CN107398292A - A kind of preparation method of selenides/graphite phase carbon nitride photocatalysis composite - Google Patents
A kind of preparation method of selenides/graphite phase carbon nitride photocatalysis composite Download PDFInfo
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- CN107398292A CN107398292A CN201710366797.0A CN201710366797A CN107398292A CN 107398292 A CN107398292 A CN 107398292A CN 201710366797 A CN201710366797 A CN 201710366797A CN 107398292 A CN107398292 A CN 107398292A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 239000010439 graphite Substances 0.000 title claims abstract description 61
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 61
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 150000003346 selenoethers Chemical class 0.000 title claims abstract description 42
- 239000002131 composite material Substances 0.000 title claims abstract description 37
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 36
- 238000007146 photocatalysis Methods 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 45
- -1 cobaltous selenides Chemical class 0.000 claims abstract description 21
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000011941 photocatalyst Substances 0.000 claims abstract description 11
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 8
- 239000011669 selenium Substances 0.000 claims abstract description 7
- 150000002815 nickel Chemical class 0.000 claims abstract 2
- 239000013153 zeolitic imidazolate framework Substances 0.000 claims description 20
- 239000000843 powder Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 239000004570 mortar (masonry) Substances 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 21
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 21
- 239000001257 hydrogen Substances 0.000 abstract description 21
- 238000004519 manufacturing process Methods 0.000 abstract description 12
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 150000001875 compounds Chemical class 0.000 abstract description 7
- 239000003426 co-catalyst Substances 0.000 abstract description 5
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- 230000009467 reduction Effects 0.000 abstract description 2
- 230000008021 deposition Effects 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- 239000010457 zeolite Substances 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 description 2
- OQUOOEBLAKQCOP-UHFFFAOYSA-N nitric acid;hexahydrate Chemical compound O.O.O.O.O.O.O[N+]([O-])=O OQUOOEBLAKQCOP-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 229920000877 Melamine resin Polymers 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000007233 catalytic pyrolysis Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 230000002079 cooperative effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 210000004709 eyebrow Anatomy 0.000 description 1
- 210000000720 eyelash Anatomy 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 210000004209 hair Anatomy 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000003020 moisturizing effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- 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
-
- 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 present invention relates to a kind of preparation method of selenides/graphite phase carbon nitride photocatalysis composite.It is formed by selenides nanoparticle deposition on lamellar graphite phase carbon nitride surface, and selenides is using the carrying capacity mass percent that selenium element is counted as 2.5 12.5% in the composite photocatalyst material；Described selenides is two cobaltous selenides, two selenizing nickel composites.Photocatalysis composite provided by the invention can effectively increase the compound of reaction contact area, reduction light induced electron and hole, so that two cobaltous selenides, two nickelous selenides effectively raise the Photocatalyzed Hydrogen Production performance of graphite phase carbon nitride as co-catalyst.Therefore, this selenides/graphite phase carbon nitride photocatalysis composite is with a wide range of applications in fields such as photocatalysis, the energy and environment.
Description
Technical field
The present invention relates to a kind of preparation method of selenides/graphite phase carbon nitride photocatalysis composite, belong to material
Preparation and field of energy environment.
