CN104368383A - Preparation method of fluffy carbon nitride nano catalytic material with high catalytic activity - Google Patents
Preparation method of fluffy carbon nitride nano catalytic material with high catalytic activity Download PDFInfo
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- CN104368383A CN104368383A CN201310348730.6A CN201310348730A CN104368383A CN 104368383 A CN104368383 A CN 104368383A CN 201310348730 A CN201310348730 A CN 201310348730A CN 104368383 A CN104368383 A CN 104368383A
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- 239000000463 material Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 230000003197 catalytic effect Effects 0.000 title claims description 19
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title abstract description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 32
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000004202 carbamide Substances 0.000 claims abstract description 17
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 13
- 229910052799 carbon Inorganic materials 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 13
- 238000005245 sintering Methods 0.000 claims description 5
- 239000003708 ampul Substances 0.000 claims description 3
- 229910052573 porcelain Inorganic materials 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 abstract description 21
- 239000010439 graphite Substances 0.000 abstract description 21
- 238000000034 method Methods 0.000 abstract description 15
- 239000002994 raw material Substances 0.000 abstract description 13
- 238000011160 research Methods 0.000 abstract description 6
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 abstract description 5
- 239000002086 nanomaterial Substances 0.000 abstract description 5
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 238000007796 conventional method Methods 0.000 abstract description 2
- 238000000197 pyrolysis Methods 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 abstract 1
- 230000003287 optical effect Effects 0.000 abstract 1
- 238000007146 photocatalysis Methods 0.000 abstract 1
- 230000001699 photocatalysis Effects 0.000 abstract 1
- 229920000877 Melamine resin Polymers 0.000 description 8
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 8
- 230000015556 catabolic process Effects 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 239000000975 dye Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000205 computational method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 239000010919 dye waste Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- YSRVJVDFHZYRPA-UHFFFAOYSA-N melem Chemical compound NC1=NC(N23)=NC(N)=NC2=NC(N)=NC3=N1 YSRVJVDFHZYRPA-UHFFFAOYSA-N 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 230000007281 self degradation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000007704 wet chemistry method Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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Abstract
The graphite-phase carbon nitride has the excellent properties of carbon-nitrogen materials, and moreover the energy gap of the graphite-phase carbon nitride is very small, so that the graphite-phase carbon nitride has a great application potential in the photo catalysis field. At present, there are a plurality of preparation methods that can prepare the graphite carbon nitride from a plurality of materials, while the crystal size of the C3N4 prepared by common methods is big, C3N4 with a micro-nano size is difficult to prepare, and thus the applications of C3N4 in the fields of catalysis, photoconduction, and optical waveguide are limited, so how to prepare controllable C3N4 with multiple morphologies and a micro-nano structure has become an important and difficult research in the material field. In the provided preparation method, cheap urea is taken as the raw material to prepare C3N4, the urea is directly subjected to high temperature pyrolysis, and through controlling the heating speed in different heating areas, fluffy graphite-phase carbon nitride can be produced. The volume of the prepared carbon nitride is 5 times as big as that of carbon nitride which is prepared through a conventional method, and the provided carbon nitride has a sheet structure.
Description
Technical field
The invention belongs to technical field prepared by nano material, in particular to a kind of preparation method of azotized carbon nano catalysis material of high catalytic activity, the method, mainly through the control to thermograde, successfully prepares the graphite phase carbon nitride of fluffy high catalytic activity.
Background technology
Since Liu and M.L.Cohen in 1989 foretells in theory, β-C
3n
4may be a kind of novel superhard material also harder than diamond
[1,2].Tete in 1996 etc. then adopt first principle pseudo potential computational methods to calculate the theoretical construct of carbonitride, think that this compound may exist five kinds of thing phases, that is: α phase, β phase, Emission in Cubic, class Emission in Cubic and class graphite-phase
[3].Class graphite phase carbon nitride is gained the name because having the layer structure of similar graphite, is therefore also called graphite phase carbon nitride, be these five kinds of things mutually in the most stable crystalline phase.So people start the research boom to this New Type of Carbon nitrogen material.Domestic and international thousands of laboratories all attracted in this research, and they utilize known various attainable experimental technique to synthesize this material.People's reported first such as Wang in 2009, successful pyrolysis cyanamide prepares graphite-phase C
3n
4and (λ >420nm) hydrogen production by water decomposition under visible light
[4].After this, prelude has been pulled open in the relevant light-catalysed research of carbonitride in succession.
