CN103785434A - g-C3N4 nanosheet/CdS composite visible-light-driven photocatalyst - Google Patents

g-C3N4 nanosheet/CdS composite visible-light-driven photocatalyst Download PDF

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CN103785434A
CN103785434A CN201410082715.6A CN201410082715A CN103785434A CN 103785434 A CN103785434 A CN 103785434A CN 201410082715 A CN201410082715 A CN 201410082715A CN 103785434 A CN103785434 A CN 103785434A
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cds
nanometer sheet
catalyst
visible light
cds composite
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CN103785434B (en
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刘平
卢美良
戴文新
付贤智
裴增夏
翁孙贤
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Fuzhou University
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Abstract

The invention discloses a g-C3N4 nanosheet/CdS composite visible-light-driven photocatalyst and a preparing method and application thereof and belongs to the technical field of material preparation and photocatalysis. The catalyst is directly obtained with the solvothermal method by taking two-dimensional ultra-thin g-C3N4 nanosheets as the matrix, cadmium acetate dihydrate and thioacetamide as raw materials, and ethyl alcohol as the solvent. Compared with general block g-C3N4/CdS, the two-dimensional ultra-thin g-C3N4 nanosheet/CdS composite photocatalyst prepared with the method has the advantages that the two substances are in tighter contact, the specific surface area is larger, photon-generated electron-hole can be better separated, and photocatalytic efficiency is higher. Under the shining of sunlight, the composite photocatalyst enables catalytic degradation of organic pollutants such as methyl orange in water to be achieved well. The preparing method is easy, raw materials are easy to obtain, visible light catalysis efficiency is high, and the application prospect is wide in the photocatalysis field.

