CN104891460A - Method for preparing graphite-phase carbon nitride nanosheets by using solution phase - Google Patents

Method for preparing graphite-phase carbon nitride nanosheets by using solution phase Download PDF

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CN104891460A
CN104891460A CN201510288723.0A CN201510288723A CN104891460A CN 104891460 A CN104891460 A CN 104891460A CN 201510288723 A CN201510288723 A CN 201510288723A CN 104891460 A CN104891460 A CN 104891460A
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nanometer sheet
carbon nitride
phase carbon
graphite phase
solution prepares
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CN104891460B (en
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邓顺柳
宋雪欢
冯蓝
谢素原
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Xiamen University
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Abstract

The invention provides a method for preparing graphite-phase carbon nitride nanosheets by using a solution phase and belongs to the technical field of preparation of nano materials. The method comprises the following steps: calcining dicyanodiamine into a ceramic crucible with a cover, thereby obtaining a g-C3N4 polymer material; adding the g-C3N4 polymer material into a tetrahydrofuran solution of an alkali metal lithium or sodium, performing ultrasonic dispersion, adding halogenated organic solvent, and sequentially washing a solid product obtained by reaction with toluene, ethanol and water, thereby obtaining the g-C3N4 nanosheets. The preparation method has the advantages of cheap raw materials, simple process, high preparation efficiency and the like; the obtained g-C3N4 nanosheets are greatly enlarged in specific surface area, have good dispersibility in an organic phase and a water phase, and have favorable photocatalytic performance.

