CN110104622A - A kind of preparation method of graphite phase carbon nitride nanotube - Google Patents
A kind of preparation method of graphite phase carbon nitride nanotube Download PDFInfo
- Publication number
- CN110104622A CN110104622A CN201910425629.3A CN201910425629A CN110104622A CN 110104622 A CN110104622 A CN 110104622A CN 201910425629 A CN201910425629 A CN 201910425629A CN 110104622 A CN110104622 A CN 110104622A
- Authority
- CN
- China
- Prior art keywords
- preparation
- graphite phase
- carbon nitride
- phase carbon
- nitride nanotube
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0605—Binary compounds of nitrogen with carbon
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/13—Nanotubes
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a kind of preparation methods of graphite phase carbon nitride nanotube, which comprises (1) melamine powder is added in crucible and is put into heating calcining 2h in Muffle furnace, heating rate is 10 DEG C/min；(2) ultrasonic cut in ethyl alcohol is put into after the product that step (1) obtains being pulverized, the dosage of ethyl alcohol is 50mL；(3) it will be transferred in Muffle furnace and calcine after product filtering drying that step (2) obtains, heating rate is 10 DEG C/min；(4) product that step (3) obtains quickly is transferred in ice water and is stirred, calcine 12h at 80 DEG C after filtering, obtain azotized carbon nano pipe.The present invention has the characteristics that low in cost, simple and easy, azotized carbon nano pipe regular appearance made from this method and without breakage.
Description
Technical field
The present invention relates to inorganic photocatalysis nano material field more particularly to a kind of preparations of graphite phase carbon nitride nanotube
Method.
Background technique
As energy crisis and environmental pollution are got worse, there is an urgent need to develop renewable energy technologies by people.Artificial light
Catalysis technique is considered as a kind of high efficiency method not polluted.Nowadays, there are hundreds of semiconductor materials available.However,
In view of high cost, higher forbidden bandwidth and lower separation of charge rate, practical application are greatly hindered[1].Most
Closely, researcher develops a kind of photochemical catalyst graphite phase carbon nitride of novel visible driving, it has excellent photochemistry
Stability and suitable position of energy band[2].But efficiency has also suffered from the influence of low specific surface area and high charge recombination rate.
This problem can be solved by preparing the carbon nitride material of different-shape, thus the structural property of reinforcing material
And photocatalysis performance.At present in document it has been reported that a variety of nitridation carbon structures, such as: cellular, nanobelt, nanometer sheet are received
Mitron and nanosphere[3].Wherein, azotized carbon nano pipe has unique one-dimensional geometry, outstanding electronics and optical property,
High-specific surface area and chemical active sites, have received widespread attention.
Currently, azotized carbon nano pipe can be prepared by direct synthesis technique and chemical template method.Although scientists from all over the world develop
The method that some experiments prepare azotized carbon nano pipe is gone out, for example, Huaming Li seminar, which develops two-step method preparation, to be had
The azotized carbon nano pipe of defect, but scanning electron microscope image shows that many pipes are curved[4].Jinlong Gong class
Topic group reports the azotized carbon nano pipe of controllable preparation, however, the disadvantage is that having the nanotube of irregular alignment on surface[5].It adopts
It prepares azotized carbon nano pipe from ethylenediamine and carbon tetrachloride presoma with template also to have been reported that, researcher even attempts
Orderly nanotube growth is handled under different heating atmospheres.But the preparation section is complicated, equipment is expensive, and the production cycle is unrestrained
It is long[6].Therefore it is badly in need of a kind of production regular appearance of environmental protection and the short-cut method of unabroken azotized carbon nano pipe at present, thus
It lays a good foundation for the practical application of the material.
Bibliography:
[1]S.Y.Tee,K.Y.Win,W.S.Teo,L.D.Koh,S.Liu,C.P.Teng,M.Y.Han,Adv.Sci.4
(5),1600337(2017).
[2]S.Cao,J.Low,J.Yu,and M.Jaroniec,Adv.Mater.27,2150-2176(2015).
[3]S.Cao,J.Yu,J.Phys.Chem.Lett.5(12),2101-2107(2014).
[4]Z.Mo,H.Xu,Z.Chen,X.She,Y.Song,J.Wu,P.Yan,L.Xu,Y.Lei,S.Yuan,H.Li,
Appl.Catal.B-Environ 225,154-161(2018).
[5]S.Wang,C.Li,T.Wang,P.Zhang,A.Li,J.Gong,J.Mater.Chem.A 2(9),2885-
2890(2014).
[6]X.Lu,H.Wang,S.Zhang,D.Cui,Q.Wang,Solid State Sci.11(2),428-432
(2009).
