CN109078648A - A kind of preparation method of three-dimensional grapheme/nickel/graphite phase carbon nitride composite photocatalyst material - Google Patents
A kind of preparation method of three-dimensional grapheme/nickel/graphite phase carbon nitride composite photocatalyst material Download PDFInfo
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- CN109078648A CN109078648A CN201810863120.2A CN201810863120A CN109078648A CN 109078648 A CN109078648 A CN 109078648A CN 201810863120 A CN201810863120 A CN 201810863120A CN 109078648 A CN109078648 A CN 109078648A
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 69
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000002131 composite material Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 16
- 239000000463 material Substances 0.000 title claims abstract description 12
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 10
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 9
- 239000010439 graphite Substances 0.000 title claims abstract description 9
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 8
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 41
- 239000007787 solid Substances 0.000 claims abstract description 29
- 239000000843 powder Substances 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 230000000903 blocking effect Effects 0.000 claims abstract description 17
- 238000010792 warming Methods 0.000 claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 15
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 15
- 239000001257 hydrogen Substances 0.000 claims abstract description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 13
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 9
- 238000004108 freeze drying Methods 0.000 claims abstract description 6
- 230000008018 melting Effects 0.000 claims abstract description 4
- 238000002844 melting Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 3
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims abstract 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 8
- 229910052783 alkali metal Inorganic materials 0.000 claims description 8
- -1 alkali metal salt Chemical class 0.000 claims description 8
- 239000004202 carbamide Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 239000003054 catalyst Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 229930006000 Sucrose Natural products 0.000 claims description 2
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 2
- 238000007710 freezing Methods 0.000 claims description 2
- 230000008014 freezing Effects 0.000 claims description 2
- 239000008103 glucose Substances 0.000 claims description 2
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000005720 sucrose Substances 0.000 claims description 2
- 229920000877 Melamine resin Polymers 0.000 claims 1
- 239000003513 alkali Substances 0.000 claims 1
- 229910000288 alkali metal carbonate Inorganic materials 0.000 claims 1
- 229910001514 alkali metal chloride Inorganic materials 0.000 claims 1
- 229910052936 alkali metal sulfate Inorganic materials 0.000 claims 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 10
- 239000002245 particle Substances 0.000 description 7
- GZCGUPFRVQAUEE-SLPGGIOYSA-N aldehydo-D-glucose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O GZCGUPFRVQAUEE-SLPGGIOYSA-N 0.000 description 6
- 239000012298 atmosphere Substances 0.000 description 6
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 6
- 239000011780 sodium chloride Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000001291 vacuum drying Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 230000032900 absorption of visible light Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000010406 interfacial reaction Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 239000011787 zinc oxide Substances 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—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0027—Powdering
- B01J37/0036—Grinding
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0081—Preparation by melting
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
Abstract
The present invention relates to a kind of preparation methods of three-dimensional grapheme/nickel/graphite phase carbon nitride composite photocatalyst material, including the following steps: 1) preparation of the 3D graphene of Ni particulate load；2) after blocking material freeze drying will be freezed, light-blue solid powder is obtained；3) powder that freeze-drying obtains is put into Noah's ark or crucible, under hydrogen, is warming up to 600-750 DEG C with 5-15 DEG C/min, keeps the temperature 1-2h, then cleaned several times with deionized water, drying obtains the 3D graphene of Ni particulate load；4) 3D graphene/Ni/g-C3N4 preparation: the presoma of the 3D graphene of Ni particulate load and g-C3N4 are mixed by the way of melting, under an argon atmosphere, it is warming up to 500-600 DEG C with 5-15 DEG C/min, 2-4h is kept the temperature, obtains 3D graphene/Ni/g-C3N4 composite material.
Description
Technical field
The invention belongs to photocatalysis technology fields, and in particular to a kind of three-dimensional (3D) graphene/nickel (Ni)/graphite-phase nitridation
Carbon (g-C3N4) composite photocatalyst material preparation method.
Background technique
In recent years due to the raising of the quickening of process of industrialization and human living standard, consumption of the mankind to the energy
The fossil energies such as coal, petroleum, the natural gas for increasing year by year, but storing on the earth are extremely limited, therefore pass through photocatalysis technology
The Hydrogen Energy for converting solar energy into cleanliness without any pollution becomes the most effective means for solving energy crisis at present.
Most study is inorganic semiconductor during photocatalysis technology develops, such as titanium oxide, zinc oxide and cadmium sulfide,
But most of oxide, which cannot absorb visible light, sulfide, to be easy to happen photoetch these problems during the reaction and limits
Its application in photocatalysis field.And g-C3N4A kind of organic semiconductor as no metal attracted researcher's note that
g-C3N4Have the advantages that stability height, good environmental adaptability, band gap size suitable (2.7eV or so), visible light can be absorbed.
