defined by the appended claims, can to the application into
Row variations and modifications, these change and modification are also included in scope of the present application.
By above technical scheme it is found that this application discloses the class graphene carbonitrides that a kind of interlayer adulterates seven water potassium phosphates
Then urea and seven water phosphorus are added the method includes deionized water to be added in crucible in photochemical catalyst and preparation method thereof
Sour potassium obtains photochemical catalyst presoma;The photochemical catalyst is recrystallized, recrystallized product is obtained;By the recrystallized product
It is heat-treated in Muffle furnace, obtains the class graphene carbon nitride photocatalyst that interlayer adulterates seven water potassium phosphates.The application is real
The class graphene carbon nitride photocatalyst that the interlayer that the preparation method exemplified prepares adulterates seven water potassium phosphates is applied, by by K+
And PO4 3-It is entrained between class graphene carbon nitride layer, can speed up class graphene carbonitride light induced electron and point in hole in this way
From, introduce fault of construction in class graphene carbonitride, promote the promotion of efficiency of light absorption, and then improve class graphene nitridation
The activity of carbon visible light photocatalysis.Interlayer provided by the invention adulterates the class graphene carbon nitride photocatalyst item of seven water potassium phosphates
Part is mild, prepares simply, is suitable for large-scale production.
Those skilled in the art after considering the specification and implementing the invention disclosed here, will readily occur to its of the application
Its embodiment.This application is intended to cover any modification of the application, the variation of purposes or adaptability, these modifications, purposes
Or adaptive change follow the general principle of the application and include the application it is undocumented in the art it is known often
Knowledge or conventional techniques.Description and embodiments are considered only as inertia, and the true scope and spirit of the application are by following
Claim is paid.
It should be understood that the application is not limited to the precision architecture for being described above and being shown in the accompanying drawings, and
And various modifications and changes may be made without departing from the scope thereof.Scope of the present application is only limited by the accompanying claims.
Claims (9)
1. a kind of interlayer adulterates the preparation method of the class graphene carbon nitride photocatalyst of seven water potassium phosphates, which is characterized in that institute
The method of stating includes:
Step S101, deionized water is added in crucible, urea and seven water potassium phosphates is then added, obtain photochemical catalyst forerunner
Body;
Step S102, the photochemical catalyst is recrystallized, obtains recrystallized product;
Step S103, the recrystallized product is heat-treated in Muffle furnace, obtains the class that interlayer adulterates seven water potassium phosphates
Graphene carbon nitride photocatalyst.
2. the method as described in claim 1, which is characterized in that the quality of the seven water potassium phosphate is 0.018-0.110g.
3. method as claimed in claim 2, which is characterized in that the quality of the seven water potassium phosphate is 0.073g.
4. the method as described in claim 1, which is characterized in that the temperature of the recrystallization is 60-80 DEG C.
5. method as claimed in claim 4, which is characterized in that the temperature of the recrystallization is 60 DEG C.
6. the method as described in claim 1, which is characterized in that the temperature of the heat treatment is 550-575 DEG C.
7. method as claimed in claim 6, which is characterized in that the temperature of the heat treatment is 550 DEG C.
8. the method as described in claim 1, which is characterized in that the time of the heat treatment is 2-4h.
9. a kind of interlayer adulterates the class graphene carbon nitride photocatalyst of seven water potassium phosphates, which is characterized in that the interlayer doping
The class graphene carbon nitride photocatalyst of seven water potassium phosphates by described in claim 1-8 any one preparation method prepare and
At;
The class graphene carbon nitride photocatalyst of seven water potassium phosphates of the interlayer doping is under conditions of radiation of visible light to NO's
Removal rate is 27.41%-35.81%.
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Application publication date: 20181023 |