Summary of the invention
The present invention provides a kind of preparation method of graphite phase carbon nitride nanotube, the present invention has low in cost, simple
Easy feature, azotized carbon nano pipe regular appearance made from this method and without breakage are described below:
A kind of preparation method of graphite phase carbon nitride nanotube, the described method comprises the following steps:
(1) melamine powder is added in crucible to and is put into Muffle furnace heating calcining 2h, heating rate is 10 DEG C/
min；
(2) ultrasonic cut in ethyl alcohol is put into after the product that step (1) obtains being pulverized, the dosage of ethyl alcohol is 50mL；
(3) it being transferred in Muffle furnace and calcine after product filtering drying that step (2) obtains, heating rate is 10 DEG C/
min；
(4) product that step (3) obtains quickly is transferred in ice water and is stirred, calcined 12h at 80 DEG C after filtering, obtain
Azotized carbon nano pipe.
When specific implementation, the temperature kept after heating in step (1) is 550 DEG C.
Preferably, the time of ultrasonic cut is 1h in step (2).The temperature kept after heating in step (3) is 350 DEG C.
Further, the time for keeping temperature in step (3) after heating is 10min.
Further, mixing time is 30min in ice water in step (4)；Calcination atmosphere is vacuum.
The beneficial effect of the technical scheme provided by the present invention is that:
1, the present invention solve the problems, such as it is existing prepare nanotube method, such as: complex process, pattern are not advised
It is whole, high production cost and the problems such as being difficult to the template completely removed；
2, the present invention does not use additional template during preparing azotized carbon nano pipe, is conducive to keep nitrogen
The original physicochemical properties of carbon nano tube；Use melamine for predecessor, material source is extensive and cheap；
3, preparation method of the present invention is simple, with short production cycle；The nanotube regular appearance prepared, does not break
Damage；Productivity is up to 65% or more.
In short, the method for environmental protection disclosed by the invention can be mass the azotized carbon nano pipe of regular appearance, it is that one kind has
Practical straightforward procedure is imitated, is suitble to laboratory preparation and industrialized production, there is huge development space and application prospect.
Detailed description of the invention
Fig. 1 is a kind of flow chart of the preparation method of graphite phase carbon nitride nanotube；
Fig. 2 is transmission electron microscope (TEM) photo figure of prepared azotized carbon nano pipe.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, embodiment of the present invention is made below further
Ground detailed description.
Embodiment 1
A kind of preparation method of graphite phase carbon nitride nanotube, referring to Fig. 1, method includes the following steps:
(1) melamine powder is added in crucible to and is put into Muffle furnace heating calcining 2h, heating rate is 10 DEG C/
Min, the temperature kept after heating are 550 DEG C；
(2) ultrasonic cut in ethyl alcohol is put into after product obtained in step (1) being pulverized, the dosage of ethyl alcohol is
50mL, the time of ultrasonic cut are 1h；
(3) it will be transferred in Muffle furnace and calcined after product filtering drying obtained in step (2), heating rate 10
DEG C/min, the temperature kept after heating is 350 DEG C, and the time of kept temperature is 10min after heating；
(4) at high temperature, product obtained in step (3) is quickly transferred in ice water to and is stirred 30min, is existed after filtering
Calcining 12h is under 80 DEG C and vacuum condition to get arriving azotized carbon nano pipe.
Transmission electron microscope (TEM) result of the azotized carbon nano pipe as prepared by embodiment 1 is as shown in Fig. 2, can from Fig. 2
Out, nanotube is regular and without breakage.
Embodiment 2
It is 600 DEG C by the temperature kept after heating in (1) the step of embodiment 1, other conditions are constant.
Embodiment 3
It is 2h by the time of ultrasonic cut in (2) the step of embodiment 1, other conditions are constant.
Embodiment 4
It is 400 DEG C by the temperature kept after heating in (3) the step of embodiment 1, other conditions are constant.
Embodiment 5
Time by kept temperature after heating in (3) the step of embodiment 1 is 20min, and other conditions are constant.
Embodiment 6
It is 1h by mixing time in ice water in (4) the step of embodiment 1, other conditions are constant.
Embodiment 7
It is under air condition by (4) calcination condition the step of embodiment 1, other conditions are constant.
It will be appreciated by those skilled in the art that attached drawing is the schematic diagram of a preferred embodiment, the embodiments of the present invention
Serial number is for illustration only, does not represent the advantages or disadvantages of the embodiments.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (7)
1. a kind of preparation method of graphite phase carbon nitride nanotube, which is characterized in that the described method comprises the following steps:
(1) melamine powder is added in crucible and is put into heating calcining 2h in Muffle furnace, heating rate is 10 DEG C/min；
(2) ultrasonic cut in ethyl alcohol is put into after the product that step (1) obtains being pulverized, the dosage of ethyl alcohol is 50mL；
(3) it will be transferred in Muffle furnace and calcine after product filtering drying that step (2) obtains, heating rate is 10 DEG C/min；
(4) product that step (3) obtains quickly is transferred in ice water and is stirred, calcined 12h at 80 DEG C after filtering, nitrogenized
Carbon nanotube.
2. a kind of preparation method of graphite phase carbon nitride nanotube according to claim 1, which is characterized in that step (1)
The temperature kept after middle heating is 550 DEG C.
