CN106744806A - Nitrogen-doped porous carbon material and its application of the metal organic framework for template - Google Patents
Nitrogen-doped porous carbon material and its application of the metal organic framework for template Download PDFInfo
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- CN106744806A CN106744806A CN201710066246.2A CN201710066246A CN106744806A CN 106744806 A CN106744806 A CN 106744806A CN 201710066246 A CN201710066246 A CN 201710066246A CN 106744806 A CN106744806 A CN 106744806A
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- 239000012621 metal-organic framework Substances 0.000 title claims abstract description 39
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 36
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000013078 crystal Substances 0.000 claims abstract description 10
- 239000001301 oxygen Substances 0.000 claims abstract description 10
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 10
- 239000007789 gas Substances 0.000 claims abstract description 7
- 239000013110 organic ligand Substances 0.000 claims abstract description 6
- 229910052786 argon Inorganic materials 0.000 claims abstract description 5
- 239000000446 fuel Substances 0.000 claims abstract description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 238000001548 drop coating Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 150000003460 sulfonic acids Chemical class 0.000 claims description 3
- 238000003786 synthesis reaction Methods 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000012300 argon atmosphere Substances 0.000 claims description 2
- 230000005611 electricity Effects 0.000 claims description 2
- 238000006722 reduction reaction Methods 0.000 abstract description 5
- 239000012298 atmosphere Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 238000003756 stirring Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 10
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910021607 Silver chloride Inorganic materials 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 3
- 102100029503 E3 ubiquitin-protein ligase TRIM32 Human genes 0.000 description 2
- 101000634982 Homo sapiens E3 ubiquitin-protein ligase TRIM32 Proteins 0.000 description 2
- 230000010757 Reduction Activity Effects 0.000 description 2
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 2
- 238000004502 linear sweep voltammetry Methods 0.000 description 2
- 239000002082 metal nanoparticle Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000013112 stability test Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002717 carbon nanostructure Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 125000005909 ethyl alcohol group Chemical group 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/96—Carbon-based electrodes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/08—Intercalated structures, i.e. with atoms or molecules intercalated in their structure
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
- C01P2004/34—Spheres hollow
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
-
- 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
- Y02E60/50—Fuel cells
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inert Electrodes (AREA)
- Carbon And Carbon Compounds (AREA)
- Catalysts (AREA)
Abstract
The nitrogen-doped porous carbon material for template and its application the present invention relates to metal organic framework.The technical scheme of use is：By Ni (NO3)2, organic ligand H6TATIP, N, N dimethylformamide and H2O is added in container, in stirring under normal temperature；After container is sealed, it is placed in baking oven, under 358K, is kept for 34 days；It is slowly cooled to room temperature; green crystal is obtained, washed, filtered and dry, the crystal that will be obtained is placed in vacuum tube furnace 800 DEG C in argon gas protection atmosphere; the carbide obtained under the conditions of 3 hours adulterates wherein N element as template, and further high temperature cabonization obtains target product.Metal organic framework prepared by the present invention is that the porous carbon materials electro-chemical activity of the N doping of template is strong, is conducive to improving fuel battery negative pole oxygen reduction reaction efficiency.
Description
Technical field
The present invention relates to a kind of carbon material, specifically, be related to it is a kind of have oxygen reduction activity based on metal organic framework
It is the N doped porous carbon material materials of template.
Background technology
In the past few decades, metal organic framework (MOFs) is widely studied as a kind of functional material, MOFs tools
There is the porosity of big specific surface area and Geng Gao.Structure and function are more various, can be applied to separate, and ion exchange, gas is deposited
Storage and fluorescent optical sensor.Recent years, MOFs is used as template or presoma to synthesize the porous carbon materials of N doping, and due to
His various pore structure and carbon content high cause people widely to pay close attention to.It shows electrical conductive activities high, and corrosion resistance is good
Good surface property and low cost.Therefore, the porous carbon materials of N doping have good application prospect.
The content of the invention
The purpose of the present invention is, by the use of MOFs as template, under certain hot conditions, to be carbonized, then carries out nitrogen unit
Element doping, synthesis metal organic framework is the N doped porous carbon materials of template.
