CN106207197A - A kind of method using hair to prepare bifunctional electrocatalyst - Google Patents
A kind of method using hair to prepare bifunctional electrocatalyst Download PDFInfo
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- CN106207197A CN106207197A CN201610534672.XA CN201610534672A CN106207197A CN 106207197 A CN106207197 A CN 106207197A CN 201610534672 A CN201610534672 A CN 201610534672A CN 106207197 A CN106207197 A CN 106207197A
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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
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
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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
- H01M4/90—Selection of catalytic material
- H01M4/9091—Unsupported catalytic particles; loose particulate catalytic materials, e.g. in fluidised state
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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
- Y02E60/50—Fuel cells
Abstract
A kind of method using hair to prepare bifunctional electrocatalyst, belongs to catalyst technical field.Biomass hair, via pre-carbonization, activation doping, high temperature pyrolysis process, obtains the material with carbon element with the grade pore structure of different element doping, and material has hydrogen reduction and the oxygen precipitation electrocatalysis characteristic of excellence.With traditional preparation method is compared, the present invention uses that storage is big, price is low, eco-friendly biomass hair is raw material, and preparation process is simple and is not related to toxic reagent, can realize large-scale production.The bifunctional electrocatalyst of the present invention for fuel cell, electrolytic water device, can the field such as air cell of discharge and recharge have a wide range of applications.
Description
Technical field
The present invention relates to the preparation method of a kind of bifunctional electrocatalyst, specifically by biomass-based hair system of adulterating
The new method of standby bifunctional electrocatalyst, belongs to catalyst technical field.
Background technology
Fuel cell is a kind of TRT that chemical energy is converted directly into electric energy by chemical reaction, with traditional change
Stone fuel combustion is compared, and has energy conversion efficiency height, product cleaning, the feature of sustainable generating.But fuel battery negative pole
The Pt/C catalyst that oxygen reduction reaction is used, due to expensive, storage is rare, methanol tolerance poor stability, preparation technology are multiple
The various shortcoming such as miscellaneous, significantly limit the large-scale application of fuel cell, therefore, exploitation efficiently, stable, cheap hydrogen reduction
Catalysts, for promoting fuel cell extensively to apply and to alleviate Pressure on Energy significant.
Hydrogen, owing to its energy density is high, product cleans without CO2 emission, is more and more applied in petrochemical industry
In industry and fuel cell, in current technology of preparing, water electrolysis hydrogen production efficiency is high, technique is simple, technically reliable, but due to
The catalyst IrO that anodic oxygen evolution reaction is conventional2Or RuO2Expensive rareness and less stable, limit the big of water electrolysis hydrogen production
Sizable application.
Can discharge and recharge air cell be following portable equipment, the energy development direction of electric motor car, wherein, oxygen reduction reaction and
Oxygen evolution reaction correspondence electric discharge and charging process respectively.In current research, the catalyst of preparation mostly is simple function catalyst, only
Single oxygen reduction reaction catalysis demand can be met or oxygen separates out catalysis demand, so can increase can discharge and recharge air cell this
Plant technology difficulty and the cost of the device with dual catalytic demand, therefore, it is necessary to develop bifunctional base metal electricity
Catalyst.
In the research substituting noble metal-based catalysts, it is excellent that the porous carbon materials of Heteroatom doping is proved to have electric conductivity
Different, specific surface area is high, the advantage of good stability.Many studies have shown that, (N, S, P etc.) nano-carbon material of Heteroatom doping has
Good catalysis activity and stability.
Hair is as biomass rich in abundant organic matter, and after processing high temperature cabonization, product has high-ratio surface
Long-pending grade pore passage structure, abundant nitrogen content and sulfur content, is eelctro-catalyst elite clone.In addition, hair storage is rich
Rich, with low cost, environmental friendliness and renewable, is the very good material meeting energy demand.
Summary of the invention
It is an object of the invention to provide and a kind of prepare having of multiple element codope using biomass hair as raw material
The method of the porous carbon materials of difunctional electrocatalysis characteristic, it is simple to operate, easily realizes, can scale synthesis and environmental friendliness.
A kind of method using hair to prepare bifunctional electrocatalyst, it is characterised in that under atmosphere of inert gases, biological
Matter hair is via cleaning, pre-carbonization, interpolation activator and the compound of doping and carries out activating and high temperature pyrolysis process, obtains different
Atom doped grade hole material with carbon element bifunctional catalyst.