The preparation method of graphite phase carbon nitride mainly contains two kinds: solvent-thermal process method and high-temperature polymerization.Solvent-thermal process method refers in airtight container, solvent is as reaction medium, under the condition of high temperature and high pressure (pressure produced when solvent becomes steam), prepare the heterogeneous synthetic method of one of nano material, be one of wet chemistry method preparing powder.In recent years, this synthetic method is widely used, 1999, and Montigaud etc. take melamine as raw material, with NH
2nH
2for solvent, be 3GPa at pressure, synthesize the carbonitride of graphite-phase under condition between temperature 800 DEG C-850 DEG C
[5].The people such as Bai, under the prerequisite not using any catalyst, adopt NH
4c1 and CCl
4in 400 DEG C of solvent thermal reactions, obtain graphite phase carbon nitride nanocrystalline, the average grain size that XRD and TEM provides is about 11nm, and has a small amount of monocrystalline to produce
[6].
High-temperature polymerization prepares a kind of comparatively conventional method of carbonitride.Because cyanamide at high temperature can polymerization reaction take place, polycondensation is dicyandiamide successively, and melamine, melem, finally obtains carbon nitride product.Cyanamide is heated between 400 DEG C-600 DEG C by Wang etc., and is incubated the carbonitride that 4h synthesis obtains graphite-phase.The people such as Zou utilize a kind of more cheap raw material melamine to be heated to 500 DEG C respectively at ambient pressure, 520 DEG C, 550 DEG C and 580 DEG C of constant temperature 2h also obtain graphite phase carbon nitride, and the carbonitride prepared by finding has good performance in light degradation methylene blue
[4].The people such as Niu utilize dicyandiamide two-step method to prepare the laminar structured of graphite phase carbon nitride, and obtain having higher catalytic efficiency than body phase graphite phase carbon nitride
[7].The people such as Zou with more cheap urea for raw material TiO
2for catalyst utilizes, under the condition of air, prepare graphite phase carbon nitride
[8].But, the graphite-phase C that ordinary sinter method is prepared
3n
4sample has larger crystallite dimension, the C of micro nano structure
3n
4more difficult preparation, therefore, this significantly limit graphite-phase C
3n
4in the application in the fields such as catalytic field, photoconductive field and fiber waveguide.Thus prepare controlled different morphologies and there is the graphite-phase C of micro-nano structure
3n
4become the Focal point and difficult point of this investigation of materials.
In recent years, lot of domestic and international group all expands exploration to novel graphite phase carbon-nitrogen material and research, and the preparation of material is the only way from basic research to practical application, is the important channel of improving quality of materials and reducing costs.Can the discovery realizing material structure and performance design and new material obtain practical application, depends on preparation technology and cost.Up to the present, synthesized this Novel photo material although there are many reports to claim, main also in the laboratory exploratory stage.Can say, remain focus in face of researcher and a difficult problem with method a large amount of synthesis of high purity New Type of Carbon nitrogen material material that is simple, low cost.
Bibliography:
[1]M.L.Cohen,Calculation of bulk moduli of diamond and zinc-blende solids,Phys.Rev.B1985,32,7988-7991
[2]A.Y.Liu,M.L.Cohen,Prediction of new low compressibility solids,Science.1989,245,841-842
[3]D.M.Teter,R.J.Hemley,Low-compressibility carbon nitrid,Science.1996,271,53-55
[4]X.C.Wang,K.Maeda,A.Thomas,K.Takanabe,G.Xin,J.M.Carlsson,K.Domen,M.Antonietti,Ametal-free polymeric photocatalyst for hydrogen production from water under visible light,Nat.Mater.2009,8,76–80
[5]H.Montigaud,B.Tanguy,G.Demazeau,I.Alves,M.Birot,J.Dunogues,Solvothermalsynthesis of the graphitic form of C
3N
4as macroscopic Sample.Diam.Relat.Mater.1999,8,1707-1710
[6]Y.J.Bai,B.Lu,Z.G.Liu,L.Li,D.L.Cui,X.G.Xu,Q.L.Wang,Solvothermal preparation ofgraphite-like C
3N
4nanocrystals,Crvst.Growth.2003,247,505-508
[7]P.Niu,L.L.Zhang,G.Liu,H.M.Cheng,Graphene-like carbon nitride nanosheets forimproved photocatalytic activities,Adv.Funct.Mater.2012,22,4763-4770
[8]X.X.Zou,G.D.Li,Y.N.Wang,J.Zhao,C.Yan,M.Y.Guo,L.Li,J.S.Chen,Directconversion of urea into graphitic carbon nitride over mesoporous TiO
2spheres under mildcondition,Chem.Commun.2011,47,1066-1068
Summary of the invention
The object of the invention is a large amount of preparation methods of the graphite phase carbon nitride material of openly a kind of fluffy high catalytic activity, the method is simple, and repetitive rate is high.