The technical solution adopted by the present invention is as follows：Metal organic framework is the nitrogen-doped porous carbon material of template, including with
Lower synthesis step：
1) by Ni (NO3)2, organic ligand H6TATIP, N,N-dimethylformamide and H2O is added in container, in normal temperature
Lower stirring；
Described organic ligand H6The structural formula of TATIP is as follows：
2) after container is sealed, it is placed in baking oven, under 358-368K, is kept for 3-4 days；
3) it is slowly cooled to room temperature, stands at least 1 day, obtain crystal, by crystal washing, filters and dry；
4) dried crystal is placed in the high temperature process furnances of argon atmosphere, in 800 DEG C, is heated 3-4 hours, be cooled to
Room temperature, obtains carbide；
5) carbide that will be obtained, is washed with watery hydrochloric acid, then is washed to neutrality with distillation, is vacuum dried 3~5 hours；
6) dried carbide is soaked in the methanol solution containing nitrogen source, soaking at room temperature 12 hours, is washed, done
It is dry；
7) by dried product in the vacuum tube furnace full of argon gas, at 900 DEG C, heat 1 hour, be cooled to
Room temperature obtains target product.
Above-mentioned metal organic framework is the nitrogen-doped porous carbon material of template, in molar ratio, Ni (NO3)2:Organic ligand
H6TATIP=1:0.1-0.2.
Above-mentioned metal organic framework is the nitrogen-doped porous carbon material of template, and described nitrogen source is urea.
Above-mentioned metal organic framework is the nitrogen-doped porous carbon material application in a fuel cell of template.Preferably,
Described metal organic framework is modified in work for the nitrogen-doped porous carbon material of template as Cathodic oxygen reduction catalyst
On electrode.Method is as follows：Absolute ethyl alcohol and perfluorinated sulfonic acid are added drop-wise to the N doping that above-mentioned metal organic framework is template many
In the carbon material of hole, ultrasonic disperse obtains ink black solution, will prepare ink black solution drop coating on glass-carbon electrode, at room temperature
Dry.
The metal organic framework that the present invention synthesizes is the N doped porous carbon materials of template, is with homogeneous pore structure
Hollow ball, diameter is about 8.25nm, does not contain metal nanoparticle, and hollow carbon edge ring is around a large amount of graphitized carbon nano knots
Structure, and there is high-visible lattice under ESEM, spacing of lattice is about 0.284nm.
The beneficial effects of the invention are as follows：Metal organic framework prepared by the present invention is the N doped porous carbon materials of template
With preferable electro-chemical activity, preparation method is simple, has great application prospect.
Brief description of the drawings
Fig. 1 is the electron microscope of the nitrogen-doped porous carbon material that metal organic framework of the present invention is template.
Fig. 2 is the circulation volt under the nitrogen-doped porous carbon material different atmosphere environment that metal organic framework of the present invention is template
Peace curve map.
Fig. 3 is the linear scan volt under the nitrogen-doped porous carbon material different rotating speeds that metal organic framework of the present invention is template
Peace curve map.
Fig. 4 is the current versus time curve figure of the nitrogen-doped porous carbon material that metal organic framework of the present invention is template.
Specific embodiment
The metal organic framework of embodiment 1 is the nitrogen-doped porous carbon material of template
By the Ni (NO of 0.103mmol3)2, 0.016mmol H6The N,N-dimethylformamide and 0.5mL of TATIP and 2mL
H2O is added in vial, in stirring 30 minutes under normal temperature.Then it is sealed against, is placed in baking oven, under 358K, protects
Hold 3-4 days.It is slowly cooled to room temperature that (rate of temperature fall is 3-8Kh-1), at least 1 day is stood, obtain green crystal, washing, filtering
And dry.Dried crystal is placed in high temperature process furnances, in argon gas protection atmosphere, at 800 DEG C, is heated 3 hours, obtained
To carbide, room temperature is cooled to.The carbide that will be obtained is washed with 20% watery hydrochloric acid, to remove inorganic metal impurity, then is used
Distillation is washed to neutrality, is vacuum dried 3~5 hours.Dried carbide is soaked in the methanol solution (30% containing urea
W/w in), soaking at room temperature 12 hours, washing is dried.By dried product, 900 in the vacuum tube furnace full of argon gas
Under the conditions of DEG C, heat 1 hour, be cooled to room temperature and obtain target product, metal organic framework is the nitrogen-doped porous carbon of template
Material.
