CN107597169A - A kind of multi-functional composite catalyst of biomass-based N doping porous carbon, preparation method and applications - Google Patents
A kind of multi-functional composite catalyst of biomass-based N doping porous carbon, preparation method and applications Download PDFInfo
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- CN107597169A CN107597169A CN201711088670.3A CN201711088670A CN107597169A CN 107597169 A CN107597169 A CN 107597169A CN 201711088670 A CN201711088670 A CN 201711088670A CN 107597169 A CN107597169 A CN 107597169A
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- 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 multi-functional composite catalyst of biomass-based N doping porous carbon, preparation method and applications, belong to electro-catalysis technical field.It is then to be dried overnight with deionized water rinsing cicada slough with removing the dust on surface at 70~90 DEG C first；The cicada slough that above-mentioned pretreatment is obtained again and ZnCl2It is 1 by weight：2~6 ratio mechanical mixture, gained mixture is with 300~600rpm rotating speed ball milling 5~10 hours；Again by obtained solid powder in 800~950 DEG C, N2Handled 5~10 hours in atmosphere；After being cooled to room temperature, with 0.2~1.0M HNO3Product is rinsed to remove possible metal deposit with 0.5~2M HCl mixed liquors, is fully washed with deionized water, is finally dried overnight under the conditions of 70~90 DEG C, that is, obtains the biomass-based multi-functional composite catalyst of N doping porous carbon of the present invention.The catalyst in the range of the full pH hydrogen reduction catalysis, can be applied in oxygen evolution reaction catalysis and the reduction of electro-catalysis nitrogen in alkaline range.
Description
Technical field
The invention belongs to electro-catalysis technical field, and in particular to one kind possesses the reversible catalysis (ORR, OER) of oxygen and nitrogen reduction
(NRR) the multi-functional composite catalyst of biomass-based N doping porous carbon, preparation method and applications.
Background technology
ORR and OER reactions are fuel cell and the important electrochemical reaction process of electrolysis water respectively, but complicated in reacting
Multielectron transfer process can cause high overpotential so that they react slow, therefore these are reacted to rate limiting step
Suddenly, thus need to find efficient catalyst to improve reaction rate to adapt to the needs in practical application.At present, performance is best
ORR catalyst be Pt base catalyst, the best OER catalyst of performance is RuO2Or IrO2.However, the OER of Pt base catalyst
Energy and RuO2Or IrO2ORR performances and bad, largely use high expensive, durability caused by noble metal catalyst in addition
It is bad to be unfavorable for its large-scale application.Therefore, finding alternative effective catalyst turns into these energy conversions and memory device
The key of widespread commercialization application.Research and develop aboundresources, it is cheap and easy to get, there is the prominent reversible catalytic activity of oxygen and stably
Property non-platinum catalyst substitute the platinum based catalyst of costliness to be key technology difficulty that current scientific circles' needs are captured.
Porous carbon materials have the spies such as high specific surface area, porosity, regulatable aperture, excellent chemical stability
Point, therefore be widely used in adsorbing, be catalyzed, separate, the field such as energy storage.
Biological qualitative diversity determines that its constituent is also varied.Charcoal is to be pyrolyzed the one kind obtained after biomass
Carbon containing high solid residue, it is a current international study hotspot.Charcoal pore structure is flourishing, environmental stability is high,
Electric conductivity is good.Catalysis reversible to oxygen without activity, and by doping and modification (as introduced nitrogen-atoms), changes carbon material in itself
The surface texture of material, the basic sites for increasing material surface, enhance its hydrophily, and carbon material can be made to produce the reversible catalysis of oxygen
Activity.Thus, a kind of biomass carbon sill with the reversible catalytic performance of oxygen is developed, will effectively reduce material cost,
Stability is improved, there is good commercial application prospect.
