CN108598507B - Preparation method of composite nano material - Google Patents
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- CN108598507B CN108598507B CN201810469690.3A CN201810469690A CN108598507B CN 108598507 B CN108598507 B CN 108598507B CN 201810469690 A CN201810469690 A CN 201810469690A CN 108598507 B CN108598507 B CN 108598507B
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/16—Biochemical fuel cells, i.e. cells in which microorganisms function as catalysts
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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
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention provides a preparation method of a composite nano material, which is synthesized by a two-step hydrothermal method for the first time, has the advantages of simple process, low cost, short period, environmental friendliness and the like, and can be suitable for industrial large-scale production; the composite nano material prepared by the method is fibrous, the diameter of the fiber is 5-20 nm, the length of the fiber is 500-1000 nm, and the specific surface area of the material is 900-1000 m2A pore volume of 0.3 to 0.4cm3The specific conductivity is 5-8S/cm; when the composite material is applied to an electrode material, compared with a microbial fuel cell assembled by taking conventional Pt/C as a cathode catalyst, the composite material has the advantages of higher output power, better running stability, easy preparation and low price, and lays a good foundation for the commercialization of the microbial fuel cell.
Description
The application is a divisional application, the application number of the original application is 201610612938.8, the application date is 2016, 7 and 29, and the invention is named as 'a composite nano material and a preparation method and application thereof'.
Technical Field
The invention belongs to the technical field of application of nano materials, and particularly relates to a preparation method of a composite nano material.
Background
The research on the nano material is a leading field in the scientific research nowadays and is a hot spot of research of many scientists all over the world. The curiosity and the aspects which are not known by people of the nanometer material draw extensive attention of people; the research and application of the preparation of the nano material are more hot and difficult points at present and are also key points for developing high technology.
Carbon nitride is a novel carbon material, and in recent years, nitrogen-containing carbon materials are widely considered as potential new materials due to their excellent electrocatalytic activity, photocatalytic activity, low cost, environmental friendliness and continuous and efficient characteristics (literature Science, 2009, 323, 760-material 764; Journal of the American chemical society,2011, 133, 20116-material 20119). Wherein the graphite phase carbon nitride (g-C)3N4) Is a typical nitrogen-rich non-metallic carbon material, has a graphite-like structure, and is the most stable allotrope in carbon and nitrogen compounds. g-C3N4Has been proved to exhibit excellent catalytic activity for oxygen reduction reaction and the like(document Energy)&Environmental
Science,2012,5,6717-6731) mainly because it has an abundant pyridine nitrogen active component. However, due to g-C3N4The use thereof as a cathode catalyst is inevitably restricted due to poor conductivity and low specific surface area.
Many studies have been made on carbon nitride composite materials, and there are documents (appl. mater. inter,
2014,6,1011; j. mater. chem.,2012,22,2721) reports that a graphite oxide-modified carbon nitride composite material is prepared by an ultrasonic chemical method, and after modification, the optical absorption and the transmission efficiency of photo-generated electrons of carbon nitride are enhanced. Therefore, compared with the activity before modification, the activity of the compound for photocatalytic degradation of rhodamine B and 2, 4-dichlorophenol is obviously improved. However, sonochemical methods take much time (more than 10 hours); in addition, the method is not suitable for large-scale application due to poor dispersibility of carbon nitride in water. However, there are few studies and reports on carbon nitride and carbon nanofiber composites, and there is much room for development and research on such composites.
Disclosure of Invention
The invention aims to provide a preparation method of a composite nano material, which has the advantages of simple process, high yield, good repeatability, overcoming the defects of complex preparation procedure, high cost and the like, and having more advantages in application.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
a preparation method of a composite nano material comprises the following steps:
(1) preparing a solution: weighing sucrose, concentrated nitric acid, water and a template agent polyethylene glycol PEG-2000 according to the weight ratio of 1: 0.05-0.15: 1-10: 0.5-1, mixing, and uniformly stirring for 3-6 hours to obtain a solution A; weighing a proper amount of carbon-nitrogen source according to the content of carbon nitride in the composite material, then adding a certain amount of solvent methanol, and stirring at room temperature for 1-2 hours to obtain a solution B;
(2) preparing a composite nano material: transferring the solution A into a reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction for 8-12 h at 120-180 ℃, cooling to room temperature after the reaction is finished, opening the reaction kettle, adding the solution B into the reaction kettle, then carrying out hydrothermal reaction for 6-10 h at 120-180 ℃, carrying out centrifugal separation and washing on a product after the reaction is finished, and roasting for 3-5 h at about 350-450 ℃ in a nitrogen atmosphere to obtain a composite nano material;
the composite nano material comprises 15-35 wt% of carbon nitride and 65-85 wt% of carbon nano fibers.