Further, the present invention solves the technical scheme that above-mentioned technical problem is used, and specifically includes following steps:
(1) using the hair of cleaning as presoma, pre-carbonization in the temperature programming tube furnace of protective gas atmosphere, will be pre-
Product after carbonization grinds, and obtains powder 1；
(2) add activator and the compound of doping of certain mass ratio, grind, in the temperature programming of atmosphere of inert gases
High-temperature activation in tube furnace, the product after activation, through pickling, washing, sucking filtration, vacuum drying, obtains powder 2；
(3) by powder 2 high temperature cabonization in temperature programming tube furnace, i.e. available with hair for raw material prepare difunctional
Eelctro-catalyst powder.
Demonstrated by a series of signs such as scanning electron microscope, transmission electron microscope, Raman spectrum, X-ray photoelectron spectroscopic analysis
Prepared material is high dispersive codope porous carbon materials.
Carry out pretreatment before the step (1): cleaned by hair and be cut into segment and be placed in tube furnace, tube furnace is being carried out
Before intensification, first evacuation, in order to the gas of absorption and other impurity in removal system, it is passed through noble gas；
Further, step (1) protection gas is noble gas, can be nitrogen, argon, helium, neon, Krypton, xenon or radon
Gas etc..
Further, the programming rate of step (1) pre-carbonisation is 0.5～20 DEG C/min.The temperature of pre-carbonization be 150～
400 DEG C, insulation 0.5～5h, naturally cools to room temperature at such a temperature.
Further, the temperature that step (2) activates is 400～900 DEG C, and insulation 0.5～7h, naturally cools at such a temperature
Room temperature.
Further, the activator of employing can be preferably KOH, NaOH, ZnCl2One or more in Deng.Powder 1 and institute
The mass ratio adding activator is (0.01～1): (1～9.99), during high-temperature activation under anaerobic, at activator
Effect under, material formed high-specific surface area multi-stage artery structure.
Further, the compound of doping for doping secondary carbon source or/and (carbon, carbon nitrogen source are little molecular effect in secondary nitrogen source
Preferably), the compound of doping is selected from glucose, sucrose, xylitol, carbamide, tripolycyanamide, dicyandiamide, cyanamide, thiourea, sulfur generation
One or more in the multiple compounds such as acetamide, powder 1 is (0.01～1) with the mass ratio of the compound adding doping:
(1～9.99).
The temperature of the final high temperature cabonization of step (3) is 600～1100 DEG C further, insulation 0.5～8h at such a temperature.From
So it is cooled to room temperature.Meanwhile, rear Buwen's degree of such scheme is more than or equal to back temperature, and all under protective atmosphere.
Further, pickling uses the mass fraction 36～HCl of 38%, washing to use deionized water, until pH reaches neutral.
Further, vacuum drying temperature is 40-100 DEG C, and the time is 4～18h.
The compound of doping is possible not only to complete in activation process, it is also possible to replace with in step (3) high temperature pyrolysis mistake
Journey completes.
Beneficial effects of the present invention is as follows:
1) present invention is with biomass hair as raw material, has successfully prepared sulfur, the porous carbon materials of nitrogen codope, hetero atom
Doping provide substantial amounts of avtive spot, promote the electrocatalysis characteristic of product.
2) porous carbon materials that biomass hair is obtained by activation and pyrolysis has the electric conductivity of excellence, high-specific surface area
And there is micropore, grade pore structure that mesoporous and macropore coexists, be more beneficial for the transmission of mass transfer and electric charge.
3) classes of compounds adulterated by change and doping, it is possible to achieve doped chemical kind and the control of content,
The degree of graphitization of char-forming material is regulated and controled also dependent on carburizing temperature and heating rate.
4) preparation process of the present invention avoids and uses toxic reagent and complicated synthesis technique, and preparation process is simple, operation
Convenient, easily realize large-scale production.
5) present invention uses biomass hair as raw material, and storage is abundant, with low cost, environmental friendliness and renewable,
Meet the demand of sustainable development instantly.
6) present invention has the difunctional electrocatalysis characteristic of excellence, for fuel cell, electrolytic water device, especially can fill
The air cell of electric discharge has broad application prospects.
Accompanying drawing explanation
Fig. 1 is to use hair to prepare the synthetic method schematic diagram of bifunctional electrocatalyst in embodiment 1.
Fig. 2 is the electron scanning micrograph of bifunctional electrocatalyst in embodiment 1.
Fig. 3 is the transmission electron microscope photo of bifunctional electrocatalyst in embodiment 1
Fig. 4 is the Raman spectrogram of bifunctional electrocatalyst in embodiment 1.
