CN105800571A - Preparation method for two-dimensional nanosheet carbon nitride material - Google Patents
Preparation method for two-dimensional nanosheet carbon nitride material Download PDFInfo
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- CN105800571A CN105800571A CN201610109416.6A CN201610109416A CN105800571A CN 105800571 A CN105800571 A CN 105800571A CN 201610109416 A CN201610109416 A CN 201610109416A CN 105800571 A CN105800571 A CN 105800571A
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- 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
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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
Abstract
The invention discloses a preparation method for a two-dimensional nanosheet carbon nitride material with low cost and process easy to control. The preparation method comprises the following steps: 1) heating melamine powder to 500-600 DEG C and carrying out heat preservation for 2-8 hours, then cooling to obtain solid blocky yellow g- C3N4, and then preparing into powder, so that yellow powder is obtained; and 2) adding the yellow powder into ethanol amine, uniformly mixing to obtain a uniform turbid liquid, carrying out heat preservation on the turbid liquid for 2-8 hours at the temperature of 50-200 DEG C, then cooling to obtain a reaction product, and then treating the reaction product, so that the two-dimensional nanosheet carbon nitride material is obtained. The preparation method disclosed by the invention adopts a pyrolysis process and a solvothermal method and is low in cost and easy to control, product synthesis yield is high, and a technology is relatively simple.
Description
Technical field
The present invention relates to the preparation field of carbon-nitrogen material, be specifically related to a kind of two-dimensional nano sheet carbon-nitrogen material
Preparation method.
Background technology
Carbon-nitrogen material always due in electricity, mechanics, the aspect such as optics show the most excellent performance and
All the time receive much concern.Such as, class graphite phase carbon nitride material has the photocatalysis performance of excellence, shows
Can be with degradable organic pollutant and hydrogen production by water decomposition in the case of visible ray.β-C3N4According to calculating on mechanics
It is the material harder than diamond.Meanwhile, research shows, noncrystal membrane carbon-nitrogen material have wearability,
Hydrogen storage property, excellent field emission performance and air-sensitive performance etc..Meanwhile, the carbon nitrogen of different carbon-nitrogen ratios
Material is also to there is difference on resistance, heat conductivity and heat stability.This shows, carbon-nitrogen material has
There is huge application potential.
Meanwhile, along with University of Manchester's successful synthesizing graphite alkene material, two-dimensional material is only because of it
Special optics, mechanics, electromagnetism and gas-sensitive property and show the prospect of being widely applied.
Therefore, prepare two-dimensional nano sheet carbon-nitrogen material and there is important researching value and using value.Synthesis
Two-dimensional nano sheet carbon-nitrogen material typically uses thermal oxide etching method, chemical stripping method, liquid solution stripping method
Deng.And solvent-thermal method is easy and simple to handle, the reaction temperature hot by adjusting solvent and temperature retention time etc. are because of usually
Control crystal growth, synthesize two-dimensional nano sheet carbon-nitrogen material, the complexity of other Two-dimensional Carbon nitrogen materials that compare
Technique synthesizes, technique relative ease, relative inexpensiveness.
The Chinese invention of application publication number CN 104401948 A (Application No. 201410653994.7) is special
Profit application discloses the preparation method of a kind of mono-layer graphite type azotized carbon nano sheet solution, including following step
Rapid: 1) to choose tripolycyanamide, carbamide or dimerization cdicynanmide be presoma, obtained by heat polymerization
Graphite type carbon nitride powder body；Choose the aqueous solution of a kind of polar solvent or surfactant, to selected
The aqueous solution of polar solvent or surfactant adds graphite type carbon nitride powder body, obtains solution A, so
After solution A is put in ball grinder, be placed on jar mill carrying out ball milling 12～24h, obtain carbonitride
Suspension solution；Wherein, in solution A, the concentration of carbonitride powder body is 2.5～5mg/mL；2) process is taken out
Carbonitride suspension solution after ball-milling treatment, is placed in ultrasonic disperse instrument and carries out ultrasonic stripping, interim, ultrasonic
Power 100～200w, ultrasonic time 0.5～1h；3) solution after ultrasonic stripping is centrifuged
Process 0.5～1h, centrifuge speed 3000～4000rpm, take the supernatant and i.e. obtain mono-layer graphite type nitrogen
Change carbon nanosheet solution.This preparation method preparation process is complicated, and by ultrasonic stripping after ball milling, its
Pattern is uncontrollable.