Background technology
The development of today's society be unable to do without the energy, and the existing energy depends on the burning of fossil fuel mostly.But fossil fires
Material has the problem of rare surplus, secondary pollution while the energy is provided for us, and therefore, development clean energy resource is compeled in eyebrow
Eyelash.In numerous clean energy resourcies, Hydrogen Energy is of great interest.Production hydrogen technology mainly has oil pyrolysis, electrolysis water, light at present
Catalytic pyrolysis water etc..But the method for oil pyrolysis is still restricted by fossil energy, the method for electrolysis water then consumes substantial amounts of electric energy,
This low cost production hydrogen approach of Gu Guangcuihualiexieshui turns into optimal selection.It is various to urge to improve the efficiency of photocatalytic cleavage water
Agent is introduced into reaction system.Graphite phase carbon nitride prepares cheap, chemical stability preferably and with great due to it
Researching value, however, graphite phase carbon nitride is simultaneously there is the shortcomings that photo-generate electron-hole recombination rate is fast, specific surface area is small,
It is unfavorable for its application in light-catalyzed reaction, can be effectively improved and urged with graphite phase carbon nitride progress compound using co-catalyst
The production hydrogen efficiency of agent.Conventional co-catalyst usually contains precious metal element, such as platinum, improves the cost of reaction.This hair
Transition metal selenium that is bright to have abandoned precious metal element, being generated using ZIF-67CoNi zeolitic imidazolate framework materials as raw material
The cobaltous selenide of compound two, two nickelous selenides have the property that particle diameter is small, specific surface area is big, and because selenium atom radius is big, electronegativity is low,
Small to the outer-shell electron active force of cobalt, nickel, these electronics can promote the progress of redox reaction, and be nitrogenized in conjunction with graphite-phase
Carbon photocatalyst material produces cooperative effect, so that the cobaltous selenide of transition metal selenides two, two nickelous selenides are as co-catalyst
Compound material is advantageous to the transmission of electronics in Photocatalyzed Hydrogen Production reaction with graphite phase carbon nitride, while decreases electronics-sky
Cave is compound.But in existing research, this composite is not yet prepared with the inventive method and not in Photocatalyzed Hydrogen Production side
Applied in face.
The content of the invention
The goal of the invention of the present invention is the provision of a kind of system of selenides/graphite phase carbon nitride photocatalysis composite
Preparation Method.The preparation method has the features such as preparation technology is simple, easily controllable, synthesis cost is low.The selenizing of gained nanoscale two
Cobalt, two nickelous selenide cocatalyst materials load in graphite phase carbon nitride, high for Photocatalyzed Hydrogen Production catalytic activity.
A kind of preparation method of selenides/graphite phase carbon nitride photocatalysis composite, it is by two cobaltous selenides, two selenizings
Nano nickel particles are deposited on lamellar graphite phase carbon nitride surface and formed, and described selenides is that two cobaltous selenides, two nickelous selenides are compound
Thing, the carrying capacity mass percent that selenides is counted using selenium element in the composite photocatalyst material is 2.5-12.5%.
A kind of preparation method of selenides/graphite phase carbon nitride photocatalysis composite, comprises the following steps：
（1）Prepare ZIF-67CoNi zeolitic imidazolate framework materials；
（2）Prepare graphite phase carbon nitride powder；
（3）ZIF-67CoNi zeolitic imidazolate framework materials, selenium powder and graphite phase carbon nitride powder are mixed by a certain percentage
Close, agate mortar grinding certain time, in N2After being calcined under atmosphere, selenides/graphite phase carbon nitride composite photo-catalyst is obtained
Material；
By such scheme, step（3）The calcination process is warming up to 300 ~ 350 DEG C for 5 ~ 10 DEG C/min and is incubated 3 ~ 5 hours.
Two cobaltous selenides of the present invention, two nickelous selenides are using selenium powder and ZIF-67CoNi zeolitic imidazolate framework materials as raw material system
It is standby, a kind of selenides/graphite phase carbon nitride photocatalysis composite can be obtained using method of calcination, this method can ensure to receive
The cobaltous selenide of meter level two, two nickelous selenides load in graphite phase carbon nitride.Thus obtained selenides/graphite phase carbon nitride complex light
Catalyst material can effectively increase the compound of reaction contact area, reduction light induced electron and hole, so that two cobaltous selenides,
Two nickelous selenides effectively raise the Photocatalyzed Hydrogen Production performance of graphite phase carbon nitride as co-catalyst.Therefore, this selenides/
Graphite phase carbon nitride photocatalysis composite is with a wide range of applications in fields such as photocatalysis, the energy and environment.
Preparation method provided by the invention and its obtained material have advantages below：
（1）Preparation technology provided by the invention is simple, easy to operate, and synthesis cost is low, and resulting materials heat endurance and chemistry are steady
It is qualitative good, it is easily stored, and choose different load percentages and can control its performance；
（2）Selenides prepared by the present invention/graphite phase carbon nitride photocatalysis composite efficiently solves single graphite-phase nitrogen
The problem of photo-generate electron-hole of change carbon material is high to recombination rate, improves light-catalyzed reaction speed, further increases production hydrogen
Efficiency.
Brief description of the drawings
Fig. 1 is the X ray powder of selenides/graphite phase carbon nitride composite photocatalyst material prepared by different embodiments of the invention
Last diffraction detection figure.
