CN103623849A - Graphene/BiOCl<x>Br<1-x> micro-nano compound photocatalyst and preparation method thereof - Google Patents
Graphene/BiOCl<x>Br<1-x> micro-nano compound photocatalyst and preparation method thereof Download PDFInfo
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- CN103623849A CN103623849A CN201310539758.8A CN201310539758A CN103623849A CN 103623849 A CN103623849 A CN 103623849A CN 201310539758 A CN201310539758 A CN 201310539758A CN 103623849 A CN103623849 A CN 103623849A
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Abstract
The invention relates to a graphene/BiOCl<x>Br<1-x> micro-nano compound photocatalyst and a preparation method thereof. The photocatalyst is a compound photocatalyst which takes graphene as a carrier and is loaded with BiOCl<x>Br<1-x> micro-nanospheres, wherein Cl:Br is equal to 7:3. Through reductive modification of oxidized graphene, the photocatalyst has stronger electron transport capacity. By carrying out loading modification on the graphene surface with the BiOCl<x>Br<1-x> micro-nanospheres, migration of photon-generated electrons from BiOCl<x>Br<1-x> to the graphene surface is promoted. The prepared graphene-loaded BiOCl<x>Br<1-x> photocatalyst has high ultraviolet and visible light photocatalytic activities.
Description
Technical field
The present invention relates to a kind of photochemical catalyst and preparation method thereof, relate in particular to a kind of Graphene/BiOCl
xbr
1-xmicro-nano composite photo-catalyst and preparation method thereof.
Background technology
Since having delivered, Fujishima in 1972 etc. utilize TiO
2since the achievement in research of electrode photocatalysis hydrogen production, nano semiconductor material photocatalysis technology is subject to showing great attention to of lot of domestic and foreign scholar, modern industry and economic develop rapidly, the negative effect that environment is caused also becomes seriously, photocatalysis technology as a kind of novel method to environmental pollutants and the utilization of regenerative resource there is good prospect.
Photochemical catalyst based on Bi system has been developed and recently for clean environment field, as a kind of novel visible light-responded photochemical catalyst, BiOX(X is Cl, Br, I) photochemical catalyst has unique electronic structure and band structure because of it, under Uv and visible light irradiates, aspect photocatalytically degradating organic dye, shows the catalytic degradation performance that is better than other type semiconductor; But activity is lower when degradating organic dye for independent BiOX (X is Cl, Br, I), research shows BiOI
xcl
1-x(Dalton Trans.2011,40,6751-6758), BiOBr
xi
1-x(Catal. Commun.2011,13, than single BiOX(X, be all 63-68) Cl, Br, I)) catalytic activity want high.
Various material with carbon elements, comprise active carbon, carbon black, and graphite, CNT (CNTs) plays an important role in heterogeneous catalysis, no matter is as catalyst or catalyst carrier; Graphene, a kind of novel material with carbon element, its crystal structure is the sp of individual layer
2the alveolate texture of the carbon atom densification of-hydridization, in basic research and industrial application, it has been produced to great interest, concerning charge carrier, Graphene can be used as excellent conductive channel, Graphene is compared metal and is had carrier mobility faster, add the special physics and chemistry character of Graphene, make it aspect catalysis, there is good application prospect; Because composite semiconductor has the carrier separation effectively that the system of making produces under optical excitation, the effect that has extended the time-to-live of photohole, is conducive to the raising of semiconductor degradation of organic substances photocatalytic activity; So in the present invention, we have prepared the Graphene/BiOCl of high catalytic performance by an easy hydrothermal method
xbr
1-xnano composite photocatalytic material.
Summary of the invention
The object of this invention is to provide a kind of Graphene/BiOCl
xbr
1-xmicro-nano composite photo-catalyst and preparation method thereof, the method is with graphene oxide, and bismuth salt is raw material, adds He Lv source, a certain proportion of bromine source, reduced graphene oxide serving synthetic BiOCl under hydrothermal reaction condition
xbr
1-x, obtain Graphene/BiOCl
xbr
1-xmicro-nano composite photo-catalyst, this preparation method is simple, convenient, efficient.
