CN107435155A - A kind of preparation method and application of porous carbon nano-composite material catalyst - Google Patents
A kind of preparation method and application of porous carbon nano-composite material catalyst Download PDFInfo
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- CN107435155A CN107435155A CN201710791400.2A CN201710791400A CN107435155A CN 107435155 A CN107435155 A CN 107435155A CN 201710791400 A CN201710791400 A CN 201710791400A CN 107435155 A CN107435155 A CN 107435155A
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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
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
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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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- 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 preparation method of porous carbon nano-composite material catalyst, belong to nano material, high molecular polymer and catalyst technical field.Using polymerizing impregnated pyrolysis dipping method, carbon@Fe are prepared2O3@Co (II) nano composite material catalyst.The raw materials used cost of the catalyst preparation is low, and preparation technology is simple, and energy consumption of reaction is low, has prospects for commercial application.The catalyst is used for catalytic electrolysis elutriation oxygen, has good analysis oxygen electro catalytic activity and electrochemical stability.
Description
Technical field
The present invention relates to a kind of preparation method and application of porous carbon nano-composite material catalyst, belong to nano material,
High molecular polymer and electro-catalysis technical field.
Background technology
Fast development and scientific and technological continuous progress with economy, the energy and environment have extremely important in social development
Effect.In past 50 years, a large number of researchers are directed to studying, develop efficient, economic, the renewable sustainable energy.
To realize that target of sustainable development, searching and exploitation green energy resource and high efficient energy sources equipment are extremely urgent.It is worth noting that, hydrogen
Can be considered as the energy clean the most, efficient, obtaining Hydrogen Energy can be by the separation of natural air, the cracking of fossil energy
Separation or partial oxidation, photocatalysis Decomposition, biomass ferment conversion, electrolysis water；Wherein, electro-catalysis hydrolytic hydrogen production and oxygen processed cause
The extensive concern of global scientists, and electrolysis water is considered as one of method of production Hydrogen Energy of most prospect.
Electrolysis water is that aqueous water is decomposed into oxygen (O by the electric power2) and hydrogen (H2) phenomenon.Due to the half of electrolysis water
Reaction（Analyse oxygen half-reaction）Need larger overpotential to occur, considerably increase the energy consumption of hydrogen manufacturing, therefore, exploitation is efficiently urged
It is very necessary to change raising of the catalyst of oxygen evolution reaction for hydrogen producing technology, while in hydrogen energy source, chlorine industry and solar energy
Use is all very significant.
Metal Co (II) cations and its polymer have relatively low overpotential in alkaline medium, not only cost it is low and
And have good stability, corrosion resistance is also stronger.
Polyureas (polyurea) be by binary or multicomponent isocyanate with amine or a kind of strand of water reaction generation containing-
The organic polymer of NH-CO-NH- (urea groups) chain link.Because being rich in active amine (NH in its strand2), urea groups, it has lonely right
The amido N atoms of electronics so that polyureas almost can form stable complex with all metal ions.And polyureas shape after pyrolysis
Into nanometer polymer, because of the dimension of its nanometer of category, can more show the characteristic that macroscopic material can not compare.It is so far
Only, the exploitation report based on polyureas high molecular polymer electro-catalysis analysis oxygen is few.
The content of the invention
One of technical assignment of the present invention is to make up the deficiencies in the prior art, there is provided a kind of nano combined material of porous carbon
Expect its preparation method of catalyst, the raw materials used cost of this method is low, and synthesis technique is simple, and energy consumption of reaction is low, has extensive
Application prospect.
The two of the technical assignment of the present invention are to provide the purposes of porous carbon nano-composite material catalyst, and the catalyst is used for
Electrochemical catalysis analyses oxygen, has good analysis oxygen electro catalytic activity and electrochemical stability.
