CN109174188A - A kind of preparation of Heteroatom doping carbon material/Ni-MOF composite electrocatalyst - Google Patents
A kind of preparation of Heteroatom doping carbon material/Ni-MOF composite electrocatalyst Download PDFInfo
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- CN109174188A CN109174188A CN201811044661.9A CN201811044661A CN109174188A CN 109174188 A CN109174188 A CN 109174188A CN 201811044661 A CN201811044661 A CN 201811044661A CN 109174188 A CN109174188 A CN 109174188A
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- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 36
- 239000013099 nickel-based metal-organic framework Substances 0.000 title claims abstract description 26
- 125000005842 heteroatom Chemical group 0.000 title claims abstract description 23
- 239000002131 composite material Substances 0.000 title claims abstract description 19
- 239000010411 electrocatalyst Substances 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 21
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 9
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000005864 Sulphur Substances 0.000 claims abstract description 8
- 235000005074 zinc chloride Nutrition 0.000 claims abstract description 6
- 239000011592 zinc chloride Substances 0.000 claims abstract description 6
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 5
- 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 abstract description 3
- 239000008103 glucose Substances 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000003054 catalyst Substances 0.000 claims description 14
- QMKYBPDZANOJGF-UHFFFAOYSA-N benzene-1,3,5-tricarboxylic acid Chemical compound OC(=O)C1=CC(C(O)=O)=CC(C(O)=O)=C1 QMKYBPDZANOJGF-UHFFFAOYSA-N 0.000 claims description 10
- 235000019441 ethanol Nutrition 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 5
- GZCGUPFRVQAUEE-VANKVMQKSA-N aldehydo-L-glucose Chemical compound OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)C=O GZCGUPFRVQAUEE-VANKVMQKSA-N 0.000 claims description 4
- 238000004090 dissolution Methods 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- 238000003763 carbonization Methods 0.000 claims description 3
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 238000002242 deionisation method Methods 0.000 claims 1
- 239000006185 dispersion Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 21
- 230000003197 catalytic effect Effects 0.000 abstract description 10
- 239000012621 metal-organic framework Substances 0.000 abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 8
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052799 carbon Inorganic materials 0.000 abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052717 sulfur Inorganic materials 0.000 abstract description 5
- 238000006555 catalytic reaction Methods 0.000 abstract description 4
- 239000003795 chemical substances by application Substances 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 150000001721 carbon Chemical group 0.000 abstract description 2
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 abstract description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 10
- 229910052697 platinum Inorganic materials 0.000 description 5
- 125000004429 atom Chemical group 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000013110 organic ligand Substances 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- -1 cation salt Chemical class 0.000 description 1
- 210000003850 cellular structure Anatomy 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/22—Organic complexes
- B01J31/2204—Organic complexes the ligands containing oxygen or sulfur as complexing atoms
- B01J31/2208—Oxygen, e.g. acetylacetonates
- B01J31/2226—Anionic ligands, i.e. the overall ligand carries at least one formal negative charge
- B01J31/223—At least two oxygen atoms present in one at least bidentate or bridging ligand
- B01J31/2239—Bridging ligands, e.g. OAc in Cr2(OAc)4, Pt4(OAc)8 or dicarboxylate ligands
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
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- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Electrochemistry (AREA)
- Metallurgy (AREA)
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Abstract
The invention belongs to new energy source technology field, especially a kind of preparation of Heteroatom doping carbon material/Ni-MOF composite electrocatalyst.The present invention is mainly to change the charge density of adjacent carbon atom using the synergistic effect of N, S element codope, spin density in basis material is caused to be redistributed, to form active site abundant in prepared catalytic composite material, be conducive to catalysis reaction to carry out, and then improve the catalytic performance of MOF sill.Using glucose as carbon source, thiocarbamide as sulphur source and nitrogen source, zinc chloride be structure directing agent, carbon material is tentatively synthesized using hydro-thermal method and carries out dezincify processing, it is dried after washing at 110 DEG C, then through tube furnace high temperature cabonization, obtains sulphur, N doping porous carbon (SNPC) material.Heteroatom doping carbon material and the composite electrocatalyst (SNPC/Ni-MOF) of Ni-MOF are prepared using hydro-thermal method again, by test discovery composite material electrolysis water performance be improved significantly.
Description
Technical field
The invention belongs to new energy source technology field, relates to a kind of Heteroatom doping carbon material/Ni-MOF compound electric and urge
The preparation of agent.
