CN104009242A - Preparation method of metal/metal oxide loaded nitrogen-doped porous carbon network-structure material - Google Patents
Preparation method of metal/metal oxide loaded nitrogen-doped porous carbon network-structure material Download PDFInfo
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- CN104009242A CN104009242A CN201410181761.1A CN201410181761A CN104009242A CN 104009242 A CN104009242 A CN 104009242A CN 201410181761 A CN201410181761 A CN 201410181761A CN 104009242 A CN104009242 A CN 104009242A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
- H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- Y02E60/13—Energy storage using capacitors
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
A preparation method of a metal/metal oxide loaded nitrogen-doped porous carbon network-structure material is provided. With natural macromolecules as raw materials, a metal salt solution is added, a sol is formed, and then a hydrogel is obtained by adding an alkaline substance; the hydrogel is washed and freeze-dried to obtain a dried gel; the dried gel is subjected to heat treatment with a nitrogen atmosphere in a tube furnace to obtain the product. The preparation method has the beneficial effects that: 1, the natural macromolecules are used as a carbon source and a nitrogen source, have natural sources, can be recycled, and have large biomass; 2, the prepared material is the metal/metal oxide loaded porous carbon network-structure material; and 3, the material prepared by the method has quite excellent oxygen electro-catalytic reduction performance. The material also has potential application values in many fields such as super capacitors, lithium ion batteries, organic catalysis, photocatalysis and gas adsorption.
Description
Technical field
The invention belongs to carbon composite nano-material field, relate in particular to a kind of preparation method of nitrogen doping porous carbon composite network structural material.
Background technology
Porous carbon materials, owing to having large specific area, is widely used at aspects such as electro-catalysis, organic catalysis, ultracapacitor, photocatalysis, sewage disposal, gas absorption.Because nitrogen adulterates, can change very many-sided performance of material with carbon element, the porous carbon materials of nitrogen doping has potential application in a lot of fields.For example, in fuel battery cathod catalyst method, the porous carbon materials of nitrogen doping is desirable catalyst carrier.Metal oxide can be worked in coordination with the performance (improving oxygen Electrochemical Properties) that strengthens fuel battery cathod catalyst with the material with carbon element of nitrogen doping.Developing simple to operate, the raw material cheap method of originating comes the fuel battery cathod catalyst that processability is good significant.
Summary of the invention
In view of this, it is the porous carbon network structure material that raw material is prepared the nitrogen doping of metal/metal oxide load with natural polymer that the technical problem to be solved in the present invention is to provide a kind of, and the network combined structural material of porous carbon provided by the invention shows significant oxygen Electrochemical Properties.
Take natural polymer chitosan as raw material, add metal salt solution, form colloidal sol, by adding alkaline matter, obtain hydrogel, to its wash, freeze drying, obtain dry gel, dry gel is used to nitrogen atmosphere heat treatment in tube furnace, obtain product.
The present invention adopts following technical scheme to achieve these goals:
A porous carbon network structure material preparation method for the nitrogen doping of metal/metal oxide load, is characterized in that: comprise the following steps:
A) take natural polymer chitosan as raw material, add metal salt solution, form colloidal sol;
B) by slowly adding alkalescent material, obtain hydrogel, to its wash, freeze drying, obtain dry gel;
C) dry gel is used to nitrogen atmosphere heat treatment in tube furnace, temperature is 750-850
oc, the time is 0.5-2.5 h, obtains product.
The porous carbon network structure material preparation method of the nitrogen doping of described a kind of metal/metal oxide load, is characterized in that: the weight ratio of shitosan and metal salt solution is 2-4:6-10.
The porous carbon network structure material preparation method of the nitrogen doping of described a kind of metal/metal oxide load, is characterized in that: described step a) specifically comprises: take appropriate shitosan, with the acetate dissolution of 5% left and right, add wherein Co (NO
3)
2, or Mn (NO
3)
2or Ni (NO
3)
2,magnetic agitation, forms uniform colloidal sol.
The porous carbon network structure material preparation method of the nitrogen doping of described a kind of metal/metal oxide load, it is characterized in that: described step b) specifically comprises: be placed in the atmosphere of ammonia or slowly add ammoniacal liquor with buret, after 1-8 hour, obtain hydrogel, to its wash, freeze drying, obtain dry gel.
Compared with prior art, the invention provides a kind of porous carbon network structure material preparation method of nitrogen doping of metal/metal oxide load, the present invention has following features:
1. with natural polymer chitosan, be Carbon and nitrogen sources, source nature, can circulate, and this biological quality is large.Whole material preparation method is simple, is easy to realize industrialization.
