CN108816262A - A kind of preparation method of nickel oxide-nitridation carbon composite photocatalyst - Google Patents
A kind of preparation method of nickel oxide-nitridation carbon composite photocatalyst Download PDFInfo
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- CN108816262A CN108816262A CN201810378248.XA CN201810378248A CN108816262A CN 108816262 A CN108816262 A CN 108816262A CN 201810378248 A CN201810378248 A CN 201810378248A CN 108816262 A CN108816262 A CN 108816262A
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- 239000002131 composite material Substances 0.000 title claims abstract description 24
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 18
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 18
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 55
- 239000007788 liquid Substances 0.000 claims abstract description 34
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910000480 nickel oxide Inorganic materials 0.000 claims abstract description 23
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims abstract description 23
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004202 carbamide Substances 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 12
- SHWZFQPXYGHRKT-FDGPNNRMSA-N (z)-4-hydroxypent-3-en-2-one;nickel Chemical compound [Ni].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O SHWZFQPXYGHRKT-FDGPNNRMSA-N 0.000 claims abstract 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000006185 dispersion Substances 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 14
- 229910052593 corundum Inorganic materials 0.000 claims description 10
- 239000010431 corundum Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- 238000003760 magnetic stirring Methods 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 2
- XUCNUKMRBVNAPB-UHFFFAOYSA-N fluoroethene Chemical compound FC=C XUCNUKMRBVNAPB-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 10
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 8
- 239000001257 hydrogen Substances 0.000 abstract description 8
- 239000002105 nanoparticle Substances 0.000 abstract description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 7
- 239000003054 catalyst Substances 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000000428 dust Substances 0.000 abstract description 4
- 230000001699 photocatalysis Effects 0.000 abstract description 4
- 238000007146 photocatalysis Methods 0.000 abstract description 4
- 230000004048 modification Effects 0.000 abstract description 3
- 238000012986 modification Methods 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 239000011858 nanopowder Substances 0.000 abstract description 2
- 238000001354 calcination Methods 0.000 abstract 1
- BMGNSKKZFQMGDH-FDGPNNRMSA-L nickel(2+);(z)-4-oxopent-2-en-2-olate Chemical compound [Ni+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O BMGNSKKZFQMGDH-FDGPNNRMSA-L 0.000 description 21
- 239000000463 material Substances 0.000 description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 229960004424 carbon dioxide Drugs 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002737 fuel gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 230000000243 photosynthetic effect Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000007704 wet chemistry method Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/39—
-
- B01J35/393—
-
- B01J35/396—
Abstract
A kind of nickel oxide-carbonitride high-efficiency composite photocatalyst preparation method obtains nitridation carbon dust first by calcining urea under certain condition；Then by ultrasonic disperse at a certain temperature, nitridation carbon dust is dispersed in the tert-butyl alcohol of certain volume, a certain amount of nickel acetylacetonate is added into mixed liquor again later, is stirred by ultrasonic disperse and continuing magnetic force, obtains pioneer's liquid.Solvent thermal reaction is carried out finally by pioneer's liquid, obtains the azotized carbon nano powder that surface modification has nickel oxide nanoparticle.It is an advantage of the invention that：(1) it is compared with other methods, this method simple process, is not necessarily to complex device and harsh environment, it is at low cost；(2) this method controls nickel oxide nanoparticle in the load capacity of nitridation carbon surface in which can be convenient；(3) nickel oxide prepared by this method-nitridation carbon composite photocatalyst has excellent photocatalysis hydrogen production ability, and after loading nickel oxide nanoparticle, catalyst hydrogen manufacturing amount is significantly improved.
Description
Technical field
The invention belongs to visible-light photocatalyst field of material technology, and in particular to a kind of nickel oxide-carbonitride complex light
The preparation method of catalyst.
