CN108598507A - A kind of preparation method of composite nano materials - Google Patents
A kind of preparation method of composite nano materials Download PDFInfo
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- CN108598507A CN108598507A CN201810469690.3A CN201810469690A CN108598507A CN 108598507 A CN108598507 A CN 108598507A CN 201810469690 A CN201810469690 A CN 201810469690A CN 108598507 A CN108598507 A CN 108598507A
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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Abstract
The present invention provides a kind of preparation methods of composite nano materials, are synthesized for the first time using two one-step hydrothermals, this is simple for process, of low cost, the period is short, advantages of environment protection, can be adapted for industrialization large-scale production；The composite nano materials being prepared by the method are in threadiness, and a diameter of 5~20 nm of fiber, length is 500~1000 nm, and material specific surface area is 900~1000 m20.3~0.4cm of/g, Kong Rongwei3/ g, conductivity are 5~8S/cm；By the composite material be applied to electrode material in use, with conventional Pt/C be cathod catalyst assembling microbiological fuel cell compared with, output power higher, operation stability is more preferably, and it is easily prepared, it is cheap, establish good basis for the commercialization of microbiological fuel cell.
Description
The application is divisional application, original application application No. is 201610612938.8, the applying date is July 29 in 2016
Day, it is entitled " a kind of composite nano materials and its preparation method and application ".
Technical field
The invention belongs to technical field of nano material application, and in particular to a kind of preparation method of composite nano materials.
Background technology
Research to nano material is a Disciplinary Frontiers and many scientific workers in the whole world in current scientific research
The hot spot of research.The magical place of nano material and the aspect that do not known by people also are even more to cause the extensive concern of people；
The research that prepared to nano material and application are even more current hot and difficult issue, and the high-tech emphasis of development.
Carbonitride is a kind of novel carbon material, in recent years, nitrogenous carbon material, due to its excellent electro catalytic activity, light
Catalytic activity, cheap cost is environmentally friendly and continue and efficient feature, is generally considered a kind of potentiality that have much
New material (document Science, 2009,323,760-764; Journal of the American Chemical
Society, 2011,133,20116-20119).Wherein, graphite phase carbon nitride (g-C3N4) it is a kind of typical rich in nitrogen
Non-metal carbon material, have graphite-like structure, be most stable of allotrope in carboritride.g-C3N4Oneself is through being demonstrate,proved
It is bright that excellent catalytic activity (document Energy ＆ Environmental can be shown to oxygen reduction reaction etc.
Science, 2012,5,6717-6731), reason essentially consists in it with abundant pyridine nitrogen active component.However, by
In g-C3N4It is influenced by poor conductance ability and low specific surface area, the application as cathod catalyst can be inevitable
It is restricted.
The research of composite material in relation to carbonitride is also more, have document (Appl.Mater.Inter.,
2014,6,1011；J.Mater.Chem., 2012,22,2721) report and be prepared for aoxidizing by the method for sonochemistry
The nitridation carbon composite of graphite modification, after modification, the optical absorption of carbonitride and the efficiency of transmission of light induced electron are added
By force.Therefore, the activity of photocatalysis rhodamine B and 2, the degradation of 4- chlorophenesic acids significantly improves compared with before modification.However, ultrasonic
Chemical method is more time-consuming (10 hours or more)；In addition, since the dispersibility of carbonitride in water is poor, this method is caused to be not suitable for
In large-scale application.However, the research and report about carbonitride and carbon nano-fiber composite material are also less, for such multiple
The R and D of condensation material also have much room.
Invention content
The object of the present invention is to provide a kind of preparation methods of composite nano materials, and this method is simple for process, and yield is larger,
Repeatability is good, overcomes the deficiencies of preparation procedure is complicated, of high cost, upper advantageously in application.
To solve the above problems, the technical solution adopted by the present invention is：
A kind of preparation method of composite nano materials, includes the following steps：
（1）The preparation of solution：Sucrose, concentrated nitric acid, water and template are weighed according to weight ratio 1: 0.05~0.15: 1~10: 0.5~1
Agent polyethylene glycol PEG-2000, uniform stirring 3~6 hours, obtain solution A after mixing；Contain according to carbonitride in composite material
Amount weighs proper amount of carbon nitrogen source, and a certain amount of solvent methanol is then added, 1~2h is stirred at room temperature, obtains solution B；
（2）The preparation of composite nano materials：First solution A is transferred in the reaction kettle with polytetrafluoroethyllining lining, 120~
8~12h of hydro-thermal reaction, is cooled to room temperature after reaction at 180 DEG C, then opens reaction kettle, then solution B is added to reaction
In kettle, continue 6~10h of hydro-thermal reaction at 120~180 DEG C later, after reaction, product be centrifuged, is washed,
And 3~5h is roasted up to composite nano materials in nitrogen atmosphere at about 350~450 DEG C.
