CN103254200A - C3N4 nanosheet with molecular-scale thickness as well as preparation method and application thereof - Google Patents

C3N4 nanosheet with molecular-scale thickness as well as preparation method and application thereof Download PDF

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CN103254200A
CN103254200A CN2013101906786A CN201310190678A CN103254200A CN 103254200 A CN103254200 A CN 103254200A CN 2013101906786 A CN2013101906786 A CN 2013101906786A CN 201310190678 A CN201310190678 A CN 201310190678A CN 103254200 A CN103254200 A CN 103254200A
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nanometer sheet
molecular level
preparation
level thickness
nanosheet
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CN103254200B (en
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梁诗景
林秋燕
毕进红
刘明华
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Fuzhou University
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Abstract

The invention discloses a C3N4 nanosheet with a molecular-scale thickness as well as a preparation method and an application thereof, which belong to the technical fields of material preparation and photocatalysis. The C3N4 nanosheet photocatalyst with a molecular-scale thickness disclosed by the invention is prepared in a water/ethanol mixed system via an ultrasonic treatment-stirring combination method. The preparation method of the catalyst comprises the following two steps of: step 1, synthesising a bulk-phase C3N4 precursor via a solid-phase thermal polymerization method; and step 2, stripping via ultrasonic treatment-stirring combination to prepare the C3N4 nanosheet. The C3N4 nanosheet photocatalyst prepared by the preparation method is high in specific surface area and photon-generated carrier separation efficiency, capable of efficiently degrading organic pollutants, and particularly efficiently decolouring printing and dyeing wastewater, and high in activity in the aspects of hydrogen production from photocatalytic water splitting and photocatalytic selective oxidation for alcohols simultaneously. The catalyst is simple in preparation process, low in cost, green and environment-friendly in production process, high in stability, capable of meeting actual production needs, and high in application potential.