Preferably, the hydrothermal reaction is carried out in a homogeneous reactor, and the temperature rise rate of the roasting is 2 ℃/min.
Preferably, the carbon-nitrogen source is melamine or cyanamide.
In addition, the invention also claims a composite nano material prepared by the preparation method, which comprises 15-35 wt% of carbon nitride and 65-85 wt% of carbon nano fibers, wherein the composite nano material is fibrous, the diameter of the fiber is 5-20 nm, the length of the fiber is 500-1000 nm, and the specific surface area of the material is 900-1000 m2A pore volume of 0.3 to 0.4cm3The specific conductivity is 5-8S/cm.
Preferably, the composite nano material is fibrous, the diameter of the fiber is 10-15 nm, the length of the fiber is 600-800 nm, and the specific surface area of the material is 920-960 m2A pore volume of 0.32 to 0.36 cm/g3The specific conductivity is 6-7S/cm.
In addition, the invention also provides application of the composite nano material in a microbial fuel cell.
The method for preparing the catalytic electrode by using the composite nano material comprises the following steps: and mixing the composite nano material, the conductive material and the binder, adding a solvent into the mixture, uniformly mixing, performing ultrasonic dispersion, uniformly coating the ultrasonic mixture on a conductive substrate, and naturally drying to obtain the composite catalytic electrode.
The conductive material is carbon black, activated carbon or graphite; the binder is polytetrafluoroethylene or 5wt% Nafion solution; the solvent is isopropanol.
The invention also provides application of the composite nano material in hydrogen production by photolysis of water.
The invention has the technical effects that: (1) the invention realizes the controllable synthesis of the composite material, the carbon nitride and carbon fiber composite nano material is synthesized by adopting a two-step hydrothermal method for the first time, the formed composite nano material has a uniform fibrous shape, the diameter of the composite nano material is 5-20 nm, the length of the composite nano material is 500-1000 nm, and the specific surface area of the material is 900-1000 m2Has excellent surface properties per gram.
(2) The invention has the advantages of simple process, low cost, short period, environmental protection and the like, can be suitable for industrialized large-scale production, and when the composite material is applied to an electrode material, compared with a microbial fuel cell assembled by taking conventional Pt/C as a cathode catalyst, the composite material has higher output power, better operation stability, easy preparation and low price, and lays a good foundation for commercialization of the microbial fuel cell.
Drawings
FIG. 1 is an SEM image of a composite nanomaterial of example 1 of the present invention.
Detailed Description
The technical scheme of the invention is further explained by combining the embodiment as follows:
example 1
The composite nano material consists of 15wt% of carbon nitride and 85wt% of carbon nano fibers, wherein the composite nano material is fibrous, the diameter of the fibers is 10 nm, the length of the fibers is 600 nm, and the specific surface area of the material is 900 m2Per g, pore volume of 0.3cm3The specific conductivity is 6S/cm;
the preparation method of the composite nano material comprises the following steps:
(1) preparing a solution: weighing sucrose, concentrated nitric acid, water and a template agent polyethylene glycol PEG-2000 according to the weight ratio of 1: 0.01: 6: 0.7, mixing, and uniformly stirring for 5 hours to obtain a solution A; weighing a proper amount of carbon-nitrogen source according to the content of carbon nitride in the composite material, then adding a certain amount of solvent methanol, and stirring for 2 hours at room temperature to obtain a solution B;
(2) preparing a composite nano material: transferring the solution A into a reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction at 160 ℃ for 9h, cooling to room temperature after the reaction is finished, opening the reaction kettle, adding the solution B into the reaction kettle, carrying out hydrothermal reaction at 150 ℃ for 8h, carrying out centrifugal separation and washing on a product after the reaction is finished, and roasting at 400 ℃ for 4h in a nitrogen atmosphere to obtain the composite nano material.
Example 2
The composite nano material consists of 25wt% of carbon nitride and 75wt% of carbon nano fibers, wherein the composite nano material is fibrous, the diameter of the fibers is 10 nm, the length of the fibers is 800 nm, and the specific surface area of the material is 950 m2Per g, pore volume of 0.35cm3The specific conductivity is 6S/cm;
the preparation method of the composite nano material comprises the following steps:
(1) preparing a solution: weighing sucrose, concentrated nitric acid, water and a template agent polyethylene glycol PEG-2000 according to the weight ratio of 1: 0.1: 6: 0.8, mixing, and uniformly stirring for 5 hours to obtain a solution A; weighing a proper amount of carbon-nitrogen source according to the content of carbon nitride in the composite material, then adding a certain amount of solvent methanol, and stirring for 2 hours at room temperature to obtain a solution B;
(2) preparing a composite nano material: transferring the solution A into a reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction for 10h at 150 ℃, cooling to room temperature after the reaction is finished, opening the reaction kettle, adding the solution B into the reaction kettle, carrying out hydrothermal reaction for 8h at 160 ℃, carrying out centrifugal separation and washing on a product after the reaction is finished, and roasting for 5h at 380 ℃ in a nitrogen atmosphere to obtain the composite nano material.