Technical scheme of the present invention is as follows:
(1) graphene oxide is synthetic: with native graphite, be raw material, in ice bath, add while stirring a certain amount of 365 concentrated sulfuric acids, sodium nitrate also stirs a period of time, then slowly add a certain amount of potassium permanganate, after potassium permanganate dissolves completely, reaction system is transferred to 35 ℃ of stirred in water bath and react half an hour, in the reaction system that a certain amount of deionized water is added slowly, continue to stir, add again a certain amount of hydrogenperoxide steam generator, finally above-mentioned solution centrifugal is filtered, repeatedly wash with water, until solution is extremely neutral after PH test paper test washing, be dried and can make graphene oxide,
(2) prepare graphene oxide dispersion liquid: the ratio by graphene oxide with 0.1 g/L-0.3 g/L is distributed in organic solvent and carries out ultrasonic processing;
(3) by Bi (NO
3)
35H
2o is dissolved in the ethylene glycol solution that contains ,Lv source, bromine source and is stirred to evenly, forms stabilizing solution;
(4) the graphene oxide dispersion liquid that is 1:1 by volume ratio mixes with stabilizing solution is ultrasonic, then the solution mixing is poured into in teflon-lined stainless steel cauldron, and is reacted at a certain temperature naturally cooling after a period of time;
(5) utilize deionized water to carry out repeatedly after centrifuge washing product, by the dry micro-nano composite photocatalyst material of Graphene/BiOClxBr1-x that obtains of product.
The organic solvent of described step (2) refers to the mixed solvent that ethanol, ethylene glycol or ethanol and ethylene glycol volume ratio are 1:1; Ultrasonic 30 ~ 60min.
In described step (3), in every liter of stabilizing solution, contain bismuth salt Bi (NO
3)
35H
2o9-40g, He Xiu source, chlorine source is respectively tetradecyl trimethyl ammonium chloride (TTAC) and softex kw (CTAB), the ratio of both amount of substances is 7:3, and the sum of TTAC and CTAB amount of substance equals the amount of substance of bismuth salt.
Stirring in described step (3) is magnetic agitation, and the time is 10 ~ 30min.
In described step (4), reaction temperature is 160 ℃-200 ℃, and the reaction time is 12h-24h.
Described product Graphene/BiOClxBr1-x, wherein x=0.7; Graphene and BiOCl
xbr
1-xthe ratio of the amount of physics is 1:1-10.
This method have technique simply, the advantage such as rapidly and efficiently, by BiOCl
xbr
1-xwell be coated on graphene nanometer sheet; Graphene/BiOCl that the present invention prepares
xbr
1-xmicro-nano composite photocatalyst material crystallinity is good, and appearance and size is controlled; Graphene/BiOCl that this method is synthetic
xbr
1-xmicro-nano composite photocatalyst material has potential using value aspect photocatalytically degradating organic dye; For 1 * 10
-1mol/L Rh B solution, in the time of 90 minutes, degradation rate reaches 95%, and degradation effect is better than simple BiOCl
xbr
1-x, have good catalytic degradation effect.
Accompanying drawing explanation
Fig. 1 be embodiment 1 prepare Graphene/BiOCl
xbr
1-xthe X ray diffracting spectrum of micro-nano composite photocatalyst material;
Fig. 2 is the Graphene/BiOCl of embodiment 1 preparation
xbr
1-xthe electron scanning micrograph of micro-nano composite photocatalyst material;
Fig. 3 be prepare Graphene/BiOCl
xbr
1-xthe UV-vis spectrogram of micro-nano composite photocatalyst material;
Fig. 4 be prepare Graphene/BiOCl
xbr
1-xdegrade under the visible ray photocatalysis effect figure of RhB of micro-nano composite photocatalyst material.