Description

A kind of C of molecular level thickness 3N 4Nanometer sheet and its preparation method and application
Technical field
The invention belongs to material preparation and photocatalysis technology field, be specifically related to a kind of C of molecular level thickness 3N 4Nanometer sheet and the preparation method and application in water/ethanol mixed system thereof.
Background technology
Photocatalysis technology since its reaction thoroughly, reaction conditions is gentle, have advantage such as redox ability concurrently, develops rapidly in recent years to a kind of sun power that utilizes carries out the new technology that environmental purification and the energy transform, and becomes research focus of greatest concern at present.But still there is the low key core problem in science that waits of quantum yield in conductor photocatalysis at present, makes its development be subjected to very big restriction.And the key that solves still is on the photocatalyst, therefore, Chinese scholars is being done a large amount of exploration work aspect the photo-quantum efficiency that improves photocatalyst: as, done a large amount of explorations and obtained certain progress at aspects such as the modification of titanium dioxide optical catalyst, modifications, simultaneously the also novel non-titanium dioxide optical catalyst of active development.Though these research work have promoted the photochemical catalysis development greatly, photocatalyst increases for its quantum yield of specific reaction, and activity of such catalysts and stability are still undesirable in the practical application.Therefore seek and development of new photocatalyst efficiently, remain at present and even the research focus in the interior photocatalysis field of quite a long period from now on.
In the various new photocatalyst materials that developed, nonmetal organic polymer semi-conductor--graphite phase carbon nitride because of its raw material sources extensively, stability is high, have suitable energy band structure, to the up-and-coming photocatalyst of a class that is considered to such as visible light-responded, be applied in the conversion of visible light photocatalysis hydrogen production by water decomposition and organism, realize that sun power is to the conversion of chemical energy.Yet the carbonitride photocatalyst of the body phase of having reported exists some intrinsic defectives, makes its photocatalytic activity lower.At present, the carbonitride of body phase mainly is that the solid-phase synthesis by high temperature, high pressure prepares, and this makes prepared sample have a large amount of boundary defects, has caused that the interface of photo-generated carrier is compound serious.Though some investigators by the exploitation mesoporous carbonitride ( Energy Environ. Sci. 2011,4,4668-4674), nonmetal doping modification (Angew. Chem. Int. Ed.2010 , 49, 441-444; J. Am. Chem. Soc.2010 , 132, 11642-11648) changes energy band structure and its absorbing properties of enhancing of carbonitride, and then improve its photocatalytic activity, but the quantum yield of carbonitride is still quite low.
Studies show that, the two-dimensional nano sheet of molecular level thickness (0.5-3 nm) is because quantum size effect and surface tissue effect have high electric conductivity and photoresponse, photo-generated carrier separation rate height, the ultrahigh activity site exposes ratio (near 100%), big specific surface area.Therefore, if the two-dimensional nano sheet of carbonitride photocatalyst exploitation prepared composition sub level thickness will effectively can be solved the problem that above-mentioned carbonitride photocatalyst exists, improve its photocatalysis performance greatly.Based on this thinking, had been found that some carbonitride two-dimensional nano sheets show excellent photocatalysis activity aspect photolysis water hydrogen, as Liu etc. ( Adv. Funct. Mater.2012, 22, 4763-4770) utilize the method for hot etching to prepare carbonitride two-dimensional nano sheet, its photodissociation aquatic products hydrogen performance has improved 4.4 times, and the life-span of 70% photo-generated carrier obtains prolonging.Though this method technology is simple, also has a lot of problems, and is not strong as controllability, the nanometer sheet of preparation is thicker, productive rate very low (<6%).Xie( J. Am. Chem. Soc. 2012,135,18-21) and Yang(Adv. Mater.2013, 25, 2452-2456) wait the employing liquid phase method, in single water, Virahol, methane amide, acetone equal solvent, the body phase carbon nitride of commodity is made carbonitride two-dimensional nano sheet.The visible light photodissociation outlet capacity of prepared azotized carbon nano sheet is effectively strengthened.Though the method that they grow up can prepare the azotized carbon nano sheet, key issue such as the nanometer sheet suspension liquid concentration for preparing low (≤0.15 mg/mL), lamellar spacing big (〉=3 nm), productive rate are low is still unresolved.
Summary of the invention
The object of the present invention is to provide a kind of C of molecular level thickness 3N 4Nanometer sheet and its preparation method and application solves preparation C at present 3N 4Low, the problems such as suspension liquid concentration is too low, the nanometer sheet productive rate is low, toxic organic solvent use of charge stripping efficiency that nanometer sheet exists.The C of molecular level thickness of the present invention 3N 4Nanometer sheet, the separation efficiency height of photo-generated carrier all shows very high photocatalytic activity in fields such as photochemical catalysis wastewater treatment, photodissociation water and selective oxidation alcohols.This preparation method is simple, the production process environmental protection, do not need cost and complex equipment, synthesis condition gentleness, and cost is low, and catalyst stability is good, has bigger application potential.
For achieving the above object, the present invention adopts following technical scheme:
A kind of C of molecular level thickness 3N 4Nanometer sheet is graphite phase C 3N 4Organic polymer semi-conductor, its specific surface area are 50-300 m 2/ g, sheet thickness are 0.5-3 nm, and length and width are 100-2000 nm, and energy gap can effectively be separated photo-generated carrier greater than 2.8 eV.