Technical scheme is as follows：
A kind of 1. preparation method of porous carbon nano-composite material catalyst
(1) 0.40-0.80 g ferric nitrate is dissolved in 4-8 mL ethanol, adds 0.20-0.40g polyphenyl urea powder PU, stir
After mixing uniformly, after 120 W ultrasound 12-15 min, steeped overnight, 60 DEG C of dryings, porous Fe (III)-polyphenyl urea coordination is made
Polymeric material;
(2) porous Fe (III)-polyphenyl urea coordination polymer material is placed in tube furnace, under air atmosphere, heating rate 3-
5 DEG C/min, 300-500 DEG C is heated to, 1.5-2.5 h is incubated, then, room temperature is cooled to 2 DEG C/min rate of temperature fall, is made
Obtain porous carbon Fe2O3Nano composite material;
(3) 0.60-1.20g cobalt nitrate is dissolved in 4-8 mL ethanol, adds 0.10-0.50g porous carbon@Fe2O3Nanometer
Composite, after 120 W ultrasound 12-15 min, steeped overnight, 60 DEG C of dryings, porous carbon@Fe are made2O3@Co (II) nanometer
Composite, i.e., porous carbon nano-composite material catalyst.
Polyphenyl urea powder PU, its structural formula are as follows described in step (1)：
Polyphenyl urea powder PU, preparation process are as follows described in step (1)：
Under electric stirring, the p-phenylenediamine of 17.0 g acetone and 2.47-3.07 mmol is dissolved into the solution of clarification, adds 8-
12 g water, after ice bath cools down 10 min, with 300 rpm stir speed (S.S.), 22-24 mmol toluene di-isocyanate(TDI)s are added dropwise in constant speed
With the blended liquid of 8-10 g acetone, 30min is dripped off, and is warming up to 30 DEG C, is incubated the h of polymerisation 3, and product is filtered and separated, and
Washed the solid three times, obtained with the water and acetone mixture that mass ratio is 3/7 and be dried to constant weight in 70 DEG C of baking oven, that is, made
Polyphenyl urea powder PU was obtained, yield is 81-89 %.
Polyphenyl urea powder PU described in step (1) and porous Fe (III)-polyphenyl urea coordination polymer material, are three-dimensional
Porous material, its it is porous by micropore, mesoporous and less than 4 um macropore forms.
Porous carbon@Fe described in step (2)2O3Nano composite material, it is porous graphite base material load Fe2O3Nano-particle
The composite of composition, its it is porous by micropore, mesoporous and less than 6 um macropore form, Fe2O3Nano particle diameter is 20-30
nm。
Porous carbon@Fe described in step (3)2O3@Co (II) nano composite material, it is porous carbon@Fe2O3It is nano combined
Material load Co (II) cation form three-dimensional manometer composite, its it is porous by micropore, mesoporous and less than 6 um macropore
Composition.
2. porous carbon nano-composite material catalyst prepared by preparation method as described above is used for electrochemical catalysis analysis oxygen
Application
(1) in the surface construction porous carbon@Fe that basal electrode is glass-carbon electrode2O3@Co (II) nano composite material, prepare
Carbon@Fe2O3@Co (II) nano composite material working electrode；
The surface construction carbon@Fe2O3@Co (II) nano composite material, it is successively with 1.0,0.3,0.05 μ by glass-carbon electrode
M Al2O3Powder polishes, and is cleaned by ultrasonic successively in ultra-pure water, dust technology, ultra-pure water and ethanol, after room temperature is dried, at it
The uL carbon@Fe of surface drop coating 62O3@Co (II) nano composite material, room temperature dry obtained working electrode；
The carbon@Fe2O3@Co (II) Nanocomposite solution, it is by 4 mg carbon@Fe2O3@Co (II) nano composite material
It is scattered in 250 μ L ethanol, 720 μ L water and 30 μ L Nafion, room temperature ultrasound 15min, mixed liquor is made；
(2) reference electrode, the working electrode prepared to electrode and above-mentioned steps (1) are connected on electrochemical workstation, reference
Electrode is Ag/AgCl electrodes (saturation KCl solution), is platinum plate electrode to electrode, and electrolyte is to be surveyed in the 0.5 M KOH aqueous solution
Try the water-based energy of electrocatalytic decomposition;
(3) above-mentioned carbon@Fe2O3@Co (II) nano composite materials working electrode is electrolysed elutriation oxygen, as the mA/ of current density, J=10
cm2When, current potential is 1.53 V vs RHE）；Tafel slope is 71 mV dec-1, illustrate that the material efficiently analyses oxygen catalysis
Activity；Before and after circulation 500 times, such material polarization curve does not have to find obvious change, shows that catalyst has well
Stability.