The object of the present invention is achieved like this, and the method adopts cheap urea to do raw material, and in the tube furnace of length 1 meter, diameter 25mm, carry out high-temperature heating according to certain thermograde, obtain a large amount of flake graphite phase carbon nitride material, its concrete preparation method is as follows:
Analytically pure urea raw material is put in porcelain boat, then the drying box being warmed up to 80 DEG C is put into, carry out drying, drying time is 12 hours, after drying terminates, urea raw material taken out and put into the zone line of quartz ampoule, and sinter in tube furnace, sintering temperature before 100 DEG C with 1.5 DEG C/min ramp, then 200 DEG C are warmed up to 1 DEG C/min, 450 DEG C are warmed up to 2 DEG C/min, 550 DEG C are warmed up to 1 DEG C/min, finally under the condition of 550 DEG C, be incubated 2 hours, to be cooled to room temperature, namely the azotized carbon nano catalysis material of fluffy high catalytic activity is obtained.
The present invention has the following advantages and good effect:
1, the urea low in raw material price that the present invention is used, only need simple dry process in early stage, a large amount of graphite phase carbon nitride materials is synthesized by the thermograde controlling high temperature sintering, this material has significantly absorption and catalytic action to rhdamine B, and by carrying out XRD detection to it after the circulation absorption of three times and catalytic process, find that catalyst of the present invention has good chemical stability.
2, simple, the environmental protection of method of the present invention, low cost; Detect rapid, repeatable high; Industrial organic dye waste water degraded detection is had broad application prospects.
3, the present invention is prepared by physical method, can obtain a large amount of product, for the large-scale production of new function carbon-nitrogen material and application lay the foundation.
Accompanying drawing explanation
Fig. 1 to be the present invention with urea be 50mg graphite phase carbon nitride that raw material prepare and take melamine as the azotized carbon nano catalysis material volume vs figure of the 50mg that raw material are prepared.
Fig. 2 is the SEM figure of the graphite phase carbon nitride that the present invention prepares.
Fig. 3 is that the graphite phase carbon nitride nanometer sheet prepared of the present invention and the body phase graphite phase carbon nitride prepared with melamine are to rhodamine catalytic activity comparison diagram under visible light.
Fig. 4 is the XRD comparison diagram of the azotized carbon nano catalysis material prepared of the present invention and the azotized carbon nano catalysis material after repeatedly catalytic reaction.
Detailed description of the invention
Analytically pure for 50mg urea raw material is put in porcelain boat, then puts into the drying box being warmed up to 80 DEG C, carry out drying, drying time is 12 hours, after drying terminates, urea taken out and put into the zone line of quartz ampoule (diameter 25mm, long 1000mm), and sintering in tube furnace.Sintering temperature with 1.5 DEG C/min ramp, was then warmed up to 200 DEG C with 1 DEG C/min before 100 DEG C, was warmed up to 450 DEG C with 2 DEG C/min, was warmed up to 550 DEG C with 1 DEG C/min, finally under the condition of 550 DEG C, was incubated 2 hours.To be cooled to room temperature, the azotized carbon nano catalysis material of fluffy high catalytic activity can be collected, do not need further process.
Conclusion: be the 50mg graphite phase carbon nitride prepared for raw material with melamine (left side) and urea (right side) respectively shown in Fig. 1, find to take urea as sample that raw material are prepared by picture contrast is 5 times that prepare 50mg sample volume of melamine under the quality of same 50mg, illustrate that the sample prepared with urea passes through the control to thermograde, make sample more fluffy, not easily reunite.
Figure 2 shows that the SEM image of the sample prepared with urea, under SEM image, present fluffy state by the known sample of image viewing, can be observed sample by the SEM image of high power and present curling laminated structure, and sheet has hole not of uniform size.
