CN103623849B - A kind of Graphene/BiOCl xbr 1-xmicro-nano composite photo-catalyst and preparation method thereof - Google Patents
A kind of Graphene/BiOCl xbr 1-xmicro-nano composite photo-catalyst and preparation method thereof Download PDFInfo
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- CN103623849B CN103623849B CN201310539758.8A CN201310539758A CN103623849B CN 103623849 B CN103623849 B CN 103623849B CN 201310539758 A CN201310539758 A CN 201310539758A CN 103623849 B CN103623849 B CN 103623849B
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Abstract
The present invention relates to a kind of Graphene/BiOCl
xbr
1-xmicro-nano composite photo-catalyst and preparation method thereof.This photochemical catalyst is carrier with Graphene, and load has BiOCl
xbr
1-xthe composite photocatalyst of micro-nano ball: wherein Cl:Br=7:3, to the modified with reduction of graphene oxide, makes it have stronger electron transport ability; BiOCl is carried out to graphenic surface
xbr
1-xmicro-nano ball loaded modified, facilitates light induced electron from BiOCl
xbr
1-xto the migration of graphenic surface, the graphene-supported BiOCl of preparation
xbr
1-xphotochemical catalyst has high ultraviolet and visible light photocatalysis active.
Description
Technical field
The present invention relates to a kind of photochemical catalyst and preparation method thereof, particularly relate to a kind of Graphene/BiOCl
xbr
1-xmicro-nano composite photo-catalyst and preparation method thereof.
Background technology
TiO is utilized since Fujishima in 1972 etc. have delivered
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, the develop rapidly of modern industry and economy, the negative effect that environment causes also is become serious, 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, show the catalytic degradation performance being better than other type semiconductor in photocatalytically degradating organic dye; But activity is lower when degradating organic dye for independent BiOX (X is Cl, Br, I), research shows BiOI
xcl
1-x(DaltonTrans.2011,40,6751-6758), BiOBr
xi
1-x(Catal.Commun.2011,13,63-68) is all Cl than single BiOX(X, Br, I)) catalytic activity want high.
Various material with carbon element, comprises active carbon, carbon black, graphite, and 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, to which creating great interest, can as the conductive channel of excellence concerning Graphene charge carrier, Graphene is compared metal and is had carrier mobility faster, add the physics and chemistry character that Graphene is special, make it in catalysis, have good application prospect; Effectively be separated because composite semiconductor has the carrier making system produce under optical excitation, extend the effect of the time-to-live of photohole, be 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 a certain proportion of bromine source and chlorine source, and reduced graphene oxide serving under hydrothermal reaction condition also synthesizes BiOCl
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) synthesis of graphene oxide: be raw material with native graphite, in ice bath, add a certain amount of 365 concentrated sulfuric acids while stirring, sodium nitrate also stirs a period of time, then a certain amount of potassium permanganate is slowly added, after potassium permanganate dissolves completely, reaction system is transferred to 35 DEG C 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 a certain amount of hydrogenperoxide steam generator again, finally above-mentioned solution centrifugal is filtered, repeatedly wash with water, until solution is extremely neutral after PH test paper test washing, drying can obtain graphene oxide,
(2) graphene oxide dispersion is prepared: to be distributed in organic solvent with the ratio of 0.1g/L-0.3g/L by graphene oxide and to carry out ultrasonic process;
(3) by Bi (NO
3)
35H
2o to be dissolved in the ethylene glycol solution containing bromine source, chlorine source and to be stirred to evenly, forms stabilizing solution;
(4) be that the graphene oxide dispersion of 1:1 mixes with stabilizing solution is ultrasonic by volume ratio, then the solution mixed poured into in teflon-lined stainless steel cauldron, and cooling naturally after reacting a period of time at a certain temperature;
(5), after utilizing deionized water to carry out repeatedly centrifuge washing to product, product drying is obtained the micro-nano composite photocatalyst material of Graphene/BiOClxBr1-x.