Description

A kind of g-C 3n 4nanometer sheet/CdS composite visible light catalyst
Technical field
The invention belongs to the technical field that belongs to material preparation and visible light photocatalysis, be specifically related to a kind of two-dimentional ultra-thin g-C 3n 4the preparation of nanometer sheet/CdS composite visible light catalyst and the application of catalytic degradation organic pollutants under visible ray thereof.
Background technology
Current energy and environment problem is day by day serious, has caused the extensive attention in global range.Photocatalysis technology is the potential desirable approach of one that solves these two problems of energy and environment.Be mainly that solar energy utilization ratio is low, thereby photochemical catalyst stability cannot recycle not etc. and restrict at present reason that photochemical catalyst applies in actual production.Therefore,, in order to utilize solar energy, prepare efficient, stable visible light catalyst and there is far reaching significance to solving the current energy and environmental problem.
After having found Graphene, two-dimensional material has caused great concern because it has unique advantage such as electricity and optical property.G-C 3n 4being that band gap is 2.7eV visible light catalyst, is the most stable a kind of carboritride, is also a kind of material with stratiform two-dimensional structure, g-C 3n 4and semiconductor compound photocatalyst also has potential application foreground aspect water-splitting and the depollution of environment under visible ray.The g-C of block 3n 4exist photo-generated carrier to be easy to compound defect, the separative efficiency in light induced electron-hole is low, and quantum efficiency is low, can not well utilize sunshine.And pass through the g-C of block 3n 4peel off into two-dimentional ultra-thin g-C 3n 4after nanometer sheet, not only increase its specific area, more avtive spot is provided, and improved the separative efficiency of photo-generated carrier.CdS is that energy gap is the semiconductor of 2.4eV, has good visible absorption performance.But being easily oxidized by photohole under illumination, CdS there is photoetch phenomenon.Photoetch phenomenon makes the bad stability of CdS catalyst, and photocatalytic activity reduces.In order to improve photostability and the photocatalytic activity of CdS, preparing its composite photo-catalyst becomes research emphasis.Due to g-C 3n 4there are the band structure of mating very much, g-C between the two with CdS 3n 4thereby can effectively lead away the upper photohole producing of CdS and suppress photoetch effect.Based on above analysis, in conjunction with two-dimentional ultra-thin g-C 3n 4with CdS advantage separately, prepare two-dimentional ultra-thin g-C 3n 4/ CdS compound, can be conducive to the separative efficiency of photo-generated carrier, effectively improves stability and the photocatalytic activity of catalyst simultaneously.
CN10319766A discloses a kind of CdS/g-C 3n 4composite visible light catalyst, preparation method and application.This catalyst is to prepare by chemical precipitation method, is applied to the degraded of methylene blue and crystal violet solution under visible ray, has good degradation effect.But that this patent system is standby is block g-C 3n 4, do not possess two-dimentional ultra-thin g-C 3n 4the special nature having, is also difficult to realize two-dimentional ultra-thin g-C 3n 4the close contact such with CdS, therefore photocatalysis efficiency is low.And we utilize ultrasonic stripping method by block g-C 3n 4peel off into two-dimentional ultra-thin g-C 3n 4, and obtain the ultra-thin g-C of two dimension of both close contacts at its surface in situ growth CdS nano particle by solvent-thermal method 3n 4/ CdS visible light catalyst, photo-generated carrier transfer impedance is little between the two, and separative efficiency is high.Experiment showed, two-dimentional ultra-thin g-C 3n 4/ CdS composite photo-catalyst is obviously better than block g-C at this pollutant of degraded methyl orange 3n 4the photocatalysis effect of/CdS composite photo-catalyst.
Summary of the invention
The object of the present invention is to provide one to overcome block g-C 3n 4deficiency that photo-generated carrier separative efficiency is low, suppress CdS photoetch, there is the ultra-thin g-C of two dimension of efficient visible light activity 3n 4the preparation method of nanometer sheet/CdS composite photo-catalyst, and the application of catalytic degradation organic pollutants under visible ray.The ultra-thin g-C of two dimension that the present invention prepares 3n 4nanometer sheet/CdS and general block g-C 3n 4/ CdS compares, two-dimentional ultra-thin g-C 3n 4between nanometer sheet/CdS composite photo-catalyst two materials, have contact more closely, and specific area is larger, thereby light induced electron-cavity energy separates better, photocatalysis efficiency is higher.
For achieving the above object, the present invention adopts following technical scheme:
The ultra-thin g-C of two dimension of the present invention 3n 4nanometer sheet/CdS composite visible light catalyst is by by block g-C 3n 4peel off into two-dimentional ultra-thin g-C 3n 4nanometer sheet, and obtain at its surface in situ growth CdS nano particle by solvent-thermal method.G-C in catalyst 3n 4the mass ratio of nanometer sheet and CdS is 1:100-90:100.
Preparation method comprises the following steps:
(1) by melamine or urea through calcining, cooling, grind and make block g-C 3n 4;
(2) by block g-C 3n 4join in isopropyl alcohol, ultrasonic 5-20 hour, forms the suspension disperseing; Low-speed centrifugal is removed thicker block g-C 3n 4, the more remaining suspension of high speed centrifugation, the dry ultra-thin g-C that obtains two dimension 3n 4nanometer sheet;
(3) by the ultra-thin g-C of two dimension 3n 4nanometer sheet joins in the ethanolic solution of two hydration cadmium acetates, and ultrasonic, stirring, forms homodisperse suspension;
(4) in the suspension of step (3), add thioacetamide, after stirring makes it to dissolve completely, carry out solvent thermal reaction;
(5) by step (4) products therefrom through centrifugal, washing, the dry ultra-thin g-C that makes two dimension 3n 4nanometer sheet/CdS composite visible light catalyst.
In step (1), calcining heat is 400-600 ℃.
Described catalyst is for the visible light photocatalytic degradation of water target contaminant.
Described target contaminant is methyl orange.