Description

A kind of solution prepares the method for graphite phase carbon nitride nanometer sheet mutually
Technical field
The invention belongs to technical field of nanometer material preparation, relate to a kind of solution and prepare graphite phase carbon nitride (g-C mutually 3n 4) method of nanometer sheet.
Background technology
In five kinds of allotropic substances of carbonitride, graphite phase carbon nitride, i.e. g-C 3n 4it is the most stable one.In recent years, g-C 3n 4because of its good chemical stability, unique semiconductor energy band structure, nontoxic and raw material is easy to get, not the excellent specific property such as containing metal get more and more people's extensive concerning in fields such as photochemical catalysis contaminant degradation, photolysis water hydrogen, photochemical catalysis organic syntheses.But, as a kind of polymer semiconducting material, by g-C 3n 4also there are some problems, (~ 10m as little in specific surface area as photocatalyst 2/ g), the exciton binding energy of photo-generated carrier is high, photo-generate electron-hole compound serious, visible ray utilization ratio is low.For these problems, people are from g-C 3n 4the aspects such as optimum synthesis, the physics of photocatalyst are composite modified, chemical doping modification, modification by copolymerization, finishing, nano modification to its physico-chemical property, as semiconductor energy band structure, optical absorption property etc. adjust, to improve g-C 3n 4photocatalysis performance.
Compared with body phase material, through the g-C of nano modification 3n 4photocatalyst specific surface area increases, degree of crystallinity improves, and its photocatalysis performance obviously improves.At present, people have synthesized with template and non-template method and have obtained a series of g-C with special appearance 3n 4nano-photocatalyst, as mesoporous g-C 3n 4, g-C 3n 4nanometer rod, g-C 3n 4nano particles etc., effectively facilitate g-C 3n 4the development of photocatalyst material.Due to g-C 3n 4there is class graphite laminate structure, also can by g-C 3n 4peel off into nano flake or single layer structure, stripping means conventional at present has hot stripping method or solvent stripping method.Hot stripping method is by g-C 3n 4heat-treat in atmosphere, body phase material is decomposed into nano flake (Niu P etc., Adv.Funct.Mater. gradually, 2012,22:4763-4770), and the solvent that solvent stripping method is commonly used is water (Zhang X D etc., J.Am.Chem.Soc., 2013,135,18-21) and Virahol (Yang S etc., Adv.Mater., 2013,25:2452), peel off the g-C obtained 3n 4laminated structure is comparatively complete, defect is few, has higher photocatalysis efficiency.But still there is experiment poor controllability in hot stripping method and solvent stripping method, the g-C prepared 3n 4the key issues such as lamella dispersiveness is bad, thickness is large, productive rate is low not yet solve.
Summary of the invention
The object of the present invention is to provide one to solve and prepare g-C at present 3n 4the solution of the problems such as nanometer sheet efficiency is low, thickness large, bad dispersibility prepares graphite phase carbon nitride (g-C mutually 3n 4) method of nanometer sheet.
For achieving the above object, first the inventive method is presoma with Dicyanodiamide, obtains g-C by heat polymerization 3n 4polymer materials, then under halogenated organic reagent exists, carries out g-C in the tetrahydrofuran solution of basic metal and naphthalene 3n 4the solution of nanometer sheet is prepared mutually.
A kind of solution prepares graphite phase carbon nitride (g-C mutually 3n 4) method of nanometer sheet, comprise the following steps:
1) take Dicyanodiamide as raw material, calcine, obtain yellow g-C 3n 4polymer materials;
2) by step 1) gained g-C 3n 4polymer materials is dispersed in tetrahydrofuran solution, ultrasonic disperse under nitrogen protection condition, the g-C obtained 3n 4dispersion liquid, at g-C 3n 4add basic metal and naphthalene successively in dispersion liquid, Keep agitation, then add halo organic reagent, react under nitrogen protection condition, after reaction terminates, gained solid product is washed with toluene, second alcohol and water successively, obtains graphite phase carbon nitride (g-C 3n 4) nanometer sheet;
Step 1) in, described calcining is calcined in retort furnace in ceramic crucible with cover, and the temperature of calcining can be 450 ~ 550 DEG C, and the time of calcining can be 2 ~ 4h.
Step 2) in, described basic metal can be metallic lithium or sodium Metal 99.5.
Step 2) in, described g-C 3n 4polymer materials and alkali-metal mol ratio (C 3n 4: basic metal) can be 1:7 ~ 150, the mol ratio >1 of basic metal and naphthalene.
Step 2) in, described halogenated organic reagent can be brominated alkanes Br (CH 2) ncH 3(n is integer, 4≤n≤12) and alkane iodide I (CH 2) ncH 3one in (n is integer, 4≤n≤12).
Step 2) in, described halo organic reagent and alkali-metal mol ratio are preferably 1: 1.
Step 2) in, the time of described reaction can be 5 ~ 24h.
Step 2) in, the time of described Keep agitation can be 30 ~ 120min.
G-C is obtained prepared by the present invention 3n 4nanometer sheet preparation efficiency is high, and by detecting, specific surface area can reach 53m 2/ g, the good dispersity in water and conventional organic solvent, has good photocatalysis performance, and atomic force microscope (AFM) shows, g-C 3n 4the thickness of nano flake is about 1 ~ 2nm.
The advantage that the present invention is compared with prior art possessed:
(1) the invention provides a kind of g-C 3n 4the molten liquid phase preparation process of nanometer sheet, the method preparation efficiency is high, controllability strong, the g-C prepared 3n 4nanometer sheet thickness and size adjustable;
(2) g-C for preparing of the present invention 3n 4nanometer sheet has good dispersiveness in water and common organic solvents;
(3) g-C for preparing of the present invention 3n 4nanometer sheet specific surface area is large, is conducive to effective separation of photo-generated carrier under illumination condition, improves photocatalysis performance;