Preferably, the hydro-thermal reaction is carried out in homogeneous reactor, and the heating rate of the roasting is 2 DEG C/min.
Preferably, the carbon nitrogen source is melamine or cyanamide.
In addition, the present invention is also claimed by the preparation-obtained composite nano materials of the preparation method, it is compound by accounting for
The carbonitride of 15~35wt% of material percentage composition and the carbon nano-fiber composition of 65~85wt%, the composite nano materials are in fibre
Shape, a diameter of 5~20 nm of fiber are tieed up, length is 500~1000 nm, and material specific surface area is 900~1000 m2/ g, hole
It is 0.3~0.4cm to hold3/ g, conductivity are 5~8S/cm.
Wherein, as the preferred composite nano materials in threadiness, a diameter of 10~15 nm of fiber, length 600
~800 nm, material specific surface area are 920~960 m20.32~0.36cm of/g, Kong Rongwei3/ g, conductivity are 6~7S/cm.
In addition, the application the present invention also provides the composite nano materials in microbiological fuel cell.
The method that the composite nano materials prepare catalysis electrode, includes the following steps：By composite nano materials, conduction material
Material and binder mixing, are uniformly mixed, ultrasonic disperse, then equably by ultrasonic mixing object after solvent is added into mixture
Coated in conductive substrates, natural air drying is to get to composite material catalysis electrode.
The conductive material is carbon black, activated carbon or graphite；The binder is polytetrafluoroethylene (PTFE) or 5wt%Nafion
Solution；The solvent is isopropanol.
The present invention also provides application of the composite nano materials in photolysis water hydrogen.
The present invention technique effect be：（1）The present invention realizes the controlledly synthesis of composite material, uses two step hydro-thermals for the first time
Method has synthesized carbonitride and the compound nano material of carbon fiber, and uniform fiber is presented in the pattern for being formed by composite nano materials
Shape, a diameter of 5~20 nm, length are 500~1000 nm, and material specific surface area is even more to reach 900~1000 m2/ g, tool
There is very excellent surface nature.
（2）The present invention have it is simple for process, of low cost, the period is short, advantages of environment protection, can be adapted for industrializing
The composite material is applied to electrode material in use, being micro- life that cathod catalyst assembles with conventional Pt/C by large-scale production
Object fuel cell is compared, output power higher, and operation stability is more preferably, and easily prepared, cheap, is Microbial fuel
Good basis has been established in the commercialization of battery.
Description of the drawings
Fig. 1 is that the SEM of 1 composite nano materials of the embodiment of the present invention schemes.
Specific implementation mode
Technical scheme of the present invention is further elaborated with reference to embodiment：
Embodiment 1
A kind of composite nano materials, by accounting for the carbonitride of composite material percentage composition 15wt% and the carbon nano-fiber group of 85wt%
At the composite nano materials are 600 nm, material specific surface area 900 in threadiness, a diameter of 10 nm of fiber, length
m2/ g, Kong Rongwei 0.3cm3/ g, conductivity 6S/cm；
Wherein, the preparation method of the composite nano materials includes the following steps：
（1）The preparation of solution：Sucrose, concentrated nitric acid, water and template polyethylene glycol are weighed according to weight ratio 1: 0.01: 6: 0.7
PEG-2000, uniform stirring 5 hours, obtain solution A after mixing；It is weighed according to the content of carbonitride in composite material proper amount of
Then carbon nitrogen source is added a certain amount of solvent methanol, 2h is stirred at room temperature, obtains solution B；
（2）The preparation of composite nano materials：First solution A is transferred in the reaction kettle with polytetrafluoroethyllining lining, at 160 DEG C
Lower hydro-thermal reaction 9h, is cooled to room temperature after reaction, then opens reaction kettle, then solution B is added in reaction kettle, later
Continue the hydro-thermal reaction 8h at 150 DEG C product is centrifuged, washs after reaction, and the nitrogen gas at 400 DEG C
4h is roasted in atmosphere up to composite nano materials.