Fig. 2 is selenides/graphite phase carbon nitride photocatalysis composite scanning electron microscope (SEM) photograph in the embodiment of the present invention 2.
Fig. 3 is selenides/graphite phase carbon nitride photocatalysis composite elementary analysis figure in the embodiment of the present invention 2.
Fig. 4 is selenides/graphite phase carbon nitride composite photo-catalyst, single graphite prepared by different embodiments of the invention
Phase carbon nitride material visible-light photochemical catalyzing hydrogen-producing speed comparison diagram.
Embodiment
The embodiment of the present invention is described in detail below.
Specific embodiment 1
ZIF-67CoNi zeolitic imidazolate framework materials and graphite phase carbon nitride powder are mixed, make ZIF-67CoNi zeolites
Mass ratio shared by imidazate framework material is 2.5%, the selenium of the quality such as addition and ZIF-67CoNi zeolitic imidazolate framework materials
Powder, after grinding 15min in agate mortar, in N2Under atmosphere, with 5 DEG C/min be warming up to 350 DEG C insulation 2 hours after, natural cooling
To room temperature.
Specific embodiment 2
ZIF-67CoNi zeolitic imidazolate framework materials and graphite phase carbon nitride powder are mixed, make ZIF-67CoNi zeolites
Mass ratio shared by imidazate framework material is 5%, the selenium powder of the quality such as addition and ZIF-67CoNi zeolitic imidazolate framework materials,
After grinding 15min in agate mortar, in N2Under atmosphere, with 5 DEG C/min be warming up to 350 DEG C insulation 2 hours after, naturally cool to
Room temperature.
Specific embodiment 3
ZIF-67CoNi zeolitic imidazolate framework materials and graphite phase carbon nitride powder are mixed, make ZIF-67CoNi zeolites
Mass ratio shared by imidazate framework material is 10%, the selenium powder of the quality such as addition and ZIF-67CoNi zeolitic imidazolate framework materials,
After grinding 15min in agate mortar, in N2Under atmosphere, with 5 DEG C/min be warming up to 350 DEG C insulation 2 hours after, naturally cool to
Room temperature.
Specific embodiment 4
ZIF-67CoNi zeolitic imidazolate framework materials and graphite phase carbon nitride powder are mixed, make ZIF-67CoNi zeolites
Mass ratio shared by imidazate framework material is 12.5%, the selenium of the quality such as addition and ZIF-67CoNi zeolitic imidazolate framework materials
Powder, after grinding 15min in agate mortar, in N2Under atmosphere, with 5 DEG C/min be warming up to 350 DEG C insulation 2 hours after, natural cooling
To room temperature.
Photocatalysis Decomposition aquatic products hydrogen is tested
Aquatic products hydrogen effect is catalytically decomposed under visible light to investigate selenides/graphite phase carbon nitride photocatalysis composite, this
Inventor is tested its visible light photocatalysis H2-producing capacity by the following method.Test process is as follows：Photocatalyzed Hydrogen Production is tested
Carried out in photocatalytic activity evaluation on-line analysis system, before reaction starts, condenser system is opened, by vavuum pump exclusion system
Air.300W xenon lamp is as light source.It is as follows in typical Photocatalyzed Hydrogen Production experiment process：By selenides ground 30mg/
Graphite phase carbon nitride photocatalysis composite is added in 50mL 20vol% triethanolamine solution, and utilizes ultrasonic machine ultrasound
15min is allowed to form uniform suspension.Then, 40min vacuum pumpings are carried out to reaction system system, to drain air.
Then, reactor is placed on agitator lasting stirring and illumination 4h, makes photochemical catalyst in the dispersed shape of experimentation moisturizing
State and uniform illumination, the content of the hydrogen in gaseous sample are analyzed by gas chromatograph.Separately nitrogenized with single graphite-phase
Carbon material makees catalyst, forms control experiment.
