CN109876859A - A kind of composite material and preparation method of ion liquid functionalization carbon nanotube - Google Patents
A kind of composite material and preparation method of ion liquid functionalization carbon nanotube Download PDFInfo
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- CN109876859A CN109876859A CN201910232339.7A CN201910232339A CN109876859A CN 109876859 A CN109876859 A CN 109876859A CN 201910232339 A CN201910232339 A CN 201910232339A CN 109876859 A CN109876859 A CN 109876859A
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- carbon nanotube
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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
Abstract
The invention discloses a kind of composite materials of ion liquid functionalization carbon nanotube, ionic liquid imidazole radicals is cation, iodide ion, tetrafluoride boron, phosphorus hexafluoride and bis- (fluoroform sulphonyl) imines are respectively as anion, ionic liquid is connected directly between carbon nano tube surface by covalent bond, connects between the two without other atoms.The invention also discloses the preparation method of the composite material, by functional amido carbon nanotube and formaldehyde, glyoxal, ammonium acetate hybrid reaction in methyl alcohol.Iodomethane is added in product later, finally obtains methylimidazole salt compounded of iodine functionalized carbon nano-tube.Then by anion exchange, other ion liquid functionalization carbon nanotubes are obtained.The present invention is applied to the above composite material as liberation of hydrogen catalyst in electrolysis water, and Ionic Liquid Modified carbon nanotube has excellent catalytic activity for hydrogen evolution, and ionic liquid can also play the role of adhesive.
Description
Technical field
The invention belongs to carbon nano tube compound material technical field more particularly to a kind of ion liquid functionalization carbon nanotubes
Composite material more particularly relates to a kind of preparation method of ion liquid functionalization carbon nano-tube material and its is catalyzed as liberation of hydrogen
The application of agent.
Background technique
At present, the energy crisis and problem of environmental pollution that the whole world is faced are increasingly serious, threaten the life of the mankind
It deposits and develops；At the same time, nearly exhausted with non-renewable energy resources such as coal, natural gas and petroleum, and caused by this kind of energy
It pollutes very serious.Therefore, Renewable Energy Development, walking sustainable development path becomes the focus of scholars' research.Each
In kind of novel renewable energy, solar energy, wind energy etc. is easy by landform, the such environmental effects such as weather, and be not easy storage and
Transport has very big application limitation.And Hydrogen Energy has fossil fuel and incomparable advantage (such as resource of other new energy
Abundant, circulation is renewable, and high-efficiency environment friendly can store, widely used etc.).Therefore, Hydrogen Energy increasingly attracts people's attention, and is recognized
For a kind of ideal free of contamination green energy resource.In various hydrogen producing technologies, it is most widely used and mature that electrolysis water, which is no different,
's.Its simple process will not generate pollution, and hydrogen production process generates hydrogen and oxygen by raw material of water, is that hydrogen reacts life with oxygen
The inverse process of Cheng Shui.
It is electrolytic cell in the core of water electrolysis hydrogen production technology, and the key component of electrolytic cell is to load on the electrode
Catalyst.Liberation of hydrogen overvoltage can be effectively reduced in outstanding cathod catalyst, guarantee while reducing energy consumption and electrolysis cost
Good liberation of hydrogen efficiency.Currently, there are two main classes for electrolysis water cathode for hydrogen evolution catalyst.One kind is traditional Pt, Pd and its alloy.