Metal organic framework for template nitrogen-doped porous carbon material electron microscope as shown in figure 1, the carbide be with
The hollow ball of homogeneous pore structure, bore dia is about 8.25nm, does not contain metal nanoparticle, and hollow carbon edge ring is around a large amount of
Graphitized carbon nano structure, and there is high-visible lattice under ESEM, spacing of lattice is about 0.284nm.
The metal organic framework of embodiment 2 reacts for the nitrogen-doped porous carbon material catalytic oxidation-reduction of template
(1) preparation method：Nitrogen-doped porous carbon material of the metal organic framework as template prepared using embodiment 1 as
Catalyst oxygen reduction reaction
Metal organic framework prepared by the embodiment 1 that the perfluorinated sulfonic acid of 1mL absolute ethyl alcohols and 50 μ L is added drop-wise to 5mg is mould
In the nitrogen-doped porous carbon material of plate, the ultrasonic disperse in supersonic cleaning machine obtains homogeneous ink black solution.Take 5 μ L dispersions
Good ink black solution, by its drop coating on polished glass-carbon electrode, dries at room temperature, and it is template to obtain metal organic framework
The working electrode of nitrogen-doped porous carbon material modification.
(2) cyclic voltammetry curve test
Using electrochemical workstation, volt-ampere curve test is circulated in three-electrode system, electrolyte is oxygen saturation
0.1M KOH solution, test voltage scope be -1~0.2V, Ag/AgCl electrodes be reference electrode, to electrode be platinum filament electricity
Pole, as a result as shown in Fig. 2 in saturation oxygen, being shown in -0.2V places and being observed that obvious reduction peak, and it is lazy in saturation
Property gas Ar in there is no reduction peak, illustrate that nitrogen-doped porous carbon material that metal organic framework of the invention is template has obvious
Oxygen reduction activity.
(3) linear sweep voltammetry curve test
Using electrochemical workstation, rotating disk electrode (r.d.e) carries out linear sweep voltammetry curve test in three-electrode system,
Electrolyte is the KOH solution of the 0.1M of oxygen saturation, and test voltage scope is -1~0.2V, and Ag/AgCl electrodes are reference electrode,
It is platinum electrode to electrode, the rotating disk electrode (r.d.e) range of speeds is 400~2400rpm, as a result such as Fig. 3.Fig. 3 shows, from test
In it is observed that gradually increasing with the increase electric current of rotating speed.
(4) current-vs-time stability test
Using electrochemical workstation, rotating disk electrode (r.d.e) carries out current-vs-time stability test in three-electrode system,
Electrolyte is the KOH solution of the 0.1M of oxygen saturation, and test voltage is -0.2V, and Ag/AgCl electrodes are reference electrode, to electrode
It is platinum electrode, rotating disk electrode (r.d.e) rotating speed is 1600rpm, and the testing time is 20000s, as a result such as Fig. 4.Fig. 4 shows, from survey
Can be observed in test result, metal organic framework of the present invention is the stability of the nitrogen-doped porous carbon material (NPC-900) of template
Very well, the only minimal amount loss of application for a long time, still retains 75% after 20000s, and Pt/C only remains 48%, illustrates the present invention
Metal organic framework have more preferable stability than Pt/C for the nitrogen-doped porous carbon material of template.
Claims (6)
1. metal organic framework is the nitrogen-doped porous carbon material of template, it is characterised in that including following synthesis step：
1) by Ni (NO3)2, organic ligand H6TATIP, N,N-dimethylformamide and H2O is added in container, is stirred under normal temperature
Mix；
2) after container is sealed, it is placed in baking oven, under 358-368K, is kept for 3-4 days；
3) it is slowly cooled to room temperature, stands at least 1 day, obtain crystal, by crystal washing, filters and dry；
4) dried crystal is placed in the high temperature process furnances of argon atmosphere, in 800 DEG C, is heated 3-4 hours, be cooled to room
Temperature, obtains carbide；
5) carbide that will be obtained, is washed with watery hydrochloric acid, then is washed to neutrality with distillation, is vacuum dried 3~5 hours；
6) dried carbide is soaked in the methanol solution containing nitrogen source, soaking at room temperature 12 hours, is washed, dried；
7) by dried product in the vacuum tube furnace full of argon gas, at 900 DEG C, heat 1 hour, be cooled to room temperature
Obtain target product.
