CN108425128A - A kind of porous amino functional graphene catalysis material and preparation and application - Google Patents
A kind of porous amino functional graphene catalysis material and preparation and application Download PDFInfo
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- CN108425128A CN108425128A CN201810200317.8A CN201810200317A CN108425128A CN 108425128 A CN108425128 A CN 108425128A CN 201810200317 A CN201810200317 A CN 201810200317A CN 108425128 A CN108425128 A CN 108425128A
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Abstract
The invention belongs to electrochemical material field, a kind of porous amino functional graphene catalysis material and preparation and application are disclosed.Graphene oxide and ammonia source are added in solvent, stirring and dissolving uniformly carries out hydro-thermal process afterwards, and product obtains amino functional graphene through centrifuge washing, freeze-drying；By amino functional graphene dispersion in strong base solution, heating stirring etching reaction transfers to progress ball milling punching in ball grinder, and with sour neutralization reaction liquid, solid product separating, washing, freeze-drying obtain porous amino functional grapheme material.Preparation method of the present invention is simple, it is only necessary to be carried out under 80 DEG C and alkaline condition, there is gained catalysis material good electrochemical hydrogen catalytic performance and preferable stability is precipitated, and can promote the development of scale water electrolysis catalyst material.
Description
Technical field
The invention belongs to electrochemical material fields, and in particular to a kind of porous amino functional graphene catalysis material and system
It is standby with application.
Background technology
It is also most gently the most abundant element of content that hydrogen, which is on the earth, and the product after burning only has water, is ＂ truly
No pollution ＂ fuel, thus most attraction.In recent decades, with the lasting rising of worldwide energy demand, exploitation is found
New energy receives more and more attention come the research for replacing oneself to have fossil fuel.Hydrogen Energy has cleaning, efficiently, easily stores, peace
Entirely, many advantages, such as can transporting.With the exhaustion of fossil fuel and the getting worse of environmental problem, this secondary energy sources are clearly
A kind of free of contamination new century ideal green energy, Hydrogen Energy are increasingly valued by people.Now industrial general use is split
Fossil oil hydrogen making or water-gas method hydrogen manufacturing, the reserves that sample presentation not only consumes petroleum with coal, while also will produce and a large amount of toxic have
Evil gas, endangers environment for the survival of mankind.Water reserve is abundant on the earth, and there are about 71% to be covered with water for earth surface, photodissociation
Water hydrogen manufacturing and water electrolysis hydrogen production are the clean hydrogen manufacturing modes of comparison, and selection relatively good at present.So far, people study
Remain problems in the photocatalytic system of exploitation, for example photochemical catalyst catalytic activity in visible-range is low and light
The many factors such as the unstability in source directly limit the commerce-change of photocatalytic water.
Water electrolysis hydrogen producing is a kind of important means realized industrialization and inexpensively prepare hydrogen, is not polluted the environment, and
The hydrogen product purity arrived is high.But greatest problem existing for the technology is that power consumption is big so that production cost is higher, causes electricity
The main reason for energy consumption is big is that the overpotential of hydrogen evolution of electrolysis electrode is excessively high, therefore studies reduction oxygen overpotential to reduce electrolysis energy
It consumes particularly important.In order to reduce cathode overpotential to save energy consumption, the cathode material of low overpotential of hydrogen evolution, high catalytic activity is studied
Have great importance.The factor for influencing liberation of hydrogen material catalytic activity mainly has capacity factor and geometrical factor.Therefore, it prepares high
The cathode material for hydrogen evolution of catalytic activity, is mainly realized by two ways：First, the new catalytic material of high catalytic activity is found,
Improve the electro-chemical activity of electrode itself；Second is that improving the true specific surface area of electrode, that is, increases the surface roughness of electrode, make
The real current density of electrode surface reduces in electrolytic process, achievees the purpose that reduce overpotential of hydrogen evolution.
Currently used for electrolysis water electrode material there are expensive, specific surfaces less, electro catalytic activity is not high the shortcomings of,
Lead to that electrolysis electrode hydrogen-evolution overpotential is excessively high, energy consumption is excessive, seriously constrains the development of water electrolysis method hydrogen producing technology.
