CN109244492A - A kind of efficient two-dimentional azepine Carbon Materials and preparation method thereof and the application in energy conversion field - Google Patents
A kind of efficient two-dimentional azepine Carbon Materials and preparation method thereof and the application in energy conversion field Download PDFInfo
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Abstract
The invention belongs to energy conversion technical field, a kind of efficient two-dimentional azepine Carbon Materials and preparation method thereof and the application in energy conversion field are disclosed, especially as application of the elctro-catalyst in oxygen reduction reaction and carbon dioxide electro-reduction reaction.The preparation method of the efficiently two-dimentional azepine Carbon Materials of the present invention includes the following steps: to synthesize two-dimentional silica using double-template, nitrogenous precursor is introduced into silica template, high temperature carbonization processing, removes silica template, obtains the efficient two-dimentional azepine Carbon Materials.The present invention also provides the efficient two-dimentional azepine Carbon Materials that the above method is prepared.It can sufficiently expose active site with unique 2 D mesopore structure, while be conducive to the transmission of active specy, show excellent electrocatalysis characteristic, can be applied to electrochemical energy conversion and storing technology.Especially as the application in elctro-catalyst under alkaline condition oxygen reduction reaction and alkaline condition carbon dioxide electro-reduction reaction.
Description
Technical field
The invention belongs to energy conversion technical field, in particular to a kind of efficient two-dimentional azepine Carbon Materials and preparation method thereof
With the application in energy conversion field, especially as elctro-catalyst in oxygen reduction reaction and carbon dioxide electro-reduction reaction
Application.
Background technique
Oxygen reduction reaction is the key that one step of energy conversion electrochemical process, is mainly used in fuel cell and metal-sky
Pneumoelectric pond.Efficient oxygen reduction reaction catalyst has always been considered as being the key factor for solving fuel cell, although platinum based catalyst
Just it is widely used in fuel cell in the sixties in 19th century, but to constrain it extensive for high price due to platinum and resource shortage
Application.Therefore, it is necessary to develop develop the novel even nonmetallic oxygen reduction reaction catalyst of non-platinum group metallic catalyst.
Carbon dioxide reduction is considered as a kind of promising mode for realizing global carbon at fuel.With other conversions
Mode compares, and the conversion of carbon dioxide electroreduction can carry out under normal temperature and pressure and temperate condition, therefore, carbon dioxide electroreduction
Reaction technology is one of very promising " electric energy-chemical energy " transformation technology.
Carbon based material, especially nanoporous Carbon Materials are expected to become next-generation oxygen reduction reaction and carbon dioxide electricity also
Former catalysts.Firstly, can effectively promote catalytic performance by surface modification and the modes such as atom doped；Second, it is flourishing
Hole is conducive to transmission of the electroactive substance in electrode；Third, nanometer confinement space exchange power transformation catalysis latent active
Provide more possibilities.In addition, porous carbon based material has been successfully applied to the capture of carbon dioxide, charcoal material surface dioxy
The adsorption activation for changing carbon is the precondition for promoting its reduction reaction to occur.
It is noted that conventional three-dimensional Carbon Materials active site majority is in long-range mesoporous wall, long-range is mesoporous
In the presence of the arrival for being unfavorable for active material.Reducing material dimension is considered as that one kind effectively solves concentration polarization and improves active sites
The method of utilization efficiency.
Summary of the invention
In order to overcome the shortcomings and deficiencies of the prior art described above, the primary purpose of the present invention is that providing a kind of efficient two dimension
The preparation method of azepine Carbon Materials.
Another object of the present invention is to provide the efficient two-dimentional azepine Carbon Materials of above method preparation.
The material that the method for the present invention is prepared has unique 2 D mesopore structure, can sufficiently expose catalytic active site
Point, while being conducive to the transmission of active specy, shows excellent electrocatalysis characteristic, can be applied to electrochemical energy conversion and
Storing technology.
