CN106732659A - Graphene CdLa2S4Composite visible light catalyst and its preparation technology - Google Patents
Graphene CdLa2S4Composite visible light catalyst and its preparation technology Download PDFInfo
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- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 claims description 11
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims description 11
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- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
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- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to visible light catalyst field, a kind of Graphene CdLa is proposed2S4Composite visible light catalyst and its preparation technology.Wherein Graphene CdLa2S4Composite visible light catalyst includes Graphene and photochemical catalyst, and photochemical catalyst is attached to graphene sheet layer, and photochemical catalyst is CdLa2S4.In addition the invention further relates to a kind of above-mentioned Graphene CdLa2S4The preparation technology of composite visible light catalyst.Graphene CdLa2S4Composite visible light catalyst can realize quick separating by the transfer of photo-generate electron-hole pair, thus with relatively low electron-hole recombination rate and more excellent catalysis activity.
Description
Technical field
The present invention relates to visible light catalyst field, and more particularly to a kind of Graphene-CdLa2S4Composite visible light is catalyzed
Agent and its preparation technology.
Background technology
Problem of environmental pollution is one of significant challenge of 21 century facing mankind.Environment is the field of human survival and activity
On the one hand institute, the mankind ask for resource and the energy to meet the demand of life and production activity to environment, on the one hand again will life
In the waste discharge produced in production to environment.The direct result of environmental pollution is the deterioration of environment for human survival, influences people
The quality of life of class, healthy and production are movable.Photocatalysis technology is that a kind of energy-conserving and environment-protective can be used for the new of the depollution of environment
Technology, can be used for the degraded purification of air and water pollutant.The photochemical catalyst that traditional photocatalysis technology is used is TiO2,
Yet with TiO2With band gap wider, it is caused to carry out catalytic degradation using the visible ray for accounting for solar energy 45%
Pollutant, therefore, necessary exploitation is to visible light-responded catalysis material.
The content of the invention
It is an object of the invention to provide a kind of Graphene-CdLa2S4Composite visible light catalyst, this Graphene-
CdLa2S4Composite visible light catalyst is good using the effect of catalyzing and degrading pollutant by visible light, and with relatively low electronics-sky
Cave recombination rate and more excellent catalysis activity.
Another object of the present invention is to provide a kind of Graphene-CdLa2S4The preparation technology of composite visible light catalyst,
Graphene-the CdLa higher to prepare catalysis activity2S4Composite visible light catalyst, above-mentioned catalyst is dropped using visible light catalytic
The effect for solving pollutant is good.
The present invention is solved its technical problem and is realized using following technical scheme.
The present invention proposes a kind of Graphene-CdLa2S4Composite visible light catalyst, it includes Graphene and photochemical catalyst, light
Catalyst is attached to graphene sheet layer, and photochemical catalyst is CdLa2S4。
Preferably, CdLa2S4It is Nano microsphere CdLa2S4。
Preferably, Nano microsphere CdLa2S4By oval CdLa2S4Nanoparticle aggregate is formed.
The present invention proposes a kind of Graphene-CdLa2S4The preparation technology of composite visible light catalyst, it is comprised the following steps：
S1 steps：Prepare graphene oxide solution；
S2 steps：The first mixed liquor is made to cadmium acetate and lanthanum nitrate is added in graphene oxide solution；
S3 steps：After by thiocarbamide and polyvinylpyrrolidone dissolving in deionized water, add ethylene glycol to be made second and mix
Close liquid；
S4 steps：First mixed liquor and the second mixed liquor are mixed, and after adjusting pH to 8~11, the 3rd mixed liquor is obtained；
S5 steps：3rd mixed liquor is obtained into the 4th mixed liquor after the heating 3~9 minutes of 800 watts of micro-wave oven；Wherein,
Heating is carried out several times, is heated 8~12 seconds every time, is spaced 8~12 seconds per between heating twice；And
S6 steps：4th mixed liquor is scrubbed, dry after obtain Graphene-CdLa2S4Composite visible light catalyst.
Preferably, in S1 steps, the concentration of middle graphene oxide solution is 8~12mg/ml.
Preferably, in S2 steps, when being made the first mixed liquor, the consumption of graphene oxide solution, cadmium acetate and lanthanum nitrate
Than being 18~25ml：0.24~0.26mmol：0.48~0.52mmol.
Preferably, in S2 steps, when being made the first mixed liquor, the consumption of graphene oxide solution, cadmium acetate and lanthanum nitrate
Than being 20ml：0.25mmol：0.5mmol.
Preferably, in S3 steps, when being made the second mixed liquor, thiocarbamide, polyvinylpyrrolidone, deionized water and ethylene glycol
Amount ratio be 1~2mmol：0.001~0.003g：2~10ml：90~150ml.
Preferably, in S4 steps, when three mixed liquors is obtained, the volume ratio of the first mixed liquor and the second mixed liquor is 1：5
~6.
Preferably, pH to 8~11 is adjusted using ammoniacal liquor in S4 steps.