The beneficial technique effect of the present invention：
（1）Carbon@Fe2O3The preparation method of@Co (II) nano composite material catalyst, easy to operate, cost is cheap
The present invention use polymerization-dipping-pyrolysis-dipping method, first by high activity aromatic series toluene di-isocyanate(TDI) (TDI) and
P-phenylenediamine progressively precipitation polymerization in water and acetone, is modified without any stabilizer, pore-foaming agent and surface, prepared by one-step method
Surface is rich in the porous polyphenyl urea high polymer material of amido（PU）；By itself and transition-metal Fe (III) cation impregnation,
Porous Fe (III)-polyphenyl urea coordination polymer material has been made；Continue porous Fe (III)-polyphenyl urea coordination polymer material
Pyrolysis processing, porous carbon@Fe are made2O3Nano composite material, and porous graphite base material load Fe2O3What nano-particle was formed
Composite；Further with transition metal Co2+Impregnation, it has been made with carbon@Fe2O3@Co (II) nano composite material is catalyzed
Agent, raw materials used cheap, building-up process is simple, is easy to industrialize.
（2）The invention provides a kind of carbon@Fe2O3@Co (II) nano composite material is used for answering for electrolysis water oxygen-separating catalyst
With.Because the catalyst is by Co (II) cation, nanometer Fe2O3Particle is supported on the porous material formed on graphite, compares surface
Product is high, exposes more and different avtive spots, has played Co in composite (II) cation, nanometer Fe2O3Particle and stone
The synergy of black base material so that the catalysis analysis oxygen based on the composite, high catalytic efficiency and stability is good.
Embodiment
With reference to embodiment, the invention will be further described, but protection scope of the present invention is not only limited to implement
Example, the change that professionals in the field is made to technical solution of the present invention, all should belong in protection scope of the present invention.
A kind of preparation method of porous carbon nano-composite material catalyst of embodiment 1
(1) 0.40-0.80 g ferric nitrate is dissolved in 4-8 mL ethanol, adds 0.20-0.40g polyphenyl urea powder PU,
After stirring, after 120 W ultrasound 12-15 min, steeped overnight, 60 DEG C of dryings, porous Fe (III)-polyphenyl urea is made and matches somebody with somebody
Position polymeric material;
(2) porous Fe (III)-polyphenyl urea coordination polymer material is placed in tube furnace, under air atmosphere, heating rate 3-
5 DEG C/min, 300-500 DEG C is heated to, 1.5-2.5 h is incubated, then, room temperature is cooled to 2 DEG C/min rate of temperature fall, is made
Obtain porous carbon Fe2O3Nano composite material;
(3) 0.60-1.20g cobalt nitrate is dissolved in 4-8 mL ethanol, adds 0.10-0.50g porous carbon@Fe2O3Nanometer
Composite, after 120 W ultrasound 12-15 min, steeped overnight, 60 DEG C of dryings, porous carbon@Fe are made2O3@Co (II) nanometer
Composite, i.e., porous carbon nano-composite material catalyst.
A kind of preparation method of porous carbon nano-composite material catalyst of embodiment 2
(1) 0.40-0.80 g ferric nitrate is dissolved in 4-8 mL ethanol, adds 0.20-0.40g polyphenyl urea powder PU,
After stirring, after 120 W ultrasound 12-15 min, steeped overnight, 60 DEG C of dryings, porous Fe (III)-polyphenyl urea is made and matches somebody with somebody
Position polymeric material;
(2) porous Fe (III)-polyphenyl urea coordination polymer material is placed in tube furnace, under air atmosphere, heating rate 3-
5 DEG C/min, 300-500 DEG C is heated to, 1.5-2.5 h is incubated, then, room temperature is cooled to 2 DEG C/min rate of temperature fall, is made
Obtain porous carbon Fe2O3Nano composite material;
(3) 0.60-1.20g cobalt nitrate is dissolved in 4-8 mL ethanol, adds 0.10-0.50g porous carbon@Fe2O3Nanometer
Composite, after 120 W ultrasound 12-15 min, steeped overnight, 60 DEG C of dryings, porous carbon@Fe are made2O3@Co (II) nanometer
Composite, i.e., porous carbon nano-composite material catalyst.
