CN110385146A - A kind of Ni0.85Se/PDA/g-C3N4Composite photo-catalyst and its application - Google Patents
A kind of Ni0.85Se/PDA/g-C3N4Composite photo-catalyst and its application Download PDFInfo
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- CN110385146A CN110385146A CN201910731656.3A CN201910731656A CN110385146A CN 110385146 A CN110385146 A CN 110385146A CN 201910731656 A CN201910731656 A CN 201910731656A CN 110385146 A CN110385146 A CN 110385146A
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 32
- 229920001690 polydopamine Polymers 0.000 claims abstract description 79
- 239000002131 composite material Substances 0.000 claims abstract description 37
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 31
- 239000003054 catalyst Substances 0.000 claims abstract description 30
- 239000002105 nanoparticle Substances 0.000 claims abstract description 27
- 238000002360 preparation method Methods 0.000 claims abstract description 23
- 239000001257 hydrogen Substances 0.000 claims abstract description 20
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 20
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000006303 photolysis reaction Methods 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 239000002135 nanosheet Substances 0.000 claims abstract description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 81
- 239000011669 selenium Substances 0.000 claims description 80
- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 claims description 18
- 239000012530 fluid Substances 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 18
- 238000002604 ultrasonography Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- 238000005303 weighing Methods 0.000 claims description 11
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims description 10
- 229960001149 dopamine hydrochloride Drugs 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 8
- 239000004202 carbamide Substances 0.000 claims description 8
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 6
- 239000012279 sodium borohydride Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000006116 polymerization reaction Methods 0.000 claims description 5
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 4
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 230000015556 catabolic process Effects 0.000 claims description 3
- 238000006731 degradation reaction Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000000975 dye Substances 0.000 claims description 3
- 238000005984 hydrogenation reaction Methods 0.000 claims description 3
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 claims description 3
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 3
- 229910052724 xenon Inorganic materials 0.000 claims description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 2
- 238000005286 illumination Methods 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims 2
- 229910052757 nitrogen Inorganic materials 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract description 6
- 239000003426 co-catalyst Substances 0.000 abstract description 6
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 abstract description 3
- 238000011068 loading method Methods 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 11
- 239000003795 chemical substances by application Substances 0.000 description 9
- 150000001875 compounds Chemical class 0.000 description 8
- 238000006555 catalytic reaction Methods 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 4
- 239000004570 mortar (masonry) Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 230000003139 buffering effect Effects 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 2
- 230000015843 photosynthesis, light reaction Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000013019 agitation Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical group OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 229960003638 dopamine Drugs 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052961 molybdenite Inorganic materials 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- -1 nickelous selenide Chemical class 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000003504 photosensitizing agent Substances 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/28—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of the platinum group metals, iron group metals or copper
-
- B01J35/39—
-
- 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
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- 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
- C01B2203/1047—Group VIII metal catalysts
- C01B2203/1052—Nickel or cobalt catalysts
- C01B2203/1058—Nickel catalysts
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
-
- 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 a kind of Ni0.85Se/PDA/g‑C3N4Composite photo-catalyst and its preparation method and application, the composite photocatalyst material have loaded poly-dopamine (PDA) and Ni using azotized carbon nano piece as carrier, in azotized carbon nano on piece0.85Se nano particle.The composite catalyst has many advantages, such as that environmental-friendly, photo-generated carrier separative efficiency is high, visible absorption region is big；Raw material is easy to get simultaneously, and preparation process is simple, and operation is easy, and has repeatability and higher photocatalytic activity well.By optimizing Ni0.85The loading capacity of Se co-catalyst, hydrogen generating quantity is 3.17 times higher than purity nitrogen carbon nanosheet, compares PDA/g-C3N4Composite catalyst is 2.4 times high.Therefore, there is good application prospect in photodissociation aquatic products hydrogen field.
Description
Technical field
The invention belongs to polynary semiconductor composite technical field more particularly to a kind of Ni0.85Se/PDA/g-C3N4It is multiple
Light combination catalyst and its application in photodissociation aquatic products hydrogen direction.
