CN108686690A - One kind being based on graphite phase carbon nitride g-C3N4Photochemical catalyst and its preparation method and application - Google Patents
One kind being based on graphite phase carbon nitride g-C3N4Photochemical catalyst and its preparation method and application Download PDFInfo
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- CN108686690A CN108686690A CN201710236277.8A CN201710236277A CN108686690A CN 108686690 A CN108686690 A CN 108686690A CN 201710236277 A CN201710236277 A CN 201710236277A CN 108686690 A CN108686690 A CN 108686690A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 239000003054 catalyst Substances 0.000 title claims abstract description 55
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 54
- 239000010439 graphite Substances 0.000 title claims abstract description 54
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000001257 hydrogen Substances 0.000 claims abstract description 29
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 29
- 238000004519 manufacturing process Methods 0.000 claims abstract description 19
- 230000001699 photocatalysis Effects 0.000 claims abstract description 13
- 238000007146 photocatalysis Methods 0.000 claims abstract description 9
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000015556 catabolic process Effects 0.000 claims abstract description 8
- 238000006731 degradation reaction Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 6
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 4
- 239000000356 contaminant Substances 0.000 claims abstract description 4
- 239000000446 fuel Substances 0.000 claims abstract description 4
- 230000009467 reduction Effects 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 7
- 239000003513 alkali Substances 0.000 claims description 7
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- 229920000877 Melamine resin Polymers 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 5
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical group C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 claims description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 239000005416 organic matter Substances 0.000 claims description 4
- 238000000053 physical method Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 238000002604 ultrasonography Methods 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 3
- 238000006471 dimerization reaction Methods 0.000 claims description 3
- 239000002086 nanomaterial Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 238000000354 decomposition reaction Methods 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 238000012644 addition polymerization Methods 0.000 claims 1
- 229910001873 dinitrogen Inorganic materials 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 13
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000012071 phase Substances 0.000 description 54
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000000634 powder X-ray diffraction Methods 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000006303 photolysis reaction Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 238000004630 atomic force microscopy Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 150000007522 mineralic acids Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical class OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 235000011054 acetic acid Nutrition 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000012612 commercial material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011943 nanocatalyst Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 150000002825 nitriles Chemical group 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 125000004193 piperazinyl group Chemical group 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000003643 water by type 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/39—
-
- B01J35/613—
-
- B01J35/615—
-
- B01J35/647—
-
- B01J35/651—
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
- C01B2203/1088—Non-supported catalysts
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention discloses one kind being based on graphite phase carbon nitride g-C3N4Photochemical catalyst and its preparation method and application.It is described to be based on graphite phase carbon nitride g-C3N4Photochemical catalyst have higher Photocatalyzed Hydrogen Production activity, production hydrogen activity can be higher than 600 μm of olg-1·h-1, significantly improve body phase graphite phase carbon nitride g-C3N4Photocatalyzed Hydrogen Production activity.It is described to be based on graphite phase carbon nitride g-C3N4The preparation method of photochemical catalyst be with body phase g-C3N4G-C is obtained by physical or chemical treatment for raw material3N4Nanometer sheet, then by high-temperature roasting, be prepared with different photocatalytic activities based on graphite phase carbon nitride g-C3N4Photochemical catalyst;The preparation method is simple, the operation cycle is short, it is at low cost, be suitable for large-scale industrial production.It is described to be based on graphite phase carbon nitride g-C3N4Photochemical catalyst can be used for the fields such as photocatalytic water splitting hydrogen manufacturing, photocatalysis carbon dioxide reduction, degradation of fuel, contaminant degradation.
Description
Technical field
The invention mainly relates to nano material and catalyst for preparing hydrogen technical fields, and in particular to one kind is nitrogenized based on graphite-phase
Carbon g-C3N4Photochemical catalyst and its preparation method and application.