The specific embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Graphene oxide is distributed in ethanol, and ultrasonic processing 30min, obtains the graphene oxide dispersion liquid of 30ml, the graphene oxide that contains 3 mg; By 1.2g Bi (NO
3)
35H
2o be dissolved in containing in the ethylene glycol solution of 0.51g TTAC and 0.27g CTAB and magnetic agitation 10min form the stabilizing solution of 30 mL, then mixes with graphene oxide solution, ultrasonic even; Mixed solution is poured into in teflon-lined stainless steel cauldron, reactor is put into baking oven, 160 ℃ of temperature, 24 hours reaction time; Question response finishes, and reactor is down to room temperature, by centrifuge, washs, and wash solution is distilled water and absolute ethyl alcohol, and centrifugal number of times 3 ~ 5 times, puts into baking oven by sample, dries for 60 ℃, can obtain Graphene/BiOCl
0.7br
0.3micro-nano composite photocatalyst material.
Graphene oxide is distributed in the mixed solution that ethanol and ethylene glycol volume ratio are 1:1, and ultrasonic processing 60 min, obtain the graphene oxide dispersion liquid of 30ml, the graphene oxide that contains 6 mg; By 1.2g Bi (NO
3)
35H
2o be dissolved in containing in the ethylene glycol solution of 0.51 g TTAC and 0.27 g CTAB and magnetic agitation 20min form the stabilizing solution of 30 mL, then mixes with graphene oxide solution, ultrasonic even; Mixed solution is poured into in teflon-lined stainless steel cauldron, reactor is put into baking oven, 180 ℃ of temperature, 18 hours reaction time.Question response finishes, and reactor is down to room temperature, by centrifuge, washs, and wash solution is distilled water and absolute ethyl alcohol, and centrifugal number of times 3 ~ 5 times, puts into baking oven by sample, dries for 60 ℃.Can obtain Graphene/BiOCl
0.7br
0.3micro-nano composite photocatalyst material.
Graphene oxide is distributed in ethylene glycol, and ultrasonic processing 45min, obtains the graphene oxide dispersion liquid of 30ml, the graphene oxide that contains 6 mg; By 0.485 g Bi (NO
3)
35H
2o be dissolved in containing in the ethylene glycol solution of 0.2 g TTAC and 0.11 g CTAB and magnetic agitation 20min form the stabilizing solution of 30 mL, then mixes with graphene oxide solution, ultrasonic even; Mixed solution is poured into in teflon-lined stainless steel cauldron, reactor is put into baking oven, 180 ℃ of temperature, 18 hours reaction time.Question response finishes, and reactor is down to room temperature, by centrifuge, washs, and wash solution is distilled water and absolute ethyl alcohol, and centrifugal number of times 3 ~ 5 times, puts into baking oven by sample, dries for 60 ℃.Can obtain Graphene/BiOCl
0.7br
0.3micro-nano composite photocatalyst material.
Embodiment 4
Graphene oxide is distributed in ethanol, and ultrasonic processing 60min, obtains the graphene oxide dispersion liquid of 30ml, the graphene oxide that contains 9mg; By 0.36 g Bi (NO
3)
35H
2o be dissolved in containing in the ethylene glycol solution of 0.15g TTAC and 0.08g CTAB and magnetic agitation 30min form the stabilizing solution of 30 mL, then mixes with graphene oxide solution, ultrasonic even; Mixed solution is poured into in teflon-lined stainless steel cauldron, reactor is put into baking oven, 200 ℃ of temperature, 12 hours reaction time.Question response finishes, and reactor is down to room temperature, by centrifuge, washs, and wash solution is distilled water and absolute ethyl alcohol, and centrifugal number of times 3 ~ 5 times, puts into baking oven by sample, dries for 60 ℃.Can obtain Graphene/BiOCl
0.7br
0.3micro-nano composite photocatalyst material.
Photocatalysis experiment
Prepared to Graphene/BiOCl in order to check
xbr
1-xthe degradation property of micro-nano composite photocatalyst material, the present invention selects rhodamine B as photocatalytic degradation object.Respectively the sample in embodiment is carried out to Photocatalytic Degradation Property test, the catalyst of preparing with embodiment 1-4 is numbered respectively 0#, 1#, and 2#, the 3# rhodamine B in degradation water (Rh B) molecule under visible ray condition is evaluated.Light source is the xenon lamp of 500W, by 1 * 10 of 100mL
-1mol/LRh B solution is put into beaker, adds the photochemical catalyst of 0.05g, and the ultrasonic mark 10min of lucifuge stirs 20min, makes Rh B reach adsorption equilibrium in photocatalyst surface.Turn on light to irradiate and carry out photocatalytic degradation reaction, after 3 hours, sample respectively 4mL, with centrifuge centrifugation catalyst granules, get supernatant, with UV-vis spectrophotometer, monitor the absorbance of Rh B, and then follow the tracks of the change in concentration of Rh B in solution, obtain the activity figure of photocatalytic degradation RhB.