Background technique
Hydrogen Energy is a kind of clean energy resource.Hydrogen Energy, Ke Yitong are converted by sustainable solar energy using semiconductor catalyst
When reduce that fossil fuel is exhausted and problem of environmental pollution.Graphite phase carbon nitride (g-C3N4) it is the first metal-free semiconductor
Polymer, nontoxic because of its visible absorption, low cost, in light the advantages that excellent chemical and thermal stability and environment friendly
Catalysis energy conversion field causes great concern.But since carbonitride specific surface area is smaller, photo-generated carrier is easily compound,
Visible light region edge absorption (absorbing wavelength < 455), electric conductivity is poor etc. to limit carbonitride in the reality in photolysis water hydrogen field
Border application.
Recent research indicate that by being to improve light induced electron and hole in nitridation carbon surface load carbon material or co-catalyst
Low separation efficiency and improve visible absorption, to realize the most simple of effective photodissociation aquatic products hydrogen activity, most efficient method it
One.Noble metal platinum has proven to a kind of outstanding co-catalyst, but it there are scarcity of resources and it is expensive the disadvantages of.
In recent years, Transition-metal dichalcogenide, such as MoS2, NiS, CoS, MoSe2Deng, be widely used as substitute platinum gC3N4's
Co-catalyst.
Dopamine be it is a kind of come biological micromolecule, under weak basic condition can spontaneous polymerization on any surface generate it is tight
Close poly-dopamine (PDA) coating.PDA itself does not have the ability of photodissociation aquatic products hydrogen as a kind of carbon material.But due to
PDA has outstanding light capture ability, good photoconduction and catechol group abundant, effectively can shift and separate light
Raw carrier.Recent studies have shown that carbonitride can be improved after PDA is used to modify carbonitride as polymer nanocomposite coating
Photocatalytic activity.
Summary of the invention
In order to overcome defect present in the prior art, the present invention provides a kind of Ni0.85Se/PDA/g-C3N4Tri compound
Photochemical catalyst is used for photolysis water hydrogen and degradation of organic dyes, reduces catalysis cost to reach, improves the purpose of catalytic efficiency.
To achieve the above object, the present invention adopts the following technical scheme:
The first aspect of the invention is to provide a kind of Ni0.85Se/PDA/g-C3N4Composite photo-catalyst, the complex light are urged
Agent material loads poly-dopamine PDA and Ni using azotized carbon nano piece as carrier, in the azotized carbon nano on piece0.85Se nanometers
Grain.
Further, Ni in the composite photo-catalyst0.85The load capacity of Se nano particle is 3wt%~20wt%.More
Preferably, Ni0.85The load capacity of Se nano particle is 8wt%-12wt%；Most preferably, Ni0.85The load capacity of Se nano particle
For 10wt%.
Further, the preparation step of the composite photo-catalyst includes:
Dopamine hydrochloride is added by after azotized carbon nano piece and alkalescent Tris-HCl buffer ultrasonic mixing in step 1),
Strong stirring 15~25 hours；
Step 2) is by a certain amount of Ni0.85Se nano particle and alkalescent Tris-HCl buffer ultrasonic mixing, obtain
Ni0.85Se homogenizing fluid；By the Ni0.85Se homogenizing fluid is added dropwise in the solution that the step 1) obtains, and is stirred 6~10 hours；It produces
For object by filtering, drying obtains Ni after grinding0.85Se/PDA/g-C3N4Three-element composite photocatalyst.
Further, the preparation step of the azotized carbon nano piece includes: using urea as raw material, by calcining and hot soarfing
From preparing azotized carbon nano piece.
Further, the Ni0.85The preparation step of Se nano particle includes: with selenium powder, sodium borohydride, and nickel chloride is original
Material prepares Ni by solvent thermal reaction0.85Se nano particle.
Further, the dosage of Dopamine hydrochloride is the 8~15% of azotized carbon nano tablet quality in the step 1),；More
Preferably, the dosage of Dopamine hydrochloride is the 10% of azotized carbon nano tablet quality, and polymerization time is 20 hours.
Further, the pH of the alkalescent Tris-HCl buffer is 8~9；More preferably, 8.5 pH.
Further, in the step 2), mixing time is 8 hours.