Fig. 5 is the X-ray photoelectron spectroscopic analysis of bifunctional electrocatalyst in embodiment 1
Fig. 6 is the distribution diagram of element of bifunctional electrocatalyst in embodiment 1.
Fig. 7 is the nitrogen adsorption curve of bifunctional electrocatalyst in embodiment 1.
Fig. 8 is the pore-size distribution of bifunctional electrocatalyst in embodiment 1.
Fig. 9 is the hydrogen reduction catalytic performance comparison diagram of the eelctro-catalyst in embodiment 1 and business Pt/C.
Figure 10 is the transfer electron number comparison diagram of the eelctro-catalyst in embodiment 1 and business Pt/C.
Figure 11 is the hydrogen peroxide yield comparison diagram of the eelctro-catalyst in embodiment 1 and business Pt/C.
Figure 12 is that the oxygen of the eelctro-catalyst in embodiment 1 and business Pt/C separates out catalytic performance comparison diagram.
Figure 13 is to use hair to prepare the electron scanning micrograph of bifunctional electrocatalyst in embodiment 2.
Figure 14 is to use hair to prepare the transmission electron microscope photo of bifunctional electrocatalyst in embodiment 2.
Figure 15 is to use hair to prepare the electron scanning micrograph of bifunctional electrocatalyst in embodiment 3.
Figure 16 is to use hair to prepare the transmission electron microscope photo of bifunctional electrocatalyst in embodiment 3.
Detailed description of the invention
In order to be illustrated more clearly that the present invention, below in conjunction with preferred embodiments and drawings, the present invention is done further
Bright.It will be appreciated by those skilled in the art that following specifically described content is illustrative and be not restrictive, should be with this
Limit the scope of the invention.Experimental drug derive from commercial channel (An Naiji, traditional Chinese medicines group, Beijing Chemical Plant, Du Pont,
AlfaAesar), purify the most further；
Embodiment 1: the method preparing bifunctional electrocatalyst for raw material with biomass hair
1) by hair at the acetone of 1:1: ethanol solution soaks, ultrasonic, to remove surface impurity, hair is being immersed in
In deionized water ultrasonic, washing several times, be then placed in the vacuum drying oven of 60 DEG C be dried 12h.
2) the uniform segment that the hair cleaned up is cut into about 5mm inserts little porcelain boat, and little porcelain boat is inserted program
In intensification tube furnace, first evacuation, it is then charged with noble gas, is heated to 250 DEG C with the heating rate of 5 DEG C/min, insulation
150min, naturally cools to room temperature.After being cooled to room temperature, by product mortar grinder, obtain powder 1.
3) taking 0.7g powder 1, add 2.1g NaOH, 2.8g carbamide, 2.1g glucose, mix homogeneously also grinds, inserts journey
Sequence intensification tube furnace, first evacuation, then pour noble gas, be heated to 600 DEG C with the heating rate of 5 DEG C/min, insulation
60min, naturally cools to room temperature.By the HCl washing that product mass fraction is 36-38% and some with deionized water rinsing
Secondary until pH=7.Product is dried in the vacuum drying oven of 60 DEG C 12h, obtains powder 2.
4) powder 2 is put in temperature programming tube furnace, then pass to noble gas.From room temperature with the speed of 5 DEG C/min
It is warmed up to 900 DEG C, is incubated 180min at such a temperature, naturally cools to room temperature, i.e. can get high dispersive S of black, N codope
Porous carbon materials H-Carbon-G-U.
Embodiment 2: the method preparing bifunctional electrocatalyst for raw material with biomass hair
1) by hair at the acetone of 1:1: ethanol solution soaks, ultrasonic, to remove surface impurity, hair is being immersed in
In deionized water ultrasonic, washing several times, be then placed in the vacuum drying oven of 60 DEG C be dried 12h.
2) the uniform segment that the hair cleaned up is cut into about 5mm inserts little porcelain boat, and little porcelain boat is inserted program
In intensification tube furnace, first evacuation, it is then charged with noble gas, is heated to 250 DEG C with the heating rate of 5 DEG C/min, insulation
150min, naturally cools to room temperature.After being cooled to room temperature, by product mortar grinder, obtain powder 1.