This kind of electrode has very low overpotential of hydrogen evolution, but content is rare and expensive, is not suitable for large-scale application.It is another kind of be Mo,
The alloys such as Ni, Fe or metal oxygen (sulphur) compound.Compared to precious metals such as Pt, such electrode reduce costs maintain compared with
Low overvoltage, but such electrode still will use such as Mo " rare metal ", while its synthesis process is still to consumption mass energy
And it is had certain limitations in stability and corrosion resistance.Recently, conductive polymer material (polyaniline, polypyrrole, polyaniline-
Polypyrrole) be applied in water electrolysis hydrogen production as nonmetallic elctro-catalyst, but its there is still a need for Pt pieces as carrier and catalytic performance
Do not have and obviously mentions；C3N4And C60(OH)8There is catalysis performance well as nonmetallic liberation of hydrogen catalyst, but it synthesizes item
Part is complicated and preparation cost is higher.In addition, the above most liberation of hydrogen catalyst requires expensive Nafion as adhesive
It loads on electrode.Therefore, a kind of novel metalloid liberation of hydrogen catalyst cheap and easily-available while that there is good catalytic efficiency is developed
It is more and more important, and ionic liquid-carbon nano tube compound material is exactly a kind of ideal potential substitute as catalyst.
Ionic liquid (Ionic liquids, ILs) is that the fusing point that organic cation and various anion are constituted is lower than 100
DEG C molten salt system, there is electrochemical window mouth width, conductivity is high, and toxicity is low, excellent dissolution ability and stronger chemical stability etc.
Advantage.Therefore, ionic liquid is widely applied to organic synthesis, in abstraction technique and electrochemistry.Carbon nanotube (Carbon
Nanotubes, CNTs) it is a kind of coaxial circles of the single layer (wall) being made of the carbon atom of hexagonal array to tens of layers (wall)
Pipe carbon molecules.Its with special mechanics, electricity and chemical property, such as high intensity, high-melting-point, outstanding electron conduction and
Heat conductivity.In electro-catalysis, carbon nanotube is widely used as catalyst carrier.Therefore, it is excellent to be provided simultaneously with both of the above
The Ionic Liquid Modified carbon nano tube compound material of point is paid close attention to by various countries researcher naturally, is widely applied to every electrochemistry
In research, and the key issues of its application and those skilled in the art's research as liberation of hydrogen catalyst in electrolysis water.
Summary of the invention
In view of this, it is an object of the invention to: a kind of ion liquid functionalization carbon nanotube (IL-CNTs) (1) is provided
Preparation method.(2) prepare ionic liquid directly connect with carbon nanotube, between there is no other atoms.(3) pass through the side
The preparation of ion liquid functionalization carbon nanotube is completed in method preparation while synthesizing ionic liquid, simple and quick.(4) ion
Liquid functional carbon nano tube has good chemical property as electrolysis water cathode for hydrogen evolution catalyst.
In order to achieve the above objectives, the invention provides the following technical scheme:
1. ion liquid functionalization preparation method of carbon nano-tube, comprising the following steps:
(1) formaldehyde is mixed with glyoxal solution according to molar ratio 1:1, and ammonium acetate and functional amido carbon nanotube are added later,
80oIt is reacted 6 hours in C methanol；Head product obtains imidazoles functionalized carbon nano-tube after sodium hydroxide washs；The vinegar
Sour ammonium and formaldehyde mole ratio are 1:2；
(2) above-mentioned imidazoles functionalized carbon nano-tube is added in iodomethane, 80oIt reacts 6 hours, finally obtains in C methanol
Methylimidazole metal iodide ions liquid functional carbon nano tube；The mass ratio 1 of the imidazoles functionalized carbon nano-tube and iodomethane:
1；The molar ratio of the iodomethane and formaldehyde is 1:1；
(3) methylimidazole metal iodide ions liquid functional carbon nano tube and excessive ion exchange reagent are subjected to anion exchange
Reaction, obtains the imidazolium ionic liquid functionalized carbon nano-tube of different anions；The ion-exchanger be sodium fluoborate,
One of Potassium Hexafluorophosphate and double trifluoromethanesulfonimide lithiums.
2. being catalyzed as liberation of hydrogen in electrolysis water using the ion liquid functionalization carbon nanotube prepared by method described above
Application in liberation of hydrogen.