Summary of the invention
It is an object of the invention to provide two-dimensional nano sheet carbon nitrogen a kind of with low cost, that process is easily controllable
The preparation method of material.
The preparation method of a kind of two-dimensional nano sheet carbon-nitrogen material, comprises the following steps:
1) melamine powder it is heated to 500 DEG C～600 DEG C and is incubated 2～8h, then cooling down, obtain
Solid block yellow g-C3N4, make powder afterwards, obtain yellow powder；
2) yellow powder is added ethanolamine, mix homogeneously, obtain uniform suspension, will be the most suspended
Liquid is incubated 2～8h at 50 DEG C～200 DEG C, cools down afterwards, obtains product, and product is post-treated
Obtain two-dimensional nano sheet carbon-nitrogen material.
In the present invention, use pyrolysismethod and solvent-thermal method, in crucible, first heat appropriate tripolycyanamide,
In Muffle furnace, g-C is synthesized with suitable Technology for Heating Processing with semi-closed state3N4, and grind into powder storage
Deposit；Then, with the g-C of synthesis3N4Yellow powder be raw material, ethanolamine is solvent, puts after stirring
Enter in reactor, and by the regulation and control response time, carry out solvent thermal reaction process, prepare two-dimensional nano sheet
Carbon-nitrogen material.This preparation method is with low cost, it is easy to control, and Product formation yield is high, and technique is the simplest
Single.
Following as the preferred technical solution of the present invention:
Step 1) in, melamine powder is heated to 500 DEG C with the heating rate of 2～5 DEG C/min
～600 DEG C and be incubated 2～8h.Further preferably, by melamine powder with the heating rate of 3～4 DEG C/min
It is heated to 530 DEG C～570 DEG C and is incubated 3～5h.Most preferably, by melamine powder with 3.5 DEG C/min's
Heating rate is heated to 550 DEG C and is incubated 4h.
It is subsequently cooled to ambient temperature, is i.e. cooled to 0 DEG C～35 DEG C.
Step 2) in, mix homogeneously is realized by magnetic agitation 1h～5h, and further preferably, mixing is all
Even realized by magnetic agitation 2h.
It is cooled to ambient temperature afterwards, is i.e. cooled to 0 DEG C～35 DEG C.
Described post processing includes: washs and is dried.Described washing uses deionized water and dehydrated alcohol
Repeatedly clean.Described is dried 60 DEG C～80 DEG C drying, and further preferably in baking oven, 70 DEG C of insulations are dried
Dry.
Above-mentioned tripolycyanamide, ethanolamine are chemical pure.
Compared with prior art, present invention have the advantage that
The present invention prepares two-dimensional nano sheet carbon-nitrogen material by pyrolysismethod and solvent thermal.The present invention is in the first step
By thermal decomposition tripolycyanamide synthesis g-C3N4, the synthesis for nanometer sheet provides material source.On the other hand
By adding ethanolamine solvent during second step solvent thermal reaction, it is effectively controlled carbon-nitrogen material
Morphology change, is finally synthesizing two-dimensional nano sheet carbon-nitrogen material.This preparation method is easily controllable, with low cost,
Technique is relatively easy, it is possible to achieve large-scale production.Synthesized two-dimensional nano sheet carbon-nitrogen material, has
Bigger serface, stable structure, there is the property of excellence in photocatalysis, gas absorption and air-sensitive field
Energy.
Accompanying drawing explanation
Fig. 1 is solid block yellow g-C of the first step thermal decomposition preparation of embodiment 1 preparation3N4SEM
Photo；
Fig. 2 is the SEM photograph of the two-dimensional nano sheet carbon-nitrogen material of embodiment 1 preparation；
Fig. 3 is the TEM photo of the two-dimensional nano sheet carbon-nitrogen material of embodiment 1 preparation.
Detailed description of the invention
The inventive method is further illustrated below in conjunction with embodiment.