Example 3
The composite nano material consists of 30wt% of carbon nitride and 70wt% of carbon nano fibers, wherein the composite nano material is fibrous, the diameter of the fibers is 15 nm, the length of the fibers is 700 nm, and the specific surface area of the material is 900 m2Per g, poreVolume of 0.4cm3The specific conductivity is 8S/cm;
the preparation method of the composite nano material comprises the following steps:
(1) preparing a solution: weighing sucrose, concentrated nitric acid, water and a template agent polyethylene glycol PEG-2000 according to the weight ratio of 1: 0.15: 5: 0.8, mixing, and uniformly stirring for 6 hours to obtain a solution A; weighing a proper amount of carbon-nitrogen source according to the content of carbon nitride in the composite material, then adding a certain amount of solvent methanol, and stirring for 2 hours at room temperature to obtain a solution B;
(2) preparing a composite nano material: transferring the solution A into a reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction for 12 hours at 120 ℃, cooling to room temperature after the reaction is finished, opening the reaction kettle, adding the solution B into the reaction kettle, carrying out hydrothermal reaction for 6-10 hours at 180 ℃, carrying out centrifugal separation and washing on a product after the reaction is finished, and roasting for 3 hours at 450 ℃ in a nitrogen atmosphere to obtain the composite nano material.
Example 4
The composite nano material consists of 35wt% of carbon nitride and 65wt% of carbon nano fibers, wherein the composite nano material is fibrous, the diameter of the fibers is 16 nm, the length of the fibers is 800 nm, and the specific surface area of the material is 1000 m2Per g, pore volume of 0.4cm3The specific conductivity is 7S/cm;
the preparation method of the composite nano material comprises the following steps:
(1) preparing a solution: weighing sucrose, concentrated nitric acid, water and a template agent polyethylene glycol PEG-2000 according to the weight ratio of 1: 0.12: 8: 1, mixing, and uniformly stirring for 5 hours to obtain a solution A; weighing a proper amount of carbon-nitrogen source according to the content of carbon nitride in the composite material, then adding a certain amount of solvent methanol, and stirring at room temperature for 1.5h to obtain a solution B;
(2) preparing a composite nano material: transferring the solution A into a reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction at 140 ℃ for 9h, cooling to room temperature after the reaction is finished, opening the reaction kettle, adding the solution B into the reaction kettle, carrying out hydrothermal reaction at 130 ℃ for 9h, carrying out centrifugal separation and washing on a product after the reaction is finished, and roasting at 380 ℃ for 5h in a nitrogen atmosphere to obtain the composite nano material.
Comparative example 1
A composite nano material is prepared by the following steps:
(1) preparing a solution: weighing sucrose, concentrated nitric acid, water and a template agent polyethylene glycol PEG-2000 according to the weight ratio of 1: 0.01: 6: 0.7, mixing, and uniformly stirring for 5 hours to obtain a solution A; weighing a proper amount of carbon-nitrogen source according to the content of carbon nitride in the composite material, then adding a certain amount of solvent methanol, and stirring for 2 hours at room temperature to obtain a solution B;
(2) preparing a composite nano material: and mixing the solution A and the solution B, transferring the mixture into a reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction for 9 hours at 160 ℃, after the reaction is finished, carrying out centrifugal separation and washing on a product, and roasting for 4 hours at 400 ℃ in a nitrogen atmosphere to obtain the composite nano material.
Examples 1-4 of the present invention and comparative examples were applied to the performance testing of microbial fuel cells:
(I) the method comprises the following steps Preparing an electrode: fully mixing the composite materials, the conductive material carbon black and the binder PTFE of the examples and the comparative examples according to the mass ratio of 10:31:63, and adding an isopropanol reagent for ultrasonic dispersion for 30 minutes; and (3) uniformly coating the ultrasonic mixture on graphite cloth, and naturally drying for 24 hours to obtain the composite material catalytic electrode. The Pt/C catalytic electrode can be prepared by mixing a conventional Pt/C catalyst, a conductive material and a binder in the same manner.
(II) Single-chamber microbial Fuel cell Performance testing: 15mL of the electrogenic microbial liquid was charged into a single-chamber microbial fuel cell from the inlet, and the composite catalytic electrode and the Pt/C catalytic electrode of the examples and comparative examples prepared above were used as the cathode of the fuel cell, respectively. And connecting the fuel cell into a 1000-ohm external resistance circuit, starting to record the electricity generation process, and testing the performance of the fuel cell after the highest voltage output is stable.