The C for preparing aforesaid molecular level thickness 3N 4The method of nanometer sheet is the C of the stratiform that obtains with the trimeric cyanamide thermopolymerization 3N 4Be precursor, in water/ethanol mixed system by ultrasonic-stir the method combine and prepare the C that concentration is the molecular level thickness of 0.3-3 mg/mL 3N 4The nanometer sheet suspension liquid obtains C by centrifugal means at last 3N 4The nanometer sheet pressed powder.May further comprise the steps: (1) gets the trimeric cyanamide of 1-20 g in crucible, places 550 ℃ of calcinings of retort furnace, 4 h, the stratiform C of preparation body phase 3N 4Presoma; (2) get the stratiform C of 0.2-1 g body phase 3N 4Presoma is put into 500 mL beakers, adds deionized water and the ethanol of 10-205 mL, the first ultrasonication 1-6 h then of 20-150 mL in the beaker, 0.5-24 h is stirred in the back, ultrasonication 1-6 h is last centrifugal with 3000 rev/mins rotating speed again, removes the C of stratiform 3N 4Precipitate, obtain the C of the molecular level thickness of high density 3N 4The nanometer sheet suspension liquid, the last C that under 10000 rev/mins of high speed centrifugations, makes molecular level thickness 3N 4Nanometer sheet.
The C of described molecular level thickness 3N 4Nanometer sheet is used for degradation of contaminant as photocatalyst, particularly to the efficient decolorizing of dyeing waste water; Or be applied to photolysis water hydrogen and photocatalysis to selectively oxidize alcohols.
Remarkable advantage of the present invention is:
(1) the present invention utilizes water/alcohol mixed solvent first, by the stripping means that ultrasonication-stirring combines, prepares the C of the molecular level thickness of high density 3N 4Nanometer sheet, prepared nanometer sheet has big specific surface area, and photo-generated carrier such as can effectively separate at characteristics.
(2) compare with the method for bibliographical information, the solvent environment close friend that the present invention uses, the nanometer sheet suspension liquid concentration height for preparing, nanometer sheet productive rate height is avoided the use of poisonous organic solvent, and the nanometer sheet size that makes is even, adjustable size, and thickness is littler.
(3) whole technological process of the present invention is simple and easy to control, the production process environmental protection, and energy consumption is low, does not need cost and complex equipment, synthesis condition gentleness, and cost is low, and catalyst stability is good, has bigger application potential.
(4) C of molecular level thickness 3N 4Nanometer sheet is photocatalysis treatment dyeing waste water, photodissociation aquatic products hydrogen and selective oxidation alcohols etc. efficiently, has good activity stability simultaneously.The photocatalyst renewable is strong in the light-catalyzed reaction system, and the repeating utilization factor height has very high practical value and application prospect.
Description of drawings
Fig. 1 is the C of molecular level thickness 3N 4The preparation flow synoptic diagram of nanometer sheet.
Fig. 2 is the C of the molecular level thickness of embodiment 1 gained 3N 4The X-ray powder diffraction figure (XRD) of nanometer sheet.
Fig. 3 is the C of the molecular level thickness of embodiment 1 gained 3N 4The atomic power flying-spot microscope figure (AFM) of nanometer sheet.
Fig. 4 is the C of the molecular level thickness of embodiment 1 gained 3N 4The C of nanometer sheet, stratiform 3N 4With commodity TiO 2Degradation effect comparison diagram to RhB.
Embodiment
Below be several embodiments of the present invention, further specify the present invention, but the present invention is not limited only to this.
Embodiment 1
At first be body phase C 3N 4The preparation of presoma takes by weighing the trimeric cyanamide of 15 g in crucible, places 550 ℃ of calcinings of retort furnace, 4 h, and is standby after grinding; In beaker with the body phase C of 0.5 g 3N 4Presoma adds the deionized water of 90 mL and the ethanol of 105 mL, then beaker is placed ultrasonic 4 h of ultrasonic machine, after place agitator to stir 14 h in beaker, ultrasonic 4 h again, obtain suspension liquid, centrifugal under 3000 rev/mins rotating speed, remove precipitation, last again under 10000 rev/mins high speed centrifugation, can obtain the C of molecular level thickness 3N 4The nanometer sheet photocatalyst.
Embodiment 2
At first be body phase C 3N 4The preparation of presoma takes by weighing the trimeric cyanamide of 10 g in crucible, places 550 ℃ of calcinings of retort furnace, 4 h, and is standby after grinding; In beaker with the body phase C of 0.3 g 3N 4Presoma adds the deionized water of 60 mL and the ethanol of 70 mL, then beaker is placed ultrasonic 4 h of ultrasonic machine, after place agitator to stir 5 h in beaker, ultrasonic 4 h obtain suspension liquid again, centrifugal under 3000 rev/mins rotating speed, remove precipitation, last again under 10000 rev/mins high speed centrifugation, can obtain the C of molecular level thickness 3N 4The nanometer sheet photocatalyst.
Embodiment 3
At first be body phase C 3N 4The preparation of presoma takes by weighing the trimeric cyanamide of 15 g in crucible, places 550 ℃ of calcinings of retort furnace, 4 h, and is standby after grinding; In beaker with the body phase C of 1.0 g 3N 4Presoma adds the deionized water of 90 mL and the ethanol of 105 mL, then beaker is placed ultrasonic 5 h of ultrasonic machine, after place agitator to stir 14 h in beaker, ultrasonic 3 h again, obtain suspension liquid, centrifugal under 3000 rev/mins rotating speed, remove precipitation, last again under 10000 rev/mins high speed centrifugation, can obtain the C of molecular level thickness 3N 4Nanometer sheet glue photocatalyst.
From Fig. 2, can find the C of molecular level thickness 3N 4The XRD diffraction peak of nanometer sheet significantly weakens even disappears, and the C of body phase is described 3N 4The nanometer sheet of successful coverlet molecular layers thick.From Fig. 3, can find the C of prepared molecular level thickness 3N 4The thickness of nanometer sheet is about 1 nm.
The C of molecular level thickness 3N 4The test of nanometer sheet photocatalysis performance characterizes by the degraded to RhB under the xenon lamp irradiation.Adopt batch reactor, the RhB that is about 10 ppm with concentration is reaction substrate.As light source, catalyst consumption is 0.04 g with the xenon lamp of 300 W.Absorption in advance makes the RhB illumination of turning on light after adsorption-desorption balance on the catalyzer before the reaction of turning on light.As can be seen from Figure 4, behind the illumination 70min that turns on light, the C of molecular level thickness 3N 4The nanometer sheet photocatalyst to the degradation rate of RhB up to 100%.By contrast, body phase C 3N 4Catalyzer degradation efficiency to RhB in 90 min light application times is low.Simultaneously can obviously find out more also that with the titanium dioxide of commodity the azotized carbon nano piece performance of the molecular level thickness that the present invention prepares is more excellent.
The above only is preferred embodiment of the present invention, and all equalizations of doing according to the present patent application claim change and modify, and all should belong to covering scope of the present invention.