Embodiment 2
A kind of composite nano materials, by accounting for the carbonitride of composite material percentage composition 25wt% and the carbon nano-fiber group of 75wt%
At the composite nano materials are 800 nm, material specific surface area 950 in threadiness, a diameter of 10 nm of fiber, length
m2/ g, Kong Rongwei 0.35cm3/ g, conductivity 6S/cm；
Wherein, the preparation method of the composite nano materials includes the following steps：
（1）The preparation of solution：Sucrose, concentrated nitric acid, water and template polyethylene glycol PEG- are weighed according to weight ratio 1: 0.1: 6: 0.8
2000, uniform stirring 5 hours, obtain solution A after mixing；Proper amount of carbon nitrogen is weighed according to the content of carbonitride in composite material
Then source is added a certain amount of solvent methanol, 2h is stirred at room temperature, obtains solution B；
（2）The preparation of composite nano materials：First solution A is transferred in the reaction kettle with polytetrafluoroethyllining lining, at 150 DEG C
Lower hydro-thermal reaction 10h, is cooled to room temperature after reaction, then opens reaction kettle, then solution B is added in reaction kettle, it
After continue the hydro-thermal reaction 8h at 160 DEG C, after reaction, product is centrifuged, is washed, and the nitrogen at 380 DEG C
5h is roasted in atmosphere up to composite nano materials.
Embodiment 3
A kind of composite nano materials, by accounting for the carbonitride of composite material percentage composition 30wt% and the carbon nano-fiber group of 70wt%
At the composite nano materials are 700 nm, material specific surface area 900 in threadiness, a diameter of 15 nm of fiber, length
m2/ g, Kong Rongwei 0.4cm3/ g, conductivity 8S/cm；
Wherein, the preparation method of the composite nano materials includes the following steps：
（1）The preparation of solution：Sucrose, concentrated nitric acid, water and template polyethylene glycol are weighed according to weight ratio 1: 0.15: 5: 0.8
PEG-2000, uniform stirring 6 hours, obtain solution A after mixing；It is weighed according to the content of carbonitride in composite material proper amount of
Then carbon nitrogen source is added a certain amount of solvent methanol, 2h is stirred at room temperature, obtains solution B；
（2）The preparation of composite nano materials：First solution A is transferred in the reaction kettle with polytetrafluoroethyllining lining, at 120 DEG C
Lower hydro-thermal reaction 12h, is cooled to room temperature after reaction, then opens reaction kettle, then solution B is added in reaction kettle, it
After continue 6~10h of hydro-thermal reaction at 180 DEG C, after reaction, product is centrifuged, is washed, and at 450 DEG C
3h is roasted in nitrogen atmosphere up to composite nano materials.
Embodiment 4
A kind of composite nano materials, by accounting for the carbonitride of composite material percentage composition 35wt% and the carbon nano-fiber group of 65wt%
At the composite nano materials are 800 nm, material specific surface area 1000 in threadiness, a diameter of 16 nm of fiber, length
m2/ g, Kong Rongwei 0.4cm3/ g, conductivity 7S/cm；
Wherein, the preparation method of the composite nano materials includes the following steps：
（1）The preparation of solution：Sucrose, concentrated nitric acid, water and template polyethylene glycol PEG- are weighed according to weight ratio 1: 0.12: 8: 1
2000, uniform stirring 5 hours, obtain solution A after mixing；Proper amount of carbon nitrogen is weighed according to the content of carbonitride in composite material
Then source is added a certain amount of solvent methanol, 1.5h is stirred at room temperature, obtains solution B；
（2）The preparation of composite nano materials：First solution A is transferred in the reaction kettle with polytetrafluoroethyllining lining, at 140 DEG C
Lower hydro-thermal reaction 9h, is cooled to room temperature after reaction, then opens reaction kettle, then solution B is added in reaction kettle, later
Continue the hydro-thermal reaction 9h at 130 DEG C product is centrifuged, washs after reaction, and the nitrogen gas at 380 DEG C
5h is roasted in atmosphere up to composite nano materials.
Comparative example 1
A kind of composite nano materials, preparation method include the following steps：
（1）The preparation of solution：Sucrose, concentrated nitric acid, water and template polyethylene glycol are weighed according to weight ratio 1: 0.01: 6: 0.7
PEG-2000, uniform stirring 5 hours, obtain solution A after mixing；It is weighed according to the content of carbonitride in composite material proper amount of
Then carbon nitrogen source is added a certain amount of solvent methanol, 2h is stirred at room temperature, obtains solution B；
（2）The preparation of composite nano materials：It is transferred to the reaction with polytetrafluoroethyllining lining after solution A and solution B are mixed
In kettle, product is centrifuged, washs after reaction by the hydro-thermal reaction 9h at 160 DEG C, and the nitrogen gas at 400 DEG C
4h is roasted in atmosphere up to composite nano materials.