The beneficial effects of the present invention are: the present invention provides a kind of directly in carbon nano tube surface connection ionic liquid
Preparation method does not have the connection of any other atom between ionic liquid and carbon nanotube.The preparation method of offer is in synthesis ion
The preparation of functionalized carbon nano-tube is completed while liquid, process is simple and quick.Such ion liquid functionalization carbon nanotube is made
Higher catalyst activity and good stability are shown for electrolysis water cathode for hydrogen evolution catalyst, and ionic liquid can also rise
To the effect of adhesive, it is not necessarily to additional Nafion, reduces use cost.
Detailed description of the invention
In order to keep the purpose of the present invention, technical scheme and beneficial effects clearer, the present invention provides following attached drawing:
Fig. 1 is the schematic diagram that ion liquid functionalization carbon nanotube is prepared in embodiment 1.
Fig. 2 is the scanning electron microscope (SEM) photograph of ion liquid functionalization carbon nanotube prepared by embodiment 1.
Fig. 3 is the infrared figure of 1 gained ion liquid functionalization carbon nanotube of embodiment.
Fig. 4 is the electrolysis water Electrocatalytic Property for Hydrogen Evolution figure of ion liquid functionalization carbon nanotube described in embodiment 1.
Specific embodiment
Below in conjunction with attached drawing, a preferred embodiment of the present invention will be described in detail.
The preparation of 1 ion liquid functionalization carbon nanotube of embodiment
The preparation step schematic diagram of methylimidazolyl ion liquid functionalization carbon nanotube is as shown in Figure 1, the specific steps are as follows:
1) ammonium acetate and functional amido carbon nanometer is added according to molar ratio 1:1 ultrasonic mixing in formaldehyde and glyoxal solution later
Pipe, 80oIt is reacted 6 hours in C methanol.Head product obtains imidazoles functionalized carbon after the washing of (0.1 M) sodium hydroxide solution and receives
Mitron；Wherein the molar ratio of ammonium acetate and formaldehyde is 1:2；
2) above-mentioned imidazoles functionalized carbon nano-tube is added in iodomethane solution, 80oIt is reacted 6 hours in C methanol, final
To methylimidazole metal iodide ions liquid functional carbon nano tube MIM-I-CNTs；Wherein imidazoles functionalized carbon nano-tube and iodomethane
Mass ratio 1:1；The molar ratio of iodomethane and formaldehyde is 1:1；
3) by the MIM-I-CNTs of preparation and excess amount of ions exchanger sodium fluoborate NaBF4, Potassium Hexafluorophosphate KPF6With double trifluoros
Sulfonyl methane imine lithium LiNTf2Anion exchange reaction is carried out, respectively obtains and is received containing methylimidazole tetrafluoride boron functionalized carbon
Mitron MIM-BF4- CNTs, methylimidazole phosphorus hexafluoride functionalized carbon nano-tube MIM-PF6- CNTs and the double fluoroforms of methylimidazole
Alkane sulfimide functionalized carbon nano-tube MIM-NTf2-CNTs。
Fig. 2 is the scanning electron microscope (SEM) photograph of prepared ion liquid functionalization carbon nanotube, it can be seen that ion liquid functionalization
Afterwards, the basic pattern of carbon nanotube does not change, and basic framework remains intact.
Fig. 3 is the infrared figure of gained ion liquid functionalization carbon nanotube, it can be seen that Fig. 3 (a) is raw material amido function
The infrared spectrum of carbon nano tube, the characteristic peak with amido etc.；And Fig. 3 (b) is product ion liquid functional carbon nano tube
Infrared spectrum, with imidazole radicals characteristic peak.Prove that ion liquid functionalization carbon nanotube is successfully prepared.
Methylimidazolyl ion liquid functionalization carbon nanotube is surveyed as electrolysis water liberation of hydrogen catalyst and chemical property
Examination:
MIM-I-CNTs, MIM-BF of preparation are taken respectively4-CNTs、MIM-PF6- CNTs and MIM-NTf2- CNTs is urged as liberation of hydrogen
Agent is equably coated on glass-carbon electrode (about 5 mm of diameter).Water electrolysis hydrogen production experiment carries out on electrochemical workstation, with 3
Electrode system (working electrode: the glass-carbon electrode of supported catalyst；To electrode: platinum plate electrode；Reference electrode: saturation calomel electricity
Pole).Solution containing 100 μ g catalyst be added in working electrode surface then each dry Electrolytic Water Experiment in triplicate it is above with
Guarantee that data are accurate and reliable.