Claims (5)

1. the C of a molecular level thickness 3N 4Nanometer sheet is characterized in that: described C 3N 4Nanometer sheet is graphite phase C 3N 4The organic polymer semi-conductor.
2. the C of molecular level thickness according to claim 1 3N 4Nanometer sheet is characterized in that: described C 3N 4The specific surface area of nanometer sheet is 50-300 m 2/ g, sheet thickness are 0.5-3 nm, and length and width are 100-2000 nm, and energy gap can effectively be separated photo-generated carrier greater than 2.8 eV.
3. C who prepares molecular level thickness as claimed in claim 1 3N 4The method of nanometer sheet is characterized in that: the C of the stratiform that obtains with the trimeric cyanamide thermopolymerization 3N 4Be precursor, in water/ethanol mixed system by ultrasonic-stir the method combine and prepare the C that concentration is the molecular level thickness of 0.3-3 mg/mL 3N 4The nanometer sheet suspension liquid obtains C by centrifugal means at last 3N 4The nanometer sheet pressed powder.
4. the C of molecular level thickness according to claim 3 3N 4The preparation method of nanometer sheet is characterized in that: may further comprise the steps:
(1) trimeric cyanamide of getting 1-20 g places 550 ℃ of calcinings of retort furnace, 4 h in crucible, the stratiform C of preparation body phase 3N 4Presoma;
(2) get the stratiform C of 0.2-1 g body phase 3N 4Presoma is put into 500 mL beakers, adds deionized water and the ethanol of 10-205 mL, the first ultrasonication 1-6 h then of 20-150 mL in the beaker, 0.5-24 h is stirred in the back, ultrasonication 1-6 h is last centrifugal with 3000 rev/mins rotating speed again, removes the C of stratiform 3N 4Precipitate, obtain the C of the molecular level thickness of high density 3N 4The nanometer sheet suspension liquid, the last C that under 10000 rev/mins of high speed centrifugations, makes molecular level thickness 3N 4Nanometer sheet.
5. the C of a molecular level thickness as claimed in claim 1 3N 4The application of nanometer sheet is characterized in that: described C 3N 4Nanometer sheet is used for degradation of contaminant as photocatalyst, particularly to the efficient decolorizing of dyeing waste water; Or be applied to photolysis water hydrogen and photocatalysis to selectively oxidize alcohols.
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CN104401948A (en) * 2014-11-17 2015-03-11 长安大学 Preparation method for single-layer graphite-type carbon nitride nanosheet solution
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CN104525258A (en) * 2015-01-07 2015-04-22 福州大学 Covalence triazine organic polymer visible-light-driven photocatalyst and preparing method and application thereof
CN104617306A (en) * 2015-01-17 2015-05-13 哈尔滨工业大学 Platinum-based catalyst carrier of proton exchange membrane fuel cell (PEMFC) and preparation method of platinum-based catalyst carrier
CN105925954A (en) * 2016-05-27 2016-09-07 清华大学 Preparation method of semiconductor carbon nitride films
CN106268897A (en) * 2015-06-02 2017-01-04 中国科学院金属研究所 A kind of preparation method of the decrystallized graphite state carbonitride of optical absorption edge significantly red shift
CN107098323A (en) * 2017-04-25 2017-08-29 中南大学 A kind of g C3N4Nanometer sheet and preparation method and application
CN108408700A (en) * 2018-04-04 2018-08-17 南京工业大学 A kind of method that non-solvent in-situ carburization prepares blue-fluorescence carbon nitrogen nanometer sheet on a large scale
CN108470647A (en) * 2018-05-08 2018-08-31 上海应用技术大学 A kind of ultracapacitor PEDOT:PSS@g-C3N4Combination electrode material and preparation method thereof
CN108772085A (en) * 2018-03-13 2018-11-09 合肥工业大学 A kind of preparation method of broad stopband carbon nitrogen polymer
CN109286009A (en) * 2018-09-25 2019-01-29 陕西科技大学 A kind of preparation method of nanometer sheet self assembled three-dimensional nano flower artificial gold/graphitization carbonitride lithium ion battery negative material
CN112717973A (en) * 2020-11-16 2021-04-30 中北大学 Preparation of rod-like g-C by microwave hydrothermal method3N4Method and application of nanosheet
CN113321818A (en) * 2021-05-11 2021-08-31 中山大学 Composite hydrogel and preparation method and application thereof