Still a further object of the present invention is to provide application of the above-mentioned efficient two-dimentional azepine Carbon Materials in energy conversion field, special
It is not the application as elctro-catalyst in oxygen reduction reaction and carbon dioxide electro-reduction reaction.
The purpose of the present invention is realized by following proposal:
A kind of preparation method of efficient two-dimentional azepine Carbon Materials, includes the following steps: to synthesize two-dimentional dioxy using double-template
Nitrogenous precursor is introduced into silica template by SiClx, and high temperature carbonization processing removes silica template, obtains the height
Imitate two-dimentional azepine Carbon Materials.
In above-mentioned preparation method, the double-template is preferably graphene oxide (GO) and polyethylene oxide-polycyclic
Ethylene Oxide-polyethylene oxide triblock copolymer (P123).
In above-mentioned preparation method, in the double-template, the concentration of graphene oxide is preferably 1.0~5.0mg/mL,
The concentration of P123 is preferably 0.5~4.5mM.
In above-mentioned preparation method, the method for using double-template to synthesize two-dimentional silica is conventional dual-mode plate method
Step.Concretely: graphene oxide and P123 uniformly being mixed in the solution, assembling hydrolysis in acid condition obtains
Two-dimensional silica.The solution is aqueous solution, refers to and is adjusted to acid aqueous solution.
In above-mentioned preparation method, the nitrogenous charcoal source presoma includes but is not limited to Phen, pyrroles, aniline
At least one of.
In above-mentioned preparation method, the method that nitrogenous precursor is introduced into silica template can include: first immersion
Stain method, capillary condensation infusion process or ultrasonic immersing method etc..It specifically can comprise the following steps that incipient wetness impregnation method is by nitrogenous forerunner
Body is added in silica template, and 20~40 DEG C of vacuum impregnations 20~for 24 hours.Capillary condensation infusion process is by nitrogenous precursor
It is added in reaction kettle with silica template, 130~190 DEG C of 2~5h of holding are cooled to room temperature.Ultrasonic immersing method is that will contain
Nitrogen presoma is uniformly mixed with silica template, 6~10h of ultrasound, solvent evaporated at 20~50 DEG C.
In above-mentioned preparation method, the high temperature carbonization processing roasts 4 to be 650~1050 DEG C in inert atmosphere temperature
~6h.The inert atmosphere can be argon gas.
In above-mentioned preparation method, the removing silica template can be removed by alkali cleaning, as 8~10M can be used
Dipping by lye processing 20~for 24 hours.The lye can be sodium hydroxide solution.It is carried out under high temperature known to the immersion, such as 110 DEG C.
The present invention also provides the efficient two-dimentional azepine Carbon Materials that the above method is prepared.It is with unique 2 D mesopore
Structure can sufficiently expose active site, while be conducive to the transmission of active specy, show excellent electrocatalysis
Can, it can be applied in energy conversion field, especially as elctro-catalyst in oxygen reduction reaction and carbon dioxide electro-reduction reaction
In application.
The present invention compared with the existing technology, have the following advantages and the utility model has the advantages that
(1) the method for the present invention uses metal-free Carbon Materials, to realize oxygen reduction reaction and carbon dioxide electroreduction
Catalysts it is non-metallic；
(2) the method for the present invention introduces double-template in synthesis, reduces the dimension of Carbon Materials, has obtained high-specific surface area
Two-dimensional material.
(3) the method for the present invention realizes the Effective Doping of nitrogen using Phen, pyrroles, aniline as nitrogen source and charcoal source.
(4) catalyst that the method for the present invention is prepared both has excellent catalytic effect to oxygen reduction reaction, while to dioxy
Changing carbon reduction reaction has preferable performance.
Detailed description of the invention
Fig. 1 is the electron micrograph of the two-dimentional azepine Carbon Materials of 1 gained of embodiment.
Fig. 2 is the atomic force microscopy of the two-dimentional azepine Carbon Materials of 1 gained of embodiment.
Fig. 3 is the nitrogen Adsorption and desorption isotherms figure of the two-dimentional azepine Carbon Materials of 1 gained of embodiment.