Embodiment 1
1) weigh melamine powder to add in crucible, and cover crucible cover and make sample be in semiclosed shape
State, puts in Muffle furnace.It is heated to 550 DEG C with the heating rate of 3.5 DEG C/min and is incubated 4h, then
Furnace cooling, to room temperature 25 DEG C, obtains solid block yellow g-C3N4；
2) by step 1) solid block yellow g-C of gained3N4Grind into powder, obtains yellow powder,
And store；
3) by step 2) prepared by yellow powder weigh 1g, put in the beaker of 50ml.Measure
The ethanolamine of 40ml is poured in beaker, magnetic agitation 2h, make the abundant disperse of yellow powder in ethanolamine,
Obtain uniform suspension；
4) in step 3) the uniform suspension of gained transfers in reactor inner bag, airtight, puts into baking oven
In 200 DEG C be incubated 2h, furnace cooling, to room temperature 25 DEG C, obtains product；
5) in step 4) product of gained, repeatedly clean with deionized water and dehydrated alcohol, put into
Drying baker, dries 70 DEG C of insulations, obtains carbon-nitrogen material two-dimensional nano sheet.
Fig. 1 is solid block yellow g-C of first step thermal decomposition preparation3N4SEM photograph, Fig. 2 is
The SEM photograph of two-dimensional nano sheet carbon-nitrogen material, Fig. 3 is the TEM photo of two-dimensional nano sheet carbon-nitrogen material.
Embodiment 2
1) weigh melamine powder to add in crucible, and cover crucible cover and make sample be in semiclosed shape
State, puts in Muffle furnace.It is heated to 550 DEG C with the heating rate of 3.5 DEG C/min and is incubated 4h, then
Furnace cooling, to room temperature 25 DEG C, obtains solid block yellow g-C3N4；
2) by step 1) solid block yellow g-C of gained3N4Grind into powder, obtains yellow powder,
And store；
3) by step 2) prepared by yellow powder weigh 1g, put in the beaker of 50ml.Measure 40ml
Ethanolamine pour in beaker, magnetic agitation 2h, make the abundant disperse of yellow powder in ethanolamine, obtain
Uniformly suspension；
4) in step 3) the uniform suspension of gained transfers in reactor inner bag, airtight, puts into baking oven
In 200 DEG C be incubated 8h, furnace cooling, to room temperature 25 DEG C, obtains product；
5) in step 4) product of gained, repeatedly clean with deionized water and dehydrated alcohol, put into
Drying baker, dries 70 DEG C of insulations, obtains carbon-nitrogen material two-dimensional nano sheet.
Embodiment 3
1) weigh melamine powder to add in crucible, and cover crucible cover and make sample be in semiclosed shape
State, puts in Muffle furnace.It is heated to 550 DEG C with the heating rate of 3.5 DEG C/min and is incubated 4h, then
Furnace cooling, to room temperature 25 DEG C, obtains solid block yellow g-C3N4；
2) by step 1) solid block yellow g-C of gained3N4Grind into powder, obtains yellow powder,
And store；
3) by step 2) prepared by yellow powder weigh 1g, put in the beaker of 50ml.Measure 40ml
Ethanolamine pour in beaker, magnetic agitation 2h, make the abundant disperse of yellow powder in ethanolamine, obtain
Uniformly suspension；
4) in step 3) the uniform suspension of gained transfers in reactor inner bag, airtight, puts into baking oven
In 150 DEG C be incubated 6h, furnace cooling, to room temperature 25 DEG C, obtains product；
5) in step 4) product of gained, repeatedly clean with deionized water and dehydrated alcohol, put into
Drying baker, dries 70 DEG C of insulations, obtains carbon-nitrogen material two-dimensional nano sheet.
Claims (9)
1. the preparation method of a two-dimensional nano sheet carbon-nitrogen material, it is characterised in that comprise the following steps:
1) melamine powder it is heated to 500 DEG C～600 DEG C and is incubated 2～8h, then cooling down, obtain
Solid block yellow g-C3N4, make powder afterwards, obtain yellow powder；
2) yellow powder is added ethanolamine, mix homogeneously, obtain uniform suspension, will be the most suspended
Liquid is incubated 2～8h at 50 DEG C～200 DEG C, cools down afterwards, obtains product, and product is post-treated
Obtain two-dimensional nano sheet carbon-nitrogen material.
The preparation method of two-dimensional nano sheet carbon-nitrogen material the most according to claim 1, its feature exists
In, step 1) in, melamine powder is heated to 500 DEG C～600 DEG C with the heating rate of 2～5 DEG C/min
And it is incubated 2～8h.
