CN105800571B - A kind of preparation method of two-dimensional nano piece carbon-nitrogen material - Google Patents
A kind of preparation method of two-dimensional nano piece carbon-nitrogen material Download PDFInfo
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- CN105800571B CN105800571B CN201610109416.6A CN201610109416A CN105800571B CN 105800571 B CN105800571 B CN 105800571B CN 201610109416 A CN201610109416 A CN 201610109416A CN 105800571 B CN105800571 B CN 105800571B
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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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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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Abstract
The invention discloses a kind of of low cost, the preparation method of the easily controllable two-dimensional nano piece carbon-nitrogen material of process, comprises the following steps：1) melamine powder is heated to 500 DEG C~600 DEG C and keeps the temperature 2~8h, then cooled down, obtain solid block yellow g C3N4, powder is made afterwards, obtains yellow powder；2) yellow powder is added into monoethanolamine, be uniformly mixed, obtain uniform suspension, by uniform suspension 50 DEG C~200 DEG C keep the temperature 2~8h, postcooling, obtain reaction product, reaction product is post-treated to obtain two-dimensional nano piece carbon-nitrogen material.The present invention uses pyrolysismethod and solvent-thermal method, and the preparation method is of low cost, easily controllable, and Product formation yield is high, and technique is relatively easy.
Description
Technical field
The present invention relates to the preparation field of carbon-nitrogen material, and in particular to a kind of preparation side of two-dimensional nano piece carbon-nitrogen material
Method.
Background technology
Carbon-nitrogen material enjoys all the time due to showing very excellent performance in electricity, mechanics, optics etc. always
Concern.For example, class graphite phase carbon nitride material has excellent photocatalysis performance, can degrade in the case of showing visible ray
Organic pollution and hydrogen production by water decomposition.β-C3N4On mechanics according to calculate be the material harder than diamond.Meanwhile research shows,
Noncrystal membrane carbon-nitrogen material has wearability, hydrogen storage property, excellent field emission performance and air-sensitive performance etc..At the same time, no
Carbon-nitrogen material with carbon-nitrogen ratio is also that there is difference on resistance, heat conductivity and heat endurance.This shows that carbon-nitrogen material has
There is huge application potential.
At the same time, with the successful synthesizing graphite alkene material of University of Manchester, two-dimensional material because its unique optics,
Mechanics, electromagnetism and gas-sensitive property and show the prospect of being widely applied.
Therefore, preparing two-dimensional nano piece carbon-nitrogen material has important researching value and application value.Synthesize two-dimensional nano
Piece carbon-nitrogen material is generally using thermal oxide etching method, chemical stripping method, liquid solution stripping method etc..And solvent-thermal method operation letter
Just, two-dimensional nano piece carbon nitrogen is synthesized because usually controlling crystal growth by the reaction temperature of adjusting solvent heat and soaking time etc.
Material, the complicated technology synthesis for other two-dimentional carbon-nitrogen materials that compare, technique relative ease, relative inexpensiveness.
The Chinese invention patent application of 104401948 A of application publication number CN (Application No. 201410653994.7) is public
A kind of preparation method of mono-layer graphite type azotized carbon nano piece solution has been opened, has been comprised the following steps：1) melamine, urea are chosen
Or dimerization cdicynanmide is presoma, graphite type carbon nitride powder is obtained by heat polymerization；Choose a kind of polar solvent or table
The aqueous solution of face activating agent, graphite type carbon nitride powder is added into the aqueous solution of selected polar solvent or surfactant
Body, obtains solution A, then solution A is put into ball grinder, is placed in carrying out 12~24h of ball milling on jar mill, obtains carbonitride
Suspension solution；Wherein, the concentration for toner body being nitrogenized in solution A is 2.5~5mg/mL；2) nitridation after ball-milling treatment is taken out
Carbon suspension solution, is placed in ultrasonic disperse instrument and carries out ultrasonic stripping, interim, 100~200w of ultrasonic power, 0.5~1h of ultrasonic time；
3) solution after ultrasound is peeled off is subjected to 0.5~1h of centrifugal treating, 3000~4000rpm of centrifuge speed, takes upper strata clear
Liquid obtains mono-layer graphite type azotized carbon nano piece solution.The preparation method preparation process is complicated, and passes through ultrasound after ball milling
Peel off, its pattern is uncontrollable.
The content of the invention
It is an object of the invention to provide a kind of of low cost, system of the easily controllable two-dimensional nano piece carbon-nitrogen material of process
Preparation Method.
A kind of preparation method of two-dimensional nano piece carbon-nitrogen material, comprises the following steps：
1) melamine powder is heated to 500 DEG C~600 DEG C and keeps the temperature 2~8h, then cooled down, obtain solid block Huang
Color g-C3N4, powder is made afterwards, obtains yellow powder；
2) yellow powder is added into monoethanolamine, be uniformly mixed, obtain uniform suspension, by uniform suspension 50 DEG C~
200 DEG C insulation 2~8h, postcooling, obtain reaction product, reaction product is post-treated to obtain two-dimensional nano piece carbon-nitrogen material.