2. the porous carbon network structure material of the nitrogen doping of the metal/metal oxide load that prepared by the method has very outstanding oxygen electrical catalyze reduction performance.
3. synthetic porous carbon network structure material, BET surface area is large, and the nitrogen element content of doping is high.This material probably also can have potential using value in various fields such as ultracapacitor, lithium ion battery, organic catalysis, photocatalysis, gas absorption.
Accompanying drawing explanation
In Fig. 1, Fig. 1 a is the stereoscan photograph of the product for preparing of the embodiment of the present invention 1; Fig. 1 b is the transmission electron microscope photo of the product for preparing of the embodiment of the present invention 1; Fig. 1 c is the high-resolution-ration transmission electric-lens photo of the product for preparing of the embodiment of the present invention 1;
Fig. 2 is the x-ray diffraction pattern of the product for preparing of the embodiment of the present invention 1;
Fig. 3 is the BET result of the product for preparing of the embodiment of the present invention 1;
Fig. 4 be the product for preparing of the embodiment of the present invention 1 oxygen electroreduction catalytic performance with and stability.
embodiment,
In order to further illustrate the present invention, below in conjunction with embodiment, product preparation method provided by the invention is described in detail.
Embodiment 1
Take 2 grams of shitosans, use 5% acetate dissolution, add wherein Co (NO
3)
25 grams, magnetic agitation 2 hours, forms uniform colloidal sol.Be placed in the atmosphere of ammonia, 2-6 hour, obtains hydrogel, to its wash, freeze drying, obtain dry gel, dry gel is used to nitrogen atmosphere heat treatment, 800 in tube furnace
oc, times 1.5 h.Obtain product.
Embodiment 2
Take 2 grams of shitosans, use 5% acetate dissolution, add wherein Co (NO
3)
210 grams, magnetic agitation 1 hour, forms uniform colloidal sol.Be placed in the atmosphere of ammonia, 3-8 hour, obtains hydrogel, to its wash, freeze drying, obtain dry gel, dry gel is used to nitrogen atmosphere heat treatment, 750 in tube furnace
oc, times 1.5 h.Obtain product.
Embodiment 3
Take 4 grams of shitosans, use 5% acetate dissolution, add wherein Co (NO
3)
210 grams, magnetic agitation 2 hours, forms uniform colloidal sol.Be placed in the atmosphere of ammonia, 4-8 hour, obtains hydrogel, to its wash, freeze drying, obtain dry gel, dry gel is used to nitrogen atmosphere heat treatment, 750 in tube furnace
oc, times 2 h.Obtain product.
Embodiment 4
Take 2 grams of shitosans, use 5% acetate dissolution, add wherein Co (NO
3)
210 grams, magnetic agitation 0.5 hour, forms uniform colloidal sol.Be placed in the atmosphere of ammonia, 3-10 hour, obtains hydrogel, to its wash, freeze drying, obtain dry gel, dry gel is used to nitrogen atmosphere heat treatment, 700 in tube furnace
oc, times 2.5 h.Obtain product.
Embodiment 5
Take 2 grams of shitosans, use 5% acetate dissolution, add wherein Co (NO
3)
24 grams, magnetic agitation 0.5 hour, forms uniform colloidal sol.Be placed in the atmosphere of ammonia, 3-6 hour, obtains hydrogel, to its wash, freeze drying, obtain dry gel, dry gel is used to nitrogen atmosphere heat treatment, 750 in tube furnace
oc, time 1 h.Obtain product.
Embodiment 6
Take 2 grams of shitosans, use 5% acetate dissolution, add wherein Co (NO
3)
26 grams, magnetic agitation 1.5 hours, forms uniform colloidal sol.Be placed in the atmosphere of ammonia, 2-3 hour, obtains hydrogel, to its wash, freeze drying, obtain dry gel, dry gel is used to nitrogen atmosphere heat treatment, 750 in tube furnace
oc, times 2 h.Obtain product.
Embodiment 7
Take 2 grams of shitosans, use 5% acetate dissolution, add wherein Ni (NO
3)
26 grams, magnetic agitation 1.5 hours, forms uniform colloidal sol.Be placed in the atmosphere of ammonia, 3-6 hour, obtains hydrogel, to its wash, freeze drying, obtain dry gel, dry gel is used to nitrogen atmosphere heat treatment, 750 in tube furnace
oc, time 1 h.Obtain product.