In addition, ammonia is one of important inorganic chemical product, ammonia synthesizing industry occupies critical role in national economy.It is logical
Classical Haber-Bosch techniques are crossed by N2It is converted into NH3, it is necessary to using iron-based material as catalyst, under severe reaction conditions
Carry out (15~25MPa, 300~550 DEG C).The 1~2% of world energy supplies need to be consumed by providing reaction condition, about be produced every year
2.3 tons of carbon dioxide.It is presently used for NH3The raw material of synthesis --- hydrogen about consumes the world every year essentially from the reformation of methane
The 3~5% of gas production, and discharge substantial amounts of carbon monoxide and carbon dioxide.In view of fossil fuel shortages and global gas
Change is waited, the energy demand by reducing fixed nitrogen process is a challenging and target for chronicity.Once there is document report
Cross and the carbon-supported catalysts of N doping are applied to the reduction of photocatalysis nitrogen, and electro-catalysis NRR is also rarely reported.
The content of the invention
The carbon-supported catalysts of Heteroatom doping show the catalytic performance and stability of exceptional, by researchers'
Extensive concern.The present invention is prepared for a kind of new life with high specific surface area, abundant multi-stage porous using cicada slough as raw material
The multi-functional composite catalyst of material base N doping porous carbon.
For this method using cheap cicada slough as raw material, zinc chloride is activator, by after ball milling mixing in nitrogen atmosphere
Lower high-temperature calcination, then prepare after pickling, washing, drying the biomass-based nitrogen of high-specific surface area, big pore volume, hierarchical porous structure
Adulterate the multi-functional composite catalyst of porous carbon.Shown through electromicroscopic photograph：The material of preparation is the pore passage structure of three-dimensional foam shape,
XPS analysis show that nitrogen content is 1.73~2.20%, and its specific surface area is 1112.24~1547.13m2/g.By obtained nitrogen
Carbon material is adulterated as the OER catalyst under the ORR catalyst and alkalescence condition in the range of full pH, high activity is respectively provided with and height is steady
It is qualitative.In addition, also applying it under normal temperature and pressure on electro-catalysis fixed nitrogen, production ammonia performance well is also achieved.The preparation side
Method is simple, and raw material green is friendly, cheap, and yield is high, can effectively reduce cost, increase economic efficiency.
A kind of preparation method of biomass-based multi-functional composite catalyst of N doping porous carbon of the present invention, its step
It is as follows：
(1) then it is dried overnight with deionized water rinsing cicada slough with removing the dust on surface at 70~90 DEG C；Again will
The cicada slough and ZnCl that above-mentioned pretreatment obtains2It is 1 by weight：2~6 ratio mechanical mixture, gained mixture with 300~
600rpm rotating speed ball milling 5~10 hours；
(2) by the solid powder that step (1) obtains in 800~950 DEG C, N2Handled 5~10 hours in atmosphere；It is cooled to room
Wen Hou, with 0.2~1.0M HNO3Product is rinsed to remove possible metal deposit with 0.5~2M HCl mixed liquors, then is used
Deionized water is fully washed, and is finally dried overnight under the conditions of 70~90 DEG C, that is, is obtained biomass-based nitrogen of the present invention and mixed
The miscellaneous multi-functional composite catalyst of porous carbon.
A kind of biomass-based multi-functional composite catalyst of N doping porous carbon, it is that the above method is prepared.
Application of the biomass-based multi-functional composite catalyst of N doping porous carbon in hydrogen reduction catalysis in the range of full pH.
The biomass-based multi-functional composite catalyst of N doping porous carbon answering in oxygen evolution reaction catalysis in alkaline range
With.
Application of the biomass-based multi-functional composite catalyst of N doping porous carbon in the reduction of electro-catalysis nitrogen.
A kind of preparation method of N doping porous carbon of the present invention, this method its advantage and have compared with prior art
Beneficial effect is：
1. application effect is good.Biomass carbon-supported catalysts show higher oxygen as a kind of non-metal kind elctro-catalyst
Reduction reaction activity and stability, especially in the basic conditions, its catalytic effect has been over business platinum carbon.
It is 2. multi-functional.
3. present invention process flow is simple, the cycle is short, high-specific surface area, the carbon-based catalysis of biomass of high stability can be prepared
Agent；It is the reagent safety that is used in biomass carbon sill preparation process, nontoxic, it is environmentally safe.
4. biomass of the present invention can prepare pore structure and specific surface area is controllable by controlling the temperature of different heat treatment
Biomass carbon sill.
