CN103785434B - A kind of g-C 3n 4nanometer sheet/CdS composite visible light catalyst - Google Patents
A kind of g-C 3n 4nanometer sheet/CdS composite visible light catalyst Download PDFInfo
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- CN103785434B CN103785434B CN201410082715.6A CN201410082715A CN103785434B CN 103785434 B CN103785434 B CN 103785434B CN 201410082715 A CN201410082715 A CN 201410082715A CN 103785434 B CN103785434 B CN 103785434B
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Abstract
The invention discloses a kind of graphite phase carbon nitride (g-C
3n
4) nanometer sheet/cadmium sulfide (CdS) composite visible light catalyst and its preparation method and application, belong to material preparation and light-catalysed technical field.This catalyst is with two-dimensional ultrathin g-C
3n
4nanometer sheet is matrix, with two acetate hydrate cadmiums and thioacetamide for raw material, is directly obtained by the solvent thermal process of ethanol as solvent.The two-dimensional ultrathin g-C that the present invention prepares
3n
4nanometer sheet/CdS and general block g-C
3n
4/ CdS compares, two-dimensional ultrathin g-C
3n
4have between nanometer sheet/CdS composite photo-catalyst two material and contact more closely, and specific area is larger, thus photo-generate electron-hole can be separated better, photocatalysis efficiency is higher.This composite photo-catalyst, under sunlight, has good catalytic degradation effect to this kind of 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.
Description
Technical field
The invention belongs to the technical field belonging to material preparation and visible light photocatalysis, be specifically related to a kind of two-dimensional ultrathin g-C
3n
4the application of the preparation of nanometer sheet/CdS composite visible light catalyst and under visible light catalytic degradation organic pollutants.
Background technology
Current energy and environment problem is day by day serious, causes the extensive attention in global range.Photocatalysis technology is then the potential desirable route of one solving this two problems of energy and environment.And mainly low, the photochemical catalyst stability of solar energy utilization ratio is not thus cannot recycle to restrict reason that photochemical catalyst applies in actual production at present.Therefore, in order to can better solar energy be utilized, prepare efficient, stable visible light catalyst, to the current energy of solution and environmental problem, there is far reaching significance.
After having found Graphene, two-dimensional material has had the advantages such as unique electricity and optical property and has caused great concern because of it.G-C
3n
4be band gap be 2.7eV visible light catalyst, being 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 there is potential application foreground water-splitting and depollution of environment aspect under visible light.The g-C of block
3n
4there is the defect that photo-generated carrier is easy to compound, the separative efficiency of photo-generate electron-hole is low, and quantum efficiency is low, well can not utilize sunshine.And pass through the g-C of block
3n
4peel off into two-dimensional ultrathin g-C
3n
4after nanometer sheet, not only increase its specific area, more avtive spot is provided, and improve the separative efficiency of photo-generated carrier.The semiconductor of CdS to be energy gap be 2.4eV, has good visible absorption performance.But CdS is easily oxidized by photohole under light illumination and photoetch phenomenon occurs.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
4the band structure of mating is had very much between the two, g-C with CdS
3n
4effectively can lead away photohole thus suppression photoetch effect that CdS produces.Based on above analysis, in conjunction with two-dimensional ultrathin g-C
3n
4with CdS advantage separately, prepare two-dimensional ultrathin 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 prepared 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-dimensional ultrathin g-C
3n
4the special nature had, is also difficult to realize two-dimensional ultrathin 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-dimensional ultrathin g-C
3n
4, and obtained the two-dimensional ultrathin g-C 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 proves, two-dimensional ultrathin 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
One is the object of the present invention is to provide to overcome block g-C
3n
4the deficiency that photo-generated carrier separative efficiency is low, the two-dimensional ultrathin g-C suppressing CdS photoetch, there is 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 light.The two-dimensional ultrathin g-C that the present invention prepares
3n
4nanometer sheet/CdS and general block g-C
3n
4/ CdS compares, two-dimensional ultrathin g-C
3n
4have between nanometer sheet/CdS composite photo-catalyst two material and contact more closely, and specific area is larger, thus photo-generate electron-hole can be separated better, photocatalysis efficiency is higher.