Invention content
In place of the above shortcoming and defect of the existing technology, the primary purpose of the present invention is that providing a kind of porous
The preparation method of amino functional graphene catalysis material.The present invention has by corroding the method punched, gained catalysis material
Large specific surface area, electrocatalytic hydrogen evolution activity be strong, water electrolysis hydrogen production the advantages that low energy consumption, efficient.
Another object of the present invention is to provide a kind of porous amino functional graphites being prepared by the above method
Alkene catalysis material.
It is still another object of the present invention to provide above-mentioned porous amino functional graphene catalysis materials in electrolysis aquatic products hydrogen
Application in catalysis.
The object of the invention is achieved through the following technical solutions：
A kind of preparation method of porous amino functional graphene catalysis material, including following preparation process：
(1) graphene oxide and ammonia source are added in solvent, stirring and dissolving uniformly carries out hydro-thermal process afterwards, product pass through from
The heart washs, and freeze-drying obtains amino functional graphene；
(2) by amino functional graphene dispersion in strong base solution, heating stirring etching reaction transfers to ball grinder
Middle progress ball milling punching, with sour neutralization reaction liquid, solid product separating, washing, freeze-drying obtain porous amino functional
Grapheme material.
Preferably, ammonia source described in step (1) is at least one in ammonium hydroxide, melamine and polyvinylpyrrolidone
Kind.
Preferably, it is (25~100) that quality and the mass ratio in ammonia source, which is added, in graphene oxide described in step (1):1.
Preferably, solvent described in step (1) is at least one of DMF, water and absolute ethyl alcohol.
Preferably, the temperature of hydro-thermal process described in step (1) is 150~200 DEG C, the time is 10~15h.
Preferably, washing described in step (1) is to be washed with water 3~5 times；The freeze-drying refers to being freeze-dried
Dry 24~48h in case.
Preferably, strong base solution described in step (2) refers to the KOH solution of 6~10M.
Preferably, the temperature of heating stirring etching reaction described in step (2) be 80~100 DEG C, the time be 10~
24h。
Preferably, the condition of the punching of ball milling described in step (2) is：Rotational speed of ball-mill is 400~1100rpm, and the time is
30~60h, abrading-ball are the zirconia ball that diameter is 1.5~3mm.
Preferably, washing described in step (2) refers to being washed with water 3~5 times.
Preferably, freeze-drying described in step (2) refers to dry 24~48h in freeze drying box.
A kind of porous amino functional graphene catalysis material, is prepared by the above method.The porous amino functional
Graphite alkene material is made of the graphite flake of lamella, and surface is distributed hole not of uniform size, there is apparent fold.
Application of the above-mentioned porous amino functional graphene catalysis material in being electrolysed aquatic products hydrogen catalysis.
The present invention preparation method and obtained product has the following advantages that and advantageous effect：
(1) since graphene has good electric conductivity, punching processing is eroded on surface, the surface for increasing electrode is thick
Rugosity makes the real current density of porous amino functional grapheme material electrode surface during electrolytic catalysis reduce, reaches
To the purpose for reducing overpotential of hydrogen evolution.Meanwhile after punching processing, there is no destroy for the self stability of graphitic carbon material.
(2) there are the doping of nitrogen, the carbon material of N doping that can also improve material in present invention gained catalysis material
Active site and electric conductivity.
(3) it is very simple to corrode drilling method by the present invention, it is only necessary to carried out under 80 DEG C and alkaline condition, therefore synthesize at
This is cheap, and energy consumption is relatively low, environmental-friendly, can promote the development of scale water electrolysis catalyst material.
Description of the drawings
Fig. 1 is the XPS figures of the porous amino functional graphene catalysis material nitrogen of gained in the embodiment of the present invention 1.
Fig. 2 is the Raman spectrogram of the porous amino functional graphene catalysis material of gained in the embodiment of the present invention 1.
Fig. 3 is the XRD diagram of the porous amino functional graphene catalysis material of gained in the embodiment of the present invention 1.
Fig. 4 is the SEM figures of the porous amino functional graphene catalysis material of gained in the embodiment of the present invention 1.
Fig. 5 is the TEM figures of the porous amino functional graphene catalysis material of gained in the embodiment of the present invention 1.