5. catalyst cost of the present invention is cheap, has wide range of applications.Compared with the noble metals such as conventional Pt, material cost
Substantially reduce.
A kind of preparation method of N doping porous carbon of the present invention, the novelty of this method are with cheap
Biomass is raw material, prepares nitrogen-doped porous carbon material.Relative to SiO2Masterplate method, ammonia facture, the present invention not only operate
Simply, without adding masterplate post-treating and other steps, so as to reduce old, its economic benefit is improved.
Brief description of the drawings
Fig. 1：The XRD of the biomass-based multi-functional composite catalyst of N doping porous carbon prepared for the embodiment of the present invention 3,
It is the structure of a standard class graphene to show the material.Abscissa represents 2 θ angles in figure.
Fig. 2：The scanning electricity of the biomass-based multi-functional composite catalyst of N doping porous carbon prepared for the embodiment of the present invention 3
Mirror photo, it can be seen that the porous carbon shows the pore structure pattern of three-dimensional foam shape.
Fig. 3：The nitrogen of the biomass-based multi-functional composite catalyst of N doping porous carbon prepared for the embodiment of the present invention 3 is inhaled
Desorption isotherm, it can be seen that there is desorption hysteresis winding, show the prepared biomass-based more work(of N doping porous carbon
Energy composite catalyst has meso-hole structure.In addition, it can be seen that respectively in micropore (P/P0=0~0.2) pressure span and
Mesoporous (P/P0>0.4) there is obvious hysteresis curve pressure span, is attributed to micropore and mesoporous respectively.Ordinate, which represents, in figure inhales
Attached nitrogen volume, abscissa represent relative pressure.
Fig. 4：The aperture point of the biomass-based multi-functional composite catalyst of N doping porous carbon prepared for the embodiment of the present invention 3
Butut, it can be seen that prepared material is a kind of containing a large amount of micropores and a certain amount of mesoporous multilevel hole material；
Fig. 5：The XPS of the biomass-based multi-functional composite catalyst of N doping porous carbon prepared for the embodiment of the present invention 3 is complete
Spectrogram, it can be seen that the material for preparing of the present invention mainly contains C, N, O elements, elementary analysis shows that nitrogen content is
1.73~2.20%, further demonstrate nitrogen-atoms and be successfully doped into carbon material.Wherein abscissa represents electron energy.
Embodiment
Below by embodiment, the present invention is described in detail, but the present invention is not limited only to embodiment.
Embodiment 1
1. then it is dried overnight with deionized water rinsing cicada slough with removing the dust on surface at 80 DEG C.Then will be pre-
The 1g cicada sloughs of processing and 4g ZnCl2Mechanical mixture, the mixture of gained is in planetary ball mill instrument with 500rpm rotating speed ball milling 10
Hour, the mesh number for obtaining material is 200~400 mesh.
2. the solid powder of gained is placed in tube furnace, at 800 DEG C, N2Handled 6 hours in atmosphere.
3. after tube furnace is cooled to environment temperature, with 0.5M HNO3Product is rinsed to remove with 1M HCl mixed liquors
Possible metal deposit, then fully washed with deionized water, finally it is dried overnight in 80 DEG C of baking oven, that is, obtains biomass
The multi-functional composite catalyst of base N doping porous carbon.
Embodiment 2
1. then it is dried overnight with deionized water rinsing cicada slough with removing the dust on surface at 80 DEG C.Then will be pre-
The 1g cicada sloughs of processing and 4g ZnCl2Mechanical mixture, the mixture of gained is in planetary ball mill instrument with 500rpm rotating speed ball milling 10
Hour, the mesh number for obtaining material is 200~400 mesh.
2. the solid powder of gained is placed in tube furnace, at 850 DEG C, N2Handled 6 hours in atmosphere.
3. after tube furnace is cooled to environment temperature, with 0.5M HNO3Product is rinsed to remove with 1M HCl mixed liquors
Possible metal deposit, then fully washed with deionized water, finally it is dried overnight in 80 DEG C of baking oven, that is, obtains biomass
The multi-functional composite catalyst of base N doping porous carbon.