Fig. 1, Fig. 2 proves and has successfully prepared Graphene/BiOCl from composition and structure
xbr
1-xmicro-nano composite photocatalyst material; Fig. 3, Fig. 4 is by different uv drses, and photocatalysis effect figure illustrates embodiment 3 Graphenes and BiOCl
xbr
1-xthe ratio of the amount of physics has best visible light photocatalysis effect while being 1:5, for 1 * 10
-1mol/LRh B solution, in the time of 90 minutes, degradation rate reaches 95%.
Claims (7)
1. a Graphene/BiOCl
xbr
1-xmicro-nano composite photo-catalyst, with graphene oxide, bismuth salt, ，Lv source, bromine source is raw material, it is characterized in that reduced graphene oxide serving synthetic BiOCl under hydrothermal reaction condition
xbr
1-x, obtaining take Graphene as carrier, load has BiOCl
xbr
1-xthe composite photocatalyst of micro-nano ball.
2. a kind of Graphene/BiOCl as claimed in claim 1
xbr
1-xthe preparation method of micro-nano composite photo-catalyst, is characterized in that, comprises the steps:
(1) prepare graphene oxide dispersion liquid: graphene oxide is distributed in organic solvent and carries out the graphene oxide dispersion liquid that ultrasonic processing obtains 0.1 g/L-0.3 g/L;
(2) by Bi (NO
3)
35H
2o is dissolved in the ethylene glycol solution that contains ,Lv source, bromine source and is stirred to evenly, forms stabilizing solution;
(3) the graphene oxide dispersion liquid that is 1:1 by volume ratio mixes with stabilizing solution is ultrasonic, then the solution mixing is poured into reacting in teflon-lined stainless steel cauldron, and reaction finishes rear naturally cooling;
(4) utilize deionized water to carry out centrifuge washing to product, after being dried, obtain the micro-nano composite photocatalyst material of Graphene/BiOClxBr1-x.
3. a kind of Graphene/BiOCl as claimed in claim 2
xbr
1-xthe preparation method of micro-nano composite photo-catalyst, is characterized in that, in step (1), organic solvent refers to the mixed solvent that ethanol, ethylene glycol or ethanol and ethylene glycol volume ratio are 1:1; Ultrasonic time is 30 ~ 60min.
4. a kind of Graphene/BiOCl as claimed in claim 2
xbr
1-xthe preparation method of micro-nano composite photo-catalyst, it is characterized in that, in step (2), He Xiu source, described chlorine source is respectively tetradecyl trimethyl ammonium chloride and softex kw, the ratio of both amount of substances is 7:3, and TTAC amount of substance and CTAB amount of substance sum equal the amount of substance of bismuth salt; In described every liter of stabilizing solution, contain bismuth salt Bi (NO
3)
35H
2o 9-40g.
5. a kind of Graphene/BiOCl as claimed in claim 2
xbr
1-xthe preparation method of micro-nano composite photo-catalyst, is characterized in that, in step (2), described stirring is magnetic agitation, and the time is 10 ~ 30min.
6. a kind of Graphene/BiOCl as claimed in claim 2
xbr
1-xthe preparation method of micro-nano composite photo-catalyst, is characterized in that, in step (3), described reaction temperature is 160-200 ℃, and the reaction time is 12-24h.
7. a kind of Graphene/BiOCl as claimed in claim 2
xbr
1-xthe preparation method of micro-nano composite photo-catalyst, is characterized in that, described product Graphene/BiOCl
xbr
1-x, x=0.7 wherein; Graphene and BiOCl
xbr
1-xthe ratio of the amount of physics is 1:1-10.
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