Further, the preparation step of the composite photo-catalyst specifically includes:
Step 1: the urea of predetermined amount is weighed, with the heating rate of 4~6 DEG C/min, calcine 2 at 520~580 DEG C~
6h after being cooled to room temperature, is ground into fine powder；Fine powder is forged at 470~530 DEG C with the heating rate of 4~6 DEG C/min again
1~3h is burnt, obtains azotized carbon nano piece after being cooled to room temperature；
Step 2: weighing the selenium powder and sodium borohydride of predetermined amount, be put into a certain amount of DMF, stir 0.5~2h；It adds
The Nickel dichloride hexahydrate of predetermined amount continues 20~40min of stirring, and 18~30h is reacted at 140~180 DEG C；Obtained black produces
Object ethyl alcohol and deionized water are washed repeatedly, and dry 8~16 hours, grind into powder obtain Ni at 50~70 DEG C0.85Se
Nano particle.
Step 3: azotized carbon nano piece prepared by the step 1 of predetermined amount is weighed, is put into alkalescent Tris-HCl buffer,
Ultrasound makes its homogeneous；The Dopamine hydrochloride for adding predetermined amount, is vigorously stirred 15~25h；
Step 4: weighing Ni prepared by the step 2 of predetermined amount0.85Se nano particle is put into alkalescent Tris-HCl buffer
In, interval 0.5~2min of ultrasound obtains homogenizing fluid；Homogenizing fluid is added drop-wise in the solution of step 3,6~10h is vigorously stirred；
Step 5: for the product that step 4 obtains by repeatedly filtering, drying obtains poly-dopamine PDA and Ni after grinding0.85Se
The ternary complex catalyst Ni of load0.85Se/PDA/g-C3N4。
Further, the preparation step of the composite photo-catalyst specifically includes:
Step 1: weighing the urea of predetermined amount, with the heating rate of 5 DEG C/min, calcine 4h at 550 DEG C, be cooled to room
Wen Hou is ground into fine powder；Fine powder is calcined into 2h at 500 DEG C with the heating rate of 5 DEG C/min again, is obtained after being cooled to room temperature
To azotized carbon nano piece；
Step 2: weighing the selenium powder and sodium borohydride of predetermined amount, be put into a certain amount of DMF, stir 1h；It adds predetermined
The Nickel dichloride hexahydrate of amount continues to stir 30min, react for 24 hours at 160 DEG C；Obtained black product ethyl alcohol and deionization
Water washs repeatedly, and dry 12 hours, grind into powder obtain Ni at 60 DEG C0.85Se nano particle.
Step 3: weighing azotized carbon nano piece prepared by the step 1 of predetermined amount, be put into the Tris-HCl buffer of pH=8.5
In, ultrasound makes its homogeneous；The Dopamine hydrochloride for adding predetermined amount, is vigorously stirred 20h；
Step 4: weighing Ni prepared by the step 2 of predetermined amount0.85Se nano particle, the Tris-HCl for being put into pH=8.5 are slow
In fliud flushing, interval ultrasound 1min obtains homogenizing fluid；Homogenizing fluid is added drop-wise in the solution of step 3,8h is vigorously stirred；
Step 5: for the product that step 4 obtains by repeatedly filtering, drying obtains poly-dopamine PDA and Ni after grinding0.85Se
The ternary complex catalyst Ni of load0.85Se/PDA/g-C3N4。
The second aspect of the invention is to provide a kind of any above-mentioned Ni0.85Se/PDA/g-C3N4Photochemical catalyst is in photodissociation
Application in aquatic products hydrogen or degradation of organic dyes.
Further, the method for the photodissociation aquatic products hydrogen include the following steps: to weigh the composite photo-catalyst of predetermined amount with
The triethanolamine aqueous solution of predetermined amount mixes, ultrasound；It vacuumizes mixed solution is closed, carries out light with xenon lamp simulated solar irradiation
According to prepare hydrogen.
Compared with prior art, the present invention has the advantages that by adopting the above technical scheme
(1) raw material of the present invention is easy to get, and preparation process is simple, and operation is easy, nontoxic, and has repeatability well, has
Conducive to the promotion and application of technique.
(2) in the present invention, the compound azotized carbon nano piece that not only significantly improves of poly-dopamine (PDA) is in visible region
The absorption region and photo-generated carrier separative efficiency in domain, while binder can be served as in its polymerization process and closely fix selenium
Change nano nickel particles.
(3) Ni in the present invention0.85Se/PDA/g-C3N4Three-element composite photocatalyst has excellent photodissociation aquatic products hydrogen activity.