As shown in fig. 4 a, electro-chemical test has been carried out by IL-CNTs of the linear voltammetry to preparation.It can reflect out
Under the conditions of same, there is highest current density (j) and lower overpotential of hydrogen evolution (E by MIM-I-CNTsonset).Pass through meter
The Tafel curve for calculating the above catalyst hydrolysis obtains as shown in Figure 4 b as a result, MIM-I-CNTs has best liberation of hydrogen power
Learn characteristic.By the way that ac impedance measurement (EIS) is carried out, as illustrated in fig. 4 c, discovery MIM-I-CNTs material is effectively reduced
Faradaic impedance, conductivity are high.By LSV curve test in Fig. 4 d, it is found that MIM-I-CNTs after 700 circle CV circulations, is catalyzed
Activity does not reduce, and has good electrochemical stability.
It can verify that ionic liquid-carbon nano tube compound material disclosed by the invention with excellent using test experiments by above
Different catalytic activity for hydrogen evolution, and ionic liquid also plays the effect of adhesive, IL-CNTs directly can be loaded to electrolysis
On, without separately adding Nafion.
Finally, it is stated that preferred embodiment above is only used to illustrate the technical scheme of the present invention and not to limit it, although logical
It crosses above preferred embodiment the present invention is described in detail, however, those skilled in the art should understand that, can be
Various changes are made to it in form and in details, without departing from claims of the present invention limited range.
Claims (3)
1. a kind of preparation method of the composite material of ion liquid functionalization carbon nanotube, which is characterized in that including following preparation
Step:
(1) formaldehyde is mixed with glyoxal solution according to molar ratio 1:1, and ammonium acetate and functional amido carbon nanotube are added later,
80oIt is reacted 6 hours in C methanol；Imidazoles functionalized carbon nano-tube is obtained after sodium hydroxide washing；The ammonium acetate and first
The molar ratio of aldehyde is 1:2；
(2) above-mentioned imidazoles functionalized carbon nano-tube is added in iodomethane, 80oIt is reacted 6 hours in C methanol, finally obtains first
Base iodonium imidazolide salts ion liquid functionalization carbon nanotube；The mass ratio 1:1 of the imidazoles functionalized carbon nano-tube and iodomethane；
The molar ratio of the iodomethane and formaldehyde is 1:1;
(3) then by carrying out yin to methylimidazole metal iodide ions liquid functional carbon nano tube and excessive ion exchange reagent
Ion-exchange reactions obtains the imidazolium ionic liquid functionalized carbon nano-tube of different anions.
2. a kind of preparation method of the composite material of ion liquid functionalization carbon nanotube according to claim 2, special
Sign is that ion-exchanger described in step (3) is in sodium fluoborate, Potassium Hexafluorophosphate and double trifluoromethanesulfonimide lithiums
It is a kind of.
3. the composite material of ion liquid functionalization carbon nanotube according to claim 1, can load on the cathode electrode
It is applied in electrolysis water as liberation of hydrogen catalyst.
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| CN113264516A (en) * | 2021-07-21 | 2021-08-17 | 温州玖源锂电池科技发展有限公司 | Preparation method of lithium iron vanadium phosphate carbon nanotube modified ternary cathode material |
| CN113755075A (en) * | 2021-09-18 | 2021-12-07 | 浙江树人学院（浙江树人大学） | Ionic liquid functionalized carbon nanotube super-anticorrosion paint |
| CN114232012A (en) * | 2021-09-29 | 2022-03-25 | 中国科学院金属研究所 | Ionic liquid modified nano carbon material catalyst and preparation method and application thereof |
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