CN102941105A - Preparation method for bismuth oxyiodide/graphene oxide compound visible light catalytic material - Google Patents
Preparation method for bismuth oxyiodide/graphene oxide compound visible light catalytic material Download PDFInfo
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- CN102941105A CN102941105A CN2012104828144A CN201210482814A CN102941105A CN 102941105 A CN102941105 A CN 102941105A CN 2012104828144 A CN2012104828144 A CN 2012104828144A CN 201210482814 A CN201210482814 A CN 201210482814A CN 102941105 A CN102941105 A CN 102941105A
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Abstract
A preparation method for a bismuth oxyiodide/graphene oxide compound visible light catalytic material relates to a preparation method of the visible light catalytic material. The preparation method aims at solving the problems in the compound light catalytic material prepared through the existing method of being complex in operation, long in periodicity, high in requirement for devices and not suitable for large-scale production. The bismuth oxyiodide/graphene oxide compound visible light catalytic material is prepared through iodide, Bi(NO3)3-5H2O and the graphene oxide dispersion liquid. The method includes: 1 preparing graphene oxide dispersion liquid; 2 mixing and stirring iodide, Bi(NO3)3-5H2O and the graphene oxide dispersion liquid to obtain turbid liquid; and 3 conducting ultrasonic processing, then filtering, washing and drying sequentially to obtain the bismuth oxyiodide/graphene oxide compound visible light catalytic material. The preparation method is mainly used for preparing the bismuth oxyiodide/graphene oxide compound visible light catalytic material.
Description
Technical field
The present invention relates to a kind of preparation method of visible light catalytic material.
Background technology
In recent years, be accompanied by the development of modern industry and the raising of living standards of the people, environmental contaminants, organic wastewater, soil pollution etc. are day by day serious on the impact of environment and human health, and the whole world faces the severe challenge of energy crisis and environmental pollution.Therefore, technology is polluted in the improvement of exploitation practicality and high efficiency rate has become facing mankind and key subjects to be solved has been arranged.The people such as 20 century 70s Japan scientist Fijishima and Honda have delivered about n-type semiconductor TiO
2The paper of photodissociation water on the electrode is with TiO
2Headed by nano semiconductor material obtained various countries scientist's extensive concern as photochemical catalyst.Although TiO
2Have low price, nontoxic, to organic matter degradation non-selectivity in the water pollutant, mineralising thoroughly, the advantage such as non-secondary pollution, still, TiO
2Energy gap is wider, can only absorb the sunshine medium wavelength less than the ultraviolet light of 387nm, only has about 3% ~ 5% sunshine to be utilized, and this has limited TiO to a great extent
2Application, therefore, in the urgent need to the development of new catalysis material.
Halogenation oxygen bismuth BiOX(X=F, Cl, Br, I) be a kind of highly anisotropic layer structure semiconductor that has.Its photocatalytic activity generally is better than TiO
2And along with the increase photocatalytic activity of halogen atom ordinal number strengthens gradually, wherein, that catalytic efficiency is the highest is the BiOI of energy gap narrower (1.7-1.9eV) (P25); Be that " composite photo-catalyst BiOCl/BiOI and preparation method thereof " (application number is: CN201110077156.6 at patent name, inventor: prepare composite photo-catalyst BiOCl/BiOI Chen Gang etc.), the 20%BiOCl/BiOI methyl orange of degrading in 30min can reach 93%, has very high photocatalysis performance, what but this patent system Preparation Method was taked is two step synthetic methods, go out the BiOI powder with the hydro-thermal legal system is standby first, again with NaCl, Bi (NO
3)
3Ethanolic solution mix, hydro-thermal method is prepared composite photo-catalyst BiOCl/BiOI.This causes this preparation process complicated operation, and is periodically long, high to equipment requirement, is not suitable for large-scale industrial production.
Summary of the invention
There is complicated operation in the composite photo-catalyst that the objective of the invention is to solve existing method preparation, periodically long, high to equipment requirement, be not suitable for the problem of large-scale production, and the preparation method of a kind of bismuthyl iodide/graphene oxide composite visible light catalysis material is provided.