Fig. 6 is that the porous amino functional graphene catalysis material of gained is urged as Hydrogen evolving reaction in the embodiment of the present invention 1
Change linear sweep voltammetry curve (LSV) performance map of material.
Fig. 7 is that the porous amino functional graphene catalysis material of gained is urged as Hydrogen evolving reaction in the embodiment of the present invention 1
Change the CV stable circulation performance figures of material.
Specific implementation mode
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
Embodiment 1
(1) graphene oxide gel for measuring 100mg is dissolved into the deionized water of 40mL, is stirred by ultrasonic at room temperature
After 30min, uniformly mixed solution is obtained, the ammonium hydroxide of 2mL is then added, it, will be obtained above molten after stirring 30min at room temperature
Liquid is transferred in the reaction kettle of 50mL, and hydro-thermal reaction 12h is carried out at 180 DEG C.Hydro-thermal reaction product is centrifuged, is used
It after water washing 5 times, is dried in vacuum freezing drying oven for 24 hours, obtains amino functional graphene (AFNG).
(2) the amino functional graphene dispersion of 20mg is weighed in 80mL 6M KOH solutions, is heated to 80 DEG C, and stir
It mixes and corrodes 12h, then above-mentioned solution is transferred in the ball grinder of polytetrafluoroethylene (PTFE), ball milling 30h, obtains at rotating speed 400rpm
Dark solution first washed to neutrality with 1M HCl, be finally centrifuged, after being washed with water 5 times, in vacuum freeze drying
It is dried in case for 24 hours, obtains porous amino functional graphene (HT-AFNG) catalysis material.
The XPS figures of porous amino functional graphene catalysis material nitrogen obtained by the present embodiment are as shown in Figure 1.X-ray
Photoelectron spectroscopy (XPS) is analysis shows the form of the nitrogen adulterated in the product of gained is ammoniacal nitrogen, pyrroles's nitrogen, pyridine nitrogen, graphite
The content of nitrogen and nitrogen oxide, the nitrogen of doping is higher, illustrates that nitrating effect is good.The porous amino functional graphene catalysis material of gained
Raman spectrogram it is as shown in Figure 2.It can be seen that, the peaks G appear in 1350cm from Raman spectrograms-1Left and right, the peaks D appear in
1580cm-1Left and right illustrates the carbon having in the obtained product of the present invention based on amorphous carbon.The porous amino functional of gained
The XRD diagram of graphene catalysis material is as shown in Figure 3.X-ray powder diffraction (XRD) has 002 analysis shows the product of gained is carbon
Crystal face and 100 crystal faces illustrate that the appearance of material is carbon peak.The porous amino functional graphene catalysis material of gained SEM figure and
TEM figures are as shown in Figure 4 and Figure 5 respectively.From scanning electron microscope (SEM) and transmission electron microscope (TEM) it can be seen from the figure that by piece
The graphite flake of layer is constituted, and surface is distributed hole not of uniform size, there is apparent fold.
Catalytic performance test is precipitated in the hydrogen of porous amino functional graphene catalysis material obtained by the present embodiment：
The Nafion (5wt.%) for pipetting 80 μ L is dissolved in second alcohol and water (volume ratio=1 of 1mL:4) second is prepared in mixed liquor
Alcohol-water-Nafion solution is spare.It weighs 4.0mg HT-AFNG to be scattered in matched alcohol-water-Nafion solution, ultrasonic 1h systems
Standby suspension is spare.Then the dispersant liquid drop for pipetting 20 μ L is coated onto on glass-carbon electrode, and naturally dry has obtained HT-AFNG-
The electrode of Nafion modifications.Working electrode, saturated calomel electrode is precipitated as hydrogen in the HT-AFNG-Nafion electrodes of above-mentioned preparation
As reference electrode, charcoal bar electrode is used as to electrode.This three electrodes one end is connected to electrochemical workstation (Shanghai Chen Hua 660E),
The other end immerses 0.5M H2SO4In electrolyte.Catalytic performance, scanning are precipitated using linear sweep voltammetry curve method test material hydrogen
Rate is 2mV/s, scanning voltage range 0V~-0.8V.The porous amino functional graphene catalysis material of gained is precipitated as hydrogen
Linear sweep voltammetry curve (LSV) performance map of catalytic reaction material is as shown in Figure 6.In 0.5M H2SO4Electrolyte in, HT-
The deposition potential of AFNG is about 100mV (relative to standard electrode potential after impedance correction)；As current density j=10mA/cm2When, electricity
Pressure is 350mV, and there is good electrochemical hydrogen catalytic performance is precipitated.The porous amino functional graphene catalysis material conduct of gained
The CV stable circulation performance figures of Hydrogen evolving reaction catalysis material are as shown in Figure 7.It is tested after 3000 circle of CV (cyclic voltammetry) scannings
Material property, deposition potential are not decayed with current density, have preferable stability.