A kind of preparation method of porous carbon nano-composite material catalyst of embodiment 3
(1) 0.40-0.80 g ferric nitrate is dissolved in 4-8 mL ethanol, adds 0.20-0.40g polyphenyl urea powder PU,
After stirring, after 120 W ultrasound 12-15 min, steeped overnight, 60 DEG C of dryings, porous Fe (III)-polyphenyl urea is made and matches somebody with somebody
Position polymeric material;
(2) porous Fe (III)-polyphenyl urea coordination polymer material is placed in tube furnace, under air atmosphere, heating rate 3-
5 DEG C/min, 300-500 DEG C is heated to, 1.5-2.5 h is incubated, then, room temperature is cooled to 2 DEG C/min rate of temperature fall, is made
Obtain porous carbon Fe2O3Nano composite material;
(3) 0.60-1.20g cobalt nitrate is dissolved in 4-8 mL ethanol, adds 0.10-0.50g porous carbon@Fe2O3Nanometer
Composite, after 120 W ultrasound 12-15 min, steeped overnight, 60 DEG C of dryings, porous carbon@Fe are made2O3@Co (II) nanometer
Composite, i.e., porous carbon nano-composite material catalyst.
Embodiment 4
Polyphenyl urea powder PU, its structural formula are as follows described in step (1)：
Polyphenyl urea powder PU, preparation process are as follows described in step (1)：
Under electric stirring, the p-phenylenediamine of 17.0 g acetone and 2.47-3.07 mmol is dissolved into the solution of clarification, adds 8-
12 g water, after ice bath cools down 10 min, with 300 rpm stir speed (S.S.), 22-24 mmol toluene di-isocyanate(TDI)s are added dropwise in constant speed
With the blended liquid of 8-10 g acetone, 30min is dripped off, and is warming up to 30 DEG C, is incubated the h of polymerisation 3, and product is filtered and separated, and
Washed the solid three times, obtained with the water and acetone mixture that mass ratio is 3/7 and be dried to constant weight in 70 DEG C of baking oven, that is, made
Polyphenyl urea powder PU was obtained, yield is 81-89 %.
Polyphenyl urea powder PU described in step (1) and porous Fe (III)-polyphenyl urea coordination polymer material, are three-dimensional
Porous material, its it is porous by micropore, mesoporous and less than 4 um macropore forms.
Embodiment 5
Porous carbon@Fe described in embodiment 1-3 steps (2)2O3Nano composite material, it is porous graphite base material load Fe2O3Nanometer
Particle form composite, its it is porous by micropore, mesoporous and less than 6 um macropore form, Fe2O3Nano particle diameter is
20-30 nm。
Embodiment 6
Porous carbon@Fe described in embodiment 1-3 steps (3)2O3@Co (II) nano composite material, it is porous carbon@Fe2O3Nanometer
Composite load C o (II) cation form three-dimensional manometer composite, its it is porous by micropore, it is mesoporous and less than 6 um
Macropore forms.
Embodiment 7
Porous carbon nano-composite material catalyst is used for the application of electrochemical catalysis analysis oxygen
(1) the porous carbon@Fe prepared in basal electrode for the surface construction embodiment 1 of glass-carbon electrode2O3@Co (II) nanometer is multiple
Condensation material, prepare carbon@Fe2O3@Co (II) nano composite material working electrode；
The surface construction carbon@Fe2O3@Co (II) nano composite material, it is successively with 1.0,0.3,0.05 μ by glass-carbon electrode
M Al2O3Powder polishes, and is cleaned by ultrasonic successively in ultra-pure water, dust technology, ultra-pure water and ethanol, after room temperature is dried, at it
The uL carbon@Fe of surface drop coating 62O3@Co (II) nano composite material, room temperature dry obtained working electrode；
The carbon@Fe2O3@Co (II) Nanocomposite solution, it is by 4 mg carbon@Fe2O3@Co (II) nano composite material
It is scattered in 250 μ L ethanol, 720 μ L water and 30 μ L Nafion, room temperature ultrasound 15min, mixed liquor is made；
(2) reference electrode, the working electrode prepared to electrode and above-mentioned steps (1) are connected on electrochemical workstation, reference
Electrode is Ag/AgCl electrodes (saturation KCl solution), is platinum plate electrode to electrode, and electrolyte is to be surveyed in the 0.5 M KOH aqueous solution
Try electro-catalysis analysis oxygen performance.