The preparation method of a kind of bismuthyl iodide/graphene oxide composite visible light catalysis material, specifically finish according to the following steps: one, preparation graphene oxide dispersion liquid: at first take graphite powder as raw material adopts improved Hummers method make graphite oxide, then be under 40Hz ~ 250Hz graphite oxide to be scattered in the deionized water in supersonic frequency, ultrasonic jitter time is 1h ~ 3h, and namely obtaining concentration is the graphene oxide dispersion liquid of 0.1mg/mL ~ 1.0mg/mL; Two, the concentration that iodide is added step 1 preparation is in the graphene oxide dispersion liquid of 0.1mg/mL ~ 1.0mg/mL, and low whipping speed is to stir 10min ~ 50min under 200r/min ~ 900r/min, adds Bi (NO again
3)
35H
2O, and to continue low whipping speed be mix and blend 10min ~ 60min under 200r/min ~ 900r/min, makes suspension; Three, be that 60 ℃ ~ 90 ℃, supersonic frequency are that 40Hz ~ 250Hz and mixing speed are that the suspension that under 200r/min ~ 900r/min condition step 2 is obtained carries out ultrasonic processing at bath temperature, the ultrasonic processing time is 1h ~ 3h, then filter, the brick-red precipitation that filtration obtains adopts deionized water washing 2 ~ 6 times, then be 40 ℃ ~ 80 ℃ dry 12h ~ 36h in temperature, namely obtain bismuthyl iodide/graphene oxide composite visible light catalysis material; The iodide that add described in the step 2 and the mass ratio of the graphite oxide described in the step 1 are (50 ~ 200): 1; I in the iodide that add described in the step 2
-With Bi (NO
3)
35H
2Bi among the O
3+Mol ratio be (0.9 ~ 1.1): 1.
Advantage of the present invention: one, the present invention is by ultrasonic dispersion, mechanical agitation, first two kinds of raw materials are evenly mixed, then utilize one step of hydrolysis to make bismuthyl iodide/graphene oxide composite material, its advantage is that raw material is common and is easy to get, with low cost, preparation process is simple and safe, reduces equipment requirement, can realize large-scale production; Two, the bismuthyl iodide of the present invention's preparation/graphene oxide composite visible light catalysis material, that the BiOI nanometer sheet is dispersed in the graphene oxide surface, both avoided the reunion of BiOI nanometer sheet, also effectively prevent the accumulation of graphene oxide sheet interlayer, and significantly improved the photocatalytic activity of BiOI behind BiOI nanometer sheet and graphene oxide compound.
Description of drawings
Fig. 1 is the degradation rate curve map over time of methyl orange, the degradation rate of methyl orange curve map over time when ■ represents not add photochemical catalyst among Fig. 1, among Fig. 1 ● the degradation rate of methyl orange curve map over time when expression adds BiOI as photochemical catalyst, among Fig. 1 ▲ the degradation rate curve map over time of methyl orange when expression adds the bismuthyl iodide of test one preparation/graphene oxide composite visible light catalysis material as photochemical catalyst.
The specific embodiment
The specific embodiment one: present embodiment is the preparation method of a kind of bismuthyl iodide/graphene oxide composite visible light catalysis material, specifically finish according to the following steps: one, preparation graphene oxide dispersion liquid: at first take graphite powder as raw material adopts improved Hummers method make graphite oxide, then be under 40Hz ~ 250Hz graphite oxide to be scattered in the deionized water in supersonic frequency, ultrasonic jitter time is 1h ~ 3h, and namely obtaining concentration is the graphene oxide dispersion liquid of 0.1mg/mL ~ 1.0mg/mL; Two, the concentration that iodide is added step 1 preparation is in the graphene oxide dispersion liquid of 0.1mg/mL ~ 1.0mg/mL, and low whipping speed is to stir 10min ~ 50min under 200r/min ~ 900r/min, adds Bi (NO again
3)
35H
2O, and to continue low whipping speed be mix and blend 10min ~ 60min under 200r/min ~ 900r/min, makes suspension; Three, be that 60 ℃ ~ 90 ℃, supersonic frequency are that 40Hz ~ 250Hz and mixing speed are that the suspension that under 200r/min ~ 900r/min condition step 2 is obtained carries out ultrasonic processing at bath temperature, the ultrasonic processing time is 1h ~ 3h, then filter, the brick-red precipitation that filtration obtains adopts deionized water washing 2 ~ 6 times, then be 40 ℃ ~ 80 ℃ dry 12h ~ 36h in temperature, namely obtain bismuthyl iodide/graphene oxide composite visible light catalysis material.
The iodide that add described in the present embodiment step 2 and the mass ratio of the graphite oxide described in the step 1 are (50 ~ 200): 1; I in the iodide that add described in the present embodiment step 2
-With Bi (NO
3)
35H
2Bi among the O
3+Mol ratio be (0.9 ~ 1.1): 1.