(4) this preparation method's mild condition, does not need expensive equipment, has the prospect of large-scale application.
Accompanying drawing explanation
Fig. 1 is g-C 3n 4polymer materials and the present invention prepare g-C 3n 4the X-ray powder diffraction figure (XRD) of nanometer sheet.
Fig. 2 is that the present invention prepares g-C 3n 4the scanning electron microscope (SEM) photograph (SEM) of nanometer sheet.
Fig. 3 is that the present invention prepares g-C 3n 4the atomic force microscope figure (AFM) of nanometer sheet.
Fig. 4 is g-C 3n 4polymer materials and the present invention prepare g-C 3n 4the UV Diffuse Reflectance Spectroscopy figure of nanometer sheet.
Fig. 5 is the change curve of 2-hydroxyterephthalic acid fluorescence intensity with light application time.
Embodiment
Embodiment 1
A kind of solution prepares graphite phase carbon nitride (g-C mutually 3n 4) method of nanometer sheet, comprise the following steps:
In the ceramic crucible with cover of 50mL, add 10g Dicyanodiamide, crucible is placed in retort furnace, be increased to 550 DEG C with the speed of 2.5 DEG C/min from room temperature, constant temperature two hours.Be cooled to room temperature after calcining terminates, sample ground in agate mortar and obtains yellow powder, i.e. g-C 3n 4polymer materials.Under nitrogen protection condition, take 108mg g-C 3n 4polymer materials adds in the tetrahydrofuran solution that 120mL fresh dried crosses; ultrasonic 5min; then in this dispersion liquid, 0.55g metallic lithium and 5.08g naphthalene is added; solution becomes blackish green rear Keep agitation one hour; in above-mentioned solution, add Dodecyl Bromide with the speed of 10mL/h with automatic injector again until solution green disappears, continue reaction 12h under nitrogen protection.After reaction terminates, in above-mentioned reactant, add ethanol remove unreacted metallic lithium, with the centrifugal 5min of the rotating speed of 8000rpm/min, gained solid product uses toluene, ethanol, water washing successively, finally obtains g-C 3n 4nanometer sheet.
The result of embodiment 1 shows: prepare g-C 3n 4nanometer sheet is than the g-C of equal in quality 3n 4polymer materials is more fluffy, gas adsorption measuring g-C 3n 4the specific surface area of nanometer sheet can reach 53m 2/ g.Compare g-C 3n 4polymer materials, g-C 3n 4the dispersiveness of nanometer sheet in different solvents (as methylene dichloride, chloroform, DMF) significantly improves.Fig. 1 is g-C 3n 4polymer materials and g-C 3n 4the XRD figure of nanometer sheet, can find g-C 3n 4the XRD diffraction peak intensity of nanometer sheet significantly weakens, and body phase g-C is described 3n 4polymer materials is successfully peeled off into nanometer sheet.Fig. 2 is that the present invention prepares g-C 3n 4the SEM figure of nanometer sheet, can find out its obvious flaky texture.The AFM figure of Fig. 3 shows, the g-C prepared 3n 4nanometer sheet thickness is about 1 ~ 2nm.Fig. 4 is g-C 3n 4polymer materials and g-C 3n 4the solid uv drs abosrption spectrogram of nanometer sheet, as seen from Figure 4, the g-C that the present invention prepares 3n 4nanometer sheet significantly improves in the absorption of visible region.Be molecular probe with terephthalic acid, contrast g-C by fluorescence technique 3n 4polymer materials and the present invention prepare g-C 3n 4the photocatalysis performance of nanometer sheet.Fig. 5 is the change curve of fluorescence intensity with light application time of photochemical catalysis product 2-hydroxyterephthalic acid under visible ray rayed.As seen from Figure 5, with g-C 3n 4when nanometer sheet is photocatalyst, the fluorescence intensity of 2-hydroxyterephthalic acid is significantly higher than g-C 3n 4polymer materials, illustrates the g-C that the present invention prepares under illumination condition 3n 4nanometer sheet can produce more OH, has more excellent photocatalysis performance.
Embodiment 2
In the ceramic crucible with cover of 50mL, add 8.43g Dicyanodiamide, crucible is placed in retort furnace, be increased to 550 DEG C with the speed of 2.5 DEG C/min from room temperature, constant temperature two hours.Be cooled to room temperature after calcining terminates, sample ground in agate mortar and obtains yellow powder, i.e. g-C 3n 4polymer materials.Under nitrogen protection condition, take 71.2mg g-C 3n 4polymer materials adds in the tetrahydrofuran solution that 100mL fresh dried crosses; ultrasonic 5min; then in this dispersion liquid, 0.81g metallic lithium and 5.22g naphthalene is added; solution becomes blackish green rear Keep agitation one hour; in above-mentioned solution, add 1-bromine normal butane with the speed of 10mL/h with automatic injector again until solution green disappears, continue reaction 12h under nitrogen protection.After reaction terminates, in above-mentioned reactant, add ethanol remove unreacted metallic lithium, with the centrifugal 5min of the rotating speed of 8000rpm/min, gained solid product uses toluene, ethanol, water washing successively, finally obtains g-C 3n 4nanometer sheet material.
Embodiment 3
In the ceramic crucible with cover of 50mL, add 10g Dicyanodiamide, crucible is placed in retort furnace, be increased to 550 DEG C with the speed of 2.5 DEG C/min from room temperature, constant temperature two hours.Be cooled to room temperature after calcining terminates, sample ground in agate mortar and obtains yellow powder, i.e. g-C 3n 4polymer materials.Under nitrogen protection condition, take 368mg g-C 3n 4polymer materials adds in the tetrahydrofuran solution that 120mL fresh dried crosses; ultrasonic 5min; then in this dispersion liquid, 0.21g metallic lithium and 2.56g naphthalene is added; solution becomes blackish green rear Keep agitation one hour; in above-mentioned solution, add 1-bromine normal hexane with the speed of 10mL/h with automatic injector again until solution green disappears, continue reaction 12h under nitrogen protection.After reaction terminates, in above-mentioned reactant, add ethanol remove unreacted metallic lithium, with the centrifugal 5min of the rotating speed of 8000rpm/min, gained solid product uses toluene, ethanol, water washing successively, finally obtains g-C 3n 4nanometer sheet material.