Embodiment 8
Take 2 grams of shitosans, use 5% acetate dissolution, add wherein Ni (NO
3)
28 grams, magnetic agitation 1 hour, forms uniform colloidal sol.Be placed in the atmosphere of ammonia, 3-6 hour, obtains hydrogel, to its wash, freeze drying, obtain dry gel, dry gel is used to nitrogen atmosphere heat treatment, 800 in tube furnace
oc, times 2 h.Obtain product.
Embodiment 9
Take 4 grams of shitosans, use 5% acetate dissolution, add wherein Ni (NO
3)
28 grams, magnetic agitation 2 hours, forms uniform colloidal sol.Be placed in the atmosphere of ammonia, 3-6 hour, obtains hydrogel, to its wash, freeze drying, obtain dry gel, dry gel is used to nitrogen atmosphere heat treatment, 700 in tube furnace
oc, time 1 h.Obtain product.
Embodiment 10
Take 4 grams of shitosans, use 5% acetate dissolution, add wherein Mn (NO
3)
28 grams, magnetic agitation 2 hours, forms uniform colloidal sol.Be placed in the atmosphere of ammonia, 2-6 hour, obtains hydrogel, to its wash, freeze drying, obtain dry gel, dry gel is used to nitrogen atmosphere heat treatment, 750 in tube furnace
oc, time 1 h.Obtain product.
Embodiment 11
Take 4 grams of shitosans, use 5% acetate dissolution, add wherein Mn (NO
3)
210 grams, magnetic agitation 2 hours, forms uniform colloidal sol.Be placed in the atmosphere of ammonia, 3-6 hour, obtains hydrogel, to its wash, freeze drying, obtain dry gel, dry gel is used to nitrogen atmosphere heat treatment, 800 in tube furnace
oc, time 1 h.Obtain product.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (4)
1. the porous carbon network structure material preparation method that the nitrogen of metal/metal oxide load adulterates, is characterized in that: comprise the following steps:
A) take natural polymer chitosan as raw material, add metal salt solution, form colloidal sol;
B) by slowly adding alkalescent material, obtain hydrogel, to its wash, freeze drying, obtain dry gel;
C) dry gel is used to nitrogen atmosphere heat treatment in tube furnace, temperature is 750-850
oc, the time is 0.5-2.5 h, obtains product.
2. the porous carbon network structure material preparation method of the nitrogen of a kind of metal/metal oxide load according to claim 1 doping, is characterized in that: the weight ratio of shitosan and metal salt solution is 2-4:6-10.
3. the porous carbon network structure material preparation method that the nitrogen of a kind of metal/metal oxide load according to claim 1 adulterates, it is characterized in that: described step a) specifically comprises: take appropriate shitosan, with the acetate dissolution of 5% left and right, add wherein Co (NO
3)
2, or Mn (NO
3)
2or Ni (NO
3)
2,magnetic agitation, forms uniform colloidal sol.
4. the porous carbon network structure material preparation method that the nitrogen of a kind of metal/metal oxide load according to claim 1 and 2 adulterates, it is characterized in that: described step b) specifically comprises: be placed in the atmosphere of ammonia or slowly add ammoniacal liquor with buret, after 1-8 hour, obtain hydrogel, to its wash, freeze drying, obtain dry gel.