The preparation of ZIF-67CoNi zeolitic imidazolate framework materials：
Cabaltous nitrate hexahydrate is dissolved in methanol, and 2-methylimidazole is dissolved in methanol and is added in above-mentioned metal salt solution,
The amount ratio of the material of cabaltous nitrate hexahydrate and 2-methylimidazole is 1：40,1 h is stirred at room temperature, centrifugation, obtains ZIF- after drying
67Co zeolitic imidazolate framework materials, gained ZIF-67Co zeolitic imidazolate framework materials take certain mass to be dissolved in methanol, add
Into Nickelous nitrate hexahydrate methanol solution, ensure ZIF-67Co zeolitic imidazolate framework materials with Nickelous nitrate hexahydrate mol ratio about
For 1：1,5min is centrifuged under ultrasonic 30min, 8000r/min, ZIF-67CoNi zeolitic imidazolate framework materials are obtained after drying.
The preparation of single graphite phase carbon nitride material：
In N2Under atmosphere, melamine is warming up to 550 DEG C with 10 DEG C/min and is incubated 4 hours, room temperature is naturally cooled to, obtains
Graphite phase carbon nitride bulk material, grinding 15min obtains powder in agate mortar；
Embodiments of the present invention are elaborated above., can be just but the present invention is not limited to above-mentioned embodiment
Made a variety of changes in true theoretical foundation.
The selenides obtained to specific embodiment 1,2,3,4/graphite phase carbon nitride photocatalysis composite carries out X ray
Powder diffraction detects, and obtain XRD as shown in Figure 1 goes out intensity and graphite phase carbon nitride simulation at 13 °, 27 ° and two of peak position
Crystal XRD data go out peak position, intensity is coincide substantially, while have the appearance of selenides diffraction maximum again, show synthesized by the method
Complex maintains graphite phase carbon nitride this component, while introduces selenides.
The selenides obtained to specific embodiment 2/graphite phase carbon nitride photocatalysis composite is scanned Electronic Speculum inspection
Survey, obtain selenides as shown in Figure 2/graphite phase carbon nitride photocatalysis composite scanning electron microscope (SEM) photograph.It can be seen by Fig. 2
Go out, selenides/graphite phase carbon nitride photocatalysis composite has bigger ratio with respect to graphite phase carbon nitride photocatalyst material
Surface area, layer block surface have been combined closely nano-particle of the diameter tens to hundreds of.
The selenides graphite phase carbon nitride photocatalysis composite obtained to specific embodiment 2 carries out elementary analysis, obtains
It is as seen from Figure 3, real to the elementary analysis figure of selenides as shown in Figure 3/graphite phase carbon nitride photocatalysis composite
Apply selenides/graphite phase carbon nitride photocatalysis composite that example 2 obtains and contain the elements such as C, N, O, Ni, Co, Se.
Selenides/the graphite phase carbon nitride obtained to single graphite phase carbon nitride material and specific embodiment 1,2,3,4
Photocatalysis composite carries out the contrast of visible light photocatalysis decomposition water hydrogen-producing speed, obtains graphite-phase nitridation as shown in Figure 4
Carbon and selenides/graphite phase carbon nitride photocatalysis composite hydrogen-producing speed comparison diagram.Single graphite prepared by the present invention
Phase carbon nitride photocatalyst material hydrogen-producing speed is up to 0.29 μm of olh-1, the selenides/graphite phase carbon nitride of the invention prepared
Photocatalysis composite hydrogen-producing speed is up to 14.1 μm of olh-1, about single graphite phase carbon nitride photocatalyst material production
48 times of hydrogen speed.
Claims (3)
1. the preparation method of a kind of selenides/graphite phase carbon nitride photocatalysis composite, it is characterised in that two cobaltous selenides, two
Nickelous selenide is prepared using selenium powder and ZIF-67CoNi zeolitic imidazolate framework materials as raw material, and the two is in lamellar graphite phase carbon nitride
Surface is combined closely, the carrying capacity mass percent that selenides is counted using selenium element in the composite photocatalyst material as 2.5-12.5%,
Described selenides is two cobaltous selenides, two selenizing nickel composites.
2. the preparation method of selenides according to claim 1/graphite phase carbon nitride photocatalysis composite, its feature
It is, comprises the following steps：
（1）Prepare ZIF-67CoNi zeolitic imidazolate framework materials；
（2）Prepare graphite phase carbon nitride powder；
（3）ZIF-67CoNi zeolitic imidazolate framework materials, selenium powder and graphite phase carbon nitride powder are mixed by a certain percentage
Close, agate mortar grinding certain time, in N2After being calcined under atmosphere, selenides/graphite phase carbon nitride composite photo-catalyst is obtained
Material.