Embodiment 8
Method is with embodiment 7, the porous carbon@Fe for only preparing embodiment 12O3@Co (II) nano composite material replaces with implementation
Porous carbon@Fe prepared by example 22O3@Co (II) nano composite material.
Embodiment 9
Method is with embodiment 7, the porous carbon@Fe for only preparing embodiment 12O3@Co (II) nano composite material replaces with implementation
Porous carbon@Fe prepared by example 32O3@Co (II) nano composite material.
Embodiment 10
Embodiment 7-9 is electrolysed elutriation oxygen, as the mA/cm of current density, J=102When, current potential is 1.53 V（vs RHE；Ta Feier is oblique
Rate is 71 mV dec-1, illustrate that the material efficiently analyses oxygen catalytic activity；Before and after circulation 500 times, the polarization of such material is bent
Line does not find obvious change, shows that catalyst has good stability.
Claims (6)
1. a kind of preparation method of porous carbon nano-composite material catalyst, it is characterised in that preparation process is as follows：
(1) 0.40-0.80 g ferric nitrate is dissolved in 4-8 mL ethanol, adds 0.20-0.40g polyphenyl urea powder PU, stir
After mixing uniformly, after 120 W ultrasound 12-15 min, steeped overnight, 60 DEG C of dryings, porous Fe (III)-polyphenyl urea coordination is made
Polymeric material;
(2) porous Fe (III)-polyphenyl urea coordination polymer material is placed in tube furnace, under air atmosphere, heating rate 3-
5 DEG C/min, 300-500 DEG C is heated to, 1.5-2.5 h is incubated, then, room temperature is cooled to 2 DEG C/min rate of temperature fall, is made
Obtain porous carbon Fe2O3Nano composite material;
(3) 0.60-1.20g cobalt nitrate is dissolved in 4-8 mL ethanol, adds 0.10-0.50g porous carbon@Fe2O3Nanometer
Composite, after 120 W ultrasound 12-15 min, steeped overnight, 60 DEG C of dryings, porous carbon@Fe are made2O3@Co (II) nanometer
Composite, i.e., porous carbon nano-composite material catalyst.
2. the preparation method of porous carbon nano-composite material catalyst as claimed in claim 1, it is characterised in that step (1)
Described in polyphenyl urea powder PU, preparation process is as follows：
Under electric stirring, the p-phenylenediamine of 17.0 g acetone and 2.47-3.07 mmol is dissolved into the solution of clarification, adds 8-
12 g water, after ice bath cools down 10 min, with 300 rpm stir speed (S.S.), 22-24 mmol toluene di-isocyanate(TDI)s are added dropwise in constant speed
With the blended liquid of 8-10 g acetone, 30min is dripped off, and is warming up to 30 DEG C, is incubated the h of polymerisation 3, and product is filtered and separated, and
Washed the solid three times, obtained with the water and acetone mixture that mass ratio is 3/7 and be dried to constant weight in 70 DEG C of baking oven, that is, made
Polyphenyl urea powder PU was obtained, yield is 81-89 %.
3. the preparation method of porous carbon nano-composite material catalyst as claimed in claim 1, it is characterised in that step (1)
Described in polyphenyl urea powder PU and porous Fe (III)-polyphenyl urea coordination polymer material, be three-dimensional porous material, its is porous
It is made up of micropore, mesoporous and less than 4 um macropore.
4. the preparation method of porous carbon nano-composite material catalyst as claimed in claim 1, it is characterised in that step (2)
Described in porous carbon@Fe2O3Nano composite material, it is porous graphite base material load Fe2O3The composite that nano-particle is formed,
Its it is porous by micropore, mesoporous and less than 6 um macropore form, Fe2O3Nano particle diameter is 20-30 nm.
5. the preparation method of porous carbon nano-composite material catalyst as claimed in claim 1, it is characterised in that step (3)
Described in porous carbon@Fe2O3@Co (II) nano composite material, it is porous carbon@Fe2O3Nano composite material load C o (II) is just
The three-dimensional manometer composite that ion is formed, its it is porous by micropore, mesoporous and less than 6 um macropore forms.
6. porous carbon nano-composite material catalyst prepared by preparation method as claimed in claim 1 is analysed for electrochemical catalysis
The application of oxygen.
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