Graphene-the CdLa of the embodiment of the present invention2S4The beneficial effect of composite visible light catalyst and its preparation technology is：
Using Graphene photoelectric properties it is excellent and and specific surface area it is larger the characteristics of, by catalyst CdLa2S4Mix with graphene oxide,
By obtaining Graphene-CdLa after reaction2S4Composite visible light catalyst.Above-mentioned Graphene-CdLa2S4Composite visible light is catalyzed
Agent, can realize quick separating by the transfer of photo-generate electron-hole pair, thus with relatively low electron-hole recombination rate and
More excellent catalysis activity.
Brief description of the drawings
Technical scheme in order to illustrate more clearly the embodiments of the present invention, below will be attached to what is used needed for embodiment
Figure is briefly described, it will be appreciated that the following drawings illustrate only certain embodiments of the present invention, thus be not construed as it is right
The restriction of scope, for those of ordinary skill in the art, on the premise of not paying creative work, can also be according to this
A little accompanying drawings obtain other related accompanying drawings.
Fig. 1 is the Graphene-CdLa of the embodiment of the present invention 1~32S4Composite visible light catalyst, the catalyst of comparative example 1
CdLa2S4, the redox graphene of comparative example 2 and the graphene oxide of comparative example 3 XRD spectrum；
Fig. 2 is the Graphene-CdLa of the embodiment of the present invention 22S4The scanning electron microscope (SEM) photograph (SEM) of composite visible light catalyst；
Fig. 3 is the Graphene-CdLa of the embodiment of the present invention 22S4Transmission electron microscope picture (the HR- of composite visible light catalyst
TEM)；
Fig. 4 is the Graphene-CdLa of the embodiment of the present invention 22S4Composite visible light catalyst is in degradation of methylene blue solution
Degradation curve；
Fig. 5 is the Graphene-CdLa of the embodiment of the present invention 1~32S4The commercially available P25 of composite visible light catalyst and comparative example
Speed constant curve of the photochemical catalyst in degradation of methylene blue solution.
Specific embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below will be in the embodiment of the present invention
Technical scheme be clearly and completely described.Unreceipted actual conditions person, builds according to normal condition or manufacturer in embodiment
The condition of view is carried out.Agents useful for same or the unreceipted production firm person of instrument, are the conventional product that can be obtained by commercially available purchase
Product.
CdLa2S4It is a kind of narrow bandgap semiconductor material, it can be 2.1eV with coefficient, under visible light illumination decomposition water system
Stronger photocatalytic activity is shown during hydrogen.
Graphene is the allotrope of a kind of new carbon being found in recent years, and it is by sp2The monolayer carbon of hydridization is former
Molecular cellular two dimensional crystal, the specific surface area with excellent mechanics, optically and electrically calorifics, performance and super large.
Below to the Graphene-CdLa of the embodiment of the present invention2S4Composite visible light catalyst and its preparation technology are carried out specifically
Explanation.
A kind of Graphene-CdLa provided in an embodiment of the present invention2S4Composite visible light catalyst, including Graphene and
CdLa2S4Photochemical catalyst, CdLa2S4Photochemical catalyst is attached to graphene sheet layer.
Further, CdLa2S4Photochemical catalyst is Nano microsphere CdLa2S4Photochemical catalyst.
Further, CdLa2S4Photochemical catalyst is Nano microsphere CdLa2S4Photochemical catalyst is by oval CdLa2S4Nanometer
Grain aggregation is formed.
Graphene-the CdLa that the present invention is provided2S4Composite visible light catalyst will be seen that photo absorption property is good
CdLa2S4It is combined with photoelectricity excellent performance and the larger Graphene of specific surface area, there is relatively low electron-hole to be combined for it
Rate, CdLa2S4Quick separating can be realized by the transfer of photo-generate electron-hole pair between photochemical catalyst and Graphene, so that upper
State Graphene-CdLa2S4Composite visible light catalyst has visible light catalysis activity higher.
Present invention also offers above-mentioned Graphene-CdLa2S4The preparation technology of composite visible light catalyst, including following step
Suddenly：
S1 steps：Prepare graphene oxide solution.
Further, in present pre-ferred embodiments, the concentration of graphene oxide solution is 8~12mg/ml, the concentration
Under graphene oxide, be conducive to CdLa2S4The deposition of photochemical catalyst.
During graphene oxide is prepared, graphene oxide can be distributed in water the ultrasound behaviour for carrying out the long period
Make, prolonged ultrasound procedure effectively can separate graphene oxide, and due to the presence of surface of graphene oxide functional group,
Uniform and stable dispersion liquid is advantageously formed, and is conducive to the CdLa of subsequent step2S4The uniform deposition of catalyst.Promote
CdLa2S4The uniform mixing of catalyst and Graphene, makes Graphene to CdLa2S4The performance improvement of catalyst it is more preferable.
S2 steps：The first mixed liquor is made to cadmium acetate and lanthanum nitrate is added in graphene oxide solution.