But g-C3N4Smaller, electron hole pair recombination rate that there is also specific surface areas is high, lacks to incomplete absorption of visible light region etc.
Point causes its photocatalysis hydrogen production rate lower.
g-C3N4It is light absorption, table/interfacial reaction, electricity applied to play crucial effect to its performance in photocatalysis research
Lotus separates three problems, main by improving g-C at present3N4To the absorption of visible light, increase reactivity site, reduction current-carrying
The recombination rate of son improves its catalytic activity.Such as the Au/g-C prepared by one-step method3N4The absorption of composite material visible region
It is largely increased, and since a characteristic absorption peak also occurs at 550nm in the plasma effect of Au.Pass through template
Either the method preparation of thermal oxide etching removing has the single layer or few layer g-C of bigger serface3N4It is more to expose
Active site.It can also be by g-C3N4It is compound with the progress of other narrow gap semiconductors, promote photoproduction electric by forming hetero-junctions
The separation of son-hole, or the compound conduction to improve material is carried out with carbon materials such as graphene, carbon quantum dot, carbon nanotubes
Property to improve the separative efficiency of carrier.
Graphene has big specific surface area, excellent conduction and heating conduction, but catalytic performance is weaker, by g-C3N4
With graphene carry out it is compound can overcome the disadvantage of two components respectively, and assign composite material superior catalytic performance.
Summary of the invention
In order to solve the problems, such as that graphite phase carbon nitride exists, the object of the present invention is to provide a kind of three-dimensional (3D) graphene/
Nickel (Ni)/graphite phase carbon nitride (g-C3N4) composite photocatalyst material preparation method, improve the production hydrogen of graphite phase carbon nitride
Energy.Technical scheme is as follows:
A kind of preparation method of three-dimensional grapheme/nickel/graphite phase carbon nitride composite photocatalyst material, including the following steps:
1) preparation of the 3D graphene of Ni particulate load: with catalyst, carbon source, alkali metal salt is raw material, catalyst, carbon
Source, the mass ratio of alkali metal salt are 1:(10-20): (100-200) is dissolved in a certain amount of water, stirs 1-2h；Then
Move in refrigerator freeze it is blocking；
2) after then freezing blocking material freeze drying, light-blue solid powder is obtained.
3) powder that freeze-drying obtains is put into Noah's ark or crucible, under hydrogen, 600- is warming up to 5-15 DEG C/min
750 DEG C, 1-2h is kept the temperature, is then cleaned several times with deionized water, drying obtains the 3D graphene of Ni particulate load；
4) 3D graphene/Ni/g-C3N4Preparation: by the 3D graphene and g-C of a certain amount of Ni particulate load3N4Before
It drives body to mix by the way of melting, the solid being mixed to get is put into Noah's ark, under an argon atmosphere, with 5-15 DEG C/min liter
Temperature arrives 500-600 DEG C, keeps the temperature 2-4h, obtains 3D graphene/Ni/g-C3N4Composite material.
Preferably, carbon source is glucose or sucrose in step 1)；Catalyst is the chloride or nitrate of nickel；Alkali metal salt
It is the chloride of alkali metal, sulfate or carbonate.The g-C3N4Presoma be thiocarbamide or cyanamide or dicyandiamide or three
Poly cyanamid or urea.
In conclusion core of the invention is the 3D graphene and fused salt-heat for preparing Ni particulate load by salt template
The mode of polymerization prepares 3D graphene/Ni/g-C3N4Composite photocatalyst material.Compared with prior art, advantages of the present invention exists
In:
(1) present invention takes full advantage of the limit of alkali metal salt using the 3D graphene of the Ni particulate load of salt template preparation
Domain effect forms three-dimensional structure, and the effect that the nickel particle of uniform load not only acts as catalyst also hinders the group of graphene
It is poly-.
(2) present invention preparation 3D graphene/Ni/g-C3N4Composite material significantly improves the production hydrogen of graphite phase carbon nitride
Performance and good performance is also shown in terms of degradation of contaminant.
(3) Preparation equipment of the present invention is simple, simple process.
(4) high reliablity of the present invention.Use alkali metal salt as template, repeatability is strong, there is good application prospect.
Detailed description of the invention
Fig. 1 is the XRD spectrum of the 3D graphene of Ni particulate load prepared by the embodiment of the present invention 1.
Fig. 2 is the SEM spectrum of the 3D graphene of Ni particulate load prepared by the embodiment of the present invention 1.