In the present invention, using pyrolysismethod and solvent-thermal method, suitable melamine is heated in crucible first, with semiclosed
State synthesizes g-C in Muffle furnace with suitable heat treatment process3N4, and grind into powder stores；Then, with the g- of synthesis
C3N4Yellow powder be raw material, monoethanolamine is solvent, is put into after stirring in reaction kettle, and by regulating and controlling the reaction time, is carried out
Solvent thermal reaction processing, is made two-dimensional nano piece carbon-nitrogen material.The preparation method is of low cost, easily controllable, Product formation production
Amount is high, and technique is relatively easy.
The preferred technical solution of the present invention is used as below：
In step 1), melamine powder is heated to 500 DEG C~600 DEG C with the heating rate of 2~5 DEG C/min and is kept the temperature
2~8h.Further preferably, melamine powder is heated to 530 DEG C~570 DEG C with the heating rate of 3~4 DEG C/min and kept the temperature
3~5h.Most preferably, melamine powder is heated to 550 DEG C with the heating rate of 3.5 DEG C/min and keeps the temperature 4h.
Environment temperature is subsequently cooled to, that is, is cooled to 0 DEG C~35 DEG C.
In step 2), it is uniformly mixed and is realized by magnetic agitation 1h~5h, further preferably, is uniformly mixed and is stirred by magnetic force
Mix 2h realizations.
Environment temperature is cooled to afterwards, that is, is cooled to 0 DEG C~35 DEG C.
The post processing includes：Washing and drying.The washing is cleaned repeatedly using deionized water and absolute ethyl alcohol.
The drying is in 60 DEG C~80 DEG C drying, 70 DEG C of insulation drying further preferably in baking oven.
Above-mentioned melamine, monoethanolamine are that chemistry is pure.
Compared with prior art, the invention has the advantages that：
The present invention passes through pyrolysismethod and solvent hot preparation two-dimensional nano piece carbon-nitrogen material.The present invention passes through heat point in the first step
Solve melamine synthesis g-C3N4, material source is provided for the synthesis of nanometer sheet.On the other hand by second step solvent thermal reaction
During add ethanol amine solvent, be effectively controlled carbon-nitrogen material pattern change, be finally synthesizing two-dimensional nano piece carbon nitrogen material
Material.The preparation method is easily controllable, of low cost, and technique is relatively easy, it is possible to achieve large-scale production.Two synthesized wieners
Rice piece carbon-nitrogen material, has bigger serface, stable structure, has excellent in photocatalysis, gas absorption and air-sensitive field
Performance.
Brief description of the drawings
Fig. 1 is solid block yellow g-C prepared by first step thermal decomposition prepared by embodiment 13N4SEM photograph；
Fig. 2 is the SEM photograph of two-dimensional nano piece carbon-nitrogen material prepared by embodiment 1；
Fig. 3 is the TEM photos of two-dimensional nano piece carbon-nitrogen material prepared by embodiment 1.
Embodiment
The method of the present invention is further illustrated with reference to embodiments.
Embodiment 1
1) weigh melamine powder to add in crucible, and covering crucible cover makes sample be in semi-closed state, is put into horse
Not in stove.550 DEG C are heated to the heating rate of 3.5 DEG C/min and keep the temperature 4h, then furnace cooling is to 25 DEG C of room temperature, consolidate
Body bulk yellow g-C3N4；
2) by the solid block yellow g-C obtained by step 1)3N4Grind into powder, obtains yellow powder, and stores；
3) yellow powder prepared by step 2) is weighed into 1g, be put into the beaker of 50ml.The monoethanolamine for measuring 40ml falls
Enter in beaker, magnetic agitation 2h, the abundant disperse of yellow powder is obtained uniform suspension in monoethanolamine；
4) it is transferred in the uniform suspension obtained by step 3) in reaction kettle liner, it is closed, it is put into baking oven in 200 DEG C of guarantors
Warm 2h, furnace cooling obtain reaction product to 25 DEG C of room temperature；
5) in the reaction product obtained by step 4), cleaned repeatedly with deionized water and absolute ethyl alcohol, be put into drying box, 70
DEG C insulation drying, obtain carbon-nitrogen material two-dimensional nano piece.
Fig. 1 is solid block yellow g-C prepared by first step thermal decomposition3N4SEM photograph, Fig. 2 is two-dimensional nano piece carbon nitrogen
The SEM photograph of material, Fig. 3 are the TEM photos of two-dimensional nano piece carbon-nitrogen material.