For achieving the above object, the present invention adopts following technical scheme:
Two-dimensional ultrathin g-C of the present invention
3n
4nanometer sheet/CdS composite visible light catalyst is by by block g-C
3n
4peel off into two-dimensional ultrathin g-C
3n
4nanometer sheet, and obtained 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) melamine or urea are obtained block g-C through calcining, cooling, grinding
3n
4;
(2) by block g-C
3n
4join in isopropyl alcohol, ultrasonic 5-20 hour, form the suspension of dispersion; Low-speed centrifugal removes thicker block g-C
3n
4, then the suspension remained by high speed centrifugation, the dry ultra-thin g-C obtaining 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 acetate hydrate cadmiums, and ultrasonic, stirring, forms homodisperse suspension;
(4) in the suspension of step (3), add thioacetamide, stir after making it to dissolve completely, carry out solvent thermal reaction;
(5) by the ultra-thin g-C of step (4) products therefrom through centrifugal, washing, dry obtained two dimension
3n
4nanometer sheet/CdS composite visible light catalyst.
In step (1), calcining heat is 400-600 DEG C.
Described catalyst is used for the visible light photocatalytic degradation of target contaminant in water.
Described target contaminant is methyl orange.
Remarkable advantage of the present invention is: two-dimensional ultrathin g-C 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 is different.Because the present invention is by the g-C of stripping method by block
3n
4peel off into two-dimensional ultrathin g-C
3n
4nanometer sheet, with block g-C
3n
4compare, two-dimensional ultrathin g-C of the present invention
3n
4nanometer sheet not only increases its specific area, provides more avtive spot, and improves separative efficiency and the photocatalysis efficiency of photo-generated carrier.This composite photo-catalyst, under sunlight, has good catalytic degradation effect to this kind of 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-dimensional ultrathin 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 two-dimensional ultrathin g-C of the present invention
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-dimensional ultrathin g-C
3n
4nanometer sheet/CdS compound is to the visible light catalytic design sketch of methyl orange.
Fig. 5 is the two-dimensional ultrathin g-C of homogenous quantities of the present invention ratio
3n
4nanometer sheet/CdS and block g-C
3n
4/ CdS composite photo-catalyst is to the visible light catalytic design sketch of methyl orange.
Detailed description of the invention
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 to put in corundum Noah's ark, be placed in the middle part of tube furnace, be heated to 550 DEG C with the heating rate of 2 DEG C/min, and 550 DEG C of insulations 4 hours, whole process is carried out in a nitrogen atmosphere, by its taking-up mortar grinder after naturally cooling, obtains yellow powder sample.
embodiment 2 two-dimensional ultrathin g-C
3
n
4
the preparation of nanometer sheet
Take 0.4 gram, sample in embodiment 1 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 and within inside ultrasonic machine ultrasonic 10 hours, makes it to form suspension, afterwards by suspension 3000 revs/min of centrifugal 10 minutes removing sediments, then upper suspension 12000 revs/min of high speed centrifugations are got off to obtain faint yellow solid sample.
embodiment 3
By the catalyst that the method for embodiment 1 and 2 is synthesized, after X-ray diffractometer scanning, seeing Fig. 1, is g-C
3n
4.
embodiment 4
By the catalyst of embodiment 1 method synthesis, through field emission microscopy observation, see Fig. 2, synthesized catalyst is the g-C of block
3n
4.
embodiment 5 block g-C
3
n
4
the preparation of/CdS composite catalyst
Take 0.072 gram, gained sample in embodiment 1 join dissolved 1.333 grams (5 mMs) two acetate hydrate cadmium 50 milliliters of absolute ethyl alcohols in, stirring makes it fully mix in 5 hours, add 0.376 gram of (5 mMs) thioacetamide again and stir dissolving mixing in 1 hour, wherein two-dimensional ultrathin g-C
3n
4be 1:10 with the mass ratio of CdS.Afterwards, put it in reactor, be incubated 12 hours at being placed in 180 DEG C, baking oven, Temperature fall is to room temperature subsequently, and gained precipitate with deionized water washs 3 times, and after absolute ethyl alcohol washes 2 times, gained is deposited in 100 DEG C of vacuum drying ovens and dries 12 hours.