By optimizing Ni0.85The loading capacity of Se loads the Ni of 10% mass ratio0.85The three-way catalyst of Se nano particle has best
Catalytic activity, H2Yield is 3.17 times higher than purity nitrogen carbon nanosheet, compares PDA/g-C3N4Composite catalyst is 2.4 times high.
Detailed description of the invention
Fig. 1 is Ni in one embodiment of the invention0.85Se/PDA/g-C3N4The preparation flow schematic diagram of ternary complex catalyst；
Fig. 2 is the 10Ni of 3 preparations according to an embodiment of the present invention0.85Se/PDA/g-C3N4The TEM of catalyst schemes；
Fig. 3 be according to an embodiment of the present invention with CN prepared by comparative example, PDA/CN and different Ni0.85The ternary of Se load capacity
The XRD diagram of catalyst；
Fig. 4 is Ni obtained in one embodiment of the invention0.85The XRD diagram of Se；
Fig. 5 is according to an embodiment of the present invention 3 and CN, PDA/CN and 10Ni prepared by comparative example0.85Se-PDA/CN catalysis
The Solid fluorescene spectrum figure of agent；
Fig. 6 is according to an embodiment of the present invention 3 and CN, PDA/CN and 10Ni prepared by comparative example0.85Se-PDA/CN catalysis
The solid ultraviolet spectrogram of agent；
Fig. 7 is the CN, PDA/CN and different Ni prepared according to an embodiment of the present invention with comparative example0.85The ternary of Se load capacity
The production hydrogen figure of catalyst progress photocatalytic water.
Specific embodiment
The present invention relates to a kind of Ni0.85Se/PDA/g-C3N4Composite photo-catalyst and its preparation method and application, this is compound
Photochemical catalyst material loads poly-dopamine PDA and Ni0.85Se using azotized carbon nano piece as carrier, in the azotized carbon nano on piece
Nano particle；Wherein, Ni in the composite photo-catalyst0.85The load capacity of Se nano particle is 3wt%~20wt%.Following realities
Apply Ni in example0.85Se/PDA/g-C3N4The preparation flow of ternary complex catalyst is as shown in Figure 1.
With reference to the accompanying drawings and examples, further description of the specific embodiments of the present invention.Following embodiment is only
For clearly illustrating technical solution of the present invention, and not intended to limit the protection scope of the present invention.
Experimental method in following embodiments is unless otherwise specified conventional method；Original as used in the following examples
Material, reagent etc. can obtain unless otherwise specified from public commercial source.
Embodiment 1
The present embodiment is Ni0.85Se load capacity is the Ni of 3wt%0.85Se/PDA/g-C3N4The one of Three-element composite photocatalyst
The preferable preparation method of kind comprising following steps:
Step 1: about 30 grams of urea is weighed in 50 milliliters of crucibles with cover, with the heating rate of 5 DEG C/min, 550
4h is calcined at DEG C, after being cooled to room temperature, with mortar grinder at fine powder.Fine powder is put into crucible not with cover again, with 5 DEG C/
The heating rate of min calcines 2h at 500 DEG C, obtains azotized carbon nano piece after being cooled to room temperature.
Step 2: weighing 0.316g selenium powder, 0.190g sodium borohydride is put into the DMF of 65mL, magnetic agitation 1h.It adds
0.808g nickel chloride (six hydrations), continues to stir 30min.It is transferred into the reaction kettle of 100mL, is reacted at 160 DEG C
24h.Obtained black product ethyl alcohol and deionized water are washed repeatedly, dry 12 hours at 60 DEG C, with mortar grinder at
Powder obtains Ni0.85Se nano particle.
Step 3: precise 0.1g carbonitride is put into 40mL Tris-HCl buffer (pH=8.5), in ultrasonic wave
With the frequency ultrasound 0.5h of 100Hz in cleaner.10mg Dopamine hydrochloride is added, 20h is vigorously stirred.
Step 4: Ni obtained in precise 3mg step 20.85Se nano particle is put into 20mL Tris-HCl buffer
(pH=8.5) in, with ultrasonic stick with the power intervals ultrasound 1min of 300W, homogenizing fluid is obtained.Homogenizing fluid is added drop-wise to step 3
In solution, it is vigorously stirred 8h.