Embodiment 3
1. then it is dried overnight with deionized water rinsing cicada slough with removing the dust on surface at 80 DEG C.Then will be pre-
The 1g cicada sloughs of processing and 4g ZnCl2Mechanical mixture, the mixture of gained is in planetary ball mill instrument with 500rpm rotating speed ball milling 10
Hour, the mesh number for obtaining material is 200~400.
2. the solid powder of gained is placed in tube furnace, at 900 DEG C, N2Handled 6 hours in atmosphere.
3. after tube furnace is cooled to environment temperature, with 0.5M HNO3Product is rinsed to remove with 1M HCl mixed liquors
Possible metal deposit, then fully washed with deionized water, finally it is dried overnight in 80 DEG C of baking oven, that is, obtains biomass
The multi-functional composite catalyst of base N doping porous carbon.
Embodiment 4
1. then it is dried overnight with deionized water rinsing cicada slough with removing the dust on surface at 80 DEG C.Then will be pre-
The 1g cicada sloughs of processing and 4g ZnCl2Mechanical mixture, the mixture of gained is in planetary ball mill instrument with 500rpm rotating speed ball milling 10
Hour, the mesh number for obtaining material is 200~400 mesh.
2. the solid powder of gained is placed in tube furnace, at 950 DEG C, N2Handled 6 hours in atmosphere.
3. after tube furnace is cooled to environment temperature, with 0.5M HNO3Product is rinsed to remove with 1M HCl mixed liquors
Possible metal deposit, then fully washed with deionized water, finally it is dried overnight in 80 DEG C of baking oven, that is, obtains biomass
The multi-functional composite catalyst of base N doping porous carbon.
Embodiment 5
The test of oxygen reduction reaction
The catalyst 30mg of the preparation of embodiment 3 is weighed, it is 5% to sequentially add 2mL ethanol and 67mg, mass fractionEmulsion, take 10 μ L drop coatings to be overlying on rotating circular disk (RDE) electrode surface in slurries of the ultrasonic disperse after uniform and obtain work
Electrode, using carbon-point as to electrode, using Hg/HgO electrodes as reference electrode under alkalescence condition (pH=13), neutrallty condition (pH=
7) and acid condition (pH=0) under using Ag/AgCl electrodes as reference electrode, with 10mV s-1Sweep speed carry out linear scan
(LSV), electrode rotating speed is 1600rpm, O2Take-off potential is 1.05V under the alkalescence condition of saturation, half wave potential 0.91V, pole
Current density of rationing the power supply is -8.66mA cm-2；In O2Take-off potential under the neutrallty condition of saturation is 0.942V, and half wave potential is
0.676V, limiting current density are -8.50mA cm-2；In O2Take-off potential under the acid condition of saturation is 0.899V, half-wave
Current potential is 0.630V, and limiting current density is -7.52mA cm-2。
Embodiment 6
The test of oxygen evolution reaction
The catalyst 30mg of the preparation of embodiment 3 is weighed, it is 5% to sequentially add 2mL ethanol and 67mg, mass fraction
Nafion emulsions, by slurries of the ultrasonic disperse after uniform take it is appropriate obtain working electrode coated on RDE electrode surfaces, using carbon-point as
To electrode, Hg/HgO electrodes are reference electrode, in O2In the 0.1M KOH solutions of saturation, with 10mV s-1Speed of sweeping circulated
Voltammetric scan, its 10mA cm-2Corresponding potential is 1.53V, and Tafel slopes are 66mV dec-1。
Embodiment 7
The test of nitrogen reduction
For N2Reduction experiment, in N2Constant potential experiment is carried out in the 0.1M HCl solutions of saturation and (uses N before measuring2Drum
Bubble sweeps HCl electrolyte 30 minutes).In H type electrolytic cells, nitrogen (99.99%) is carried out at a constant temperature respectively using 20 DEG C of recirculated waters
Also the films of reason Nafion 115.For preparation work electrode, the catalyst 4.0mg ultrasonic disperses that embodiment 3 will be weighed prepare
30 minutes in the 100 μ L ethanol solutions containing 0.05wt%Nafion.Then the dispersion liquid drop coating that will equably prepare before
It is 1 × 1cm to area2Carbon paper electrode on, and dried under the conditions of room temperature environment, be by calculating generated ammonia yield
15.66μg h-1mg-1, faradic efficiency 1.18%.