Further, in present pre-ferred embodiments, the ratio of graphene oxide solution, cadmium acetate and lanthanum nitrate is 15
~25ml：0.24~0.26mmol：0.48~0.52mmol.
Further, in present pre-ferred embodiments, the ratio of graphene oxide solution, cadmium acetate and lanthanum nitrate is
20ml：0.25mmol：0.5mmol.Now the ratio between amount of material of cadmium acetate and lanthanum nitrate and CdLa2S4Photochemical catalyst chemical formula
The metering of middle cadmium element and lanthanum element is conducive to for the chemical formula of final product being controlled to CdLa than identical2S4。
To that can carry out ultrasound procedure after adding cadmium acetate and lanthanum nitrate in graphene oxide solution, ultrasound can accelerate molten
Solution.
S3 steps：By thiocarbamide and polyvinylpyrrolidone in deionized water after, add ethylene glycol be made the second mixed liquor.
Further, in present pre-ferred embodiments, thiocarbamide, polyvinylpyrrolidone, deionized water and ethylene glycol
Ratio is 1~2mmol：0.001~0.003g：2~10ml：110~130ml.
Polyvinylpyrrolidone can effectively control CdLa as dispersant after addition2S4The growth of catalyst nucleus,
So as to reach control CdLa2S4The purpose of catalyst microspheres particle diameter.Because thiocarbamide is very low in ethylene glycol, first it is dissolved in
In ionized water, add ethylene glycol and be configured to the second mixed solution.
S4 steps：First mixed liquor and the second mixed liquor are mixed, and after adjusting pH to 8~11, obtains the 3rd mixed liquor.
PH is adjusted to alkalescence is conducive to thiocarbamide to discharge sulphion, accelerates generation CdLa2S4Photochemical catalyst.
Further, in present pre-ferred embodiments, the volume ratio of the first mixed liquor and the second mixed liquor is 1：5~6.
The addition of Graphene is proper under this ratio, the Graphene-CdLa for obtaining2S4Composite visible light catalyst catalysis activity
It is higher.
Further, in present pre-ferred embodiments, using aqueous ammonia conditions pH.Ammoniacal liquor is in alkalescent, is adjusted using ammoniacal liquor
Section pH value, can preferably control pH.
S5 steps：3rd mixed liquor is obtained into the 4th mixed liquor after the heating 3~9 minutes of 800 watts of micro-wave oven；Wherein,
Heating is carried out several times, is heated 8~12 seconds every time, is spaced 8~12 seconds per between heating twice；
By the way of heating is spaced, ethylene glycol can be avoided from being volatilized because temperature is too high.And avoid continuous heating process
In, temperature constantly rises, and reaction rate persistently changes.
S6 steps：4th mixed liquor is scrubbed, dry after obtain Graphene-CdLa2S4Composite visible light catalyst.
Feature of the invention and performance are described in further detail with reference to embodiments.
Embodiment 1
A kind of Graphene-CdLa that the present embodiment is provided2S4Composite visible light catalyst, it includes that Graphene and nanometer are micro-
Ball CdLa2S4Photochemical catalyst, wherein Nano microsphere CdLa2S4Photochemical catalyst is by oval CdLa2S4Nanoparticle aggregate is formed.Adopt
With Shimadzu XD-D1 (Japan) to the Graphene-CdLa of the present embodiment2S4Composite visible light catalyst carries out XRD analysis,
The XRD spectrum for obtaining is as shown in fig. 1A.To the Graphene-CdLa of the present embodiment2S4Composite visible light catalyst degraded is organic
The performance of pollutant is analyzed, and the speed constant curve during degradation of methylene blue solution for obtaining is as shown in a in Fig. 5.
A kind of Graphene-CdLa2S4The preparation technology of composite visible light catalyst：
S1 steps, ultrasonic 5 hours (amplitude is set as 45%) is scattered in deionized water by graphene oxide, is aoxidized
Graphene solution, concentration is 10mg/ml.
S2 steps, take above-mentioned graphene oxide solution 20ml, are added thereto to 0.25mmol (CH3COO)2Cd·2H2O and
0.5mmol La(NO3)3·6H2O, ultrasound obtains the first mixed liquor after 25 minutes, after that the first mixed liquor is transferred into 500ml is micro-
In ripple stove special utensil.
S3 steps, the polyvinylpyrrolidone (PVP) for weighing 2mmol thiocarbamides and 0.002g is dissolved in 3ml deionized waters,
120ml ethylene glycol is added to be made the second mixed liquor.
S4 steps, the first solution is transferred in the second solution, and ultrasound 60 points of magnetic agitation at room temperature after 10 minutes
Clock, is then adjusted to 8 pH value with ammoniacal liquor, obtains the 3rd mixed liquor.
S5 steps, will be equipped with the 3rd mixed liquor micro-wave oven special utensil be put into household microwave oven 800 watts of intervals plus
Heat obtains the 4th mixed liquor.Wherein, 10s is heated up at interval of 10s, the temporal summation that each heat time is added is 9 minutes
(that is, the heat time is total up to 9 minutes).