Step 5: for product by repeatedly filtering, drying obtains 3%wt Ni after grinding0.85The tri compound catalysis of Se load
Agent is named as 3Ni0.85Se-PDA/CN。
Embodiment 2
The present embodiment is Ni0.85Se load capacity is the Ni of 5wt%0.85Se/PDA/g-C3N4The one of Three-element composite photocatalyst
The preferable preparation method of kind comprising following steps:
Step 1~3 are same as Example 1.
Step 4: Ni obtained in precise 5mg step 20.85Se nano particle is put into 20mL Tris-HCl buffer
(pH=8.5) in, with ultrasonic stick with the power intervals ultrasound 1min of 300W, homogenizing fluid is obtained.Homogenizing fluid is added drop-wise to step 3
In solution, it is vigorously stirred 8h.
Step 5: for product by repeatedly filtering, drying obtains 5%wt Ni after grinding0.85The tri compound catalysis of Se load
Agent is named as 5Ni0.85Se-PDA/CN。
Embodiment 3
The present embodiment is Ni0.85Se load capacity is the Ni of 10wt%0.85Se/PDA/g-C3N4Three-element composite photocatalyst
A kind of preferable preparation method comprising following steps:
Step 1~3 are same as Example 1.
Step 4: Ni obtained in precise 10mg step 20.85Se nano particle is put into 20mL Tris-HCl buffering
In liquid (pH=8.5), with ultrasonic stick with the power intervals ultrasound 1min of 300W, homogenizing fluid is obtained.Homogenizing fluid is added drop-wise to step 3
Solution in, be vigorously stirred 8h.
Step 5: for product by repeatedly filtering, drying obtains 10%wt Ni after grinding0.85The tri compound of Se load is urged
Agent is named as 10Ni0.85Se-PDA/CN。
Embodiment 4
The present embodiment is Ni0.85Se load capacity is the Ni of 20wt%0.85Se/PDA/g-C3N4Three-element composite photocatalyst
A kind of preferable preparation method comprising following steps:
Step 1~3 are same as Example 1.
Step 4: Ni obtained in precise 20mg step 20.85Se nano particle is put into 20mL Tris-HCl buffering
In liquid (pH=8.5), with ultrasonic stick with the power intervals ultrasound 1min of 300W, homogenizing fluid is obtained.Homogenizing fluid is added drop-wise to step 3
Solution in, be vigorously stirred 8h.
Step 5: for product by repeatedly filtering, drying obtains 20%wt Ni after grinding0.85The tri compound of Se load is urged
Agent is named as 20Ni0.85Se-PDA/CN。
Comparative example 1
This comparative example is the preparation method of non-loaded azotized carbon nano piece comprising following steps:
The urea for weighing about 30 grams, with the heating rate of 5 DEG C/min, is forged in 50 milliliters of crucibles with cover at 550 DEG C
4h is burnt, after being cooled to room temperature, with mortar grinder at fine powder.Fine powder is put into crucible not with cover again, with the liter of 5 DEG C/min
Warm rate calcines 2h at 500 DEG C, obtains azotized carbon nano piece after being cooled to room temperature, is named as CN.
Comparative example 2
This comparative example is only to load the preparation method of the azotized carbon nano piece of PDA comprising following steps:
Step 1: about 30 grams of urea is weighed in 50 milliliters of crucibles with cover, with the heating rate of 5 DEG C/min, 550
4h is calcined at DEG C, after being cooled to room temperature, with mortar grinder at fine powder.Fine powder is put into crucible not with cover again, with 5 DEG C/
The heating rate of min calcines 2h at 500 DEG C, obtains azotized carbon nano piece after being cooled to room temperature.
Step 2: precise 0.1g carbonitride is put into 40mL Tris-HCl buffer (pH=8.5), in ultrasonic wave
With the frequency ultrasound 0.5h of 100Hz in cleaner.10mg Dopamine hydrochloride is added, vigorous magnetic stirs 20h.Add 20mL
Tris-Hcl buffer (pH=8.5) continues to stir 8h.For product by filtering, drying obtains poly-dopamine/nitridation after grinding
Carbon composite catalytic agent, is named as PDA/CN.
Performance characterization embodiment
The embodiment of the present invention 1~4 is taken, catalyst prepared by comparative example 1~2 characterize, specifically included:
(1)10Ni0.85The transmission electron microscope of Se-PDA/CN characterizes
Specifically, Fig. 2 shows the 10Ni prepared according to embodiment 30.85Se-PDA/CN Three-element composite photocatalyst it is saturating
Penetrate electron microscope, it is seen that PDA coating uniform is coated on stratiform g-C3N4On, the Ni of many black0.85Se nano particle is deposited over it
Surface.