The organic solvent of described step (2) refers to that ethanol, ethylene glycol or ethanol and ethylene glycol volume ratio are the mixed solvent of 1:1; Ultrasonic 30 ~ 60min.
Bismuth salt Bi (NO is contained in often liter of stabilizing solution in described step (3)
3)
35H
2o9-40g, chlorine source and bromine source are tetradecyl trimethyl ammonium chloride (TTAC) and softex kw (CTAB) respectively, and 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 DEG C-200 DEG C, 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/the BiOCl of this method synthesis
xbr
1-xmicro-nano composite photocatalyst material has potential using value in photocatalytically degradating organic dye; For 1 × 10
-1mol/LRhB solution, when 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 Graphene/BiOCl prepared by embodiment 1
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-xmicro-nano composite photocatalyst material is degraded the photocatalysis effect figure of RhB under visible light.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Embodiment 1
Be distributed to by graphene oxide in ethanol, ultrasonic process 30min, obtains the graphene oxide dispersion of 30ml, the graphene oxide containing 3mg; By 1.2gBi (NO
3)
35H
2o is dissolved in the stabilizing solution of also magnetic agitation 10min formation 30mL in the ethylene glycol solution containing 0.51gTTAC and 0.27gCTAB, then mixes with graphene oxide solution, evenly ultrasonic; Mixed solution is poured into in teflon-lined stainless steel cauldron, reactor is put into baking oven, temperature 160 DEG C, 24 hours reaction time; Question response terminates, and room temperature is down to by reactor, is washed by centrifuge, 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 DEG C, can obtain Graphene/BiOCl
0.7br
0.3micro-nano composite photocatalyst material.
Embodiment 2
Graphene oxide is distributed to ethanol and ethylene glycol volume ratio is in the mixed solution of 1:1, ultrasonic process 60min, obtains the graphene oxide dispersion of 30ml, the graphene oxide containing 6mg; By 1.2gBi (NO
3)
35H
2o is dissolved in the stabilizing solution of also magnetic agitation 20min formation 30mL in the ethylene glycol solution containing 0.51gTTAC and 0.27gCTAB, then mixes with graphene oxide solution, evenly ultrasonic; Mixed solution is poured into in teflon-lined stainless steel cauldron, reactor is put into baking oven, temperature 180 DEG C, 18 hours reaction time.Question response terminates, and room temperature is down to by reactor, is washed by centrifuge, 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 DEG C.Graphene/BiOCl can be obtained
0.7br
0.3micro-nano composite photocatalyst material.
Embodiment 3
Be distributed to by graphene oxide in ethylene glycol, ultrasonic process 45min, obtains the graphene oxide dispersion of 30ml, the graphene oxide containing 6mg; By 0.485gBi (NO
3)
35H
2o is dissolved in the stabilizing solution of also magnetic agitation 20min formation 30mL in the ethylene glycol solution containing 0.2gTTAC and 0.11gCTAB, then mixes with graphene oxide solution, evenly ultrasonic; Mixed solution is poured into in teflon-lined stainless steel cauldron, reactor is put into baking oven, temperature 180 DEG C, 18 hours reaction time.Question response terminates, and room temperature is down to by reactor, is washed by centrifuge, 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 DEG C.Graphene/BiOCl can be obtained
0.7br
0.3micro-nano composite photocatalyst material.
Embodiment 4
Be distributed to by graphene oxide in ethanol, ultrasonic process 60min, obtains the graphene oxide dispersion of 30ml, the graphene oxide containing 9mg; By 0.36gBi (NO
3)
35H
2o is dissolved in the stabilizing solution of also magnetic agitation 30min formation 30mL in the ethylene glycol solution containing 0.15gTTAC and 0.08gCTAB, then mixes with graphene oxide solution, evenly ultrasonic; Mixed solution is poured into in teflon-lined stainless steel cauldron, reactor is put into baking oven, temperature 200 DEG C, 12 hours reaction time.Question response terminates, and room temperature is down to by reactor, is washed by centrifuge, 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 DEG C.Graphene/BiOCl can be obtained
0.7br
0.3micro-nano composite photocatalyst material.