S6 steps, after question response liquid naturally cools to room temperature, the product for obtaining is adopted and is washed with deionized three times, then uses second
Alcohol centrifuge washing three times, then 120 degree of dryings 12 hours in air dry oven, obtain Graphene-CdLa2S4Composite visible light
Catalyst.
Embodiment 2
The present embodiment is differred primarily in that with embodiment 1：The consumption of thiocarbamide is different, the time of heating using microwave is different and
The drying time of compound is different with drying temperature, other specification and operating procedure all same.Using Shimadzu XD-D1
(Japan) to the Graphene-CdLa of the present embodiment2S4Composite visible light catalyst carries out XRD analysis, and the XRD spectrum for obtaining is as schemed
Shown in b in 1.To the Graphene-CdLa of the present embodiment2S4The performance of composite visible light catalyst degradable organic pollutant is carried out
Analysis, the speed constant curve during degradation of methylene blue solution for obtaining is as shown in the b in Fig. 5.To the Graphene of the present embodiment-
CdLa2S4Composite visible light catalyst is scanned Electronic Speculum and transmission electron microscope analysis, wherein result such as Fig. 2 of ESEM (SEM)
Shown, the result of transmission electron microscope (TEM) is as shown in Figure 3.Graphene-the CdLa of the present embodiment2S4Composite visible light catalyst is in drop
Degradation curve during solution methylene blue solution is as shown in Figure 4.
A kind of Graphene-CdLa that the present embodiment is provided2S4Composite visible light catalyst, it includes that Graphene and nanometer are micro-
Ball CdLa2S4Photochemical catalyst, wherein Nano microsphere CdLa2S4Photochemical catalyst is by oval CdLa2S4Nanoparticle aggregate is formed.
Fig. 2 and Fig. 3 is the Graphene-CdLa of the present embodiment2S4The SEM (Fig. 2) and HR-TEM of composite visible light catalyst
(Fig. 3) figure, can be clearly visible that Graphene-CdLa from figure2S4The compound Graphene quilt for meeting transparent lamina in photochemical catalyst
CdLa2S4Photochemical catalyst microballoon is covered, and the CdLa2S4 is Nano microsphere structure (diameter is about 150nm) by oval CdLa2S4
Nanoparticle aggregate is formed, nanometer CdLa2S4The lattice fringe spacing about 0.36nm of correspondence { 211 } crystal face.
Fig. 4 is the Graphene-CdLa of the present embodiment2S4Drop of the composite visible light catalyst in degradation of methylene blue solution
Solution curve.Specifically, degradation reaction is carried out in the photocatalytic reaction device of customization, reactor is by jacketed reactor, top illuminated
Xenon source (Solar, 500W, λ>420nm) constitute, the suspended state of photochemical catalyst in solution is maintained by magnetic agitation.
Its Methylene Blue initial concentration is 12mg/L, and volume is 75ml, and catalyst amount is 50mg.Under radiation of visible light, Mei Geyi
Fix time and pipette 4.0mL reaction solutions, after being centrifuged, taking supernatant liquor carries out uv-visible absorption spectra analysis, according to sample
The light absorption value of product characteristic absorption peak determines degradation process Methylene Blue change in concentration.From the figure, it can be seen that illumination
The degradation rate of methylene blue reaches 65%, the Graphene-CdLa of embodiment 2 after 120min2S4Composite visible light catalyst is in degraded
Excellent degradation effect is shown during methylene blue.
A kind of Graphene-CdLa2S4The preparation technology of composite visible light catalyst：
S1 steps, ultrasonic 5 hours (amplitude is set as 45%) is scattered in deionized water by graphene oxide, is aoxidized
Graphene solution, concentration is 10mg/ml.
S2 steps, take above-mentioned graphene oxide solution 20ml, are added thereto to 0.25mmol (CH3COO)2Cd·2H2O and
0.5mmol La(NO3)3·6H2O, ultrasound obtains the first mixed liquor after 25 minutes, after that the first mixed liquor is transferred into 500ml is micro-
In ripple stove special utensil.
S3 steps, the PVP for weighing 1.5mmol thiocarbamides and 0.002g is dissolved in a small amount of deionized water, adds 120ml second two
Alcohol is made the second mixed liquor.
S4 steps, the first solution is transferred in the second solution, and ultrasound 60 points of magnetic agitation at room temperature after 10 minutes
Clock, is then adjusted to 8 pH value with ammoniacal liquor, obtains the 3rd mixed liquor.
S5 steps, will be equipped with the 3rd mixed liquor micro-wave oven special utensil be put into household microwave oven 800 watts of intervals plus
Heat obtains the 4th mixed liquor.Wherein, total heat time is 6 minutes, and heating 10s stops 10s.
S6 steps, after question response liquid naturally cools to room temperature, the product for obtaining is adopted and is washed with deionized three times, then uses second
Alcohol centrifuge washing three times, then 90 degree of dryings 12 hours in air dry oven, obtain graphene/nanometer microballoon CdLa2S4It is compound
Visible light catalyst.