Background technology
Since 21st century, with the fast development of modern industrial technology, the fossil fuels quilt such as coal, oil, natural gas
A large amount of consumption, energy crisis are extremely urgent;However, the environmental problem thus brought is even more to grow in intensity.Development and utilization can be held
Continuous clean energy resource has become a kind of irresistible trend.Hydrogen energy source is considered as 21 century most potential cleaning energy
Source, if the non-renewable energy resources such as energy substitute fossil fuels, will benefit entire society.
Kroke et al. is by close Functional Theory calculation shows that with seven piperazine ring (C6N7) it is the graphite that basic structural unit is constructed
Phase carbon nitride (g-C3N4) there is higher chemical stability, and by scientist the study found that having unique electronic energy band knot
Graphite phase carbon nitride (the g-C of structure3N4) visible light can be absorbed, with good Photocatalyzed Hydrogen Production performance;In addition cheap, nothing
The advantages such as poison, abundance, non-metallic components have become the Photocatalyzed Hydrogen Production material of new generation of most application prospect.
Currently, the g-C with photocatalytic activity3N4Preparation method mainly have liquid phase reactor method and solid reaction process.So
And that these methods are usually prepared is body phase g-C3N4, come with some shortcomings place:As specific surface area is smaller, visible absorption
Insufficient, photo-generate electron-hole recombination rate is higher etc., limits its practical application in photocatalysis field.Therefore, how into
The visible light photocatalysis hydrogen production activity that one step improves graphite phase carbon nitride is a urgent problem to be solved.
Invention content
In order to solve the deficiencies in the prior art, the purpose of the present invention is to provide one kind being based on graphite phase carbon nitride g-C3N4
Photochemical catalyst and its preparation method and application.
The photochemical catalyst is to be based on graphite phase carbon nitride g-C3N4Made from roasting, photodissociation aquatic products can be effectively improved
The activity of hydrogen.
Purpose of the present invention is to what is be achieved through the following technical solutions:
One kind being based on graphite phase carbon nitride g-C3N4Photochemical catalyst preparation method, described method includes following steps:
1) by body phase graphite phase carbon nitride g-C3N4It is handled, obtains g-C3N4Nanometer sheet;
2) by above-mentioned steps 1) in obtained g-C3N4Nanometer sheet roasts, and obtains the photochemical catalyst.
According to the present invention, in step 1), the body phase graphite phase carbon nitride g-C3N4Preparation the prior art may be used
In customary preparation methods.
The body phase graphite phase carbon nitride g-C3N4Preparation may include steps of:By graphite phase carbon nitride presoma
It is placed in air or inert gas atmosphere (such as high pure nitrogen, high-purity argon gas), it is fired, that is, the body phase graphite is prepared
Phase carbon nitride g-C3N4。
Preferably, the graphite phase carbon nitride presoma, which is placed in air atmosphere, is roasted.
Preferably, the graphite phase carbon nitride presoma be selected from the organic matter (such as melamine) containing triazine structure,
Or selected from least one of the organic matter (such as cyanamide, cyanamid dimerization, urea) that can generate triazine structure by sudden reaction.
It is further preferred that the graphite phase carbon nitride presoma in melamine, cyanamid dimerization, urea, cyanamide extremely
Few one kind.
Preferably, the calcination temperature of the graphite phase carbon nitride presoma is 500~600 DEG C, and roasting time is 2~5h.
It is further preferred that the calcination temperature of the graphite phase carbon nitride presoma be 550~570 DEG C, roasting time be 3.5~
4.5h (such as 4h).
According to the present invention, in step 1), the body phase graphite phase carbon nitride g-C3N4It can be through physical method or chemistry side
Method processing, obtains g-C3N4Nanometer sheet.
According to the present invention, the physical method includes at least one of mechanical stripping, ultrasonotomography;The chemical method
Including at least one of acid or alkali process.
According to the present invention, the mechanical stripping the specific steps are:By body phase graphite phase carbon nitride g-C3N4It is placed in dispersion solvent
In, mechanical stripping is carried out to it, that is, the g-C is prepared3N4Nanometer sheet.