Embodiment 2
1) weigh melamine powder to add in crucible, and covering crucible cover makes sample be in semi-closed state, is put into horse
Not in stove.550 DEG C are heated to the heating rate of 3.5 DEG C/min and keep the temperature 4h, then furnace cooling is to 25 DEG C of room temperature, consolidate
Body bulk yellow g-C3N4；
2) by the solid block yellow g-C obtained by step 1)3N4Grind into powder, obtains yellow powder, and stores；
3) yellow powder prepared by step 2) is weighed into 1g, be put into the beaker of 50ml.The monoethanolamine for measuring 40ml pours into
In beaker, magnetic agitation 2h, makes the abundant disperse of yellow powder obtain uniform suspension in monoethanolamine；
4) it is transferred in the uniform suspension obtained by step 3) in reaction kettle liner, it is closed, it is put into baking oven in 200 DEG C of guarantors
Warm 8h, furnace cooling obtain reaction product to 25 DEG C of room temperature；
5) in the reaction product obtained by step 4), cleaned repeatedly with deionized water and absolute ethyl alcohol, be put into drying box, 70
DEG C insulation drying, obtain carbon-nitrogen material two-dimensional nano piece.
Embodiment 3
1) weigh melamine powder to add in crucible, and covering crucible cover makes sample be in semi-closed state, is put into horse
Not in stove.550 DEG C are heated to the heating rate of 3.5 DEG C/min and keep the temperature 4h, then furnace cooling is to 25 DEG C of room temperature, consolidate
Body bulk yellow g-C3N4；
2) by the solid block yellow g-C obtained by step 1)3N4Grind into powder, obtains yellow powder, and stores；
3) yellow powder prepared by step 2) is weighed into 1g, be put into the beaker of 50ml.The monoethanolamine for measuring 40ml pours into
In beaker, magnetic agitation 2h, makes the abundant disperse of yellow powder obtain uniform suspension in monoethanolamine；
4) it is transferred in the uniform suspension obtained by step 3) in reaction kettle liner, it is closed, it is put into baking oven in 150 DEG C of guarantors
Warm 6h, furnace cooling obtain reaction product to 25 DEG C of room temperature；
5) in the reaction product obtained by step 4), cleaned repeatedly with deionized water and absolute ethyl alcohol, be put into drying box, 70
DEG C insulation drying, obtain carbon-nitrogen material two-dimensional nano piece.
Claims (9)
1. a kind of preparation method of two-dimensional nano piece carbon-nitrogen material, it is characterised in that comprise the following steps：
1) melamine powder is heated to 500 DEG C~600 DEG C and keeps the temperature 2~8h, then cooled down, obtain solid block yellow g-
C3N4, powder is made afterwards, obtains yellow powder；
2) yellow powder is added into monoethanolamine, is uniformly mixed, uniform suspension is obtained, by uniform suspension at 50 DEG C~200 DEG C
Keep the temperature 2~8h, postcooling, obtain reaction product, reaction product is post-treated to obtain two-dimensional nano piece carbon-nitrogen material.
2. the preparation method of two-dimensional nano piece carbon-nitrogen material according to claim 1, it is characterised in that, will in step 1)
Melamine powder is heated to 500 DEG C~600 DEG C with the heating rate of 2~5 DEG C/min and keeps the temperature 2~8h.
3. the preparation method of two-dimensional nano piece carbon-nitrogen material according to claim 2, it is characterised in that, will in step 1)
Melamine powder is heated to 530 DEG C~570 DEG C with the heating rate of 3~4 DEG C/min and keeps the temperature 3~5h.
4. the preparation method of two-dimensional nano piece carbon-nitrogen material according to claim 1, it is characterised in that in step 1), so
Postcooling is to 0 DEG C~35 DEG C.
5. the preparation method of two-dimensional nano piece carbon-nitrogen material according to claim 1, it is characterised in that in step 2), mix
Close and realized uniformly through magnetic agitation 1h~5h.
6. the preparation method of two-dimensional nano piece carbon-nitrogen material according to claim 1, it is characterised in that in step 2), it
Postcooling is to 0 DEG C~35 DEG C.
7. the preparation method of two-dimensional nano piece carbon-nitrogen material according to claim 1, it is characterised in that in step 2), institute
The post processing stated includes：Washing and drying.
8. the preparation method of two-dimensional nano piece carbon-nitrogen material according to claim 7, it is characterised in that the washing is adopted
Cleaned repeatedly with deionized water and absolute ethyl alcohol.
9. the preparation method of two-dimensional nano piece carbon-nitrogen material according to claim 7, it is characterised in that the drying exists
60 DEG C~80 DEG C drying.
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| CN106430125A (en) * | 2016-09-27 | 2017-02-22 | 浙江大学 | Preparation method of porous g-C3N4 rod |
| CN107098321B (en) * | 2017-04-12 | 2019-03-19 | 天津大学 | The method that low temperature plasma prepares two-dimensional structure carboritride |
| 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 |
| 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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| 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 |
| CN104891460B (en) * | 2015-05-29 | 2017-04-19 | 厦门大学 | Method for preparing graphite-phase carbon nitride nanosheets by using solution phase |
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