2. metal organic framework according to claim 1 is the nitrogen-doped porous carbon material of template, it is characterised in that massage
You compare, Ni (NO3)2:Organic ligand H6TATIP=1:0.1-0.2.
3. metal organic framework according to claim 1 is the nitrogen-doped porous carbon material of template, it is characterised in that described
Nitrogen source be urea.
4. claim 1,2 or the metal organic framework described in 3 any one are the nitrogen-doped porous carbon material of template in fuel electricity
Application in pond.
5. application according to claim 4, it is characterised in that described metal organic framework is porous for the N doping of template
Carbon material is modified on the working electrode (s as Cathodic oxygen reduction catalyst.
6. application according to claim 5, it is characterised in that method is as follows：Absolute ethyl alcohol and perfluorinated sulfonic acid are added drop-wise to
1st, during the metal organic framework described in 2 or 3 any one is for the nitrogen-doped porous carbon material of template, ultrasonic disperse obtains ink black
Solution, the ink black solution drop coating that will be prepared is dried at room temperature on glass-carbon electrode.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107902654A (en) * | 2017-10-23 | 2018-04-13 | 东华大学 | A kind of coal tar asphalt is modified the preparation method and application of high-ratio surface porous carbon |
| CN108808018A (en) * | 2018-06-26 | 2018-11-13 | 西北师范大学 | A kind of preparation and application of octahedron nitrating carbon skeleton material |
| CN109686993A (en) * | 2018-12-26 | 2019-04-26 | 上海应用技术大学 | A kind of N doping mesoporous carbon spheres Nonmetal oxygen reduction catalyst, preparation method and application |
| CN109970046A (en) * | 2019-05-07 | 2019-07-05 | 江西铜业技术研究院有限公司 | A kind of preparation method of slim pipe diameter carbon nanotube |
| KR20200021217A (en) * | 2018-08-20 | 2020-02-28 | 주식회사 엘지화학 | Metal Organic Framework, Method for Preparing the Same and Method for Preparing Porous Carbon Structure Using the Same |
| CN111001428A (en) * | 2019-12-24 | 2020-04-14 | 山西大学 | Metal-free carbon-based electrocatalyst, preparation method and application |
| CN116120567A (en) * | 2022-11-18 | 2023-05-16 | 电子科技大学长三角研究院(湖州) | Preparation method and application of nitrogen-rich nickel-based coordination polymer and derivative material thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107902654A (en) * | 2017-10-23 | 2018-04-13 | 东华大学 | A kind of coal tar asphalt is modified the preparation method and application of high-ratio surface porous carbon |
| CN107902654B (en) * | 2017-10-23 | 2020-08-11 | 东华大学 | Preparation method and application of coal tar pitch modified high-specific-surface porous carbon |
| CN108808018A (en) * | 2018-06-26 | 2018-11-13 | 西北师范大学 | A kind of preparation and application of octahedron nitrating carbon skeleton material |
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| CN109686993A (en) * | 2018-12-26 | 2019-04-26 | 上海应用技术大学 | A kind of N doping mesoporous carbon spheres Nonmetal oxygen reduction catalyst, preparation method and application |
| CN109970046A (en) * | 2019-05-07 | 2019-07-05 | 江西铜业技术研究院有限公司 | A kind of preparation method of slim pipe diameter carbon nanotube |
| CN109970046B (en) * | 2019-05-07 | 2022-03-25 | 江西铜业技术研究院有限公司 | Preparation method of carbon nano tube with thin tube diameter |
| CN111001428A (en) * | 2019-12-24 | 2020-04-14 | 山西大学 | Metal-free carbon-based electrocatalyst, preparation method and application |
| CN116120567A (en) * | 2022-11-18 | 2023-05-16 | 电子科技大学长三角研究院(湖州) | Preparation method and application of nitrogen-rich nickel-based coordination polymer and derivative material thereof |
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