Background technique
The mankind have stepped into 21 century, and civilization degree is greatly improved, and the environmental consciousness of the mankind is also growing,
But how to realize that harmony between man and nature coexists and economic sustainable development remains a great problem.Currently, people still lead
Fossil fuel is used, due to the rapid development of science and technology, energy demand is growing day by day, this leads to the quick consumption of fossil fuels available
To the greatest extent, the mankind living environment is by huge destruction such as global warming, Melting Glacierss and sea level rise.It is believed that hydrogen
It can be the most environmentally friendly energy, the product for being primarily due to obtain after it is as Energy supply material burning is H2O is to be expected to replace
Fossil energy simultaneously becomes following leading energy.However, evolving hydrogen reaction (HER) and oxygen evolution reaction (OER) in electrochemistry hydrogen manufacturing
Require the help by catalyst.Current main HER and OER catalyst is all the catalyst based on platinum mostly, but
It is that large-scale commercial applications can not be carried out due to the disadvantages of actual storage amount of platinum is very limited, price is extremely expensive,
Therefore, the excellent and cheap catalyst of catalytic effect that exploration and searching can substitute platinum has important practical significance.
MOF material (metal-organic framework materials) is by rigid organic ligand (being mainly to provide lone electron pair) and metal
It is novel porous that ion or metal cluster (primarily as core component, providing unoccupied orbital) connect the one kind to be formed in the form of coordinate bond
Material possesses unlimited network cellular structure, therefore, its porosity with higher and biggish specific surface area.Meanwhile it should
Not only adjustable dimension, change pattern possess structure abundant, and raw material is simple and easy to get to material, and synthetic method is easy, more
Sample, it is most important that various chemical modifications can be carried out according to requirement of experiment.Therefore, MOF is also obtained in catalytic field in recent years
Wide research and application.There is diversified property with the carbon material that single carbon is constituted, mixed in carbon material
The physical property and chemical property of atom (such as N, S, P, B and other atoms) adjustable material, obtain more active sites
Point, this process, which can not only improve carbon material, makes it carry out catalysis reaction the absorption property of atom or molecule, improves it in electricity
It is catalyzed the performance of aspect, nor the electric conductivity of itself can be reduced.The carbon-based material of Heteroatom doping is cheap and is catalyzed
Excellent effect is expected to become the ideal material of substitution platinum based catalyst.Importantly, these are mixed with heteroatomic structure is
Research and development has the low price catalyst that catalytic activity is more preferable and the service life is longer and provides platform.Here the miscellaneous original of S, N is used
Son doping carbon material mainly can change the charge density of adjacent carbon atom using the synergistic effect of the two, will lead to basis material
Middle spin density is redistributed, and then forms active site abundant in the material, is conducive to catalysis reaction and is carried out, into
And improve the catalytic performance of single metal-organic framework materials.
Summary of the invention
The purpose of the present invention is so that composite catalyst is had more richer urge by S, N hetero atom codope carbon material
Change active site, be more conducively catalyzed the progress of reaction, is urged to provide a kind of Heteroatom doping carbon material/Ni-MOF compound electric
The preparation of agent.
Thinking of the invention: quasi- DEXTROSE ANHYDROUS (Panreac) and thiocarbamide are raw material, and zinc chloride is added and leads as structure
To agent, the porous carbon materials of sulphur, N doping are first synthesized with hydro-thermal method and high-temperature calcination carbonizatin method, then by the hetero atom of synthesis
Carbon material, metal cation salt and the organic ligand of doping are put into reaction kettle after mixing, are prepared again by hydro-thermal method
Heteroatom doping carbon material/Ni-MOF composite electrocatalyst.
Specifically sequentially include the following steps:
(1) glucose and thiocarbamide are weighed according to certain mol proportion, and zinc chloride 4.5g is added and is placed in a beaker, and 16mL is added and goes
Ionized water, glass bar are stirred to dissolution, are placed in hydrothermal reaction kettle and are reacted certain time under certain temperature, and ethyl alcohol, water repeat to take out
Filter washing, the drying of 110 DEG C of baking ovens are placed in tube furnace a certain temperature carbonization certain time under inert atmosphere and obtain hetero atom and mix
Miscellaneous porous carbon materials are labeled as SNPC；
(2)C4H6NiO4·4H2O and trimesic acid (H3BTC it) is weighed according to certain mol proportion, a certain amount of sulphur, nitrogen is added
32mL DMF and 20mL ethyl alcohol is then added in doped porous carbon material (SNPC), and magnetic agitation 1 hour or so until solution disperses
Uniformly, a certain thermotonus certain time in hydrothermal reaction kettle, the repeated multiple times washing of gained sample, 60 DEG C of drying, sample are fitted into
Labeled as SNPC/Ni-MOF.