Fig. 3 is 3D graphene/Ni/g-C prepared by the embodiment of the present invention 13N4XRD spectrum.
Fig. 4 is 3D graphene/Ni/g-C prepared by the embodiment of the present invention 13N4SEM figure.
Specific embodiment
Embodiment 1
Nickel nitrate, DEXTROSE ANHYDROUS and sodium chloride are dissolved in 125ml deionized water with the ratio of 1:10:100, stirred
1h；Then move in refrigerator freeze it is blocking；Then blocking substance will be freezed to be put into freeze drier, when by for 24 hours long
Between be lyophilized after, obtain light-blue solid powder.Then obtained light-blue solid powder is put into Noah's ark, in hydrogen atmosphere
Under, 600 DEG C are warming up to 5 DEG C/min, 1h is kept the temperature, is then cleaned twice with deionized water, be put into vacuum drying oven and dry, obtained
The 3D graphene of Ni particulate load as shown in Fig. 2.The three-dimensional grapheme and 10g urea that 5mg nickel particle is loaded are at 135 DEG C
Lower melting simultaneously stirs 1h at this temperature, then resulting solid is put into Noah's ark, under an argon atmosphere, with 5 DEG C/min liter
Temperature keeps the temperature 3h, obtained solid is ground to obtain 3D graphene/Ni/g-C to 500 DEG C3N4Composite material.
Embodiment 2
Nickel nitrate, DEXTROSE ANHYDROUS and sodium chloride are dissolved in 125ml deionized water with the ratio of 1:15:100, stirred
1h；Then move in refrigerator freeze it is blocking；Then blocking substance will be freezed to be put into freeze drier, when by for 24 hours long
Between be lyophilized after, obtain light-blue solid powder.Then obtained light-blue solid powder is put into Noah's ark, in hydrogen atmosphere
Under, 600 DEG C are warming up to 10 DEG C/min, 1h is kept the temperature, is then cleaned twice with deionized water, be put into vacuum drying oven and dry, obtained
To the 3D graphene of Ni particulate load as shown in Fig. 2.The three-dimensional grapheme and 10g urea that 5mg nickel particle is loaded are 135
It is melted at DEG C and stirs 1h at this temperature, then resulting solid is put into Noah's ark, under an argon atmosphere, with 5 DEG C/min
500 DEG C are warming up to, 3h is kept the temperature, obtained solid is ground to obtain 3D graphene/Ni/g-C3N4Composite material.
Embodiment 3
Nickel nitrate, DEXTROSE ANHYDROUS and sodium chloride are dissolved in 125ml deionized water with the ratio of 1:15:200, stirred
2h；Then move in refrigerator freeze it is blocking；Then blocking substance will be freezed to be put into freeze drier, when by for 24 hours long
Between be lyophilized after, obtain light-blue solid powder.Then obtained light-blue solid powder is put into Noah's ark, in hydrogen atmosphere
Under, 700 DEG C are warming up to 10 DEG C/min, 1h is kept the temperature, is then cleaned twice with deionized water, be put into vacuum drying oven and dry, obtained
To the 3D graphene of Ni particulate load as shown in Fig. 2.The three-dimensional grapheme and 10g urea that 5mg nickel particle is loaded are 135
It is melted at DEG C and stirs 1h at this temperature, then resulting solid is put into Noah's ark, under an argon atmosphere, with 10 DEG C/min
550 DEG C are warming up to, 3h is kept the temperature, obtained solid is ground to obtain 3D graphene/Ni/g-C3N4Composite material.
Embodiment 4
Nickel nitrate, DEXTROSE ANHYDROUS and sodium chloride are dissolved in 125ml deionized water with the ratio of 1:20:200, stirred
2h；Then move in refrigerator freeze it is blocking；Then blocking substance will be freezed to be put into freeze drier, when by for 24 hours long
Between be lyophilized after, obtain light-blue solid powder.Then obtained light-blue solid powder is put into Noah's ark, in hydrogen atmosphere
Under, 700 DEG C are warming up to 15 DEG C/min, 1h is kept the temperature, is then cleaned twice with deionized water, be put into vacuum drying oven and dry, obtained
To the 3D graphene of Ni particulate load as shown in Fig. 2.Three-dimensional grapheme and 10g urea that 10mg nickel particle loads are existed
At 135 DEG C melt and stir 2h at this temperature, then resulting solid is put into Noah's ark, under an argon atmosphere, with 10 DEG C/
Min is warming up to 550 DEG C, keeps the temperature 3h, obtained solid is ground to obtain 3D graphene/Ni/g-C3N4Composite material.