3) taking 0.7g powder 1, add 2.1g NaOH, 2.1g glucose, mix homogeneously also grinds, inserts temperature programming pipe
Formula stove, first evacuation, then pour noble gas, be heated to 600 DEG C with the heating rate of 5 DEG C/min, be incubated 60min, natural
It is cooled to room temperature.By the HCl washing that product mass fraction is 36-38%, and with deionized water rinsing several times until pH=
7.Product is dried in the vacuum drying oven of 60 DEG C 12h, obtains powder 2.
4) powder 2 is put in temperature programming tube furnace, then pass to noble gas.From room temperature with the speed of 5 DEG C/min
It is warmed up to 900 DEG C, is incubated 180min at such a temperature, naturally cools to room temperature, i.e. can get high dispersive S of black, N codope
Porous carbon materials H-Carbon-G.
Embodiment 3: the method preparing bifunctional electrocatalyst for raw material with biomass hair
1) by hair at the acetone of 1:1: ethanol solution soaks, ultrasonic, to remove surface impurity, hair is being immersed in
In deionized water ultrasonic, washing several times, be then placed in the vacuum drying oven of 60 DEG C be dried 12h.
2) the uniform segment that the hair cleaned up is cut into about 5mm inserts little porcelain boat, and little porcelain boat is inserted program
In intensification tube furnace, first evacuation, it is then charged with noble gas, is heated to 250 DEG C with the heating rate of 5 DEG C/min, insulation
150min, naturally cools to room temperature.After being cooled to room temperature, by product mortar grinder, obtain powder 1.
3) taking 0.7g powder 1, add 2.1g NaOH, 2.8g carbamide, mix homogeneously also grinds, inserts temperature programming tubular type
Stove, first evacuation, then pour noble gas, be heated to 600 DEG C with the heating rate of 5 DEG C/min, be incubated 60min, the coldest
But to room temperature.By the HCl washing that product mass fraction is 36-38%, and with deionized water rinsing several times until pH=7.
Product is dried in the vacuum drying oven of 60 DEG C 12h, obtains powder 2.
4) powder 2 is put in temperature programming tube furnace, then pass to noble gas.From room temperature with the speed of 5 DEG C/min
It is warmed up to 900 DEG C, is incubated 180min at such a temperature, naturally cools to room temperature, i.e. can get high dispersive S of black, N codope
Porous carbon materials H-Carbon-U.
Obviously, the above embodiment of the present invention is only for clearly demonstrating example of the present invention, and is not right
The restriction of embodiments of the present invention, for those of ordinary skill in the field, the most also may be used
To make other changes in different forms, cannot all of embodiment be given exhaustive here, every belong to this
What bright technical scheme was extended out obviously changes or changes the row still in protection scope of the present invention.
Fig. 4 is the Raman spectrogram of bifunctional electrocatalyst in embodiment 1, demonstrates D (1346cm in figure-1) peak, G
(1596cm-1) peak and 2D (2917cm-1) peak.D peak shows and represents the unordered of material with carbon element and defect.G peak means sp in material with carbon element2
The stretching of atom and vibration, 2D originates from peak the double resonance Raman Process that two contrary atoms of momentum participate in, passes through all
Sp prepared by chemical method2Material with carbon element is all found.
Fig. 6 shows it is the Elemental redistribution of C, O, N, S in embodiment 1, can substantially observe, N, S element is uniform
It is distributed in porous carbon materials.
Fig. 7 is the nitrogen adsorption curve of bifunctional electrocatalyst in embodiment 1, and its BET specific surface area is about 649m2/g。
Fig. 8 is the pore-size distribution of bifunctional electrocatalyst in embodiment 1, it can be seen that be that micropore, mesoporous and macropore coexist
Grade pore structure.
Claims (10)
1. one kind uses the method that hair prepares bifunctional electrocatalyst, it is characterised in that under atmosphere of inert gases, biomass
Hair is via cleaning, pre-carbonization, interpolation activator and the compound of doping and carries out activating and high temperature pyrolysis process, obtains different former
The grade hole material with carbon element bifunctional catalyst of son doping.
2. according to a kind of method using hair to prepare bifunctional electrocatalyst of claim 1, it is characterised in that specifically include
Following steps:
(1) using the hair of cleaning as presoma, pre-carbonization in the temperature programming tube furnace of protective gas atmosphere, by pre-carbonization
After product grind, obtain powder 1；
(2) add activator and the compound of doping of certain mass ratio, grind, in the temperature programming tubular type of atmosphere of inert gases
High-temperature activation in stove, the product after activation, through pickling, washing, sucking filtration, vacuum drying, obtains powder 2；
(3) by powder 2 high temperature cabonization in temperature programming tube furnace, the i.e. available difunctional electricity prepared for raw material with hair is urged
Agent powder.