Photocatalysis is tested
What obtain in order to inspection institute arrives Graphene/BiOCl
xbr
1-xthe degradation property of micro-nano composite photocatalyst material, the present invention selects rhodamine B as photocatalytic degradation object.Carry out Photocatalytic Degradation Property test to the sample in embodiment respectively, the catalyst prepared with embodiment 1-4 respectively numbering 0#, 1#, 2#, the 3# rhodamine B under visible light conditions in degradation water (RhB) molecule is evaluated.Light source is the xenon lamp of 500W, by 1 × 10 of 100mL
-1mol/LRhB solution puts into beaker, adds the photochemical catalyst of 0.05g, the ultrasonic mark 10min of lucifuge, stirs 20min, makes RhB reach adsorption equilibrium in photocatalyst surface.Photocatalytic degradation reaction is carried out in irradiation of turning on light, and samples 4mL respectively after 3 hours, uses centrifuge separating catalyst particles, get supernatant, by the absorbance of UV-vis spectrophotometer monitoring RhB, and then follow the tracks of the change in concentration of RhB in solution, obtain the activity figure of photocatalytic degradation RhB.
Fig. 1, Fig. 2 prove successfully to have prepared Graphene/BiOCl from composition and structure
xbr
1-xmicro-nano composite photocatalyst material; Fig. 3, Fig. 4 are by different uv drses, and photocatalysis effect figure illustrates embodiment 3 Graphene and BiOCl
xbr
1-xthe ratio of the amount of physics has best visible light photocatalysis effect when being 1:5, for 1 × 10
-1mol/LRhB solution, when 90 minutes, degradation rate reaches 95%.
Claims (4)
1. Graphene/BiOCl
xbr
1-xthe preparation method of micro-nano composite photo-catalyst, described Graphene/BiOCl
xbr
1-xmicro-nano composite photo-catalyst, with graphene oxide, bismuth salt, bromine source, chlorine source is raw material, and reduced graphene oxide serving under hydrothermal reaction condition also synthesizes BiOCl
xbr
1-x, obtaining with Graphene is carrier, and load has BiOCl
xbr
1-xthe composite photocatalyst of micro-nano ball, is characterized in that, comprises the steps:
(1) graphene oxide dispersion is prepared: to be distributed to by graphene oxide in organic solvent and to carry out the graphene oxide dispersion that ultrasonic process obtains 0.1g/L-0.3g/L;
(2) by Bi (NO
3)
35H
2o to be dissolved in the ethylene glycol solution containing bromine source, chlorine source and to be stirred to evenly, forms stabilizing solution;
(3) be that the graphene oxide dispersion of 1:1 mixes with stabilizing solution is ultrasonic by volume ratio, then poured into by the solution mixed and react with in teflon-lined stainless steel cauldron, reaction terminates rear cooling naturally;
(4) utilize deionized water to carry out centrifuge washing to product, after drying, obtain Graphene/BiOCl
xbr
1-xmicro-nano composite photocatalyst material;
In step (2), described chlorine source and bromine source are tetradecyl trimethyl ammonium chloride and softex kw respectively, and 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; Containing bismuth salt Bi (NO in described often liter of stabilizing solution
3)
35H
2o9-40g;
Described product Graphene/BiOCl
xbr
1-x, wherein x=0.7; Graphene and BiOCl
xbr
1-xthe ratio of amount of substance is 1:1-10.
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, in step (1), organic solvent refers to that ethanol, ethylene glycol or ethanol and ethylene glycol volume ratio are the mixed solvent of 1:1; Ultrasonic time is 30 ~ 60min.
3. 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, in step (2), described stirring is magnetic agitation, and the time is 10 ~ 30min.
4. 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, in step (3), described reaction temperature is 160-200 DEG C, and the reaction time is 12-24h.
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