Embodiment 3
The present embodiment is differred primarily in that with embodiment 1：The consumption of thiocarbamide is different, the time of heating using microwave it is different and
The drying time of compound is different with drying temperature, other specification and operating procedure all same.Using Shimadzu XD-D1
(Japan) to the Graphene-CdLa of the present embodiment2S4Composite visible light catalyst carries out XRD analysis, and the XRD spectrum for obtaining is as schemed
Shown in c in 1.To the Graphene-CdLa of the present embodiment2S4The performance of composite visible light catalyst degradable organic pollutant is carried out
Analysis, the speed constant curve during degradation of methylene blue solution for obtaining is as shown in the c in Fig. 5.
A kind of Graphene-CdLa that the present embodiment is provided2S4Composite visible light catalyst, it includes that Graphene and nanometer are micro-
Ball CdLa2S4Photochemical catalyst, wherein Nano microsphere CdLa2S4Photochemical catalyst is by oval CdLa2S4Nanoparticle aggregate is formed.
A kind of Graphene-CdLa2S4The preparation technology of composite visible light catalyst：
S1 steps, ultrasonic 5 hours (amplitude is set as 45%) is scattered in deionized water by graphene oxide, is aoxidized
Graphene solution, concentration is 10mg/ml.
S2 steps, take above-mentioned graphene oxide solution 20ml, are added thereto to 0.25mmol (CH3COO)2Cd·2H2O and
0.5mmol La(NO3)3·6H2O, ultrasound obtains the first mixed liquor after 25 minutes, after that the first mixed liquor is transferred into 500ml is micro-
In ripple stove special utensil.
S3 steps, the PVP for weighing 1mmol thiocarbamides and 0.002g is dissolved in a small amount of deionized water, adds 120ml ethylene glycol
It is made the second mixed liquor.
S4 steps, the first solution is transferred in the second solution, and ultrasound 60 points of magnetic agitation at room temperature after 10 minutes
Clock, is then adjusted to 8 pH value with ammoniacal liquor, obtains the 3rd mixed liquor.
S5 steps, will be equipped with the 3rd mixed liquor micro-wave oven special utensil be put into household microwave oven 800 watts of intervals plus
Heat obtains the 4th mixed liquor.Wherein, total heat time is 3 minutes, and heating 10s stops 10s.
S6 steps, after question response liquid naturally cools to room temperature, the product for obtaining is adopted and is washed with deionized three times, then uses second
Alcohol centrifuge washing three times, then 80 degree of dryings 24 hours in air dry oven, obtain graphene/nanometer microballoon CdLa2S4It is compound
Visible light catalyst.
Embodiment 4
The present embodiment is differred primarily in that with embodiment 1：The consumption of raw material is different, and technological parameter is different.
A kind of Graphene-CdLa that the present embodiment is provided2S4Composite visible light catalyst, it includes that Graphene and nanometer are micro-
Ball CdLa2S4Photochemical catalyst, wherein Nano microsphere CdLa2S4Photochemical catalyst is by oval CdLa2S4Nanoparticle aggregate is formed.
A kind of Graphene-CdLa2S4The preparation technology of composite visible light catalyst：
S1 steps, ultrasonic 4 hours (amplitude is set as 45%) is scattered in deionized water by graphene oxide, is aoxidized
Graphene solution, concentration is 8mg/ml.
S2 steps, take above-mentioned graphene oxide solution 18ml, are added thereto to 0.26mmol (CH3COO)2Cd·2H2O and
0.48mmol La(NO3)3·6H2O, ultrasound obtains the first mixed liquor after 25 minutes, after that the first mixed liquor is transferred into 500ml is micro-
In ripple stove special utensil.
S3 steps, the PVP for weighing 1mmol thiocarbamides and 0.003g is dissolved in 5ml deionized waters, adds 90ml ethylene glycol systems
Into the second mixed liquor.
S4 steps, the first solution is transferred in the second solution, and ultrasound 60 points of magnetic agitation at room temperature after 10 minutes
Clock, is then adjusted to 11 pH value with ammoniacal liquor, obtains the 3rd mixed liquor.
S5 steps, will be equipped with the 3rd mixed liquor micro-wave oven special utensil be put into household microwave oven 800 watts of intervals plus
Heat obtains the 4th mixed liquor.Wherein, total heat time is 3 minutes, and heating 10s stops 10s.
S6 steps, after question response liquid naturally cools to room temperature, the product for obtaining is adopted and is washed with deionized three times, then uses second
Alcohol centrifuge washing three times, then 80 degree of dryings 20 hours in air dry oven, obtain graphene/nanometer microballoon CdLa2S4It is compound
Visible light catalyst.
Embodiment 5
The present embodiment is differred primarily in that with embodiment 1：The consumption of raw material is different, and technological parameter is different.