Claims (8)

1. solution prepares a method for graphite phase carbon nitride nanometer sheet mutually, comprises the following steps:
1) take Dicyanodiamide as raw material, calcine, obtain yellow g-C 3n 4polymer materials;
2) by step 1) gained g-C 3n 4polymer materials is dispersed in tetrahydrofuran solution, and ultrasonic disperse under nitrogen protection condition, obtains g-C 3n 4dispersion liquid, at g-C 3n 4add basic metal and naphthalene successively in dispersion liquid, Keep agitation, then add halo organic reagent, react under nitrogen protection condition, after reaction terminates, gained solid product is washed with toluene, second alcohol and water successively, obtains g-C 3n 4nanometer sheet.
2. a kind of solution prepares the method for graphite phase carbon nitride nanometer sheet mutually as claimed in claim 1, it is characterized in that, step 1) in, the temperature of described calcining is 450 ~ 550 DEG C, and the time of calcining is 2 ~ 4h.
3. a kind of solution prepares the method for graphite phase carbon nitride nanometer sheet mutually as claimed in claim 1, it is characterized in that, step 2) in, described basic metal is metallic lithium or sodium Metal 99.5.
4. a kind of solution prepares the method for graphite phase carbon nitride nanometer sheet mutually as claimed in claim 1, it is characterized in that, step 2) in, described g-C 3n 4polymer materials and alkali-metal mol ratio (C 3n 4: basic metal) be 1: 7 ~ 150, the mol ratio >1 of basic metal and naphthalene.
5. a kind of solution prepares the method for graphite phase carbon nitride nanometer sheet mutually as claimed in claim 1, it is characterized in that, step 2) in, described halogenated organic reagent is brominated alkanes Br (CH 2) ncH 3, n is integer, 4≤n≤12; Or alkane iodide I (CH 2) ncH 3, n is integer, 4≤n≤12.
6. a kind of solution prepares the method for graphite phase carbon nitride nanometer sheet mutually as claimed in claim 1, it is characterized in that, step 2) in, described halo organic reagent and alkali-metal mol ratio are 1: 1.
7. a kind of solution prepares the method for graphite phase carbon nitride nanometer sheet mutually as claimed in claim 1, it is characterized in that, step 2) in, the time of described reaction is 5 ~ 24h.
8. a kind of solution prepares the method for graphite phase carbon nitride nanometer sheet mutually as claimed in claim 1, it is characterized in that, step 2) in, the time of described Keep agitation is 30 ~ 120min.
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Cited By (10)