Background technique
Since the mankind enter industrial society, fossil fuel is widely used in industrial production, and in burning, release is a large amount of dirty
Object is contaminated, atmosphere, water source and other natural environments are caused and seriously affected.At the same time, fossil fuel is non-renewable resources,
As continuous exploitation utilizes, energy crisis also at the mankind must in face of the problem of.In order to solve this problem, nothing is developed
The renewable and clean energy resource of pollution is just at inevitable choice.By inspiration photosynthetic in nature, scientific research personnel is dedicated to seeking
It looks for, construct high-efficiency photocatalysis material, and split water into hydrogen and oxygen under sunlight using them, or by carbon dioxide
It is converted to the fuel gas such as methane, methanol or liquid, to obtain clean renewable energy.Light can be absorbed in semiconductor material
Son, and electron-hole pair is inspired inside it, these electron-hole pairs can be used to complete to decompose water or progress two
The reduction reaction of carbonoxide.Therefore, the photochemical catalyst based on semiconductor material is always a research hotspot.In initial research
In, this wide bandgap semiconductor of titanium dioxide is to study a kind of material the most extensive.But the forbidden band of titanium dioxide
Width is up to 3.2eV, can not effectively utilize sunlight.Therefore, the wide high efficiency photocatalyst of optical response range how is obtained just
At the emphasis of research.
Carbon nitride material is a kind of nonmetallic compound semiconductor, and for its forbidden bandwidth in 2.7eV or so, can respond can
It is light-exposed.The research history that carbonitride is can trace back to 1834, but until 2009, graphite phase carbon nitride (g-C3N4)
Excellent H2-producing capacity is just reported under visible light, henceforth, g-C3N4Just before being received as a kind of non-metal optical catalyst
The concern not having.g-C3N4With visible-light absorptivity is high, stability is good, cheap and easy to get and advantages of environment protection, Ke Yiying
For a variety of reaction systems such as photolysis water hydrogen, reduction carbon dioxide.But the g-C of pure phase3N4There are carriers to answer for photochemical catalyst
It closes seriously, the inherent shortcomings such as quantum efficiency is low cause its photocatalysis performance not high.Therefore, how g-C is improved3N4Photocatalytic activity
Just at the most important thing.Commonly method of modifying includes：Nonmetal doping, metal-doped, to be compounded to form hetero-junctions, noble metal heavy
Product, surface sensitization, combined polymerization modification etc..
Summary of the invention
The purpose of the present invention is to provide a kind of nickel oxide-nitridation carbon composite photocatalyst preparation methods, make in this way
Standby composite photo-catalyst produces hydrogen rate and greatly improves.
In order to achieve the above objectives, the technical solution adopted by the present invention is that：
1) it takes 36g urea to be put into corundum crucible, places it in 24~48h of heat treatment in 80 DEG C of baking oven, then cover
550 DEG C are risen to the heating rate of 4.6 DEG C/min in Muffle furnace after lid, isothermal holding 3h is naturally cooling to room temperature, obtains
Yellow powdery solid C3N4, stand-by after grinding；
2) C of 184mg is added into screw socket bottle3N4Then powder adds the 30mL tert-butyl alcohol, in 35~45 DEG C of ultrasounds point
It dissipates and obtains dispersion liquid A；Then the nickel acetylacetonate of 64-514mg mM is added into dispersion liquid A, then in 35~45 DEG C of ultrasonic disperses
It is uniformly placed on 65~75 DEG C of magnetic stirring apparatus and stirs evenly to obtain mixed liquid B；
3) reaction kettle with polytetrafluoroethyllining lining is preheated to 60~70 DEG C, is then rapidly transferred to mixed liquid B
In polytetrafluoroethyllining lining, rapid sealing reaction kettle is simultaneously transferred them in the baking oven that temperature is 100 DEG C, then sets baking oven temperature
Degree is 190~210 DEG C, when temperature rises to setting temperature, starts timing, 12~30h of isothermal reaction；
4) after solvent thermal reaction, baking oven power supply is closed, after reaction kettle is cooled to room temperature with baking oven, opens reaction
Mixed liquor is centrifuged 15min by kettle under the rate of 10000~12000rpm, and with the vacuum after washes of absolute alcohol at 60 DEG C
C is dried to obtain in drying box3N4- NiO composite sample.
The urea of the step 1) fills corundum crucible.
The ultrasonic disperse time of the step 2) is 0.5~1h.
Step 2) the magnetic agitation time be 12~for 24 hours.