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CN103787290B (en) * 2014-01-16 2016-01-20 大连民族学院 Based on intercalation configuration C 3n 4nanometer sheet high-performance humidity-sensitive material and preparation method
CN103787290A (en) * 2014-01-16 2014-05-14 大连民族学院 High-performance humidity-sensitive material based on C3N4 nanosheet having intercalated structure and preparation method of high-performance humidity-sensitive material
CN104401948A (en) * 2014-11-17 2015-03-11 长安大学 Preparation method for single-layer graphite-type carbon nitride nanosheet solution
CN104399509A (en) * 2014-12-08 2015-03-11 福州大学 Hydrogen-free precursor synthesized carbon nitride photocatalyst
CN104525258A (en) * 2015-01-07 2015-04-22 福州大学 Covalence triazine organic polymer visible-light-driven photocatalyst and preparing method and application thereof
CN104525258B (en) * 2015-01-07 2016-06-29 福州大学 A kind of covalent triazine organic polymer visible light catalyst and preparation thereof and application
CN104617306B (en) * 2015-01-17 2017-04-05 哈尔滨工业大学 One proton exchanging film fuel battery platinum based catalyst carrier and preparation method thereof
CN104617306A (en) * 2015-01-17 2015-05-13 哈尔滨工业大学 Platinum-based catalyst carrier of proton exchange membrane fuel cell (PEMFC) and preparation method of platinum-based catalyst carrier
CN106268897B (en) * 2015-06-02 2019-03-29 中国科学院金属研究所 A kind of preparation method of the optical absorption edge substantially decrystallized graphite state carbonitride of red shift
CN106268897A (en) * 2015-06-02 2017-01-04 中国科学院金属研究所 A kind of preparation method of the decrystallized graphite state carbonitride of optical absorption edge significantly red shift
CN105925954B (en) * 2016-05-27 2020-04-14 清华大学 Preparation method of semiconductor carbon nitride film
CN105925954A (en) * 2016-05-27 2016-09-07 清华大学 Preparation method of semiconductor carbon nitride films
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
CN107098323A (en) * 2017-04-25 2017-08-29 中南大学 A kind of g C3N4Nanometer sheet and preparation method and application
CN108772085A (en) * 2018-03-13 2018-11-09 合肥工业大学 A kind of preparation method of broad stopband carbon nitrogen polymer
CN108772085B (en) * 2018-03-13 2021-02-23 合肥工业大学 Preparation method of wide-bandgap carbon-nitrogen polymer
CN108408700A (en) * 2018-04-04 2018-08-17 南京工业大学 A kind of method that non-solvent in-situ carburization prepares blue-fluorescence carbon nitrogen nanometer sheet on a large scale
CN108470647A (en) * 2018-05-08 2018-08-31 上海应用技术大学 A kind of ultracapacitor PEDOT:PSS@g-C3N4Combination electrode material and preparation method thereof
CN108470647B (en) * 2018-05-08 2019-07-23 上海应用技术大学 A kind of supercapacitor combination electrode material and preparation method thereof
CN109286009A (en) * 2018-09-25 2019-01-29 陕西科技大学 A kind of preparation method of nanometer sheet self assembled three-dimensional nano flower artificial gold/graphitization carbonitride lithium ion battery negative material
CN109286009B (en) * 2018-09-25 2021-06-08 陕西科技大学 Preparation method of nano-sheet self-assembled three-dimensional nano-flower tin sulfide/graphitized carbon nitride lithium ion battery cathode material
CN112717973A (en) * 2020-11-16 2021-04-30 中北大学 Preparation of rod-like g-C by microwave hydrothermal method3N4Method and application of nanosheet
CN113321818A (en) * 2021-05-11 2021-08-31 中山大学 Composite hydrogel and preparation method and application thereof

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