Fig. 4 is oxygen reduction reaction polarization curve of the two-dimentional azepine Carbon Materials of 1 gained of embodiment in 0.1M potassium hydroxide.
Fig. 5 is carbon dioxide reduction reaction polarization of the two-dimentional azepine Carbon Materials of 1 gained of embodiment in 0.1M sodium bicarbonate
Curve.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
Material involved in the following example can be obtained from commercial channel.The dosage of each material is in the following example with matter
Measure part, parts by volume meter, g/mL.
Embodiment 1
(1) synthesis of two-dimentional earth silicon material
4.6 mass parts P123 are weighed to be added in the 116 parts by volume aqueous solutions containing 0.522 mass parts graphene oxide,
It stirs at room temperature to P123 after being completely dissolved, adds the concentrated hydrochloric acid that 22.5 parts by volume mass fractions are 37%, continue 37 DEG C of water
Bath stirring 2.5h, is slowly added dropwise 9.4 parts by volume ethyl orthosilicates, continues after being vigorously stirred 25h, be transferred in reaction kettle, and 110 DEG C
Crystallization 20h is filtered, washed, dries, and then roasts 5h at 550 DEG C and removes template, obtains two-dimentional earth silicon material.
(2) prepared by N doping Pd/carbon catalyst
Weigh the FeCl that 3.2 mass parts Phens are dissolved in 25.0 parts by volume of ethanol and 25.0 parts by volume 0.2M2Solution
In, the above-mentioned two-dimentional silica of 2.85 mass parts is added, at room temperature then ultrasound 8h, solvent evaporated carbonize at 950 DEG C
5h.22h is finally handled at 110 DEG C with the NaOH of 8M removes silicon template, then the HClO with 0.1M422h is handled at 90 DEG C to remove
Remove undissolved iron species.
Electrode is made in the above-mentioned catalyst being prepared, oxygen under alkaline condition is carried out on CHI730 electrochemical workstation
Reduction reaction test.Spun gold electrode is used to electrode, reference electrode is saturated calomel electrode, and electrolyte is the KOH solution of 0.1M,
Logical half an hour oxygen before experiment, scanning speed 5mV/s, electrode revolving speed are 1600rpm.Carbon dioxide is carried out under alkaline condition
Electro-reduction reaction test uses spun gold electrode to electrode, and reference electrode is saturated calomel electrode, and electrolyte is the NaHCO of 0.1M3
Solution first leads to half an hour nitrogen, measures the electrochemical profiles of material under nitrogen atmosphere, then leads to half an hour carbon dioxide again, sweeps
Retouching speed is 20mV/s, measures the electrochemical profiles of carbon dioxide reduction reaction.Current potential as described below is converted into relatively reversible
For hydrogen electrode.
The transmission electron microscope of the material that the present embodiment is prepared as shown in Figure 1, it can be observed that it is ultra-thin, have and be orderly situated between
The Carbon Materials in hole；The Carbon Materials prepared known to atomic force microscopy (Fig. 2) are with a thickness of 1nm or so.Specific surface area test
It is as shown in Figure 3 with pore analysis result, it is known that its specific surface area is 584m2/ g, aperture are about 4.0nm.
Oxygen reduction reaction test, obtained test curve are carried out under alkaline condition using Carbon Materials prepared by the present invention
As shown in Figure 4.From fig. 4, it can be seen that starting point is 0.95V, this two-dimentional azepine carbon material catalyst prepared as the result is shown
There is excellent chemical property under alkaline condition.Using Carbon Materials prepared by the present invention 0.1M NaHCO3Under the conditions of carry out
The test of carbon dioxide electro-reduction reaction, obtained test curve are as shown in Figure 5.From fig. 5, it can be seen that the two-dimentional azepine of synthesis
Carbon Materials are active for carbon dioxide reduction reaction.