3. according to a kind of method using hair to prepare bifunctional electrocatalyst of claim 2, it is characterised in that in step
(1) pretreatment is carried out before: cleaned by hair and be cut into segment and be placed in tube furnace, before tube furnace is heated up, first take out
Vacuum, in order to the gas of absorption and other impurity in removal system, is passed through noble gas.
4. according to a kind of method using hair to prepare bifunctional electrocatalyst of claim 2, it is characterised in that step (1),
(2), (3) protection gas be noble gas, nitrogen, argon, helium, neon, Krypton, xenon or radon gas.
5. according to a kind of method using hair to prepare bifunctional electrocatalyst of claim 2, it is characterised in that step (1)
The programming rate of pre-carbonisation is 0.5～20 DEG C/min.The temperature of pre-carbonization is 150～400 DEG C, is incubated at such a temperature
0.5～5h, naturally cool to room temperature.
6. according to a kind of method using hair to prepare bifunctional electrocatalyst of claim 2, it is characterised in that step (2)
The temperature of activation is 400～900 DEG C, and insulation 0.5～7h, naturally cools to room temperature at such a temperature.
7. according to a kind of method using hair to prepare bifunctional electrocatalyst of claim 2, it is characterised in that the work of employing
Agent is KOH, NaOH, ZnCl2In one or more；Powder 1 is (0.01～1) with the mass ratio of added activator: (1
～9.99)；The compound of doping for doping secondary carbon source or/and secondary nitrogen source, the compound of doping selected from glucose, sucrose,
One or more in the multiple compounds such as xylitol, carbamide, tripolycyanamide, dicyandiamide, cyanamide, thiourea, thioacetamide, powder
End 1 is (0.01～1) with the mass ratio of the compound adding doping: (1～9.99).
8. according to a kind of method using hair to prepare bifunctional electrocatalyst of claim 2, it is characterised in that step (3)
The temperature of final high temperature cabonization is 600～1100 DEG C, at such a temperature insulation 0.5～8h.Naturally cool to room temperature；A rear Buwen
Degree is more than or equal to back temperature.
9. according to a kind of method using hair to prepare bifunctional electrocatalyst of claim 2, it is characterised in that the change of doping
Compound replaces with and completes during step (3) high temperature pyrolysis.
10. the bifunctional electrocatalyst prepared according to claim 1-9 any one method.
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Cited By (8)
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| CN106684396A (en) * | 2016-12-21 | 2017-05-17 | 北京化工大学 | Method for preparing bifunctional catalyst from peanut hull |
| CN106784832A (en) * | 2016-12-14 | 2017-05-31 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of porous material and its application in sodium-ion battery |
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| CN109301273A (en) * | 2018-11-07 | 2019-02-01 | 东莞理工学院 | A kind of biomass derived carbon material and its preparation method and application |
| CN109368640A (en) * | 2018-10-17 | 2019-02-22 | 西安理工大学 | A method of classifying porous carbon material is prepared using hair base |
| CN111957295A (en) * | 2020-07-02 | 2020-11-20 | 齐鲁工业大学 | Preparation method and application of keratin-based porous carbon material |
| CN112054188A (en) * | 2020-09-15 | 2020-12-08 | 湖南大昊科技有限公司 | Ion battery cathode material and preparation method and application thereof |
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| CN108620021A (en) * | 2018-05-25 | 2018-10-09 | 中北大学 | Adsorb the hair base Carbon Materials and preparation method thereof of heavy metal ion |
| CN109368640A (en) * | 2018-10-17 | 2019-02-22 | 西安理工大学 | A method of classifying porous carbon material is prepared using hair base |
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| CN109301273A (en) * | 2018-11-07 | 2019-02-01 | 东莞理工学院 | A kind of biomass derived carbon material and its preparation method and application |
| US20220017367A1 (en) * | 2018-11-23 | 2022-01-20 | University Of Tartu | Carbon nanomaterial for use as a catalyst |
| CN111957295A (en) * | 2020-07-02 | 2020-11-20 | 齐鲁工业大学 | Preparation method and application of keratin-based porous carbon material |
| CN112054188A (en) * | 2020-09-15 | 2020-12-08 | 湖南大昊科技有限公司 | Ion battery cathode material and preparation method and application thereof |
| CN112054188B (en) * | 2020-09-15 | 2023-03-24 | 湖南大昊科技有限公司 | Negative electrode material of ion battery and preparation method and application thereof |
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