Step 3) the reaction kettle polytetrafluoroethyllining lining volume is 50mL.
Step 4) the vacuum drying time be 12~for 24 hours.
The present invention proposes a kind of simple and effective method, and in nitridation supported on carbon surface nickel oxide nanoparticle, nickel oxide is received
Rice grain is uniformly supported on nitridation carbon surface, on the one hand it can effectively capture the hole of illumination lower semiconductor generation, resistance
Hinder the compound of electron-hole pair, on the other hand, nickel oxide can also effectively promote the formation of active site, thus
Substantially increase the utilization of visible light.It is demonstrated experimentally that Photocatalyzed Hydrogen Production rate greatly improves after load nickel oxide nanoparticle.
The present invention mainly uses wet chemistry method to prepare nickel oxide-nitridation carbon composite photocatalyst, first by certain
Under the conditions of calcine urea, obtain nitridation carbon dust；Then by ultrasonic disperse at a certain temperature, nitridation carbon dust is dispersed in
In the tert-butyl alcohol of certain volume, a certain amount of nickel acetylacetonate is added into mixed liquor again later, by ultrasonic disperse and continues
Magnetic agitation obtains pioneer's liquid.Solvent thermal reaction is carried out finally by pioneer's liquid, obtaining surface modification has nickel oxide nano
The azotized carbon nano powder of grain.Whole process has experimental facilities and environmental requirement low, and technical process is simple, reproducible to wait spies
Point.The size and load capacity of the easily controllable nickel oxide nanoparticle of method proposed by the present invention, such as by increasing in pioneer's liquid
The additive amount of nickel acetylacetonate can effectively increase the load capacity and particle size of nickel oxide nanoparticle.Importantly, should
Nickel oxide prepared by method-nitridation carbon composite photocatalyst has excellent photocatalysis hydrogen production ability, loads nickel oxide nano
After particle, catalyst hydrogen manufacturing amount is significantly improved.
Detailed description of the invention
Fig. 1 is with C containing different proportion3N4Through 210 DEG C of solvent thermal reactions, gained is compound for 24 hours with pioneer's liquid B of nickel acetylacetonate
The transmission electron microscope photo of sample.(a) pure C3N4；(b) molar ratio C3N4:Ni(acac)2=8:1；(c) molar ratio C3N4:Ni
(acac)2=4:1；(d) molar ratio C3N4:Ni(acac)2=2:1.
Fig. 2 is nickel oxide-nitridation carbon composite photocatalyst X-ray diffraction pattern of different nickel oxide loaded amounts, * in figure
C is corresponded respectively to the diffraction maximum of # mark3N4And NiO.
Specific embodiment
The present invention is described in further details with reference to the accompanying drawings and embodiments.
Embodiment 1：
1) it places it in 80 DEG C of baking oven and is heat-treated for 24 hours after taking 36g urea to fill corundum crucible, after then closeing the lid
550 DEG C are risen to the heating rate of 4.6 DEG C/min in Muffle furnace, isothermal holding 3h is naturally cooling to room temperature, obtains yellow powder
Last shape solid C3N4, stand-by after grinding；
2) C of 184mg is added into screw socket bottle3N4Then powder adds the 30mL tert-butyl alcohol, in 40 DEG C of ultrasonic disperses
0.5h obtains dispersion liquid A；Then the nickel acetylacetonate of 64mg is added into dispersion liquid A, then in 40 DEG C of ultrasonic disperse 0.5h postpositions
Mixed liquid B is obtained in stirring 12h on 70 DEG C of magnetic stirring apparatus；
3) reaction kettle with polytetrafluoroethyllining lining that volume is 50mL is preheated to 70 DEG C, then rapidly by mixed liquor
B is transferred in polytetrafluoroethyllining lining, and rapid sealing reaction kettle simultaneously transfers them in the baking oven that temperature is 100 DEG C, is then set
Determining oven temperature is 210 DEG C, when temperature rises to setting temperature, starts timing, isothermal reaction is for 24 hours；
4) after solvent thermal reaction, baking oven power supply is closed, after reaction kettle is cooled to room temperature with baking oven, opens reaction
Mixed liquor is centrifuged 15min by kettle under the rate of 10000rpm, and with after washes of absolute alcohol in 60 DEG C of vacuum oven
Dry 12h obtains C3N4- NiO composite sample.