embodiment 6 two-dimensional ultrathin g-C
3
n
4
the preparation of nanometer sheet/CdS composite catalyst
Take 0.072 gram, gained sample in embodiment 2 join dissolved 1.333 grams (5 mMs) two acetate hydrate cadmium 50 milliliters of absolute ethyl alcohols in, after ultrasonic 30 minutes, stirring makes it fully mix in 5 hours, add 0.376 gram of (5 mMs) thioacetamide again and stir dissolving mixing in 1 hour, wherein two-dimensional ultrathin g-C
3n
4be 1:10 with the mass ratio of CdS.Afterwards, put it in reactor, be incubated 12 hours at being placed in 180 DEG C, baking oven, Temperature fall is to room temperature subsequently, and gained precipitate with deionized water washs 3 times, and after absolute ethyl alcohol washes 2 times, gained is deposited in 100 DEG C 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, until its dissolve after, stirs 5 hours, then add 0.376 gram of (5 mMs) thioacetamide stir 1 hour dissolve mix.Afterwards, put it in reactor, be incubated 12 hours at being placed in 180 DEG C, baking oven, Temperature fall is to room temperature subsequently, and gained precipitate with deionized water washs 3 times, and after absolute ethyl alcohol washes 2 times, gained is deposited in 100 DEG C of vacuum drying ovens and dries 12 hours.
embodiment 8
By the catalyst that embodiment 6 and 7 method is synthesized respectively, after X-ray diffractometer scanning, see Fig. 1, synthesized catalyst is two-dimensional ultrathin g-C
3n
4nanometer sheet/CdS composite photo-catalyst and pure CdS.
embodiment 9
By the catalyst of embodiment 6 method synthesis, through field emission microscopy observation, see Fig. 3, synthesized catalyst has thickness to be the g-C of several nanometer
3n
4nanometer sheet and CdS nano particle composition.
embodiment 10 two-dimensional ultrathin g-C
3
n
4
the application of nanometer sheet/CdS composite catalyst degradable organic pollutant
Catalyst 30 milligrams obtained in Example 6, join in the methyl orange solution of 80 milliliter of 10 mg/litre, through the dark adsorption reaction of half an hour, under 800 turns of magnetic agitation, adopt xenon lamp simulated solar light source, carry out irradiation after 50 minutes, centrifugal, filter, get supernatant, detected by Carry50 ultraviolet-uisible spectrophotometer, degradation efficiency is 97.4%.
The foregoing is only preferred embodiment of the present invention, all equalizations done 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 (4)
1. a g-C
3n
4nanometer sheet/CdS composite visible light catalyst, is characterized in that: in catalyst, carbonitride is graphite phase carbon nitride nanometer sheet, and g-C
3n
4the mass ratio of nanometer sheet and CdS is 1:100-90:100;
Preparation method comprises the following steps:
(1) melamine or urea are obtained block g-C through calcining, cooling, grinding
3n
4;
(2) by block g-C
3n
4join in isopropyl alcohol, ultrasonic 5-20 hour, form the suspension of dispersion; Low-speed centrifugal removes thicker block g-C
3n
4, then the suspension remained by high speed centrifugation, dry acquisition g-C
3n
4nanometer sheet;
(3) by g-C
3n
4nanometer sheet joins in the ethanolic solution of two acetate hydrate cadmiums, and ultrasonic, stirring, forms homodisperse suspension;
(4) in the suspension of step (3), add thioacetamide, stir after making it to dissolve completely, carry out solvent thermal reaction;
(5) step (4) products therefrom is obtained g-C through centrifugal, washing, drying
3n
4nanometer sheet/CdS composite visible light catalyst.
2. g-C according to claim 1
3n
4nanometer sheet/CdS composite visible light catalyst, is characterized in that: in step (1), calcining heat is 400-600 DEG C.
3. 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 used for the visible light photocatalytic degradation of target contaminant in water.
4. application according to claim 3, is characterized in that: described target contaminant is methyl orange.
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