Embodiment 5
Nickel nitrate, DEXTROSE ANHYDROUS and sodium chloride are dissolved in 125ml deionized water with the ratio of 1:20:200, stirred
2h；Then move in refrigerator freeze it is blocking；Then blocking substance will be freezed to be put into freeze drier, when by for 24 hours long
Between be lyophilized after, obtain light-blue solid powder.Then obtained light-blue solid powder is put into Noah's ark, in hydrogen atmosphere
Under, 700 DEG C are warming up to 15 DEG C/min, 2h is kept the temperature, is then cleaned twice with deionized water, be put into vacuum drying oven and dry, obtained
To the 3D graphene of Ni particulate load as shown in Fig. 2.Three-dimensional grapheme and 10g urea that 15mg nickel particle loads are existed
At 135 DEG C melt and stir 2h at this temperature, then resulting solid is put into Noah's ark, under an argon atmosphere, with 10 DEG C/
Min is warming up to 550 DEG C, keeps the temperature 4h, obtained solid is ground to obtain 3D graphene/Ni/g-C3N4Composite material.
Embodiment 6
Nickel nitrate, DEXTROSE ANHYDROUS and sodium chloride are dissolved in 125ml deionized water with the ratio of 1:20:200, stirred
2h；Then move in refrigerator freeze it is blocking；Then blocking substance will be freezed to be put into freeze drier, when by for 24 hours long
Between be lyophilized after, obtain light-blue solid powder.Then obtained light-blue solid powder is put into Noah's ark, in hydrogen atmosphere
Under, 600 DEG C are warming up to 15 DEG C/min, 1h is kept the temperature, is then cleaned twice with deionized water, be put into vacuum drying oven and dry, obtained
To the 3D graphene of Ni particulate load as shown in Fig. 2.Three-dimensional grapheme and 10g urea that 15mg nickel particle loads are existed
At 135 DEG C melt and stir 1h at this temperature, then resulting solid is put into Noah's ark, under an argon atmosphere, with 15 DEG C/
Min is warming up to 550 DEG C, keeps the temperature 4h, obtained solid is ground to obtain 3D graphene/Ni/g-C3N4Composite material.
Claims (3)
1. a kind of preparation method of three-dimensional grapheme/nickel/graphite phase carbon nitride composite photocatalyst material, including the following steps:
1) preparation of the 3D graphene of Ni particulate load: with catalyst, carbon source, alkali metal salt is raw material, catalyst, carbon source, alkali
The mass ratio of metal salt is 1:(10-20): (100-200) is dissolved in a certain amount of water, stirs 1-2h；Then ice is moved to
It is freezed in case blocking；
2) after then freezing blocking material freeze drying, light-blue solid powder is obtained.
3) powder that freeze-drying obtains is put into Noah's ark or crucible, under hydrogen, 600-750 is warming up to 5-15 DEG C/min
DEG C, 1-2h is kept the temperature, is then cleaned several times with deionized water, drying obtains the 3D graphene of Ni particulate load；
4) 3D graphene/Ni/g-C3N4Preparation: by the 3D graphene and g-C of a certain amount of Ni particulate load3N4Presoma adopt
It is mixed with the mode of melting, the solid being mixed to get is put into Noah's ark, under an argon atmosphere, be warming up to 5-15 DEG C/min
500-600 DEG C, 2-4h is kept the temperature, 3D graphene/Ni/g-C is obtained3N4Composite material.
2. preparation method according to claim 1, which is characterized in that the method as described in claim 1, it is characterized in that institute
Carbon source is glucose or sucrose in the step 1) stated；Catalyst is the chloride or nitrate of nickel；Alkali metal salt is alkali metal
Chloride, sulfate or carbonate.
3. preparation method according to claim 1, which is characterized in that the g-C3N4Presoma be thiocarbamide or single cyanogen
Amine or dicyandiamide or melamine or urea.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN111554945A (en) * | 2020-05-27 | 2020-08-18 | 青岛科技大学 | High-efficiency carbon-based electrocatalyst and preparation method and application thereof |
| CN111841597A (en) * | 2020-06-22 | 2020-10-30 | 江苏中江材料技术研究院有限公司 | Composite photocatalytic material of cobalt-loaded nitrogen-doped graphene oxide/mesoporous thin-layer carbon nitride and preparation method thereof |
| CN116273135A (en) * | 2023-05-18 | 2023-06-23 | 苏州市相城区清智智能网联汽车创新中心 | Nitrogen-doped oxide supported metal catalyst and preparation method and application thereof |
| CN116273135B (en) * | 2023-05-18 | 2023-08-04 | 苏州市相城区清智智能网联汽车创新中心 | Nitrogen-doped oxide supported metal catalyst and preparation method and application thereof |
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