CN106345501B - A kind of method that iron phosphide is prepared based on the carbon nano-tube modified composite material of magnetic ionic liquids and products thereof and application - Google Patents
A kind of method that iron phosphide is prepared based on the carbon nano-tube modified composite material of magnetic ionic liquids and products thereof and application Download PDFInfo
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- CN106345501B CN106345501B CN201610817477.8A CN201610817477A CN106345501B CN 106345501 B CN106345501 B CN 106345501B CN 201610817477 A CN201610817477 A CN 201610817477A CN 106345501 B CN106345501 B CN 106345501B
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/185—Phosphorus; Compounds thereof with iron group metals or platinum group metals
- B01J27/1853—Phosphorus; Compounds thereof with iron group metals or platinum group metals with iron, cobalt or nickel
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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
- 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
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
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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 method preparing iron phosphide based on the carbon nano-tube modified composite material of magnetic ionic liquids and products thereof and application, the preparation method includes the following steps:1) by magnetic ionic liquids and carbon nanotube with mass ratio 0.1 0.2:Then 0.1 0.4 uniformly mixing are added methanol and continue grinding 15 45 minutes, dry to obtain composite material;2) with mass ratio 0.1 0.2:0.1 0.3, composite material prepared by step 1) is uniformly mixed with sodium hypophosphite, heats in ar gas environment tube furnace and obtains iron phosphide in 8 16 hours for 250 400 DEG C.The iron phosphide of preparation is loaded into cathode as liberation of hydrogen catalyst and is applied in electrolysis wate research, finds it with good catalytic activity.
Description
Technical field
The invention belongs to carbon nano tube compound material technical fields more particularly to a kind of use to be repaiied based on magnetic ionic liquids
The composite material for adoring carbon nanotube more particularly relates to method based on such material preparation iron phosphide and as liberation of hydrogen catalyst
Application.
Background technology
Currently, the energy crisis and problem of environmental pollution that the whole world is faced are increasingly serious, the existence of the mankind threaten
And development, it is at the same time, nearly exhausted with non-renewable energy resources such as coal, natural gas and oil and dirty caused by this kind of energy
Dye is very serious.Therefore, Renewable Energy Development, walking sustainable development path becomes the focus of scholars' research.Various
In novel renewable energy, solar energy, wind energy etc. is easy by such environmental effects such as landform, weathers, and is not easy to store and be transported
It is defeated, there is prodigious application limitation.Hydrogen Energy has fossil fuel, and (such as resource is rich with the incomparable advantage of other new energy
Richness, cycle is renewable, and high-efficiency environment friendly can store, widely used etc.).Therefore, Hydrogen Energy increasingly attracts people's attention, and is considered
A kind of ideal free of contamination green energy resource.In various hydrogen producing technologies, it is most widely used and ripe that electrolysis water, which is no different,.
Its is simple for process, not will produce pollution, and hydrogen production process generates hydrogen and oxygen by raw material of water, is that hydrogen reacts generation water with oxygen
Inverse process.
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.Excellent cathod catalyst can effectively reduce liberation of hydrogen overvoltage, ensure while reducing energy consumption and electrolysis cost
Good liberation of hydrogen efficiency.Currently, in water electrolysis hydrogen production catalyst, traditional Pt, Pd and its alloy have very low liberation of hydrogen excessively electric
Position, high catalytic efficiency, but its content are rare and expensive, are not suitable for large-scale application.Development is a kind of efficient, stable while honest and clean
The electrolysis water catalyst that valence is easy to get just is particularly important.Therefore, the metal phosphides such as Mo, Ni, Fe are widely studied and apply
Into water electrolysis hydrogen production.In such phosphide, iron phosphide due to the cheap and huge content of itself be considered as it is optimal,
The liberation of hydrogen catalyst of energy large-scale application.
Ionic liquid (Ionic liquids, ILs) is that the fusing point that organic cation and various anion are constituted is less than 100
DEG C molten salt system, have electrochemical window mouth width, conductivity high, toxicity is low, excellent dissolution ability and stronger chemical stability etc.