Improved Hummers method specific operation process described in the present embodiment step 1 is as follows: take by weighing graphite powder 2.5g, sodium nitrate 1.25g mixes grinding in mortar, and mixture added fill in the dry beaker of 57.5ml 98% concentrated sulfuric acid, put into the ice-water bath cooling, stir 30min; Take by weighing again potassium permanganate 7.5g porphyrize in mortar, slowly add under the strong agitation, continue to stir, remove ice-water bath after, adjust the temperature to about 35 ℃, constantly stir 30min; Slowly drip again 112.5ml warm water (about 40 ℃), then be warming up to 98 ℃; Add warm water (about 40 ℃) 180ml after under temperature is 98 ℃, reacting 1 hour mentioned solution is diluted to 350ml; The H that slowly adds again 10mL
2O
2(30%), become glassy yellow, suction filtration adopts 5%HCl to wash twice more while hot, then adopt deionization washing 3 times (to neutral, fully washing until in the filtrate without SO
4 2-), sample places on the surface plate, tiling, 50 ℃ of dryings 24 hours.
Present embodiment is by ultrasonic dispersion, mechanical agitation, first two kinds of raw materials are evenly mixed, then utilize one step of hydrolysis to make bismuthyl iodide/graphene oxide composite material, its advantage is that raw material is common and is easy to get, with low cost, preparation process is simple and safe, reduces equipment requirement, can realize large-scale production.
The bismuthyl iodide of present embodiment preparation/graphene oxide composite visible light catalysis material, that the BiOI nanometer sheet is dispersed in the graphene oxide surface, both avoided the reunion of BiOI nanometer sheet, also effectively prevent the accumulation of graphene oxide sheet interlayer, and significantly improved the photocatalytic activity of BiOI behind BiOI nanometer sheet and graphene oxide compound.
The specific embodiment two: the difference of present embodiment and the specific embodiment one is: be under 80Hz ~ 200Hz graphite oxide to be scattered in the deionized water in supersonic frequency in the step 1, ultrasonic jitter time is 1.5h ~ 2.5h, and namely obtaining concentration is the graphene oxide dispersion liquid of 0.1mg/mL～1.0mg/mL.Other are identical with the specific embodiment one.
The specific embodiment three: present embodiment and one of the specific embodiment one or two difference are: the mass ratio of graphite oxide described in the iodide that add described in the step 2 and the step 1 is (80 ~ 150): 1.Other are identical with the specific embodiment one or two.
The specific embodiment four: one of present embodiment and specific embodiment one to three difference is: the iodide described in the step 2 are KI or NaI.Other are identical with the specific embodiment one to three.
The specific embodiment five: one of present embodiment and specific embodiment one to four difference is: low whipping speed is to stir 20min ~ 40min under 300r/min ~ 700r/min in the step 2, adds Bi (NO again
3)
35H
2O, and to continue low whipping speed be mix and blend 20min ~ 50min under 300r/min ~ 700r/min, makes suspension.Other are identical with the specific embodiment one to four.
The specific embodiment six: one of present embodiment and specific embodiment one to five difference is: be that 70 ℃ ~ 80 ℃, supersonic frequency are that 80Hz ~ 200Hz and mixing speed are that the suspension that under 300r/min ~ 700r/min condition step 2 is obtained carries out ultrasonic processing at bath temperature in the step 3, the ultrasonic agitation time is 1.5h ~ 2.5h, then filter, the brick-red precipitation that filtration obtains adopts deionized water washing 3 ~ 5 times, and then temperature is 50 ℃ ~ 70 ℃ dry 18h ~ 30h, namely obtains bismuthyl iodide/graphene oxide composite visible light catalysis material.Other are identical with the specific embodiment one to five.
Adopt following verification experimental verification effect of the present invention:
Test one: the preparation method of a kind of bismuthyl iodide/graphene oxide composite visible light catalysis material, specifically finish according to the following steps: one, preparation graphene oxide dispersion liquid: at first take graphite powder as raw material adopts improved Hummers method make graphite oxide, then be under the 150Hz graphite oxide to be scattered in the deionized water in supersonic frequency, ultrasonic jitter time is 2h, and namely obtaining concentration is the graphene oxide dispersion liquid of 0.5mg/mL; Two, the concentration that iodide is added step 1 preparation is in the graphene oxide dispersion liquid of 0.5mg/mL, and then low whipping speed is to stir 30min under the 550r/min, adds Bi (NO again
3)
35H
2O, and to continue low whipping speed be mix and blend 35min under the 550r/min, makes suspension; Three, be that 80 ℃, supersonic frequency are that 150Hz and mixing speed are that the suspension that under the 440r/min condition step 2 is obtained carries out ultrasonic processing at bath temperature, ultrasonic time is 2h, then filter, the brick-red precipitation that filtration obtains adopts deionized water washing 4 times, and then temperature is 60 ℃ of dry 24h, namely obtains bismuthyl iodide/graphene oxide composite visible light catalysis material.