Embodiment 2
(1) graphene oxide gel for measuring 100mg is dissolved into the deionized water of 40mL, is stirred by ultrasonic at room temperature
After 30min, uniformly mixed solution is obtained, the ammonium hydroxide of 4mL is then added, it, will be obtained above molten after stirring 30min at room temperature
Liquid is transferred in the reaction kettle of 50mL, and hydro-thermal reaction 10h is carried out at 150 DEG C.Hydro-thermal reaction product is centrifuged, is used
After water washing 3 times, 48h is dried in vacuum freezing drying oven, obtains amino functional graphene (AFNG).
(2) the amino functional graphene for weighing 15mg is dissolved in 80mL 6M KOH solutions, is heated to 100 DEG C, and stir
It mixes erosion for 24 hours, then above-mentioned solution is transferred in the ball grinder of polytetrafluoroethylene (PTFE), ball milling 60h, obtains at rotating speed 1100rpm
To dark solution first washed to neutrality with 1M HCl, be finally centrifuged, it is dry in vacuum refrigeration after being washed with water 5 times
It is dried in dry case for 24 hours, obtains porous amino functional graphene (HT-AFNG) catalysis material.
Catalytic performance test is precipitated in the hydrogen of porous amino functional graphene catalysis material obtained by the present embodiment：
Using HT-AFNG-Nafion electricity made of porous amino functional graphene (HT-AFNG) manufactured in the present embodiment
Working electrode is precipitated as hydrogen in pole, and saturated calomel electrode is used as reference electrode, charcoal bar electrode to electrode, in 0.5M H2SO4
Electrolyte in, it is about 102mV that take-off potential, which is precipitated, (relative to standard electrode potential after impedance correction) in the hydrogen of AFNG；Work as current density
J=10mA/cm2When, there is voltage 366.6mV preferable electrochemical hydrogen catalytic performance is precipitated.CV (cyclic voltammetry) is scanned
Test material performance after 3000 circles, deposition potential within 10%, have preferable stability with current density attenuation rate.
Embodiment 3
(1) graphene oxide gel for measuring 100mg is dissolved into the deionized water of 40mL, is stirred by ultrasonic at room temperature
After 30min, uniformly mixed solution is obtained, the ammonium hydroxide of 2mL is then added, it, will be obtained above molten after stirring 30min at room temperature
Liquid is transferred in the reaction kettle of 50mL, and hydro-thermal reaction 15h is carried out at 200 DEG C.Hydro-thermal reaction product is centrifuged, is used
It after water washing 5 times, is dried in vacuum freezing drying oven for 24 hours, obtains amino functional graphene (AFNG).
(2) the amino functional graphene for weighing 10mg is dissolved in 80mL 10M KOH solutions, is heated to 90 DEG C, and stir
It mixes and corrodes 12h, then above-mentioned solution is transferred in the ball grinder of polytetrafluoroethylene (PTFE), ball milling 45h, obtains at rotating speed 900rpm
Dark solution first washed to neutrality with 1M HCl, be finally centrifuged, after being washed with water 5 times, in vacuum freeze drying
36h is dried in case, obtains porous amino functional graphene (HT-AFNG) catalysis material.