The fuel cell used in this experiment was an air cathode single cell Microbial Fuel Cell (MFCs) of the prior art document CN 105336964 a. The performance of the microbial fuel cells for the different catalytic electrodes is shown in table 1.
As can be seen from table 1, each composite material of the examples of the present invention, which is used as an oxygen reduction catalyst in a single-chamber microbial fuel cell, has catalytic activity and stability comparable to those of comparative example 1 and the conventional Pt/C catalyst, indicating that it possesses potential advantages to replace the Pt/C catalyst.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. The preparation method of the composite nano material is characterized by comprising the following steps of:
(1) preparing a solution: weighing sucrose, concentrated nitric acid, water and a template agent polyethylene glycol PEG-2000 according to the weight ratio of 1: 0.05-0.15: 1-10: 0.5-1, mixing, and uniformly stirring for 3-6 hours to obtain a solution A; weighing a proper amount of carbon-nitrogen source according to the content of carbon nitride in the composite material, then adding a certain amount of solvent methanol, and stirring at room temperature for 1-2 hours to obtain a solution B;
(2) preparing a composite nano material: transferring the solution A into a reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction for 8-12 h at 120-180 ℃, cooling to room temperature after the reaction is finished, opening the reaction kettle, adding the solution B into the reaction kettle, then carrying out hydrothermal reaction for 6-10 h at 120-180 ℃, carrying out centrifugal separation and washing on a product after the reaction is finished, and roasting for 3-5 h at 350-450 ℃ in a nitrogen atmosphere to obtain a composite nano material;
the composite nano material comprises 15-35 wt% of carbon nitride and 65-85 wt% of carbon nano fibers.
2. The method for preparing composite nanomaterial according to claim 1, wherein the hydrothermal reaction is carried out in a homogeneous reactor and the baking temperature rise rate is 2 ℃/min.
3. The method for preparing composite nano-materials according to claim 1, wherein the carbon-nitrogen source is melamine or cyanamide.
4. The composite nanomaterial produced by the production method according to any one of claims 1 to 3.
5. The composite nanomaterial according to claim 4, wherein the composite nanomaterial is in the form of a fiber having a diameter of 16 nm, a length of 800 nm, and a material specific surface area of 1000 m2Per g, pore volume of 0.4cm3The specific conductivity is 7S/cm.
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| CN106410139B (en) * | 2016-10-15 | 2018-09-11 | 河南海宏科技有限公司 | A kind of high stability lithium ion cell electrode silicon/carbonitride/carbon composite nano-material |
| CN106391090A (en) * | 2016-11-04 | 2017-02-15 | 南京工业大学 | Carbon-supported carbon nitride photocatalytic material and preparation method thereof |
| CN106622322B (en) * | 2016-11-08 | 2019-01-04 | 河南理工大学 | It is a kind of using bimetal nano particles as two-dimensional nano piece composite photo-catalyst of hetero-junctions and preparation method thereof |
| CN106784873B (en) * | 2016-12-12 | 2018-05-22 | 佛山市聚成生化技术研发有限公司 | A kind of carbonitride/carbon nano-composite material and its preparation method and application |
| CN109095545B (en) * | 2018-09-29 | 2021-08-10 | 吴洋洋 | Device and method for treating high-concentration organic wastewater through cooperation of electrochemistry and photocatalysis |
| CN109647475A (en) * | 2018-11-14 | 2019-04-19 | 中国地质大学（北京） | A kind of g-C3N4/ C composite photocatalyst fibrous material and preparation method thereof |
| CN111244490B (en) * | 2020-01-09 | 2021-03-16 | 中国人民解放军军事科学院军事医学研究院 | Bamboo-shaped hollow N-doped carbon nanotube and C3N4Nanosheet cross-linked composite material and preparation method and application thereof |
| CN112547109B (en) * | 2020-12-24 | 2023-07-18 | 江苏大学 | Preparation method of carbon-oxygen co-doped broad-spectrum response three-dimensional carbon nitride photocatalyst by introducing polymer molecules |
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| CN103265546A (en) * | 2013-05-08 | 2013-08-28 | 江苏大学 | Method for preparing carbon nitride nanofibers through template-free process |
| CN104485464A (en) * | 2014-12-11 | 2015-04-01 | 哈尔滨工业大学 | Prussian blue-based high-stability high-activity Pt-based catalyst for fuel cell and preparation method thereof |
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| CN108598507A (en) | 2018-09-28 |
| CN108598506B (en) | 2020-07-21 |
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