Advantage.Magnetic ionic liquids (Magnetic ionic liquids, MILs) can be adsorbed on magnet, add magnetic fields outside
The ionic liquid with certain intensity of magnetization, anion contain the transition metal such as Fe, Co down.Carbon nanotube (Carbon
Nanotubes, CNTs) it is a kind of coaxial pipe of the single layer (wall) being made of the carbon atom of hexagonal array to tens of layers (wall)
Carbon molecules.It is with special mechanics, electricity and chemical property, such as high intensity, high-melting-point, outstanding electron conduction and heat
Conductibility.In electro-catalysis, carbon nanotube is widely used as catalyst carrier.Therefore, pass through phosphatization magnetic ionic liquids
Carbon nano-tube modified composite material can effectively be combined MILs with the advantages of CNTs to prepare iron phosphide, be obtained preferably
Liberation of hydrogen catalyst.
Invention content
In view of this, the purpose of the present invention is to provide one kind being based on the carbon nano-tube modified composite material of magnetic ionic liquids
Method for preparing iron phosphide and products thereof and application, the present invention pass through synthesizing new functional magnetic ionic liquid, such ion
Liquid anion contains ferric ion, while cation is capable of the conductivity of reinforcing material to mention catalysis effect after phosphatization
Rate.
In order to achieve the above objectives, the present invention specifically provides the following technical solution:
1, a kind of method that iron phosphide is prepared based on the carbon nano-tube modified composite material of magnetic ionic liquids, including walk as follows
Suddenly:
1) by magnetic ionic liquids and carbon nanotube with mass ratio 0.1-0.2:0.1-0.4 is uniformly mixed, and first is then added
Alcohol continues grinding 15-45 minutes, dries to obtain composite material;
2) with mass ratio 0.1-0.2:0.1-0.3 uniformly mixes composite material prepared by step 1) with sodium hypophosphite,
250-400 DEG C of heating obtains iron phosphide in 8-16 hours in ar gas environment tube furnace.
Preferably, the magnetic ionic liquids are 1- amine propyl -3- methylimidazole bromine tri-chlorinations molysite, poly- (vinyl miaow
Azoles bromine tri-chlorination molysite) or N, N- bis- (4- (methoxycarbonyl) phenyl)-n- methylglucosamine bromine tri-chlorination molysite.
Magnetic ionic liquids preparation method reference literature " the Extraction of DNA by Magnetic
Ionic Liquids:Tunable Solvents for Rapid and Selective DNA Analysis
(Analytical Chemistry 2015,87,1552)”
The specific composition principle circuit of iron phosphide is as follows:
2, the iron phosphide prepared based on the carbon nano-tube modified composite material of magnetic ionic liquids obtained according to the method.
3, iron phosphide the answering as liberation of hydrogen catalyst prepared based on the carbon nano-tube modified composite material of magnetic ionic liquids
With.
The beneficial effects of the present invention are:The present invention proposes a kind of completely new based on magnetic ionic liquids modified carbon nanometer
The iron phosphide of preparation is loaded to cathode as liberation of hydrogen catalyst and is applied to electrolysis by the iron phosphide preparation method of pipe composite material
In wate research.Magnetic ionic liquids anion contains ferric ion, while the cationic dehydration carbonization after phosphatization is to enhance
The conductivity of material.Carbon nanotube is outstanding conductive material.The liberation of hydrogen efficiency of catalyst can be greatly improved above.Simultaneously
Such preparation method required temperature is relatively low, and raw material is cheap, can significantly reduce the cost of water electrolysis hydrogen production, has huge answer
Use foreground.