Embodiment 2：
1) it places it in 80 DEG C of baking oven and is heat-treated for 24 hours after taking 36g urea to fill corundum crucible, after then closeing the lid
550 DEG C are risen to the heating rate of 4.6 DEG C/min in Muffle furnace, isothermal holding 3h is naturally cooling to room temperature, obtains yellow powder
Last shape solid C3N4, stand-by after grinding；
2) C of 184mg is added into screw socket bottle3N4Then powder adds the 30mL tert-butyl alcohol, in 40 DEG C of ultrasonic disperses
0.5h obtains dispersion liquid A；Then the nickel acetylacetonate of 128mg is added into dispersion liquid A, then in 40 DEG C of ultrasonic disperse 0.5h postpositions
Mixed liquid B is obtained in stirring 12h on 70 DEG C of magnetic stirring apparatus；
3) reaction kettle with polytetrafluoroethyllining lining that volume is 50mL is preheated to 70 DEG C, then rapidly by mixed liquor
B is transferred in polytetrafluoroethyllining lining, and rapid sealing reaction kettle simultaneously transfers them in the baking oven that temperature is 100 DEG C, is then set
Determining oven temperature is 210 DEG C, when temperature rises to setting temperature, starts timing, isothermal reaction is for 24 hours；
4) after solvent thermal reaction, baking oven power supply is closed, after reaction kettle is cooled to room temperature with baking oven, opens reaction
Mixed liquor is centrifuged 15min by kettle under the rate of 10000rpm, and with after washes of absolute alcohol in 60 DEG C of vacuum oven
Dry 12h obtains C3N4- NiO composite sample.
Embodiment 3：
1) it places it in 80 DEG C of baking oven and is heat-treated for 24 hours after taking 36g urea to fill corundum crucible, after then closeing the lid
550 DEG C are risen to the heating rate of 4.6 DEG C/min in Muffle furnace, isothermal holding 3h is naturally cooling to room temperature, obtains yellow powder
Last shape solid C3N4, stand-by after grinding；
2) C of 184mg is added into screw socket bottle3N4Then powder adds the 30mL tert-butyl alcohol, in 40 DEG C of ultrasonic disperses
0.5h obtains dispersion liquid A；Then the nickel acetylacetonate of 257mg is added into dispersion liquid A, then in 40 DEG C of ultrasonic disperse 0.5h postpositions
Mixed liquid B is obtained in stirring 12h on 70 DEG C of magnetic stirring apparatus；
3) reaction kettle with polytetrafluoroethyllining lining that volume is 50mL is preheated to 70 DEG C, then rapidly by mixed liquor
B is transferred in polytetrafluoroethyllining lining, and rapid sealing reaction kettle simultaneously transfers them in the baking oven that temperature is 100 DEG C, is then set
Determining oven temperature is 210 DEG C, when temperature rises to setting temperature, starts timing, isothermal reaction is for 24 hours；
4) after solvent thermal reaction, baking oven power supply is closed, after reaction kettle is cooled to room temperature with baking oven, opens reaction
Mixed liquor is centrifuged 15min by kettle under the rate of 10000rpm, and with after washes of absolute alcohol in 60 DEG C of vacuum oven
Dry 12h obtains C3N4- NiO composite sample.