Remarkable advantage of the present invention is: the ultra-thin g-C of two dimension of the present invention 3n 4nanometer sheet/CdS catalyst is at preparation method, structure composition and catalytic performance and existing CdS/g-C 3n 4catalyst difference.Due to the present invention by stripping method by the g-C of block 3n 4peel off into two-dimentional ultra-thin g-C 3n 4nanometer sheet, with block g-C 3n 4compare the ultra-thin g-C of two dimension of the present invention 3n 4nanometer sheet has not only increased its specific area, and more avtive spot is provided, and has improved separative efficiency and the photocatalysis efficiency of photo-generated carrier.This composite photo-catalyst, under solar light irradiation, has good catalytic degradation effect to this class organic pollutants of methyl orange.Preparation method of the present invention is simple to operate, and raw material are easy to get, and visible light catalytic efficiency is high, has broad application prospects in photocatalysis field.
Accompanying drawing explanation
Fig. 1 is the pure ultra-thin g-C of the present invention 3n 4nanometer sheet, pure CdS, two-dimentional ultra-thin g-C 3n 4the XRD figure of nanometer sheet/CdS compound.
Fig. 2 is block g-C of the present invention 3n 4field emission scanning electron microscope figure.
Fig. 3 is the ultra-thin g-C of the present invention's two dimension 3n 4the field emission scanning electron microscope figure of nanometer sheet/CdS composite photo-catalyst.
Fig. 4 is the pure ultra-thin g-C of the present invention 3n 4nanometer sheet, pure CdS, two-dimentional ultra-thin g-C 3n 4the visible light catalytic design sketch of nanometer sheet/CdS compound to methyl orange.
Fig. 5 is the ultra-thin g-C of two dimension of homogenous quantities ratio of the present invention 3n 4nanometer sheet/CdS and block g-C 3n 4the visible light catalytic design sketch of/CdS composite photo-catalyst to methyl orange.
The specific embodiment
Enumerate embodiment below and further illustrate the present invention.
embodiment 1 block g-C 3 n 4 the preparation of catalyst
Take 10 grams of melamines and put in corundum Noah's ark, be placed in tube furnace middle part, be heated to 550 ℃ with the heating rate of 2 ℃/min, and 550 ℃ of insulations 4 hours, whole process is carried out under nitrogen atmosphere, is taken out with mortar grinding after naturally cooling, obtains yellow powder sample.
the two-dimentional ultra-thin g-C of embodiment 2 3 n 4 the preparation of nanometer sheet
Take in embodiment 1 0.4 gram, sample and put into wide-mouth bottle, add 80 milliliters of isopropyl alcohols, tighten bottle cap.The wide-mouth bottle that sample is housed is placed in to ultrasonic machine the inside and within ultrasonic 10 hours, makes it to form suspension, afterwards suspension is removed to sediment for centrifugal 10 minutes with 3000 revs/min, then upper strata suspension is got off to obtain faint yellow solid sample with 12000 revs/min of high speed centrifugations.
embodiment 3
Pressing the synthetic catalyst of method of embodiment 1 and 2, after X-ray diffractometer scanning, see Fig. 1, is g-C 3n 4.
embodiment 4
Press the synthetic catalyst of embodiment 1 method, through field emission microscopy observation, see Fig. 2, the g-C that the catalyst of synthesized is block 3n 4.
embodiment 5 block g-C 3 n 4 the preparation of/CdS composite catalyst
Taking in embodiment 1 0.072 gram, gained sample joins in 50 milliliters of absolute ethyl alcohols that dissolved 1.333 grams of (5 mMs) two hydration cadmium acetates, stirring fully mixes it in 5 hours, add again 0.376 gram of (5 mMs) thioacetamide to stir and within 1 hour, dissolve mixing, wherein two-dimentional ultra-thin g-C 3n 4with the mass ratio of CdS be 1:10.Afterwards, put it in reactor, be placed at 180 ℃, baking oven and be incubated 12 hours, be naturally cooled to subsequently room temperature, gained precipitate with deionized water washing 3 times, absolute ethyl alcohol is washed after 2 times, and gained is deposited in 100 ℃ of vacuum drying ovens and dries 12 hours.
the two-dimentional ultra-thin g-C of embodiment 6 3 n 4 the preparation of nanometer sheet/CdS composite catalyst
Taking in embodiment 2 0.072 gram, gained sample joins in 50 milliliters of absolute ethyl alcohols that dissolved 1.333 grams of (5 mMs) two hydration cadmium acetates, after ultrasonic 30 minutes, stirring fully mixes it in 5 hours, add again 0.376 gram of (5 mMs) thioacetamide to stir and within 1 hour, dissolve mixing, wherein two-dimentional ultra-thin g-C 3n 4with the mass ratio of CdS be 1:10.Afterwards, put it in reactor, be placed at 180 ℃, baking oven and be incubated 12 hours, be naturally cooled to subsequently room temperature, gained precipitate with deionized water washing 3 times, absolute ethyl alcohol is washed after 2 times, and gained is deposited in 100 ℃ of vacuum drying ovens and dries 12 hours.
the preparation of embodiment 7 CdS catalyst
Take 1.333 grams of (5 mMs) Cadmium diacetate dihydrates and add 50 milliliters of absolute ethyl alcohol and stirring, after it dissolves, stir 5 hours, then add 0.376 gram of (5 mMs) thioacetamide to stir dissolving mixing in 1 hour.Afterwards, put it in reactor, be placed at 180 ℃, baking oven and be incubated 12 hours, be naturally cooled to subsequently room temperature, gained precipitate with deionized water washing 3 times, absolute ethyl alcohol is washed after 2 times, and gained is deposited in 100 ℃ of vacuum drying ovens and dries 12 hours.
embodiment 8
The catalyst synthesizing respectively by embodiment 6 and 7 methods, after X-ray diffractometer scanning, is shown in Fig. 1, and the catalyst of synthesized is two-dimentional ultra-thin g-C 3n 4nanometer sheet/CdS composite photo-catalyst and pure CdS.
embodiment 9
Press the synthetic catalyst of embodiment 6 methods, through field emission microscopy observation, see Fig. 3, it is the g-C of several nanometers that the catalyst of synthesized has thickness 3n 4nanometer sheet and CdS nano particle composition.
the two-dimentional ultra-thin g-C of embodiment 10 3 n 4 the application of nanometer sheet/CdS composite catalyst degradable organic pollutant
Get 30 milligrams of the catalyst that make in embodiment 6, join in the methyl orange solution of 80 milliliter of 10 mg/litre, through the dark adsorption reaction of half an hour, turn under magnetic agitation 800, adopt xenon lamp simulated solar light source, irradiate after 50 minutes, centrifugal, filter, get supernatant, detect by Carry50 ultraviolet-uisible spectrophotometer, degradation efficiency is 97.4%.
The foregoing is only preferred embodiment of the present invention, all equalizations of doing according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.