Description of the drawings
In order to keep the purpose of the present invention, technical solution and advantageous effect clearer, the present invention provides following attached drawing:
Fig. 1 shows the iron phosphides prepared based on the carbon nano-tube modified composite material of 3 kinds of magnetic ionic liquids to be urged as liberation of hydrogen
Agent carries out the LSV curves of electro-chemical test;
Fig. 2 indicates that the iron phosphide prepared based on the carbon nano-tube modified composite material of 3 kinds of magnetic ionic liquids is urged as liberation of hydrogen
Agent carries out the Tafel curves of electro-chemical test;
Fig. 3 indicates that the iron phosphide prepared based on the carbon nano-tube modified composite material of 3 kinds of magnetic ionic liquids is urged as liberation of hydrogen
The EIS collection of illustrative plates of agent.
Specific implementation mode
The preferred embodiment of the present invention is described in detail below in conjunction with attached drawing.Specific item is not specified in embodiment
The experimental method of part, usually according to conventional conditions or according to the manufacturer's recommendations.
Embodiment 1
1, the synthesis of magnetic ionic liquids
1- amine propyl -3- methylimidazoles bromides and Iron(III) chloride hexahydrate are in molar ratio:1:2 mix in ethanol, room temperature
Stirring 24 hours, after filtering and removing excess reactant with ethyl alcohol, product is simultaneously put into the drying 24 hours of 65 DEG C of vacuum drying chamber, obtains
To magnetic ionic liquids 1- amine propyl -3- methylimidazole bromine tri-chlorination molysite (AMIM-FeCl3Br).Under same step, gather
(vinyl imidazole bromide) P (VBIM-Br) and N, N- bis- (4- (methoxycarbonyl) phenyl)-n- methylglucosamine bromides (MBMG-
Br poly- (vinyl imidazole bromine tri-chlorination molysite) [P (VBIM-FeCl) are obtained by the reaction with Iron(III) chloride hexahydrate respectively3Br)] and
N, N- bis- (4- (methoxycarbonyl) phenyl)-n- methylglucosamine bromine tri-chlorination molysite (MBMG-FeCl3Br)。
2, the preparation of magnetic ionic liquids-carbon nano-tube material
In mass ratio 1:1 uniformly mixes three classes magnetic ionic liquids with carbon nanotube in mortar respectively, adds second
Alcohol is ground 30 minutes, obtains composite A MIM- within finally dry 24 hours under conditions of 65 DEG C in vacuum drying chamber
FeCl3Br/CNTs、[P(VBIM-FeCl3Br)]/CNTs, MBMG-FeCl3Br/CNTs。
3, the preparation method of iron phosphide and the application in water electrolysis hydrogen production;
In mass ratio 1:1 uniformly mixes three kinds of composite materials with sodium hypophosphite respectively, 300 in ar gas environment tube furnace
DEG C heating 12 hours, finally obtain three kinds of iron phosphides (AMIM-FeP/CNTs, P (VBIM)-FeP/CNTs, MBMG-FeP/
CNTs).Meanwhile by Iron(III) chloride hexahydrate and MBMG-FeCl3Br is being added without carbon nanotube and other conditions are constant respectively
In the case of phosphatization obtain simple FeP and MBMG-FeP as a contrast.
Application Example
The compound application for preparing iron phosphide as liberation of hydrogen catalyst in electrolysis water of magnetic ionic liquids-carbon nanotube.
Water electrolysis hydrogen production experiment carries out on electrochemical workstation, with 3 electrode system (working electrodes:Supported catalyst
Glass-carbon electrode;To electrode:Platinum plate electrode;Reference electrode:Saturated calomel electrode).Solution containing 100 μ g catalyst is added in work
Making electrode surface, then each dry Electrolytic Water Experiment is above to ensure that data are accurate and reliable in triplicate.
As shown in Figure 1, by linear voltammetry to the AMIM-FeP/CNTs (e) of preparation, P (VBIM)-FeP/CNTs (c),
MBMG-FeP/CNTs (d) and FeP (a), MBMG-FePa (b) have carried out electro-chemical test.It can be reflected in same item by Fig. 1
Under part, the catalyst obtained than simple phosphatization by the iron phosphide of the carbon nano-tube modified preparation of magnetic ionic liquids has higher electricity
Current density (j) and lower overpotential of hydrogen evolution (Eonset).