(2) CN, PDA/CN and different Ni0.85The X-ray diffraction of the three-way catalyst of Se load capacity characterizes
Specifically, Fig. 3 clearly show Examples 1 to 4, CN, PDA/CN and difference prepared by comparative example 1~2
Ni0.85The XRD diagram of the powder of the X-ray diffraction characterization of the three-way catalyst of Se load capacity；It can be seen that all XRD spectrums show
Similar figure, the characteristic peak with most typical graphite phase carbon nitride.All ternary complex catalyst samples in Fig. 3
PDA or Ni is not detected in XRD spectrum0.85Se, this may be the Ni due to load0.85Se nano-particle content is low, PDA is crystallized
It spends lower.
(3)Ni0.85The X-ray diffraction of Se characterizes
Specifically, Fig. 4 clearly show the Ni prepared according to embodiment 10.85The XRD diagram of the powder of Se；As it can be seen that actual measurement
XRD spectrum is perfectly matched with standard card, to show prepared Ni0.85The purity is high of Se.
(4) CN, PDA/CN and 10Ni0.85The solid fluorescence of Se-PDA/CN characterizes
Specifically, Fig. 5 shows the 10Ni prepared according to embodiment 30.85Se-PDA/CN Three-element composite photocatalyst and right
The Solid fluorescene spectrum figure of CN prepared by ratio 1~2 and PDA/CN, it is seen that 10Ni0.85Se-PDA/CN catalyst fluorescent emission
Intensity is minimum, shows that the separative efficiency of the catalyst photo-generated carrier is most fast.
(5) CN, PDA/CN and 10Ni0.85It is characterized outside the solid violet of Se-PDA/CN
Specifically, the solid ultraviolet spectrogram of CN and PDA/CN prepared by Fig. 6, it is seen that the load of PDA significantly improves
Light absorption of the CN in visible light region (λ > 420nm), while 10wt%Ni0.85The load of Se further increases PDA/CN's
Visible absorption.
Application Example
This application embodiment will carry out photocatalytic water as photochemical catalyst according to Examples 1 to 4, comparative example 1~2, with preparation
Hydrogen, specifically includes the following steps:
Step 1, it weighs the photochemical catalyst of 50mg and is added in glass reaction bottle；
Step 2, the triethanolamine aqueous solution of 50mL 10%, ultrasound a period of time are added into the glass reaction bottle；
Step 3, which is connected to the multi-channel reaction device of connection gas chromatograph, it is closed to vacuumize, it uses
300W xenon lamp simulated solar irradiation carries out illumination, to prepare hydrogen.
Referring to Fig. 7, it is seen then that a kind of Ni0.85Se-PDA/CN trielement composite material is as photochemical catalyst, and triethanolamine is made
Under conditions of the sacrifice agent of hole, photocatalytic activity is improved.By optimizing the loading capacity of nickelous selenide co-catalyst,
10Ni0.85Se-PDA/CN has best catalytic activity, and hydrogen generating quantity is 3.17 times higher than purity nitrogen carbon nanosheet, compares PDA/
CN composite catalyst is 2.4 times high.It can be seen that Ni prepared by the embodiment of the present invention0.85Se/PDA/g-C3N4Three-way catalyst
Photocatalytic activity it is higher, and its be not necessarily to any photosensitizer and platinum co-catalyst under conditions of can by water decomposition be hydrogen
Gas.
Specific embodiments of the present invention are described in detail above, but it is only used as example, the present invention is not intended to limit
In particular embodiments described above.To those skilled in the art, the equivalent modifications and replace that any couple of present invention carries out
In generation, is also all among scope of the invention.Therefore, without departing from the spirit and scope of the invention made by equal transformation and repair
Change, all should be contained within the scope of the invention.
Claims (9)
1. a kind of Ni0.85Se/PDA/g-C3N4Composite photo-catalyst, which is characterized in that the composite photo-catalyst material is with carbonitride
Nanometer sheet is carrier, loads poly-dopamine PDA and Ni in the azotized carbon nano on piece0.85Se nano particle.