A kind of Graphene-CdLa that the present embodiment is provided2S4Composite visible light catalyst, it includes that Graphene and nanometer are micro-
Ball CdLa2S4Photochemical catalyst, wherein Nano microsphere CdLa2S4Photochemical catalyst is by oval CdLa2S4Nanoparticle aggregate is formed.
A kind of Graphene-CdLa2S4The preparation technology of composite visible light catalyst：
S1 steps, ultrasonic 6 hours (amplitude is set as 45%) is scattered in deionized water by graphene oxide, is aoxidized
Graphene solution, concentration is 8mg/ml.
S2 steps, take above-mentioned graphene oxide solution 25ml, are added thereto to 0.24mmol (CH3COO)2Cd·2H2O and
0.48mmol La(NO3)3·6H2O, ultrasound obtains the first mixed liquor after 25 minutes, after that the first mixed liquor is transferred into 500ml is micro-
In ripple stove special utensil.
S3 steps, the PVP for weighing 1.5mmol thiocarbamides and 0.001g is dissolved in 10ml deionized waters, adds 150ml second two
Alcohol is made the second mixed liquor.
S4 steps, the first solution is transferred in the second solution, and ultrasound 60 points of magnetic agitation at room temperature after 10 minutes
Clock, is then adjusted to 10 pH value with ammoniacal liquor, obtains the 3rd mixed liquor.
S5 steps, will be equipped with the 3rd mixed liquor micro-wave oven special utensil be put into household microwave oven 800 watts of intervals plus
Heat obtains the 4th mixed liquor.Wherein, total heat time is 6 minutes, and heating 10s stops 10s.
S6 steps, after question response liquid naturally cools to room temperature, the product for obtaining is adopted and is washed with deionized three times, then uses second
Alcohol centrifuge washing three times, then 110 degree of dryings 15 hours in air dry oven, obtain graphene/nanometer microballoon CdLa2S4It is multiple
Close visible light catalyst.
Embodiment 6
The present embodiment is differred primarily in that with embodiment 1：The consumption of raw material is different, and technological parameter is different.
A kind of Graphene-CdLa that the present embodiment is provided2S4Composite visible light catalyst, it includes that Graphene and nanometer are micro-
Ball CdLa2S4Photochemical catalyst, wherein Nano microsphere CdLa2S4Photochemical catalyst is by oval CdLa2S4Nanoparticle aggregate is formed.
A kind of Graphene-CdLa2S4The preparation technology of composite visible light catalyst：
S1 steps, ultrasonic 4 hours (amplitude is set as 45%) is scattered in deionized water by graphene oxide, is aoxidized
Graphene solution, concentration is 12mg/ml.
S2 steps, take above-mentioned graphene oxide solution 25ml, are added thereto to 0.26mmol (CH3COO)2Cd·2H2O and
0.48mmol La(NO3)3·6H2O, ultrasound obtains the first mixed liquor after 25 minutes, after that the first mixed liquor is transferred into 500ml is micro-
In ripple stove special utensil.
S3 steps, the PVP for weighing 1.5mmol thiocarbamides and 0.001g is dissolved in 7ml deionized waters, adds 125ml second two
Alcohol is made the second mixed liquor.
S4 steps, the first solution is transferred in the second solution, and ultrasound 60 points of magnetic agitation at room temperature after 10 minutes
Clock, is then adjusted to 9 pH value with ammoniacal liquor, obtains the 3rd mixed liquor.
S5 steps, will be equipped with the 3rd mixed liquor micro-wave oven special utensil be put into household microwave oven 800 watts of intervals plus
Heat obtains the 4th mixed liquor.Wherein, total heat time is 7 minutes, and heating 10s stops 10s.
S6 steps, after question response liquid naturally cools to room temperature, the product for obtaining is adopted and is washed with deionized three times, then uses second
Alcohol centrifuge washing three times, then 110 degree of dryings 15 hours in air dry oven, obtain graphene/nanometer microballoon CdLa2S4It is multiple
Close visible light catalyst.
Comparative example 1
A kind of CdLa that this comparative example is provided2S4Photochemical catalyst, its with embodiment 1 in Graphene-CdLa2S4Being combined can
That sees photochemical catalyst differs primarily in that no addition graphene oxide in building-up process.Using Shimadzu XD-D1
(Japan) to the CdLa of the present embodiment2S4Photochemical catalyst carries out XRD analysis, and the XRD spectrum for obtaining is as shown in the d in Fig. 1.