Embodiment 4：
1) it places it in 80 DEG C of baking oven and is heat-treated for 24 hours after taking 36g urea to fill corundum crucible, after then closeing the lid
550 DEG C are risen to the heating rate of 4.6 DEG C/min in Muffle furnace, isothermal holding 3h is naturally cooling to room temperature, obtains yellow powder
Last shape solid C3N4, stand-by after grinding；
2) C of 184mg is added into screw socket bottle3N4Then powder adds the 30mL tert-butyl alcohol, in 40 DEG C of ultrasonic disperses
0.5h obtains dispersion liquid A；Then the nickel acetylacetonate of 128mg is added into dispersion liquid A, then in 40 DEG C of ultrasonic disperse 0.5h postpositions
Mixed liquid B is obtained for 24 hours in stirring on 70 DEG C of magnetic stirring apparatus；
3) reaction kettle with polytetrafluoroethyllining lining that volume is 50mL is preheated to 70 DEG C, then rapidly by mixed liquor
B is transferred in polytetrafluoroethyllining lining, and rapid sealing reaction kettle simultaneously transfers them in the baking oven that temperature is 100 DEG C, is then set
Determining oven temperature is 210 DEG C, when temperature rises to setting temperature, starts timing, isothermal reaction is for 24 hours；
4) after solvent thermal reaction, baking oven power supply is closed, after reaction kettle is cooled to room temperature with baking oven, opens reaction
Mixed liquor is centrifuged 15min by kettle under the rate of 10000rpm, and with after washes of absolute alcohol in 60 DEG C of vacuum oven
Dry 12h obtains C3N4- NiO composite sample.
Fig. 1 is with C containing different proportion3N4Through 210 DEG C of solvent thermal reactions, gained is compound for 24 hours with pioneer's liquid B of nickel acetylacetonate
The transmission electron microscope photo of sample.(a) pure C3N4；(b) molar ratio C3N4:Ni(acac)2=8:1；(c) molar ratio C3N4:Ni
(acac)2=4:1；(d) molar ratio C3N4:Ni(acac)2=2:1.As it can be seen that the ratio with nickel acetylacetonate is continuously increased, oxygen
The load capacity for changing nano nickel particles is continuously increased.It is contemplated that the amount for continuing growing nickel acetylacetonate can continue to improve oxidation
The load capacity of nickel.
Fig. 2 is nickel oxide-nitridation carbon composite photocatalyst X-ray diffraction pattern of different nickel oxide loaded amounts, * in figure
C is corresponded respectively to the diffraction maximum of # mark3N4And NiO.As it can be seen that occurring wider oxygen in diffraction pattern after nickel acetylacetonate is added
Change nickel diffraction maximum, it was demonstrated that generate nickel oxide nanoparticle.Moreover, the ratio with nickel acetylacetonate is continuously increased, nickel oxide
Diffraction maximum constantly enhance load capacity and be continuously increased, illustrate that the content of nickel oxide is continuously increased.This conclusion is mutually reflected with Fig. 1
Card.
Embodiment 5：
1) it is placed it in after taking 36g urea to fill corundum crucible in 80 DEG C of baking oven and is heat-treated 36h, after then closeing the lid
550 DEG C are risen to the heating rate of 4.6 DEG C/min in Muffle furnace, isothermal holding 3h is naturally cooling to room temperature, obtains yellow powder
Last shape solid C3N4, stand-by after grinding；
2) C of 184mg is added into screw socket bottle3N4Then powder adds the 30mL tert-butyl alcohol, in 35 DEG C of ultrasonic disperse 1h
Obtain dispersion liquid A；Then the nickel acetylacetonate of 514mg is added into dispersion liquid A, then is placed on 65 DEG C in 35 DEG C of ultrasonic disperse 1h
Magnetic stirring apparatus on stir for 24 hours mixed liquid B；
3) reaction kettle with polytetrafluoroethyllining lining that volume is 50mL is preheated to 60 DEG C, then rapidly by mixed liquor
B is transferred in polytetrafluoroethyllining lining, and rapid sealing reaction kettle simultaneously transfers them in the baking oven that temperature is 100 DEG C, is then set
Determining oven temperature is 190 DEG C, when temperature rises to setting temperature, starts timing, isothermal reaction 12h；
4) after solvent thermal reaction, baking oven power supply is closed, after reaction kettle is cooled to room temperature with baking oven, opens reaction
Mixed liquor is centrifuged 15min by kettle under the rate of 11000rpm, and with after washes of absolute alcohol in 60 DEG C of vacuum oven
Drying obtains C for 24 hours3N4- NiO composite sample.