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| CN201410181761.1A CN104009242B (en) | 2014-04-30 | 2014-04-30 | The porous carbon network structure material preparation method of the N doping of a kind of fuel battery cathod catalyst metal/metal oxide load |
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| CN201410181761.1A CN104009242B (en) | 2014-04-30 | 2014-04-30 | The porous carbon network structure material preparation method of the N doping of a kind of fuel battery cathod catalyst metal/metal oxide load |
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| CN104009242B CN104009242B (en) | 2016-02-10 |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104617311A (en) * | 2014-11-20 | 2015-05-13 | 安徽大学 | Nitrogen and cobalt doped mesoporous carbon/graphene composite material and preparation method thereof |
| CN106252673A (en) * | 2016-08-22 | 2016-12-21 | 首都师范大学 | A kind of preparation method of Fe N/C oxygen reduction reaction catalyst based on natural plants tissue |
| CN106356537A (en) * | 2016-11-18 | 2017-01-25 | 中南大学 | Preparation method of nitrogen-doped porous carbon foam material and application of nitrogen-doped porous carbon foam material in metal-air battery |
| CN106783236A (en) * | 2017-02-20 | 2017-05-31 | 青岛科技大学 | A kind of N doping graphitized carbon/transition metal oxide nano composite material and preparation method thereof |
| CN107293730A (en) * | 2017-07-31 | 2017-10-24 | 中南大学 | A kind of Ni@N C composite positive poles, preparation method and the application in lithium-air battery |
| CN107578928A (en) * | 2017-09-11 | 2018-01-12 | 桂林电子科技大学 | A kind of nickel based on persimmon tannin absorption, the porous carbon composite and its preparation method and application of cobalt doped |
| CN107804836A (en) * | 2017-11-07 | 2018-03-16 | 桂林电子科技大学 | It is prepared by a kind of three-dimensional grapheme and its one-step method based on biopolymer |
| CN107958793A (en) * | 2017-11-07 | 2018-04-24 | 桂林电子科技大学 | A kind of three-dimensional grapheme and preparation method and application of CoO doping |
| CN108172413A (en) * | 2017-12-25 | 2018-06-15 | 温州大学新材料与产业技术研究院 | The preparation method and purposes of a kind of three-dimensional globular nitrogen-doped porous carbon material and nickel nickel composite material |
| CN108273536A (en) * | 2018-01-25 | 2018-07-13 | 太原理工大学 | A kind of preparation method of N doping three-dimensional porous nano ferrum-based catalyst |
| CN109678133A (en) * | 2019-01-14 | 2019-04-26 | 桂林电子科技大学 | A kind of C-base composte material and its preparation method and application of nickel oxide doping |
| CN111434607A (en) * | 2019-01-11 | 2020-07-21 | 国家纳米科学中心 | Metal phosphide and heteroatom-doped porous carbon composite material and preparation and application thereof |
| CN112151817A (en) * | 2020-10-26 | 2020-12-29 | 中北大学 | Copper-based anode catalyst for direct methanol fuel cell and preparation method thereof |
| CN112198201A (en) * | 2020-07-27 | 2021-01-08 | 重庆医科大学 | Indole electrochemical sensor constructed based on nitrogen-doped ordered mesoporous carbon modified electrode and application thereof |
| CN112736261A (en) * | 2021-01-07 | 2021-04-30 | 天津大学 | Porous carbon network supported platinum nanoparticle composite catalyst and preparation method thereof |
| CN113782743A (en) * | 2021-08-27 | 2021-12-10 | 合肥国轩高科动力能源有限公司 | Lithium ion battery positive electrode material and preparation method and application thereof |
| CN115382533A (en) * | 2022-04-11 | 2022-11-25 | 嘉兴学院 | Method for directly preparing and molding spherical metal oxide-based catalyst |
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| CN104617311A (en) * | 2014-11-20 | 2015-05-13 | 安徽大学 | Nitrogen and cobalt doped mesoporous carbon/graphene composite material and preparation method thereof |
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| CN109678133A (en) * | 2019-01-14 | 2019-04-26 | 桂林电子科技大学 | A kind of C-base composte material and its preparation method and application of nickel oxide doping |
| CN112198201A (en) * | 2020-07-27 | 2021-01-08 | 重庆医科大学 | Indole electrochemical sensor constructed based on nitrogen-doped ordered mesoporous carbon modified electrode and application thereof |
| CN112151817A (en) * | 2020-10-26 | 2020-12-29 | 中北大学 | Copper-based anode catalyst for direct methanol fuel cell and preparation method thereof |
| CN112736261A (en) * | 2021-01-07 | 2021-04-30 | 天津大学 | Porous carbon network supported platinum nanoparticle composite catalyst and preparation method thereof |
| CN113782743A (en) * | 2021-08-27 | 2021-12-10 | 合肥国轩高科动力能源有限公司 | Lithium ion battery positive electrode material and preparation method and application thereof |
| CN113782743B (en) * | 2021-08-27 | 2022-07-12 | 合肥国轩高科动力能源有限公司 | Lithium ion battery positive electrode material and preparation method and application thereof |
| CN115382533A (en) * | 2022-04-11 | 2022-11-25 | 嘉兴学院 | Method for directly preparing and molding spherical metal oxide-based catalyst |
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Application publication date: 20140827 Assignee: Chizhou Kecheng new material development Co., Ltd. Assignor: Anhui University Contract record no.: X2019340000004 Denomination of invention: Preparation method of fuel cell cathodic catalyst metal/metal oxide loaded nitrogen-doped porous carbon network-structure material Granted publication date: 20160210 License type: Exclusive License Record date: 20190926 |
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