1-4 of the embodiment of the present invention and comparative example are applied to the test of microbiological fuel cell performance：
（I）：It is prepared by electrode：By the composite material of each embodiment and comparative example, conductive material carbon black and binder PTFE according to matter
Measure ratio 10:31:63 are sufficiently mixed, and isopropanol reagent ultrasonic disperse are added 30 minutes；Ultrasonic mixing object is equably applied to
In Graphite cloth, composite material catalysis electrode is made in natural air drying 24 hours.After the same method by conventional Pt/C catalyst,
Pt/C catalysis electrodes can be made in conductive material and binder mixing.
（II）Single-chamber microbial fuel cell performance test：The electricity-producing microorganism bacterium solution of 15mL is micro- from import loading single chamber
In biological fuel cell, made respectively with the embodiment of above-mentioned preparation and comparative example composite material catalysis electrode and Pt/C catalysis electrodes
For the cathode of fuel cell.Fuel cell is accessed to 1000 ohm of outer resistance circuit, start recording electricity generation process waits for ceiling voltage
Output carries out fuel battery performance test after stablizing.
Wherein, the structure of fuel cell used by this experiment uses the air of 105336964 A of existing technical literature CN
Cathode single-chamber microbial fuel cell (MFCs).The performance of different catalysis electrode microbiological fuel cells is as shown in table 1.
| Cathod catalyst | Ceiling voltage (mV) | Peak power output (mW/m2 ) | The down ratio of peak power output after 30 periods of stable operation（%） |
| Embodiment 1 | 562 | 1601.3 | 2.0 |
| Embodiment 2 | 553 | 1618.2 | 1.8 |
| Embodiment 3 | 551 | 1630.5 | 2.2 |
| Embodiment 4 | 541 | 1615.7 | 1.9 |
| Comparative example 1 | 565 | 1523.2 | 4.8 |
| Pt/C | 591 | 1638.5 | 13.9 |
As can be seen from Table 1, each composite material of the embodiment of the present invention is fired as oxygen reduction catalyst for single-chamber microbial
Expect battery, has comparable in the catalytic activity and stability of comparative example 1 and routine Pt/C catalyst, illustrate that it possesses replacement
The potential advantages of Pt/C catalyst.
Finally it should be noted that：The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, although
Present invention has been described in detail with reference to the aforementioned embodiments, for those skilled in the art, still can be right
Technical solution recorded in foregoing embodiments is modified or equivalent replacement of some of the technical features.It is all
Within the spirit and principles in the present invention, any modification, equivalent replacement, improvement and so on should be included in the protection of the present invention
Within the scope of.
Claims (5)
1. a kind of preparation method of composite nano materials, which is characterized in that include the following steps：
（1）The preparation of solution：Sucrose, concentrated nitric acid, water and template are weighed according to weight ratio 1: 0.05~0.15: 1~10: 0.5~1
Agent polyethylene glycol PEG-2000, uniform stirring 3~6 hours, obtain solution A after mixing；Contain according to carbonitride in composite material
Amount weighs proper amount of carbon nitrogen source, and a certain amount of solvent methanol is then added, 1~2h is stirred at room temperature, obtains solution B；
（2）The preparation of composite nano materials：First solution A is transferred in the reaction kettle with polytetrafluoroethyllining lining, 120~
8~12h of hydro-thermal reaction, is cooled to room temperature after reaction at 180 DEG C, then opens reaction kettle, then solution B is added to reaction
In kettle, continue 6~10h of hydro-thermal reaction at 120~180 DEG C later, after reaction, product be centrifuged, is washed,
And 3~5h is roasted up to composite nano materials in nitrogen atmosphere at about 350~450 DEG C.
2. the preparation method of composite nano materials according to claim 1, which is characterized in that the hydro-thermal reaction is homogeneous
It is carried out in reactor, the heating rate of the roasting is 2 DEG C/min.
3. the preparation method of composite nano materials according to claim 1, which is characterized in that the carbon nitrogen source is melamine
Amine or cyanamide.
4. according to the preparation-obtained composite nano materials of any one of the claim 1-3 preparation methods.
5. composite nano materials according to claim 4, which is characterized in that the composite nano materials are fine in threadiness
A diameter of 16 nm of dimension, length are 800 nm, and material specific surface area is 1000 m2/ g, Kong Rongwei 0.4cm3/ g, conductivity are
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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| CN108598506B (en) | 2020-07-21 |
| CN106025303B (en) | 2018-10-30 |
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