Claims (5)
1. a kind of preparation method of the biomass-based multi-functional composite catalyst of N doping porous carbon, its step are as follows：
(1) then it is dried overnight with deionized water rinsing cicada slough with removing the dust on surface at 70~90 DEG C；Again will be above-mentioned
Pre-process obtained cicada slough and ZnCl2It is 1 by weight：2~6 ratio mechanical mixture, gained mixture is with 300~600rpm
Rotating speed ball milling 5~10 hours；
(2) by the solid powder that step (1) obtains in 800~950 DEG C, N2Handled 5~10 hours in atmosphere；After being cooled to room temperature,
With 0.2~1.0M HNO3Rinse product with 0.5~2M HCl mixed liquors to remove possible metal deposit, then spend from
Sub- water fully washs, and is finally dried overnight under the conditions of 70~90 DEG C, that is, it is multi-functional multiple to obtain biomass-based N doping porous carbon
Close catalyst.
A kind of 2. biomass-based multi-functional composite catalyst of N doping porous carbon, it is characterised in that：It is the side as described in claim 1
Method is prepared.
3. the biomass-based multi-functional composite catalyst of N doping porous carbon hydrogen reduction in the range of full pH described in claim 2 is urged
Application in change.
4. the biomass-based multi-functional composite catalyst of N doping porous carbon oxygen evolution reaction in alkaline range described in claim 2
Application in catalysis.
5. the biomass-based multi-functional composite catalyst of N doping porous carbon the answering in the reduction of electro-catalysis nitrogen described in claim 2
With.
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| CN108134098A (en) * | 2018-02-11 | 2018-06-08 | 中国科学院青岛生物能源与过程研究所 | A kind of efficient biomass carbon electrochemical oxygen reduction catalyst and its preparation method and application |
| CN108660481A (en) * | 2018-04-25 | 2018-10-16 | 浙江理工大学 | A kind of novel N doping biological carbon Quito hole elctro-catalyst preparation method |
| CN109569696A (en) * | 2019-01-30 | 2019-04-05 | 中国矿业大学 | A kind of preparation method and its hydrogen reduction catalytic applications of N doping biomass porous carbon |
| CN110605131A (en) * | 2019-05-07 | 2019-12-24 | 韦萍洁 | Three-dimensional nitrogen-doped carbon-based material loaded bimetallic phosphide bifunctional catalyst and preparation method and application thereof |
| CN111206256A (en) * | 2020-02-27 | 2020-05-29 | 上海理工大学 | Biochar electrochemical reforming hydrogen production method based on biomass multistage utilization |
| CN111569930A (en) * | 2020-05-19 | 2020-08-25 | 东北师范大学 | Zinc monoatomic catalyst and preparation method and application thereof |
| CN112028052A (en) * | 2020-09-18 | 2020-12-04 | 西北大学 | Preparation method and application of biomass carbon-based Fe monatomic-N doped porous carbon material |
| CN112316981A (en) * | 2019-07-19 | 2021-02-05 | 天津师范大学 | Composite material based on nano porous gold and zeolite imidazole framework and preparation method and application thereof |
| CN113134347A (en) * | 2021-03-23 | 2021-07-20 | 西安理工大学 | Preparation method and application of heteroatom porous carbon |
| CN113897625A (en) * | 2021-10-14 | 2022-01-07 | 电子科技大学广东电子信息工程研究院 | Composite catalyst and preparation method thereof |
| CN114318412A (en) * | 2022-01-27 | 2022-04-12 | 江西师范大学 | Limited-domain N-doped Fe nano-particles and preparation method and application thereof |
| CN114725328A (en) * | 2021-12-17 | 2022-07-08 | 安徽师范大学 | Nitrogen-doped biomass-derived porous carbon-supported Fe3O4Fe composite material and preparation method and application thereof |