3. the preparation method of selenides according to claim 2/graphite phase carbon nitride photocatalysis composite, it is special
Sign is, step（3）The calcination process is warming up to 300 ~ 350 DEG C for 5 ~ 10 DEG C/min and is incubated 3 ~ 5 hours.
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| CN107983387A (en) * | 2017-12-05 | 2018-05-04 | 福州大学 | A kind of preparation method of carbonitride/selenic acid bismuth composite material and application |
| CN108374179A (en) * | 2018-02-07 | 2018-08-07 | 浙江大学 | A kind of preparation method and application of the compound nitrogen-doped carbon material of two cobaltous selenide of Fe2O3 doping |
| CN109999879A (en) * | 2019-04-17 | 2019-07-12 | 吉林大学 | A kind of lamellar graphite phase carbon nitride photochemical catalyst and preparation method thereof of selenium auxiliary |
| CN110385146A (en) * | 2019-08-08 | 2019-10-29 | 上海大学 | A kind of Ni0.85Se/PDA/g-C3N4Composite photo-catalyst and its application |
| CN110404574A (en) * | 2019-07-26 | 2019-11-05 | 华东理工大学 | The method of hydrogen production by water decomposition catalyst and preparation method thereof and hydrogen production by water decomposition |
| CN110853937A (en) * | 2019-11-29 | 2020-02-28 | 江苏理工学院 | Preparation method of nickel-cobalt bimetallic selenide/carbon composite for supercapacitor |
| CN111790441A (en) * | 2020-07-03 | 2020-10-20 | 扬州大学 | Polyaniline loaded copper-iron catalyst material and preparation method and application thereof |
| CN111905788A (en) * | 2020-07-11 | 2020-11-10 | 吉林化工学院 | NiSe/g-C3N4Preparation method and application of photocatalyst |
| CN113277484A (en) * | 2020-02-19 | 2021-08-20 | 松山湖材料实验室 | High-performance alkaline zinc battery cathode material and preparation method thereof |
| CN114471625A (en) * | 2021-11-30 | 2022-05-13 | 东北农业大学 | Preparation method and application of nickel selenide/tungsten trioxide/graphene photocatalytic composite material |
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| CN109999879A (en) * | 2019-04-17 | 2019-07-12 | 吉林大学 | A kind of lamellar graphite phase carbon nitride photochemical catalyst and preparation method thereof of selenium auxiliary |
| CN110404574A (en) * | 2019-07-26 | 2019-11-05 | 华东理工大学 | The method of hydrogen production by water decomposition catalyst and preparation method thereof and hydrogen production by water decomposition |
| CN110385146A (en) * | 2019-08-08 | 2019-10-29 | 上海大学 | A kind of Ni0.85Se/PDA/g-C3N4Composite photo-catalyst and its application |
| CN110853937A (en) * | 2019-11-29 | 2020-02-28 | 江苏理工学院 | Preparation method of nickel-cobalt bimetallic selenide/carbon composite for supercapacitor |
| CN113277484A (en) * | 2020-02-19 | 2021-08-20 | 松山湖材料实验室 | High-performance alkaline zinc battery cathode material and preparation method thereof |
| CN113277484B (en) * | 2020-02-19 | 2023-04-07 | 松山湖材料实验室 | High-performance alkaline zinc battery cathode material and preparation method thereof |
| CN111790441A (en) * | 2020-07-03 | 2020-10-20 | 扬州大学 | Polyaniline loaded copper-iron catalyst material and preparation method and application thereof |
| CN111790441B (en) * | 2020-07-03 | 2022-10-25 | 扬州大学 | Polyaniline loaded copper-iron catalyst material and preparation method and application thereof |
| CN111905788A (en) * | 2020-07-11 | 2020-11-10 | 吉林化工学院 | NiSe/g-C3N4Preparation method and application of photocatalyst |
| CN114471625A (en) * | 2021-11-30 | 2022-05-13 | 东北农业大学 | Preparation method and application of nickel selenide/tungsten trioxide/graphene photocatalytic composite material |
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