Figure 3 shows that the graphitic nitralloy carbon (u-g-C that urea is prepared
3n
4) the body phase graphitic nitralloy carbon (m-g-C for preparing with melamine
3n
4) contrast of catalytic performance and catalyst-free rhodamine from degraded (blank).Sample u-g-C in the middle of process
3n
4have the adsorption effect to dyestuff higher than 60% and catalytic effect is stable and efficient, finally 180 minutes time, dyestuff is degradable.Carry out the sample m-g-C of contrast experiment therewith
3n
4adsorption effect only has about 35% and catalytic effect is unstable, and especially when dye strength is low, catalytic degradation is slow.. blank room catalyst experiment shows that dyestuff self degradation is under visible light negligible.
Figure 4 shows that sample u-g-C
3n
4by contrast, the XRD image of (Fresh) (Used) afterwards before catalytic reaction, finds that the peak position of sample XRD image of sample after catalytic reaction does not change, shows that sample has outstanding stability.
The degradation rate of the present invention's photocatalytic degradation rhodamine B under xenon lamp simulated visible light source assesses the activity of graphite phase carbon nitride, and when the reaction time is 180min, its degradation rate reaches 97%.
Claims (1)
1. a preparation method for the azotized carbon nano catalysis material of fluffy high catalytic activity, is characterized in that:
Preparation method is as follows:
Analytically pure urea sample is put in porcelain boat, then the drying box being warmed up to 80 DEG C is put into, carry out drying, drying time is 12 hours, after drying terminates, urea taken out and put into the zone line of quartz ampoule, and sinter in tube furnace, sintering temperature before 100 DEG C with 1.5 DEG C/min ramp, then 200 DEG C are warmed up to 1 DEG C/min, 450 DEG C are warmed up to 2 DEG C/min, 550 DEG C are warmed up to 1 DEG C/min, finally under the condition of 550 DEG C, be incubated 2 hours, to be cooled to room temperature, namely the azotized carbon nano catalysis material of fluffy high catalytic activity is obtained.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105152147A (en) * | 2015-08-28 | 2015-12-16 | 郑州大学 | Method for preparation of water-soluble luminous graphite-phase carbon nitride nano kelp |
| CN105289684A (en) * | 2015-09-29 | 2016-02-03 | 北京化工大学 | Method for preparing porous flake-like graphite phase carbon nitride on large scale, and application thereof |
| CN106145069A (en) * | 2016-06-29 | 2016-11-23 | 湖南大学 | Graphite mould C3n4the preparation method of material, graphite mould C3n4material and application thereof |
| CN106552660A (en) * | 2016-10-24 | 2017-04-05 | 广西民族大学 | A kind of high-specific surface area g C3N4The preparation method of photocatalyst |
| CN110560127A (en) * | 2019-09-09 | 2019-12-13 | 辽宁石油化工大学 | Preparation method of graphite phase carbon nitride with large specific surface area |
| CN110624594A (en) * | 2019-10-10 | 2019-12-31 | 吉林师范大学 | Magnetic Fe3O4/ZnO/g-C3N4Composite photocatalyst and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105152147A (en) * | 2015-08-28 | 2015-12-16 | 郑州大学 | Method for preparation of water-soluble luminous graphite-phase carbon nitride nano kelp |
| CN105289684A (en) * | 2015-09-29 | 2016-02-03 | 北京化工大学 | Method for preparing porous flake-like graphite phase carbon nitride on large scale, and application thereof |
| CN106145069A (en) * | 2016-06-29 | 2016-11-23 | 湖南大学 | Graphite mould C3n4the preparation method of material, graphite mould C3n4material and application thereof |
| CN106552660A (en) * | 2016-10-24 | 2017-04-05 | 广西民族大学 | A kind of high-specific surface area g C3N4The preparation method of photocatalyst |
| CN106552660B (en) * | 2016-10-24 | 2020-02-04 | 广西民族大学 | g-C with high specific surface area3N4Method for preparing photocatalyst |
| CN110560127A (en) * | 2019-09-09 | 2019-12-13 | 辽宁石油化工大学 | Preparation method of graphite phase carbon nitride with large specific surface area |
| CN110624594A (en) * | 2019-10-10 | 2019-12-31 | 吉林师范大学 | Magnetic Fe3O4/ZnO/g-C3N4Composite photocatalyst and preparation method thereof |
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