The preparation method of two-dimensional nano sheet carbon-nitrogen material the most according to claim 2, its feature exists
In, step 1) in, melamine powder is heated to 530 DEG C～570 DEG C with the heating rate of 3～4 DEG C/min
And it is incubated 3～5h.
The preparation method of two-dimensional nano sheet carbon-nitrogen material the most according to claim 1, its feature exists
In, step 1) in, it is subsequently cooled to 0 DEG C～35 DEG C.
The preparation method of two-dimensional nano sheet carbon-nitrogen material the most according to claim 1, its feature exists
In, step 2) in, mix homogeneously is realized by magnetic agitation 1h～5h.
The preparation method of two-dimensional nano sheet carbon-nitrogen material the most according to claim 1, its feature exists
In, step 2) in, it is cooled to 0 DEG C～35 DEG C afterwards.
The preparation method of two-dimensional nano sheet carbon-nitrogen material the most according to claim 1, its feature exists
In, step 2) in, described post processing includes: washs and is dried.
The preparation method of two-dimensional nano sheet carbon-nitrogen material the most according to claim 7, its feature exists
In, described washing uses deionized water and dehydrated alcohol repeatedly to clean.
The preparation method of two-dimensional nano sheet carbon-nitrogen material the most according to claim 7, its feature exists
In, described is dried 60 DEG C～80 DEG C drying.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106430125A (en) * | 2016-09-27 | 2017-02-22 | 浙江大学 | Preparation method of porous g-C3N4 rod |
| CN107098321A (en) * | 2017-04-12 | 2017-08-29 | 天津大学 | The method that low temperature plasma prepares two-dimensional structure carboritride |
| CN109534307A (en) * | 2019-01-16 | 2019-03-29 | 济南大学 | A kind of g-C3N4 crystal phase/amorphous phase homojunction and its preparation method and application |
| CN112142021A (en) * | 2020-09-11 | 2020-12-29 | 江苏理工学院 | Preparation method and application of carbon-nitrogen polymer two-dimensional material |
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| CN102718206A (en) * | 2011-03-29 | 2012-10-10 | 中国科学院大连化学物理研究所 | A macroscopic quantity preparation method for a nitrogen-doped graphene |
| CN104401948A (en) * | 2014-11-17 | 2015-03-11 | 长安大学 | Preparation method for single-layer graphite-type carbon nitride nanosheet solution |
| CN104891460A (en) * | 2015-05-29 | 2015-09-09 | 厦门大学 | Method for preparing graphite-phase carbon nitride nanosheets by using solution phase |
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2016
- 2016-02-26 CN CN201610109416.6A patent/CN105800571B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102718206A (en) * | 2011-03-29 | 2012-10-10 | 中国科学院大连化学物理研究所 | A macroscopic quantity preparation method for a nitrogen-doped graphene |
| CN104401948A (en) * | 2014-11-17 | 2015-03-11 | 长安大学 | Preparation method for single-layer graphite-type carbon nitride nanosheet solution |
| CN104891460A (en) * | 2015-05-29 | 2015-09-09 | 厦门大学 | Method for preparing graphite-phase carbon nitride nanosheets by using solution phase |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106430125A (en) * | 2016-09-27 | 2017-02-22 | 浙江大学 | Preparation method of porous g-C3N4 rod |
| CN107098321A (en) * | 2017-04-12 | 2017-08-29 | 天津大学 | The method that low temperature plasma prepares two-dimensional structure carboritride |
| CN109534307A (en) * | 2019-01-16 | 2019-03-29 | 济南大学 | A kind of g-C3N4 crystal phase/amorphous phase homojunction and its preparation method and application |
| CN109534307B (en) * | 2019-01-16 | 2022-03-29 | 济南大学 | g-C3N4 crystalline phase/amorphous homogeneous junction and preparation method and application thereof |
| CN112142021A (en) * | 2020-09-11 | 2020-12-29 | 江苏理工学院 | Preparation method and application of carbon-nitrogen polymer two-dimensional material |
| CN112142021B (en) * | 2020-09-11 | 2022-02-11 | 江苏理工学院 | Preparation method and application of carbon-nitrogen polymer two-dimensional material |
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