Catalytic performance test is precipitated in the hydrogen of porous amino functional graphene catalysis material obtained by the present embodiment：
Using HT-AFNG-Nafion electricity made of porous amino functional graphene (HT-AFNG) manufactured in the present embodiment
Working electrode is precipitated as hydrogen in pole, and saturated calomel electrode is used as reference electrode, charcoal bar electrode to electrode, in 0.5M H2SO4
Electrolyte in, it is about 114mV that take-off potential, which is precipitated, (relative to standard electrode potential after impedance correction) in the hydrogen of HT-AFNG；Work as electric current
Density j=10mA/cm2When, there is voltage 373mV preferable electrochemical hydrogen catalytic performance is precipitated.CV (cyclic voltammetry) is swept
Test material performance after 3000 circles is retouched, deposition potential within 10%, has preferable stability with current density attenuation rate
Energy.
Embodiment 4
(1) graphene oxide gel for measuring 100mg is dissolved into the deionized water of 40mL, is stirred by ultrasonic at room temperature
After 30min, uniformly mixed solution is obtained, the ammonium hydroxide of 1mL is then added, it, will be obtained above molten after stirring 30min at room temperature
Liquid is transferred in the reaction kettle of 50mL, and hydro-thermal reaction 15h is carried out at 200 DEG C.Hydro-thermal reaction product is centrifuged, is used
It after water washing 5 times, is dried in vacuum freezing drying oven for 24 hours, obtains amino functional graphene (AFNG).
(2) the amino functional graphene for weighing 25mg is dissolved in 80mL 10M KOH solutions, is heated to 100 DEG C, and
12h is corroded in stirring, then above-mentioned solution is transferred in the ball grinder of polytetrafluoroethylene (PTFE), the ball milling 45h at rotating speed 1100rpm,
Obtained dark solution is first washed with 1M HCl to neutrality, is finally centrifuged, after being washed with water 5 times, in vacuum refrigeration
48h is dried in drying box, obtains porous amino functional graphene (HT-AFNG) production hydrogen catalysis material.
Catalytic performance test is precipitated in the hydrogen of porous amino functional graphene catalysis material obtained by the present embodiment：
Using HT-AFNG-Nafion electricity made of porous amino functional graphene (HT-AFNG) manufactured in the present embodiment
Working electrode is precipitated as hydrogen in pole, and saturated calomel electrode is used as reference electrode, charcoal bar electrode to electrode, in 0.5M H2SO4
Electrolyte in, it is about 115mV that take-off potential, which is precipitated, (relative to standard electrode potential after impedance correction) in the hydrogen of HT-AFNG；Work as electric current
Density j=10mA/cm2When, there is voltage 375mV preferable electrochemical hydrogen catalytic performance is precipitated.CV (cyclic voltammetry) is swept
Test material performance after 3000 circles is retouched, deposition potential within 10%, has preferable stability with current density attenuation rate
Energy.
Embodiment 5
(1) graphene oxide gel for measuring 100mg is dissolved into the deionized water of 40mL, is stirred by ultrasonic at room temperature
After 30min, uniformly mixed solution is obtained, the ammonium hydroxide of 1mL is then added, it, will be obtained above molten after stirring 30min at room temperature
Liquid is transferred in the reaction kettle of 50mL, and hydro-thermal reaction 15h is carried out at 200 DEG C.Hydro-thermal reaction product is centrifuged, is used
It after water washing 5 times, is dried in vacuum freezing drying oven for 24 hours, obtains amino functional graphene (AFNG).
(2) the amino functional graphene for weighing 90mg is dissolved in 80mL 10M KOH solutions, is heated to 100 DEG C, and
12h is corroded in stirring, then above-mentioned solution is transferred in the ball grinder of polytetrafluoroethylene (PTFE), the ball milling 45h at rotating speed 1100rpm,
Obtained dark solution is first washed with 1M HCl to neutrality, is finally centrifuged, after being washed with water 5 times, in vacuum refrigeration
48h is dried in drying box, obtains porous amino functional graphene (HT-AFNG) production hydrogen catalysis material.