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CN105417507A (en) * 2015-12-10 2016-03-23 济南大学 Preparing method for carbon nitride nano particles and obtained product
CN105540557A (en) * 2015-12-17 2016-05-04 榆林学院 Method for preparing graphite-like carbon nitride in ultrasonic field
CN105688969A (en) * 2016-02-19 2016-06-22 厦门大学 Preparation method of catalyst for photo-catalytically splitting water to produce hydrogen
CN105772056A (en) * 2016-04-28 2016-07-20 成都理工大学 Preparation method and application of graphite-phase carbon nitride photocatalysis material
CN105800571A (en) * 2016-02-26 2016-07-27 浙江大学 Preparation method for two-dimensional nanosheet carbon nitride material
CN107098323A (en) * 2017-04-25 2017-08-29 中南大学 A kind of g C3N4Nanometer sheet and preparation method and application
CN108584892A (en) * 2018-04-26 2018-09-28 福州大学 A kind of preparation method and applications of crystalline phase azotized carbon nano particle
CN108927197A (en) * 2018-07-09 2018-12-04 江苏大学 A kind of g-C of high catalytic performance3N4Preparation method and purposes
CN112126946A (en) * 2020-09-15 2020-12-25 中国科学院大连化学物理研究所 Composite membrane for acid-base water electrolysis and preparation method and application thereof
CN112897484A (en) * 2021-01-14 2021-06-04 华南理工大学 g-C without defect3N4Nanosheets, two-dimensional g-C3N4Nano sheet film, preparation method and application

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CN103058182A (en) * 2013-01-27 2013-04-24 厦门大学 Method for preparing graphene by solution phase
CN103232458A (en) * 2013-04-25 2013-08-07 大连理工大学 Method for preparing graphite phase carbon nitride material with monatomic layer structure
CN103848405A (en) * 2014-03-07 2014-06-11 西北大学 Preparation method of monolayer g-C3N4 nanometer material with monatomic thickness
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CN103058182A (en) * 2013-01-27 2013-04-24 厦门大学 Method for preparing graphene by solution phase
CN103232458A (en) * 2013-04-25 2013-08-07 大连理工大学 Method for preparing graphite phase carbon nitride material with monatomic layer structure
CN103848405A (en) * 2014-03-07 2014-06-11 西北大学 Preparation method of monolayer g-C3N4 nanometer material with monatomic thickness
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CN105417507B (en) * 2015-12-10 2018-03-06 济南大学 A kind of preparation method and products obtained therefrom of azotized carbon nano particle
CN105417507A (en) * 2015-12-10 2016-03-23 济南大学 Preparing method for carbon nitride nano particles and obtained product
CN105540557A (en) * 2015-12-17 2016-05-04 榆林学院 Method for preparing graphite-like carbon nitride in ultrasonic field
CN105688969A (en) * 2016-02-19 2016-06-22 厦门大学 Preparation method of catalyst for photo-catalytically splitting water to produce hydrogen
CN105800571A (en) * 2016-02-26 2016-07-27 浙江大学 Preparation method for two-dimensional nanosheet carbon nitride material
CN105772056A (en) * 2016-04-28 2016-07-20 成都理工大学 Preparation method and application of graphite-phase carbon nitride photocatalysis material
CN107098323A (en) * 2017-04-25 2017-08-29 中南大学 A kind of g C3N4Nanometer sheet and preparation method and application
CN107098323B (en) * 2017-04-25 2019-08-30 中南大学 A kind of g-C3N4Nanometer sheet and the preparation method and application thereof
CN108584892A (en) * 2018-04-26 2018-09-28 福州大学 A kind of preparation method and applications of crystalline phase azotized carbon nano particle
CN108927197A (en) * 2018-07-09 2018-12-04 江苏大学 A kind of g-C of high catalytic performance3N4Preparation method and purposes
CN112126946A (en) * 2020-09-15 2020-12-25 中国科学院大连化学物理研究所 Composite membrane for acid-base water electrolysis and preparation method and application thereof
CN112126946B (en) * 2020-09-15 2021-08-27 中国科学院大连化学物理研究所 Composite membrane for acid-base water electrolysis and preparation method and application thereof
CN112897484A (en) * 2021-01-14 2021-06-04 华南理工大学 g-C without defect3N4Nanosheets, two-dimensional g-C3N4Nano sheet film, preparation method and application
CN112897484B (en) * 2021-01-14 2023-10-31 华南理工大学 Defect-free g-C 3 N 4 Nanoplatelets, two-dimensional g-C 3 N 4 Nanosheet film and preparation method and application thereof

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