The transmission electron microscope for the two-dimentional azepine Carbon Materials that following example is prepared is similar with Fig. 1.Gained two dimension carbon material
Atomic force microscopy it is similar with Fig. 2.The nitrogen Adsorption and desorption isotherms of gained two dimension carbon material are similar to Fig. 3.Gained two
The oxygen reduction reaction polarization curve for tieing up carbon material is similar with Fig. 4.The carbon dioxide reduction reaction of gained two dimension azepine Carbon Materials is bent
Line is similar with Fig. 5.It does not provide one by one.
Embodiment 2
(1) synthesis of two-dimentional earth silicon material
4.6 mass parts P123 are weighed to be added in the 116 parts by volume aqueous solutions containing 0.261 mass parts graphene oxide,
It stirs at room temperature to P123 after being completely dissolved, adds the concentrated hydrochloric acid that 22.5 parts by volume mass fractions are 37%, continue 37 DEG C of water
Bath stirring 2.5h, is slowly added dropwise 9.4 parts by volume ethyl orthosilicates, continues after being vigorously stirred 25h, be transferred in reaction kettle, and 110 DEG C
Crystallization 20h is filtered, washed, dries, and then roasts 5h at 550 DEG C and removes template, obtains two-dimentional earth silicon material.
(2) prepared by N doping Pd/carbon catalyst
The method for preparing N doping Pd/carbon catalyst is identical as embodiment 1 step (2).
The material characterization and electrochemical property test method of the catalyst are same as Example 1, prepared Carbon Materials ratio
Surface area is 500m2/ g, aperture are about 3.5nm, and oxygen reduction reaction take-off potential is 0.91V, carbon dioxide reduction reaction have compared with
Excellent activity.
Embodiment 3
(1) synthesis of two-dimentional earth silicon material
2.3 mass parts P123 are weighed to be added in the 116 parts by volume aqueous solutions containing 0.522 mass parts graphene oxide,
It stirs at room temperature to P123 after being completely dissolved, adds the concentrated hydrochloric acid that 22.5 parts by volume mass fractions are 37%, continue 37 DEG C of water
Bath stirring 2.5h, is slowly added dropwise 9.4 parts by volume ethyl orthosilicates, continues after being vigorously stirred 25h, be transferred in reaction kettle, and 110 DEG C
Crystallization 20h is filtered, washed, dries, and then roasts 5h at 550 DEG C and removes template, obtains two-dimentional earth silicon material.
(2) prepared by N doping Pd/carbon catalyst
Weigh the FeCl that 2.5 mass parts Phens are dissolved in 20.0 parts by volume of ethanol and 20.0 parts by volume 0.1M2Solution
In, the above-mentioned two-dimentional silica of 1.75 mass parts is added, at room temperature ultrasound 7h, solvent evaporated, the then charcoal at 1050 DEG C
Change 4h.Removing silicon template, then the HClO with 0.1M for 24 hours is finally handled at 110 DEG C with the NaOH of 9M422h is handled at 90 DEG C
Remove undissolved iron species.
The material characterization and electrochemical property test method of the catalyst are same as Example 1, prepared Carbon Materials ratio
Surface area is 500m2/ g, aperture are about 4.2nm, and oxygen reduction reaction take-off potential is 0.93V, carbon dioxide reduction reaction have compared with
Excellent activity.
Embodiment 4
(1) synthesis of two-dimentional earth silicon material
The method of two-dimentional earth silicon material is prepared with embodiment 1.
(2) prepared by N doping Pd/carbon catalyst
0.85 parts by volume pyrroles and 1.2 mass parts two dimension silica are added in reaction kettle, are put into 140 DEG C of vacuum drying oven guarantors
Hold 3h, cooled to room temperature obtains buff powder, then by the FeCl of 35 parts by volume 2.5M3Above-mentioned yellow powder is added in solution
In, stirring polymerization 20h, is then dried in vacuo at 110 DEG C, then carbonizes 5h at 950 DEG C at room temperature.Finally use the NaOH of 10M
20h is handled at 110 DEG C removes silicon template, then the HClO with 0.1M422h is handled at 90 DEG C removes undissolved iron species.