2. a kind of Ni according to claim 10.85Se/PDA/g-C3N4Composite photo-catalyst, which is characterized in that described
Ni in composite photo-catalyst0.85The load capacity of Se nano particle is 3wt%~20wt%.
3. a kind of Ni according to claim 10.85Se/PDA/g-C3N4Composite photo-catalyst, which is characterized in that described multiple
The preparation step of light combination catalyst includes:
Dopamine hydrochloride, strength is added by after azotized carbon nano piece and alkalescent Tris-HCl buffer ultrasonic mixing in step 1)
Stirring 15~25 hours；
Step 2) is by a certain amount of Ni0.85Se nano particle and alkalescent Tris-HCl buffer ultrasonic mixing, obtain Ni0.85Se
Homogenizing fluid；By the Ni0.85Se homogenizing fluid is added dropwise in the solution that the step 1) obtains, and is stirred 6~10 hours；Product passes through
It filters, drying obtains Ni after grinding0.85Se/PDA/g-C3N4Three-element composite photocatalyst.
4. a kind of Ni according to claim 30.85Se/PDA/g-C3N4Composite photo-catalyst, which is characterized in that the nitrogen
The preparation step for changing carbon nanosheet includes: using urea as raw material, by calcining and hot soarfing from preparing azotized carbon nano piece.
5. a kind of Ni according to claim 30.85Se/PDA/g-C3N4Composite photo-catalyst, which is characterized in that described
Ni0.85The preparation step of Se nano particle includes: with selenium powder, sodium borohydride, and nickel chloride is raw material, by solvent thermal reaction, system
Standby Ni0.85Se nano particle.
6. a kind of Ni according to claim 30.85Se/PDA/g-C3N4Composite photo-catalyst, which is characterized in that described
The dosage of Dopamine hydrochloride is the 8~15% of azotized carbon nano tablet quality in step 1), and polymerization pH is 8~9, polymerization time 15
~25h.
7. a kind of Ni according to claim 30.85Se/PDA/g-C3N4Composite photo-catalyst, which is characterized in that described multiple
The preparation step of light combination catalyst specifically includes:
Step 1: the urea of predetermined amount is weighed, with the heating rate of 4~6 DEG C/min, 2~6h is calcined at 520~580 DEG C, to
After being cooled to room temperature, it is ground into fine powder；Again by fine powder with the heating rate of 4~6 DEG C/min, calcine 1 at 470~530 DEG C~
3h obtains azotized carbon nano piece after being cooled to room temperature；
Step 2: weighing the selenium powder and sodium borohydride of predetermined amount, be put into a certain amount of DMF, stir 0.5~2h；It adds predetermined
The Nickel dichloride hexahydrate of amount continues 20~40min of stirring, and 18~30h is reacted at 140~180 DEG C；Obtained black product is used
Ethyl alcohol and deionized water are washed repeatedly, and dry 8~16 hours, grind into powder obtain Ni at 50~70 DEG C0.85Se nanometers
Particle.
Step 3: weighing azotized carbon nano piece prepared by the step 1 of predetermined amount, be put into alkalescent Tris-HCl buffer, ultrasound
Make its homogeneous；The Dopamine hydrochloride for adding predetermined amount, is vigorously stirred 15~25h；
Step 4: weighing Ni prepared by the step 2 of predetermined amount0.85Se nano particle is put into alkalescent Tris-HCl buffer,
0.5~2min of ultrasound of having a rest, obtains homogenizing fluid；Homogenizing fluid is added drop-wise in the solution of step 3,6~10h is vigorously stirred；
Step 5: for the product that step 4 obtains by repeatedly filtering, drying obtains poly-dopamine PDA and Ni after grinding0.85Se load
Ternary complex catalyst Ni0.85Se/PDA/g-C3N4。
8. a kind of such as Ni according to any one of claims 1 to 70.85Se/PDA/g-C3N4Composite photo-catalyst is in photodissociation aquatic products
Application in hydrogen or degradation of organic dyes.
9. application according to claim 8, which is characterized in that the method for the photodissociation aquatic products hydrogen includes the following steps: to claim
The composite photo-catalyst of predetermined amount is taken to mix with the triethanolamine aqueous solution of predetermined amount, ultrasound；It vacuumizes mixed solution is closed,
Illumination is carried out with xenon lamp simulated solar irradiation, to prepare hydrogen.
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