Positive effect obtained by the present invention is: (1) the adjustable material of N, S hetero atom is mixed in carbon material
Physical property and chemical property, changed by replacing the position of certain carbon atoms in carbon skeleton the electronic structure of material with point
Cloth, convenient for the exposure of a large amount of active sites, not only improving carbon material makes it be catalyzed anti-the absorption property of atom or molecule
It answers, and improves activity of the material in terms of electro-catalysis.(2) carbon material with excellent conductive capability is as carrier loaded
MOF sill can adjust well and improve the monolithic conductive performance of composite catalyst, facilitate the active raising of electrolysis water.
(3) by test, SNPC/Ni-MOF composite catalyst electrolysis water performance be improved significantly, show the carbon-based of Heteroatom doping
Material price is cheap and catalytic effect is excellent, is expected to become the ideal material of substitution platinum based catalyst.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of Ni-MOF.
Fig. 2 is the scanning electron microscope (SEM) photograph of SNPC/Ni-MOF.
Specific embodiment
Specific embodiment 1: a kind of Heteroatom doping carbon material/Ni-MOF composite electrocatalyst of present embodiment
Preparation is to sequentially include the following steps:
(1) glucose and thiocarbamide are weighed according to certain mol proportion, and zinc chloride 4.5g is added and is placed in a beaker, and 16mL is added and goes
Ionized water, glass bar are stirred to dissolution, are placed in hydrothermal reaction kettle and are reacted certain time under certain temperature, and ethyl alcohol, water repeat to take out
Filter washing, the drying of 110 DEG C of baking ovens are placed in tube furnace a certain temperature carbonization certain time under inert atmosphere and obtain hetero atom and mix
Miscellaneous porous carbon materials are labeled as SNPC；
(2)C4H6NiO4·4H2O and trimesic acid (H3BTC it) is weighed according to certain mol proportion, a certain amount of sulphur, nitrogen is added
32mL DMF and 20mL ethyl alcohol is then added in doped porous carbon material (SNPC), and magnetic agitation 1 hour or so until solution disperses
Uniformly, a certain thermotonus certain time in hydrothermal reaction kettle, the repeated multiple times washing of gained sample, 60 DEG C of drying, sample are fitted into
Labeled as SNPC/Ni-MOF.
Specific embodiment 2: the present embodiment is different from the first embodiment in that glucose and sulphur in step (1)
Urea is weighed according to 3:1 molar ratio, 140 DEG C of hydro-thermal reactions 10h, 700 DEG C of high temperature cabonization 2h.Other and one phase of specific embodiment
Together.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that according to 2:1 in step (2)
Molar ratio weighs, and 5mg SNPC, 180 DEG C of hydro-thermal reaction 10h is added.Other are the same as one or two specific embodiments.
A kind of Heteroatom doping carbon material/Ni-MOF composite electrocatalyst is illustrated by following embodiment and comparative example
Preparation.
Embodiment one:
(1) glucose and thiocarbamide are weighed according to 3:1 molar ratio, and zinc chloride 4.5g is added and is placed in a beaker, and 16mL is added and goes
Ionized water, glass bar are stirred to dissolution, are placed in 140 DEG C of hydro-thermal reaction 10h in hydrothermal reaction kettle, and ethyl alcohol, water repeat filtering and washing,
110 DEG C of baking oven drying are placed on the lower 700 DEG C of high temperature cabonization 2h of inert atmosphere in tube furnace and obtain Heteroatom doping porous carbon materials,
Labeled as SNPC；
(2)C4H6NiO4·4H2O and trimesic acid (H3BTC it) is weighed according to 2:1 molar ratio, 5mg sulphur, N doping is added
32mL DMF and 20mL ethyl alcohol is then added in porous carbon materials (SNPC), and magnetic agitation 1h or so is uniformly dispersed up to solution, fills
Enter 180 DEG C of hydro-thermal reaction 10h in hydrothermal reaction kettle, the repeated multiple times washing of gained sample, 60 DEG C of drying, sample is labeled as SNPC/
Ni-MOF。
Fig. 1 is the scanning electron microscope (SEM) photograph of Ni-MOF, and the pure Ni-MOF sill prepared by hydro-thermal method is uniform just in shape
Cube structure, and size is about 2~8 μm.The surface of material can be seen that apparent pore structure, this is metal organic framework
The characteristic of class material, while being also the main reason for such material is widely used in catalytic field.