3. a kind of preparation method of graphite phase carbon nitride nanotube according to claim 1, which is characterized in that step (2)
The time of middle ultrasonic cut is 1h.
4. a kind of preparation method of graphite phase carbon nitride nanotube according to claim 1, which is characterized in that step (3)
The temperature kept after middle heating is 350 DEG C.
5. a kind of preparation method of graphite phase carbon nitride nanotube according to claim 1, which is characterized in that step (3)
The time that temperature is kept after middle heating is 10min.
6. a kind of preparation method of graphite phase carbon nitride nanotube according to claim 1, which is characterized in that step (4)
Mixing time is 30min in middle ice water.
7. a kind of preparation method of graphite phase carbon nitride nanotube described in any claim in -6 according to claim 1,
It is characterized in that, the calcination atmosphere in step (4) is vacuum.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910425629.3A CN110104622A (en) | 2019-05-21 | 2019-05-21 | A kind of preparation method of graphite phase carbon nitride nanotube |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910425629.3A CN110104622A (en) | 2019-05-21 | 2019-05-21 | A kind of preparation method of graphite phase carbon nitride nanotube |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110104622A true CN110104622A (en) | 2019-08-09 |
Family
ID=67491453
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910425629.3A Pending CN110104622A (en) | 2019-05-21 | 2019-05-21 | A kind of preparation method of graphite phase carbon nitride nanotube |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110104622A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103601162A (en) * | 2013-11-26 | 2014-02-26 | 天津大学 | Preparation method of graphite type carbon nitride nanotubes |
| US20150340117A1 (en) * | 2013-01-09 | 2015-11-26 | Hanwha Chemical Corporation | Method for producing conductive film |
-
2019
- 2019-05-21 CN CN201910425629.3A patent/CN110104622A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150340117A1 (en) * | 2013-01-09 | 2015-11-26 | Hanwha Chemical Corporation | Method for producing conductive film |
| CN103601162A (en) * | 2013-11-26 | 2014-02-26 | 天津大学 | Preparation method of graphite type carbon nitride nanotubes |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107098323B (en) | A kind of g-C3N4Nanometer sheet and the preparation method and application thereof | |
| CN106732708B (en) | Graphite phase carbon nitride nanometer sheet loads single layer Bismuth tungstate nano-sheet heterojunction material and its preparation method and application | |
| CN102950016B (en) | Preparation method of ZnO/g-C3N4 composite photocatalyst | |
| CN107555470B (en) | A kind of method of two-step method synthesis zinc cadmium sulphur solid-solution material | |
| CN103601162B (en) | Preparation method of graphite type carbon nitride nanotubes | |
| CN106745226B (en) | Micro-nano titanium dioxide and preparation method and application based on eutectic solvent synthesis | |
| CN108126756B (en) | Bismuth tungstate-MIL-53 (Al) composite material, and preparation method and application thereof | |
| CN107282070B (en) | Three-dimensional flower-shaped sulfur indium zinc micro-nanowire array and preparation method and application thereof | |
| CN103736513A (en) | Preparation method of TiO2(B)@g-C3N4 composite nano-sheet photocatalyst | |
| CN102260046B (en) | Microwave synthesis method of zinc oxide film with oriented nanorod structure | |
| CN105502286B (en) | A kind of porous nano NiFe2O4Preparation method | |
| CN102126710B (en) | Method for preparing boron nitride nanowire by cracking of polymer | |
| CN107159289A (en) | A kind of preparation g C in situ3N4‑TiO2The method of nano heterojunction photocatalysis film | |
| CN108328646A (en) | A method of preparing three-dimensional flower-shaped zinc oxide-cadmium sulfide heterojunction nanometer material | |
| CN104261478A (en) | Preparation method of Mn3O4 nanowire or nanorod | |
| CN106492779A (en) | The preparation method of core shell structure rare earth titanate dioxide composite nanofiber catalysis material | |
| CN103920505A (en) | Cadmium sulfide inverse opal structure capable of producing hydrogen in high-efficiency manner through visible light photocatalysis and preparation method thereof | |
| CN103833080B (en) | A kind of preparation method of molybdic acid cadmium porous ball | |
| CN108085784B (en) | Synthetic method of NiO multi-stage micro-nano fiber and obtained product | |
| CN110104622A (en) | A kind of preparation method of graphite phase carbon nitride nanotube | |
| CN103160929A (en) | Preparation method of monocrystalline AlN nanocones and nanosheets | |
| CN107986340A (en) | A kind of porous NiO Nano compounds material of mask shape and preparation method thereof | |
| CN101870470A (en) | Preparation method of SiC nanowire in hierarchical structure | |
| CN113101952B (en) | Bi 4 O 5 I 2 /Bi 5 O 7 I composite photocatalyst and preparation method and application thereof | |
| CN111807380B (en) | Method for preparing three-dimensional multilevel structure basic nickel silicate catalyst by one pot |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20190809 |
|
| WD01 | Invention patent application deemed withdrawn after publication |