Catalytic performance test is precipitated in the hydrogen of porous amino functional graphene catalysis material obtained by the present embodiment：
Using HT-AFNG-Nafion electricity made of porous amino functional graphene (HT-AFNG) manufactured in the present embodiment
Working electrode is precipitated as hydrogen in pole, and saturated calomel electrode is used as reference electrode, charcoal bar electrode to electrode, in 0.5M H2SO4
Electrolyte in, it is about 116mV that take-off potential, which is precipitated, (relative to standard electrode potential after impedance correction) in the hydrogen of HT-AFNG；Work as electric current
Density j=10mA/cm2When, there is voltage 376mV preferable electrochemical hydrogen catalytic performance is precipitated.CV (cyclic voltammetry) is swept
Test material performance after 3000 circles is retouched, deposition potential within 10%, has preferable stability with current density attenuation rate
Energy.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of porous amino functional graphene catalysis material, it is characterised in that including following preparation process：
(1) graphene oxide and ammonia source are added in solvent, stirring and dissolving uniformly carries out hydro-thermal process afterwards, and product is washed through centrifugation
It washs, is freeze-dried, obtains amino functional graphene；
(2) by amino functional graphene dispersion in strong base solution, heating stirring etching reaction, transfer in ball grinder into
Row ball milling punches, and with sour neutralization reaction liquid, solid product separating, washing, freeze-drying obtain porous amino functional graphite
Alkene material.
2. a kind of preparation method of porous amino functional graphene catalysis material according to claim 1, feature exist
In：Ammonia source described in step (1) is at least one of ammonium hydroxide, melamine and polyvinylpyrrolidone.
3. a kind of preparation method of porous amino functional graphene catalysis material according to claim 1, feature exist
In：It is (25~100) that quality and the mass ratio in ammonia source, which is added, in graphene oxide described in step (1):1.
4. a kind of preparation method of porous amino functional graphene catalysis material according to claim 1, feature exist
In：Solvent described in step (1) is at least one of DMF, water and absolute ethyl alcohol.
5. a kind of preparation method of porous amino functional graphene catalysis material according to claim 1, feature exist
In：The temperature of hydro-thermal process described in step (1) is 150~200 DEG C, and the time is 10~15h.
6. a kind of preparation method of porous amino functional graphene catalysis material according to claim 1, feature exist
In：Strong base solution described in step (2) refers to the KOH solution of 6~10M.
7. a kind of preparation method of porous amino functional graphene catalysis material according to claim 1, feature exist
In：The temperature of heating stirring etching reaction described in step (2) be 80~100 DEG C, the time be 10~for 24 hours.
8. a kind of preparation method of porous amino functional graphene catalysis material according to claim 1, feature exist
Described in step (2) ball milling punch condition be：Rotational speed of ball-mill is 400~1100rpm, and the time is 30~60h, and abrading-ball is straight
Diameter size is the zirconia ball of 1.5~3mm.
9. a kind of porous amino functional graphene catalysis material, it is characterised in that：Described in any one of claim 1~8
Method be prepared.
10. a kind of porous amino functional graphene catalysis material answering in being electrolysed aquatic products hydrogen catalysis described in claim 9
With.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110787820A (en) * | 2019-09-05 | 2020-02-14 | 青岛科技大学 | Heteroatom nitrogen surface modification MoS2Preparation and application of nano material |
| CN113652699A (en) * | 2021-07-05 | 2021-11-16 | 南昌大学 | Method for improving activity of hydrogen production by electrocatalysis of graphene |
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| CN104973595A (en) * | 2015-06-30 | 2015-10-14 | 华南理工大学 | Three-dimensional porous graphene material, and preparation method and applications thereof |
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| CN104973595A (en) * | 2015-06-30 | 2015-10-14 | 华南理工大学 | Three-dimensional porous graphene material, and preparation method and applications thereof |
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| ZHONG-JIE JIANG ET. AL: "The role of holes in improving the performance of nitrogen-doped", 《JOURNAL OF POWER SOURCES》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110787820A (en) * | 2019-09-05 | 2020-02-14 | 青岛科技大学 | Heteroatom nitrogen surface modification MoS2Preparation and application of nano material |
| CN113652699A (en) * | 2021-07-05 | 2021-11-16 | 南昌大学 | Method for improving activity of hydrogen production by electrocatalysis of graphene |
| CN113652699B (en) * | 2021-07-05 | 2023-08-29 | 南昌大学 | Method for improving electrocatalytic hydrogen production activity of graphene |
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Application publication date: 20180821 |