Preferably, the mechanical stripping can select cell crushing instrument, remove 3~5h.
According to the present invention, the ultrasonotomography the specific steps are:By body phase graphite phase carbon nitride g-C3N4It is placed in dispersion solvent
In, it is disperseed using ultrasound, that is, the g-C is prepared3N4Nanometer sheet.
Preferably, the ultrasonic frequency when ultrasonic disperse is 1000~40000Hz, and the time of ultrasonic disperse is at least
10h。
According to the present invention, the dispersion solvent is selected from least one of water or organic solvent.
According to the present invention, the organic solvent is not particularly limited, and is suitable for reaction system of the present invention.
As illustrative, the organic solvent is selected from low boiling point organic solvent;The low boiling point organic solvent is selected from nitrile solvents (example
Such as acetonitrile);Alcohols solvent (such as methanol, ethyl alcohol, isopropanol);At least one of ketones solvent (such as acetone).
According to the present invention, it is described acid or alkali process the specific steps are:By body phase graphite phase carbon nitride g-C3N4It is placed in acid or alkali
In solution, the g-C is prepared3N4Nanometer sheet.
According to the present invention, there is no particular limitation with its concentration for the selection of the acid or alkali, is suitable for of the present invention
Reaction system.As illustrative, the acid is selected from least one of inorganic acid or organic acid;The inorganic acid choosing
From one or more in hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid;The one kind or more of the organic acid in formic acid, acetic acid, lactic acid
Kind;The alkali is one or more in ammonium hydroxide or other basic solvents.
According to the present invention, the g-C3N4The thickness of nanometer sheet is 1~10nm, preferably 1~6.8nm.
According to the present invention, in step 2), by the g-C3N4Nanometer sheet roasts under the mixed-gas atmosphere of hydrogen and nitrogen
It burns, obtains the photochemical catalyst.
Preferably, the mixed gas is H2(5~15%)/N2The mixed atmosphere of (85~95%);It is further preferred that
The mixed gas is H2(5~10%)/N2The mixed atmosphere of (90~95%).
According to the present invention, in step 2), the calcination temperature is 150~550 DEG C, preferably 300~500 DEG C;It is described
Roasting time is 2~5h, preferably 3.5~4.5h (such as 4h).
The present invention also provides one kind being based on graphite phase carbon nitride g-C3N4Photochemical catalyst, the photochemical catalyst is using upper
What the method for stating was prepared.
According to the present invention, the photochemical catalyst be nano material, grain size be 30~200nm, preferably 60~
160nm;Specific surface area is 30~200cm2/ g, preferably 42.1~100cm2/g。
There is photochemical catalyst of the present invention higher Photocatalyzed Hydrogen Production activity, production hydrogen activity can be higher than 600 μm of ol
g-1·h-1, significantly improve body phase graphite phase carbon nitride g-C3N4Photocatalyzed Hydrogen Production activity.
It is based on graphite phase carbon nitride g-C the present invention also provides above-mentioned3N4Photochemical catalyst application, can be used for photocatalysis
The fields such as water decomposition hydrogen manufacturing, photocatalysis carbon dioxide reduction, degradation of fuel, contaminant degradation.
Beneficial effects of the present invention:
The present invention provides one kind being based on graphite phase carbon nitride g-C3N4Photochemical catalyst and its preparation method and application.Institute
It states and is based on graphite phase carbon nitride g-C3N4Photochemical catalyst have higher Photocatalyzed Hydrogen Production activity, production hydrogen activity can be higher than 600
μmol·g-1·h-1, significantly improve body phase graphite phase carbon nitride g-C3N4Photocatalyzed Hydrogen Production activity.It is described to be based on graphite-phase
Carbonitride g-C3N4The preparation method of photochemical catalyst be with body phase g-C3N4G- is obtained by physical or chemical treatment for raw material
C3N4Nanometer sheet, then by high-temperature roasting, be prepared based on graphite phase carbon nitride g-C3N4Photochemical catalyst;The preparation side
Method is simple, the operation cycle is short, it is at low cost, be suitable for large-scale industrial production.It is described to be based on graphite phase carbon nitride g-C3N4Light
Catalyst can be used for the fields such as photocatalytic water splitting hydrogen manufacturing, photocatalysis carbon dioxide reduction, degradation of fuel, contaminant degradation.