Fig. 2 is the scanning electron microscope (SEM) photograph of SNPC/Ni-MOF, and after the carbon material that Heteroatom doping is added, MOF material is square
The many spherical carbon materials of body area load, and surface is by the coarse of flat and smooth change, and aperture increases than before, in this way
Structure be conducive to provide more active sites, facilitate contact of the catalyst with electrolyte, make the electricity of composite material
Catalytic performance is improved；And the carbon material of surface covering reduces the resistance of composite material, that is, increases the conduction of catalyst
Property, be conducive to promote its catalytic activity during electrolysis water.
Comparative example one:
C4H6NiO4·4H2O and trimesic acid (H3BTC) weighed according to 2:1 molar ratio, then be added 32mL DMF and
20mL ethyl alcohol is uniformly dispersed up to solution, is fitted into 180 DEG C of hydro-thermal reaction 10h in hydrothermal reaction kettle for magnetic agitation 1 hour or so,
The repeated multiple times washing of gained sample, 60 DEG C of drying, sample are labeled as Ni-MOF.
Claims (4)
1. a kind of preparation of Heteroatom doping carbon material/Ni-MOF composite electrocatalyst, it is characterised in that the catalyst be by with
Lower step carries out:
(1) glucose and thiocarbamide are weighed according to certain mol proportion, and zinc chloride 4.5g is added and is placed in a beaker, 16mL deionization is added
Water, glass bar are stirred to dissolution, are placed in hydrothermal reaction kettle and are reacted certain time under certain temperature, and ethyl alcohol, water are repeated to filter and be washed
It washs, the drying of 110 DEG C of baking ovens is placed in tube furnace a certain temperature carbonization certain time under inert atmosphere, and to obtain Heteroatom doping more
Hole carbon material is labeled as SNPC；
(2)C4H6NiO4·4H2O and trimesic acid (H3BTC it) is weighed according to certain mol proportion, a certain amount of sulphur, N doping is added
32mL DMF and 20mL ethyl alcohol is then added in porous carbon materials (SNPC), and magnetic agitation 1 hour or so until solution dispersion is equal
It is even, it is fitted into a certain thermotonus certain time in hydrothermal reaction kettle, the repeated multiple times washing of gained sample, 60 DEG C of drying, sample mark
It is denoted as SNPC/Ni-MOF.
2. a kind of preparation of Heteroatom doping carbon material/Ni-MOF composite electrocatalyst according to claim 1, feature
It is in step (1) that glucose and thiocarbamide are weighed according to 3:1 molar ratio, 140 DEG C of hydro-thermal reactions 10h, 700 DEG C of high temperature cabonization 2h.
3. a kind of preparation of Heteroatom doping carbon material/Ni-MOF composite electrocatalyst according to claim 1, feature
It is to weigh in step (2) according to 2:1 molar ratio, 5mg SNPC, 180 DEG C of hydro-thermal reaction 10h is added.
4. a kind of preparation of Heteroatom doping carbon material/Ni-MOF composite electrocatalyst according to claim 1, feature
Be prepared SNPC/Ni-MOF composite catalyst electrolysis water performance be improved significantly.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109692711A (en) * | 2019-02-12 | 2019-04-30 | 济南大学 | A kind of CeO2And Co3O4The preparation method and application of hydridization Ce-MOF/Co-MOF composite catalyst |
| CN110156120A (en) * | 2019-06-26 | 2019-08-23 | 中南大学 | Sewage-treatment plant and processing method |
| CN110586191A (en) * | 2019-09-18 | 2019-12-20 | 常州大学 | Oxygen evolution catalyst of CoCu-MOF/SNPC compounded by MOF material |
| CN110813363A (en) * | 2019-12-04 | 2020-02-21 | 南京工程学院 | Nitrogen-sulfur-doped porous carbon modified carbon nanotube supported Pt-Ni alloy catalyst and preparation method thereof |
| CN111359635A (en) * | 2020-04-13 | 2020-07-03 | 新昌县佳和工艺股份有限公司 | Porous carbon material loaded FeCo2S4Electrochemical oxygen evolution catalyst and preparation method thereof |
| CN114230807A (en) * | 2022-01-12 | 2022-03-25 | 三峡大学 | Preparation method of chiral nickel-based complex and application of chiral nickel-based complex in electrochemical detection of glucose |
| CN115784228A (en) * | 2022-12-21 | 2023-03-14 | 陕西科技大学 | Bimetal modified nitrogen-doped porous carbon nanosheet and preparation method and application thereof |
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Application publication date: 20190111 Assignee: Changzhou Zhuoyida Machinery Co.,Ltd. Assignor: CHANGZHOU University Contract record no.: X2023980053835 Denomination of invention: Preparation of a heteroatom doped carbon material/Ni MOF composite electrocatalyst Granted publication date: 20200214 License type: Common License Record date: 20231225 |
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