A kind of CdLa2S4The preparation technology of photochemical catalyst：By 0.25mmol (CH3COO)2Cd·2H2O and 0.5mmol La
(NO3)3·6H2O is dissolved in a small amount of water, and (consumption of water is to dissolve (CH3COO)2Cd·2H2O and La (NO3)3·6H2In O)
Add 30ml ethylene glycol, ultrasound 25 minutes after obtain mixed solution A, after mixed solution A is transferred to 500ml micro-wave oven special-purpose devices
In ware；1mmol thiocarbamides are weighed again and a certain amount of 0.002g polyvinylpyrrolidones (PVP) are dissolved in 3ml deionized waters, plus
Enter 120ml ethylene glycol and be made solution B.Solution B is transferred in solution A, ultrasound 60 points of magnetic agitation at room temperature after 10 minutes
Clock, the pH value of this mixed liquor is adjusted to 8 AB mixed liquors are obtained with ammoniacal liquor.The micro-wave oven special utensil that will be equipped with AB mixed liquors is put
In entering household microwave oven, using the 10 seconds mode of heatings in interval, 3 minutes total heat times, after question response liquid naturally cools to room temperature,
The product for obtaining is adopted and is washed with deionized three times, then with ethanol centrifuge washing three times, then in air dry oven 100 degree do
Dry 12 hours, obtain pure CdLa2S4Catalysis material.
Comparative example 2
This comparative example provides a kind of redox graphene, using Shimadzu XD-D1 (Japan) to the present embodiment
Redox graphene carries out XRD analysis, and the XRD spectrum for obtaining is as shown in the e in Fig. 1.
Graphene oxide is scattered in deionized water ultrasonic 5 hours (amplitude is set as 45%), graphene oxide is obtained
Solution, concentration is 10mg/ml；Above-mentioned graphene oxide 20ml is taken, adds 120ml ethylene glycol to obtain mixed liquor wherein.Will be upper
State 800 watts of interval heating of mixed liquor.Wherein, total heat time is 6 minutes, heats 10s, stops 10s.The Graphene for obtaining is molten
After liquid naturally cools to room temperature, adopt and be washed with deionized three times, then with ethanol centrifuge washing three times, it is freeze-dried after obtain
Redox graphene.
Comparative example 3
This comparative example provides a kind of commercially available graphene oxide.Using Shimadzu XD-D1 (Japan) to the present embodiment
Graphene oxide carry out XRD analysis, the XRD spectrum for obtaining is as shown in the f in Fig. 1.
Comparative example 4
This comparative example provides a kind of commercially available P25 photochemical catalysts, and above-mentioned catalyst can be catalyzed visible ray.To the present embodiment
Graphene-CdLa2S4The performance of composite visible light catalyst degradable organic pollutant is analyzed, the degraded methylene for obtaining
Speed constant curve during blue solution is as shown in the d in Fig. 5.
The XRD spectrum that X-ray diffraction analysis are obtained is as shown in figure 1, above-mentioned X-ray diffraction analysis are in instrument Shimadzu
XD-D1 (Japan) is measured.Wherein a, b, c are followed successively by the Graphene-CdLa of embodiment 1, embodiment 2, embodiment 32S4Being combined can
See photochemical catalyst, d is the CdLa of comparative example 12S4Photochemical catalyst, e is the redox graphene of comparative example 2, and f is the oxygen of comparative example 3
Graphite alkene.Therefrom it can be seen that obtained CdLa2S4Photochemical catalyst the θ of the angle of diffraction 2 be about 18.03 °, 20.74 °, 26.50 °,
27.97 °, 43.91 °, be respectively present (111), (200), (121), (220), (303), (422) crystallographic plane diffraction peak at 52.05 °,
These diffraction maximums are all CdLa2S4The characteristic peak of photochemical catalyst.After composite graphite alkene, the crystalline phase of sample does not change, but does not see
Observe the diffraction maximum corresponding to Graphene or graphene oxide, reason is that Graphene content is less and from Fig. 1 in composite sample
It can be seen that the characteristic peak and CdLa of Graphene2S4Characteristic peak partly overlap.
By the Graphene-CdLa of embodiment 1~32S4The commercially available P25 photochemical catalysts of composite visible light catalyst and comparative example
The performance of degraded organic pollutants is compared.Specific Graphene-the CdLa using above-described embodiment 1~32S4It is compound
Methylene blue (MB) in the commercially available P25 photocatalyst for degrading water of visible light catalyst and comparative example, degradation reaction is in customization
Carried out in photocatalytic reaction device, reactor is by jacketed reactor, top illuminated xenon source (Solar, 500W, λ>420nm) group
Into maintaining the suspended state of photochemical catalyst in solution by magnetic agitation.Its Methylene Blue initial concentration is 12mg/L, body
Product is 75ml, and catalyst amount is 50mg.Under radiation of visible light, 4.0mL reaction solutions are pipetted at regular intervals, be centrifuged
Afterwards, to take supernatant liquor carry out uv-visible absorption spectra analysis, and the light absorption value according to sample characteristic absworption peak determines to degrade
Journey Methylene Blue change in concentration.The situation of photocatalytic degradation methylene blue such as Fig. 5 and Fig. 4.
Fig. 5 is the Graphene-CdLa of embodiment 1~32S4The commercially available P25 photochemical catalysts of composite visible light catalyst and comparative example
Speed constant curve in degradation of methylene blue solution (when wavelength is 660nm).A, b, c are embodiment 1, embodiment 2 in Fig. 5
With the Graphene-CdLa of embodiment 32S4Composite visible light catalyst, d is commercially available P25 photochemical catalysts.It can be seen that
Graphene-the CdLa of embodiment 2 under illumination2S4Composite visible light catalyst is to the degraded highly significant of methylene blue, and its one-level is anti-
It is 8.1 × 10 to answer speed constant-3min-1(slope of fitting a straight line in figure), more than the Graphene-CdLa of other embodiment2S4It is multiple
Close visible light catalyst and commercially available P25 photochemical catalysts.