Claims (5)

1. a g-C 3n 4nanometer sheet/CdS composite visible light catalyst, is characterized in that: in catalyst, carbonitride is graphite-phase azotized carbon nano sheet, and g-C 3n 4the mass ratio of nanometer sheet and CdS is 1:100-90:100.
2. prepare g-C as claimed in claim 1 for one kind 3n 4the method of nanometer sheet/CdS composite visible light catalyst, is characterized in that: comprise the following steps:
(1) by melamine or urea through calcining, cooling, grind and make block g-C 3n 4;
(2) by block g-C 3n 4join in isopropyl alcohol, ultrasonic 5-20 hour, forms the suspension disperseing; Low-speed centrifugal is removed thicker block g-C 3n 4, the more remaining suspension of high speed centrifugation, the dry g-C that obtains 3n 4nanometer sheet;
(3) by g-C 3n 4nanometer sheet joins in the ethanolic solution of two hydration cadmium acetates, and ultrasonic, stirring, forms homodisperse suspension;
(4) in the suspension of step (3), add thioacetamide, after stirring makes it to dissolve completely, carry out solvent thermal reaction;
(5) by step (4) products therefrom through centrifugal, washing, the dry g-C that makes 3n 4nanometer sheet/CdS composite visible light catalyst.
3. g-C according to claim 2 3n 4the preparation method of nanometer sheet/CdS composite visible light catalyst, is characterized in that: in step (1), calcining heat is 400-600 ℃.
4. a g-C as claimed in claim 1 3n 4the application of nanometer sheet/CdS composite visible light catalyst, is characterized in that: described catalyst is for the visible light photocatalytic degradation of water target contaminant.
5. g-C according to claim 4 3n 4the application of nanometer sheet/CdS composite visible light catalyst, is characterized in that: described target contaminant is methyl orange.
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