The material characterization and electrochemical property test method of the catalyst are same as Example 1, and the Carbon Materials of preparation compare table
Area is 515m2/ g, aperture are about 4.5nm, and oxygen reduction reaction take-off potential is 0.93V, and carbon dioxide reduction reaction has more excellent
Activity.
Embodiment 5
(1) synthesis of two-dimentional earth silicon material
The method of two-dimentional earth silicon material is prepared with embodiment 1.
(2) prepared by N doping Pd/carbon catalyst
0.80 parts by volume aniline and 1.5 mass parts two dimension silica are added in reaction kettle, are put into 190 DEG C of vacuum drying oven guarantors
Hold 4h, cooled to room temperature obtains buff powder, then by the FeCl of 20 parts by volume 2.5M3Above-mentioned yellow powder is added in solution
In, stirring polymerization 20h, is then dried in vacuo at 110 DEG C, then carbonizes 6h at 900 DEG C at room temperature.Finally use the NaOH of 10M
20h is handled at 110 DEG C removes silicon template, then the HClO with 0.1M422h is handled at 90 DEG C removes undissolved iron species.
The material characterization and electrochemical property test method of the catalyst are same as Example 1, and the Carbon Materials of preparation compare table
Area is 461m2/ g, aperture are about 5.2nm, and oxygen reduction reaction take-off potential is 0.90V, and carbon dioxide reduction reaction has more excellent
Activity.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of efficient two-dimentional azepine Carbon Materials, it is characterised in that include the following steps: to synthesize using double-template
Two-dimentional silica, nitrogenous precursor is introduced into silica template, and high temperature carbonization processing removes silica template, obtains
To the efficient two-dimentional azepine Carbon Materials.
2. the preparation method of efficient two-dimentional azepine Carbon Materials according to claim 1, it is characterised in that: the double-template
For graphene oxide and polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer.
3. the preparation method of efficient two-dimentional azepine Carbon Materials according to claim 2, it is characterised in that: the double-template
In, the concentration of graphene oxide is 1.0~5.0mg/mL, and the concentration of P123 is 0.5~4.5mM.
4. the preparation method of efficient two-dimentional azepine Carbon Materials according to claim 2, it is characterised in that: described to use bimodulus
The method that plate synthesizes two-dimentional silica, specifically: by graphene oxide and polyethylene oxide-polypropylene oxide-polycyclic oxygen second
Alkane triblock copolymer uniformly mixes in the solution, and assembling hydrolysis in acid condition obtains two-dimensional silica.
5. the preparation method of efficient two-dimentional azepine Carbon Materials according to claim 1, it is characterised in that: the nitrogenous charcoal
Source presoma includes at least one of Phen, pyrroles, aniline.
6. the preparation method of efficient two-dimentional azepine Carbon Materials according to claim 1, it is characterised in that: it is described will be nitrogenous before
Driving the method that body is introduced into silica template includes: incipient wetness impregnation method, capillary condensation infusion process or ultrasonic immersing method.
7. the preparation method of efficient two-dimentional azepine Carbon Materials according to claim 6, it is characterised in that: the incipient wetness impregnation
Method is that nitrogenous precursor is added in silica template, 20~40 DEG C of vacuum impregnations 20~for 24 hours；The capillary condensation leaching
Stain method is that nitrogenous precursor and silica template are added in reaction kettle, and 130~190 DEG C of 2~5h of holding are cooled to room
Temperature；The ultrasonic immersing method is uniformly to mix nitrogenous precursor with silica template, and 6~10h of ultrasound at 20~50 DEG C steams
Dry solvent.
8. the preparation method of efficient two-dimentional azepine Carbon Materials according to claim 1, it is characterised in that: the high temperature carbonization
It is 650~1050 DEG C of 4~6h of roasting that processing, which is in inert atmosphere temperature,.
9. a kind of efficient two-dimentional azepine Carbon Materials, it is characterised in that described in any item preparation methods obtain according to claim 1~8
It arrives.
10. application of the efficient two-dimentional azepine Carbon Materials as claimed in claim 9 in energy conversion field.
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