Description of the drawings
Fig. 1 is the X-ray powder diffraction figure for the HCNNS-300 photochemical catalysts that embodiment 1 is prepared.
Fig. 2 is the X-ray powder diffraction figure for the HCNNS-450 photochemical catalysts that embodiment 2 is prepared.
Fig. 3 is the g-C that embodiment 1 is prepared3N4The atomic force microscopy diagram of nanometer sheet.
Fig. 4 is the transmission electron microscope picture for the HCNNS-450 photochemical catalysts that embodiment 2 is prepared.
Fig. 5 is the g-C that embodiment 1 is prepared3N4Nanometer sheet, HCNNS-300 photochemical catalysts and embodiment 2 are prepared
HCNNS-450 photochemical catalysts photodissociation aquatic products hydrogen design sketch.
Specific implementation mode
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.Furthermore, it is to be understood that after having read recorded content of the invention, this field skill
Art personnel can make various changes or modifications the present invention, and such equivalent forms equally fall within limited range of the present invention.
Unless otherwise indicated, the raw materials and reagents used in embodiment are commercial materials.
It is described to be based on graphite phase carbon nitride g-C in the present embodiment3N4Photochemical catalyst be denoted as HCNNS-T;Described in it is indicated
Based on graphite phase carbon nitride g-C3N4What nanometer sheet was prepared after T (unit, DEG C) roastings;Such as:HCNNS-300 is expressed as
The HCNNS photochemical catalysts are g-C3N4It is prepared after 300 DEG C of roastings.
In the present embodiment, the X-ray powder diffraction figure of the photochemical catalyst is by MiniFlex II type powder diffractions
Instrument is characterized.
In the present embodiment, the g-C3N4The thickness of nanometer sheet is characterized with atomic force microscope.
In the present embodiment, the transmission electron microscope picture of the photochemical catalyst is that use transmission Electronic Speculum is characterized.
In the present embodiment, the photochemical catalyst and g-C3N4The photodissociation aquatic products hydrogen design sketch of nanometer sheet is to pass through LabSolar-
III AG photocatalysis on-line analysis system and gas chromatograph GC9790 II are detected.
The testing conditions of the gas chromatograph are:Chromatogram column temperature is 100 DEG C;Post case temperature is 60 DEG C;Conductance cell temperature
Degree is 120 DEG C.
Embodiment 1
The specific preparation method of HCNNS-300 photochemical catalysts
It uses melamine for presoma, roasts in air, 4 hours are kept at 550 DEG C, then Temperature fall, i.e.,
Obtain body phase g-C3N4.Take a small amount of body phase g-C3N4In ethyl alcohol, by cell crushing instrument by body phase g-C3N4Remove into few layer
g-C3N4Nanometer sheet after drying, then puts it into ultrasound in supersonic wave cleaning machine, until being dispersed in water, then again by it
Drying, obtains g-C3N4Nanometer sheet.The g-C that will be obtained3N4Nanometer sheet is in H2(10%)/N2(90%) it is roasted in mixed gas, with 5
DEG C/heating rate of min is warming up to 300 DEG C, kept for 4 hours, then Temperature fall, that is, be prepared HCNNS-300 light and urge
Agent.
Fig. 1 is the X-ray powder diffraction figure for the photochemical catalyst that embodiment 1 is prepared.As shown in Figure 1, the light is urged
Only there are one characteristic diffraction peak, peak position corresponds to the feature diffraction of graphite-phase accumulation (002) crystal face, says agent at 27.67 °
The successful synthesis of graphite phase carbon nitride is illustrated.