By calculating the Tafel curves of above catalyst hydrolysis, obtain it is as shown in Figure 2 as a result, by Fig. 2 can reflect by
The iron phosphide of the carbon nano-tube modified preparation of magnetic ionic liquids has better liberation of hydrogen power than the catalyst that simple phosphatization obtains
Learn characteristic, it can be seen that, the addition of carbon nanotube effectively raises the electric conductivity of catalyst, and ionic liquid cation is in phosphorus
Conductivity/electric charge transfer speed that carbonization further increases catalyst can be dehydrated during change, to improve catalyst liberation of hydrogen
Activity.
By being exchanged with MBMG-FeP/CNTs (c) AMIM-FeP/CNTs (a), P (VBIM)-FeP/CNTs (b)
Testing impedance (EIS), as shown in fig. 3, it was found that MBMG-FeP/CNTs materials effectively reduce Faradaic impedance, thus into one
Carbonization occurs in parkerizing process for ionic liquid cation of the step explanation based on glucose to improve the conductivity of catalyst.
It can verify that by above application test experiments disclosed by the invention by ionic liquid-carbon nano tube compound material preparation
Iron phosphide have excellent catalytic activity for hydrogen evolution.
Finally illustrate, preferred embodiment above is merely illustrative of the technical solution of the present invention and unrestricted, 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 method preparing iron phosphide based on the carbon nano-tube modified composite material of magnetic ionic liquids, which is characterized in that packet
Include following steps:
1)By magnetic ionic liquids and carbon nanotube with mass ratio 0.1-0.2:0.1-0.4 is uniformly mixed, then be added methanol after
Continuous grinding 15-45 minutes, dries to obtain composite material;The magnetic ionic liquids are 1- amine propyl -3- methylimidazole bromine tri-chlorinations
Molysite gathers(Vinyl imidazole bromine tri-chlorination molysite)Or N, N- bis-(4 -(Methoxycarbonyl)Phenyl)- n- methylglucosamine bromines
Tri-chlorination molysite;
2)With mass ratio 0.1-0.2:0.1-0.3, by step 1)The composite material of preparation is uniformly mixed with sodium hypophosphite, in argon gas
250-400 DEG C of heating obtains iron phosphide in 8-16 hours in environment tube furnace.
2. the phosphorus prepared based on the carbon nano-tube modified composite material of magnetic ionic liquids that method obtains according to claim 1
Change iron.
3. the iron phosphide prepared based on the carbon nano-tube modified composite material of magnetic ionic liquids described in claim 2 is urged as liberation of hydrogen
The application of agent.
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CN108448120A (en) * | 2018-03-13 | 2018-08-24 | 北京化工大学 | Fe/PIL/MWCNTs fuel-cell catalysts and preparation method thereof |
CN108889323B (en) * | 2018-06-20 | 2021-04-13 | 西南大学 | Co2Microwave preparation method and application of P @ CNTs cathode material |
CN109402663B (en) * | 2018-09-04 | 2021-09-07 | 青岛科技大学 | Preparation of FePx with 3D mesoporous structure and application of FePx in hydrogen production by electrolyzing water |
CN109267094B (en) * | 2018-10-19 | 2020-07-24 | 温州大学 | Heteroatom-doped porous carbon/iron phosphide composite material |
CN109876859B (en) * | 2019-03-26 | 2021-08-06 | 西南大学 | Composite material of ionic liquid functionalized carbon nanotube and preparation method thereof |
CN110468433B (en) * | 2019-09-02 | 2021-08-20 | 江西理工大学 | Method for preparing Sm-Co alloy film by low-temperature electrodeposition |
CN116618070B (en) * | 2023-05-22 | 2024-01-05 | 福建省福能龙安热电有限公司 | Environment-friendly denitration catalyst and preparation method thereof |
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