| CN114875444A (en) * | 2022-04-27 | 2022-08-09 | 东南大学 | Preparation method of nitrogen-sulfur atom-rich doped biomass-derived hydrogen evolution electrocatalyst |
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| CN108134098B (en) * | 2018-02-11 | 2020-02-21 | 中国科学院青岛生物能源与过程研究所 | Efficient biomass carbon electrochemical oxygen reduction catalyst and preparation method and application thereof |
| CN108134098A (en) * | 2018-02-11 | 2018-06-08 | 中国科学院青岛生物能源与过程研究所 | A kind of efficient biomass carbon electrochemical oxygen reduction catalyst and its preparation method and application |
| CN108660481A (en) * | 2018-04-25 | 2018-10-16 | 浙江理工大学 | A kind of novel N doping biological carbon Quito hole elctro-catalyst preparation method |
| CN109569696A (en) * | 2019-01-30 | 2019-04-05 | 中国矿业大学 | A kind of preparation method and its hydrogen reduction catalytic applications of N doping biomass porous carbon |
| CN110605131A (en) * | 2019-05-07 | 2019-12-24 | 韦萍洁 | Three-dimensional nitrogen-doped carbon-based material loaded bimetallic phosphide bifunctional catalyst and preparation method and application thereof |
| CN112316981A (en) * | 2019-07-19 | 2021-02-05 | 天津师范大学 | Composite material based on nano porous gold and zeolite imidazole framework and preparation method and application thereof |
| CN112316981B (en) * | 2019-07-19 | 2022-07-01 | 天津师范大学 | Composite material based on nano porous gold and zeolite imidazole framework and preparation method and application thereof |
| CN111206256B (en) * | 2020-02-27 | 2021-04-30 | 上海理工大学 | Biochar electrochemical reforming hydrogen production method based on biomass multistage utilization |
| CN111206256A (en) * | 2020-02-27 | 2020-05-29 | 上海理工大学 | Biochar electrochemical reforming hydrogen production method based on biomass multistage utilization |
| CN111569930A (en) * | 2020-05-19 | 2020-08-25 | 东北师范大学 | Zinc monoatomic catalyst and preparation method and application thereof |
| CN111569930B (en) * | 2020-05-19 | 2022-12-13 | 东北师范大学 | Zinc monoatomic catalyst and preparation method and application thereof |
| CN112028052A (en) * | 2020-09-18 | 2020-12-04 | 西北大学 | Preparation method and application of biomass carbon-based Fe monatomic-N doped porous carbon material |
| CN112028052B (en) * | 2020-09-18 | 2022-03-29 | 西北大学 | Preparation method and application of biomass carbon-based Fe monatomic-N doped porous carbon material |
| CN113134347A (en) * | 2021-03-23 | 2021-07-20 | 西安理工大学 | Preparation method and application of heteroatom porous carbon |
| CN113897625B (en) * | 2021-10-14 | 2022-09-23 | 电子科技大学广东电子信息工程研究院 | Composite catalyst and preparation method thereof |
| CN113897625A (en) * | 2021-10-14 | 2022-01-07 | 电子科技大学广东电子信息工程研究院 | Composite catalyst and preparation method thereof |
| CN114725328A (en) * | 2021-12-17 | 2022-07-08 | 安徽师范大学 | Nitrogen-doped biomass-derived porous carbon-supported Fe3O4Fe composite material and preparation method and application thereof |
| CN114725328B (en) * | 2021-12-17 | 2023-10-27 | 安徽师范大学 | Nitrogen-doped biomass-derived porous carbon-loaded Fe 3 O 4 Fe composite material, preparation method and application thereof |
| CN114318412A (en) * | 2022-01-27 | 2022-04-12 | 江西师范大学 | Limited-domain N-doped Fe nano-particles and preparation method and application thereof |
| CN114875444A (en) * | 2022-04-27 | 2022-08-09 | 东南大学 | Preparation method of nitrogen-sulfur atom-rich doped biomass-derived hydrogen evolution electrocatalyst |
| CN114875444B (en) * | 2022-04-27 | 2024-02-02 | 东南大学 | Preparation method of biomass-derived hydrogen evolution electrocatalyst doped with nitrogen-rich sulfur atoms |
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