Graphene-CdLa in embodiments of the invention 4~62S4Composite visible light catalyst can also reach above-mentioned reality
Test effect.In addition, Graphene-the CdLa of embodiment 4~62S4Composite visible light catalyst be used for detect, the XRD spectrum of acquisition,
The performance test of scanning electron microscope (SEM) photograph, transmission electron microscope picture and degradation of methylene blue solution is consistent with above-mentioned result of the test, differs herein
One repeats.
In sum, the Graphene-CdLa of the embodiment of the present invention2S4Composite visible light catalyst and Graphene-CdLa2S4
Composite visible light catalyst preparation technology, by by Graphene and CdLa2S4Photochemical catalyst is combined, and improves CdLa2S4Photocatalysis
Agent carries out catalysis activity during Photocatalytic Activity for Degradation pollutant, the Graphene-CdLa for obtaining2S4Composite visible light catalyst
With relatively low electron-hole recombination rate and more excellent catalysis activity.
Embodiments described above is a part of embodiment of the invention, rather than whole embodiments.Reality of the invention
The detailed description for applying example is not intended to limit the scope of claimed invention, but is merely representative of selected implementation of the invention
Example.Based on the embodiment in the present invention, what those of ordinary skill in the art were obtained under the premise of creative work is not made
Every other embodiment, belongs to the scope of protection of the invention.
Claims (10)
1. a kind of Graphene-CdLa2S4Composite visible light catalyst, it is characterised in that it includes Graphene and photochemical catalyst, institute
State photochemical catalyst and be attached to the graphene sheet layer, the photochemical catalyst is CdLa2S4。
2. Graphene-CdLa according to claim 12S4Composite visible light catalyst, it is characterised in that the CdLa2S4
It is Nano microsphere CdLa2S4。
3. Graphene-CdLa according to claim 22S4Composite visible light catalyst, it is characterised in that the nanometer is micro-
Ball CdLa2S4By oval CdLa2S4Nanoparticle aggregate is formed.
4. Graphene-the CdLa described in a kind of any one of claims 1 to 32S4The preparation technology of composite visible light catalyst, its
It is characterised by, comprises the following steps：
S1 steps：Prepare graphene oxide solution；
S2 steps：The first mixed liquor is made to cadmium acetate and lanthanum nitrate is added in the graphene oxide solution；
S3 steps：After by thiocarbamide and polyvinylpyrrolidone dissolving in deionized water, ethylene glycol is added to be made the second mixed liquor；
S4 steps：First mixed liquor and second mixed liquor are mixed, and after adjusting pH to 8~11, is obtained the 3rd and is mixed
Close liquid；
S5 steps：3rd mixed liquor is obtained into the 4th mixed liquor after the heating 3~9 minutes of 800 watts of micro-wave oven；Wherein,
The heating is carried out several times, is heated 8~12 seconds every time, is spaced 8~12 seconds per between heating twice；And
S6 steps：4th mixed liquor is scrubbed, dry after obtain the Graphene-CdLa2S4Composite visible light catalyst.
5. Graphene-CdLa according to claim 42S4The preparation technology of composite visible light catalyst, it is characterised in that
In S1 steps, the concentration of the graphene oxide solution is 8~12mg/ml.
6. Graphene-CdLa according to claim 42S4The preparation technology of composite visible light catalyst, it is characterised in that
In S2 steps, when being made first mixed liquor, the consumption of the graphene oxide solution, the cadmium acetate and the lanthanum nitrate
Than being 18~25ml：0.24~0.26mmol：0.48~0.52mmol.
7. Graphene-CdLa according to claim 62S4The preparation technology of composite visible light catalyst, it is characterised in that
In S2 steps, when being made first mixed liquor, the consumption of the graphene oxide solution, the cadmium acetate and the lanthanum nitrate
Than being 20ml：0.25mmol：0.5mmol.
8. Graphene-CdLa according to claim 42S4The preparation technology of composite visible light catalyst, it is characterised in that
In S3 steps, when being made second mixed liquor, the thiocarbamide, the polyvinylpyrrolidone, the deionized water and described
The amount ratio of ethylene glycol is 1~2mmol：0.001~0.003g：2~10ml：90~150ml.
9. Graphene-CdLa according to claim 42S4The preparation technology of composite visible light catalyst, it is characterised in that
In S4 steps, when three mixed liquor is obtained, first mixed liquor is 1 with the volume ratio of second mixed liquor：5~6.
10. Graphene-CdLa according to claim 42S4The preparation technology of composite visible light catalyst, it is characterised in that
PH to 8~11 is adjusted using ammoniacal liquor in the S4 steps.
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