Fig. 3 is the g-C being prepared in embodiment 13N4The atomic force microscopy diagram of nanometer sheet.From the figure 3, it may be seen that described
Photochemical catalyst is nanoscale, its thickness is 1.35nm, is equivalent to 4 C-N layers of thickness.
Embodiment 2
The specific preparation method of HCNNS-450 photochemical catalysts
It uses melamine for presoma, roasts in air, 4 hours are kept at 550 DEG C, then Temperature fall, i.e.,
Obtain body phase g-C3N4.Take a small amount of body phase g-C3N4In ethyl alcohol, by cell crushing instrument by body phase g-C3N4Remove into few layer
g-C3N4Nanometer sheet after drying, then puts it into ultrasound in supersonic wave cleaning machine, until being completely dispersed in water, then again
It is baked to, obtains g-C3N4Nanometer sheet.The g-C that will be obtained3N4Nanometer sheet is in H2(10%)/N2(90%) it is roasted in mixed gas
It burns, is warming up to 450 DEG C with the heating rate of 5 DEG C/min, is kept for 4 hours, then Temperature fall, that is, be prepared HCNNS-
450 photochemical catalysts.
Fig. 2 is the X-ray powder diffraction figure for the photochemical catalyst that embodiment 2 is prepared.As shown in Figure 2, the light is urged
Agent only there are one characteristic diffraction peak, compare and deviated to high angle with 27.67 ° in Fig. 1, peak position at 27.76 ° by peak position,
Illustrate that level spacing becomes smaller, but both corresponds to the feature diffraction of graphite-phase accumulation (002) crystal face.
Fig. 4 is the transmission electron microscope picture for the photochemical catalyst that embodiment 2 is prepared.As shown in Figure 4, the photochemical catalyst is
Nanoscale, its edge illustrate that the thickness of the catalyst is very thin close to transparent.
Embodiment 3
The hydrogen yield of photochemical catalyst is tested
It is added 90 ml deionized waters into reaction kettle, 10 milliliters of triethanolamines are made in 10 milligrams of above-described embodiments 1 and 2
Standby obtained photochemical catalyst is added 33 microlitres of chloroplatinic acids (Pt load capacity is 1.56wt%) with liquid-transfering gun, reaction kettle is covered, while stirring
It mixes side and is evacuated in liquid with vacuum pump and no longer generate bubble, 300W xenon lamps (420 optical filters of UV cut) is used to irradiate.Often
Hour sampling is primary, samples six times, by sample into gas chromatograph 9790II, records peak area, calculating hydrogen output and production hydrogen
Rate.As a result referring to Fig. 5.
The result shows that:HCNNS-300 photochemical catalysts in embodiment of the present invention, HCNNS-450 photochemical catalysts and g-C3N4
The hydrogen-producing speed of nanometer sheet is respectively 670.97 μm of olg-1·h-1, 1689.51 μm of olg-1·h-1, 255.66 μm of olg-1·h-1。
Show that the HCNNS-T photochemical catalyst hydrogen production activities prepared in the embodiment of the present invention are far above g- according to the above results
C3N4Nanometer sheet Photocatalyzed Hydrogen Production activity.
More than, embodiments of the present invention are illustrated.But the present invention is not limited to the above embodiments.It is all
Within the spirit and principles in the present invention, any modification, equivalent substitution, improvement and etc. done should be included in the guarantor of the present invention
Within the scope of shield.
Claims (10)
1. one kind being based on graphite phase carbon nitride g-C3N4Photochemical catalyst preparation method, which is characterized in that the method includes such as
Lower step:
1) by body phase graphite phase carbon nitride g-C3N4It is handled, obtains g-C3N4Nanometer sheet;
2) g-C for obtaining step 1)3N4Nanometer sheet roasts, and the photochemical catalyst is prepared.