Embodiment 6：
1) it is placed it in after taking 36g urea to fill corundum crucible in 80 DEG C of baking oven and is heat-treated 48h, after then closeing the lid
550 DEG C are risen to the heating rate of 4.6 DEG C/min in Muffle furnace, isothermal holding 3h is naturally cooling to room temperature, obtains yellow powder
Last shape solid C3N4, stand-by after grinding；
2) C of 184mg is added into screw socket bottle3N4Then powder adds the 30mL tert-butyl alcohol, in 45 DEG C of ultrasonic disperse 1h
Obtain dispersion liquid A；Then the nickel acetylacetonate of 450mg is added into dispersion liquid A, then is placed on 75 DEG C in 45 DEG C of ultrasonic disperse 1h
Magnetic stirring apparatus on stirring 20h obtain mixed liquid B；
3) reaction kettle with polytetrafluoroethyllining lining that volume is 50mL is preheated to 65 DEG C, then rapidly by mixed liquor
B is transferred in polytetrafluoroethyllining lining, and rapid sealing reaction kettle simultaneously transfers them in the baking oven that temperature is 100 DEG C, is then set
Determining oven temperature is 200 DEG C, when temperature rises to setting temperature, starts timing, isothermal reaction 30h；
4) after solvent thermal reaction, baking oven power supply is closed, after reaction kettle is cooled to room temperature with baking oven, opens reaction
Mixed liquor is centrifuged 15min by kettle under the rate of 12000rpm, and with after washes of absolute alcohol in 60 DEG C of vacuum oven
Dry 18h obtains C3N4- NiO composite sample.
Claims (6)
1. a kind of nickel oxide-nitridation carbon composite photocatalyst preparation method, it is characterised in that：
1) it takes 36g urea to be put into corundum crucible, places it in 24~48h of heat treatment in 80 DEG C of baking oven, then close the lid
550 DEG C are risen to the heating rate of 4.6 DEG C/min in Muffle furnace afterwards, isothermal holding 3h is naturally cooling to room temperature, obtains yellow
Pulverulent solids C3N4, stand-by after grinding；
2) C of 184mg is added into screw socket bottle3N4Then powder adds the 30mL tert-butyl alcohol, obtain in 35~45 DEG C of ultrasonic disperses
To dispersion liquid A；Then the nickel acetylacetonate of 64-514mg is added into dispersion liquid A, then after 35~45 DEG C of ultrasonic disperses are uniform
It is placed on 65~75 DEG C of magnetic stirring apparatus and stirs evenly to obtain mixed liquid B；
3) reaction kettle with polytetrafluoroethyllining lining is preheated to 60~70 DEG C, mixed liquid B is then transferred to poly- four rapidly
In vinyl fluoride liner, rapid sealing reaction kettle simultaneously transfer them to temperature and be in 100 DEG C of baking oven then set oven temperature as
190~210 DEG C, when temperature rises to setting temperature, start timing, 12~30h of isothermal reaction；
4) after solvent thermal reaction, baking oven power supply is closed, after reaction kettle is cooled to room temperature with baking oven, opens reaction kettle, it will
Mixed liquor is centrifuged 15min under the rate of 10000~12000rpm, and with the vacuum oven after washes of absolute alcohol at 60 DEG C
In be dried to obtain C3N4- NiO composite sample.
2. nickel oxide according to claim 1-carbonitride high-efficiency composite photocatalyst preparation method, it is characterised in that：Institute
The urea for stating step 1) fills corundum crucible.
3. nickel oxide according to claim 1-carbonitride high-efficiency composite photocatalyst preparation method, it is characterised in that：Institute
The ultrasonic disperse time for stating step 2) is 0.5~1h.
4. nickel oxide according to claim 1-carbonitride high-efficiency composite photocatalyst preparation method, it is characterised in that：Institute
State step 2) the magnetic agitation time be 12~for 24 hours.
5. nickel oxide according to claim 1-carbonitride high-efficiency composite photocatalyst preparation method, it is characterised in that：Institute
Stating step 3) reaction kettle polytetrafluoroethyllining lining volume is 50mL.
6. nickel oxide according to claim 1-carbonitride high-efficiency composite photocatalyst preparation method, it is characterised in that：Institute
State step 4) vacuum drying time be 12~for 24 hours.
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