2. preparation method according to claim 1, which is characterized in that in step 1), the body phase graphite phase carbon nitride
g-C3N4Preparation specifically comprise the following steps:It is (such as high that graphite phase carbon nitride presoma is placed in air or inert gas atmosphere
Pure nitrogen gas, high-purity argon gas) in, it is fired, that is, the body phase graphite phase carbon nitride g-C is prepared3N4。
Preferably, the graphite phase carbon nitride presoma, which is placed in air atmosphere, is roasted.
Preferably, the graphite phase carbon nitride presoma is selected from the organic matter containing triazine structure or selected from can be anti-by addition polymerization
At least one of organic matter of triazine structure should be generated.
Preferably, the graphite phase carbon nitride presoma is selected from least one of melamine, cyanamid dimerization, urea, cyanamide.
3. preparation method according to claim 2, which is characterized in that the calcination temperature of the graphite phase carbon nitride presoma
It it is 500~600 DEG C, roasting time is 2~5h.
Preferably, the calcination temperature of the graphite phase carbon nitride presoma is 550~570 DEG C, and roasting time is 3.5~4.5h
(such as 4h).
4. according to the preparation method described in claim 1-3, which is characterized in that in step 1), the body phase graphite-phase
Carbonitride g-C3N4It can be handled through physical method or chemical method, obtain g-C3N4Nanometer sheet.
Preferably, the physical method includes at least one of mechanical stripping, ultrasonotomography;The chemical method include acid or
At least one of alkali process.
5. according to the preparation method described in claim 1-4, which is characterized in that the mechanical stripping the specific steps are:By body
Phase graphite phase carbon nitride g-C3N4It is placed in dispersion solvent, mechanical stripping is carried out to it, that is, the g-C is prepared3N4Nanometer
Piece.
Preferably, the mechanical stripping can select cell crushing instrument, remove 3~5h.
Preferably, the ultrasonotomography the specific steps are:By body phase graphite phase carbon nitride g-C3N4It is placed in dispersion solvent, utilizes
Ultrasound disperses it, that is, the g-C is prepared3N4Nanometer sheet.
Preferably, the ultrasonic frequency when ultrasonic disperse is 1000~40000Hz, the time at least 10h of ultrasonic disperse.
Preferably, the dispersion solvent is selected from least one of water or organic solvent.
Preferably, it is described acid or alkali process the specific steps are:By body phase graphite phase carbon nitride g-C3N4It is placed in acid or aqueous slkali,
The g-C is prepared3N4Nanometer sheet.
6. according to the preparation method described in claim 1-5, which is characterized in that the g-C3N4The thickness of nanometer sheet be 1~
10nm, preferably 1~6.8nm.
7. according to the preparation method described in claim 1-6, which is characterized in that in step 2), by the g-C3N4Nanometer sheet
It is roasted under the mixed-gas atmosphere of hydrogen and nitrogen, obtains the photochemical catalyst.
Preferably, the mixed gas is H2(5~15%)/N2The mixed atmosphere of (85~95%);It is further preferred that the mixing
Gas is H2(5~10%)/N2The mixed atmosphere of (90~95%).
Preferably, in step 2), the calcination temperature is 150~550 DEG C, preferably 300~500 DEG C;The roasting time
For 2~5h, preferably 3.5~4.5h (such as 4h).
8. one kind being based on graphite phase carbon nitride g-C3N4Photochemical catalyst, which is characterized in that the photochemical catalyst is wanted using right
The method described in 1-7 is asked to be prepared.
9. photochemical catalyst according to claim 8, which is characterized in that the photochemical catalyst is nano material, grain size
For 30~200nm, preferably 60~160nm, specific surface area is 30~200cm2/ g, preferably 42.1~100cm2/g。
10. described in claim 8 or 9 based on graphite phase carbon nitride g-C3N4Photochemical catalyst application, can be used for photocatalysis
The fields such as water decomposition hydrogen manufacturing, photocatalysis carbon dioxide reduction, degradation of fuel, contaminant degradation.
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