The iodide that add described in the present embodiment step 2 and the mass ratio of graphene oxide are 94:1; I in the iodide that add described in the present embodiment step 2
-With Bi (NO
3)
35H
2Bi among the O
3+Mol ratio be 1:1.
Improved Hummers method specific operation process described in the present embodiment step 1 is as follows: take by weighing graphite powder 2.5g, sodium nitrate 1.25g mixes grinding in mortar, and mixture added fill in the dry beaker of 57.5ml 98% concentrated sulfuric acid, put into the ice-water bath cooling, stir 30min; Take by weighing again potassium permanganate 7.5g porphyrize in mortar, slowly add under the strong agitation, continue to stir, remove ice-water bath after, adjust the temperature to about 35 ℃, constantly stir 30min; Slowly drip again 112.5ml warm water (about 40 ℃), then be warming up to 98 ℃; Add warm water (about 40 ℃) 180ml after under temperature is 98 ℃, reacting 1 hour mentioned solution is diluted to 350ml; The H that slowly adds again 10mL
2O
2(30%), become glassy yellow, suction filtration adopts 5%HCl to wash twice more while hot, then adopt deionization washing 3 times (to neutral, fully washing until in the filtrate without SO
4 2-), sample places on the surface plate, tiling, 50 ℃ of dryings 24 hours.
Adopt that photocatalytic reaction device detects the degradation rate of methyl orange when not adding photochemical catalyst, degradation rate and the degradation rate of methyl orange when adopting the bismuthyl iodide that this test prepares/graphene oxide composite visible light catalysis material as photochemical catalyst of methyl orange when adopting BiOI as photochemical catalyst, photocatalytic reaction device is furnished with the lamp box of 250W high-pressure sodium lamp, lamp source and liquid level of solution are at a distance of 15cm, agitating device is installed in lamp box, reaction vessel is that 250mL jacketed reactor and circulating water cooling device form, and detects the photocatalysis performance of sample and estimates by the degraded methyl orange solution; Light source is chosen suitable optical filter makes the optical wavelength that sees through greater than 420nm.Experiment I: get the methyl orange solution that 100mL concentration is 20mg/L, do not add photochemical catalyst, at radiation of visible light reaction 3h; Experiment II: get the methyl orange solution that 100mL concentration is 20mg/L, add BiOI as photochemical catalyst, at radiation of visible light reaction 3h; Experiment III: get the methyl orange solution that 100mL concentration is 20mg/L, add and test the bismuthyl iodide that a prepares/graphene oxide composite visible light catalysis material as photochemical catalyst, at radiation of visible light reaction 3h; Testing result is shown in 1, Fig. 1 is the degradation rate curve map over time of methyl orange, the degradation rate of methyl orange curve map over time when ■ represents not add photochemical catalyst among Fig. 1, among Fig. 1 ● the degradation rate of methyl orange curve map over time when expression adds BiOI as photochemical catalyst, among Fig. 1 ▲ the degradation rate curve map over time of methyl orange when expression adds the bismuthyl iodide of test one preparation/graphene oxide composite visible light catalysis material as photochemical catalyst; As shown in Figure 1 behind radiation of visible light 60min, the degradation rate of methyl orange can reach 95% when adding the bismuthyl iodide of test one preparation/graphene oxide composite visible light catalysis material as photochemical catalyst, and the degradation rate to methyl orange when adding BiOI as photochemical catalyst has improved 17.9 times.
Claims (6)
1. the preparation method of bismuthyl iodide/graphene oxide composite visible light catalysis material, the preparation method who it is characterized in that bismuthyl iodide/graphene oxide composite visible light catalysis material finishes according to the following steps: one, preparation graphene oxide dispersion liquid: at first take graphite powder as raw material adopts improved Hummers method make graphite oxide, then be under 40Hz ~ 250Hz graphite oxide to be scattered in the deionized water in supersonic frequency, ultrasonic jitter time is 1h ~ 3h, and namely obtaining concentration is the graphene oxide dispersion liquid of 0.1mg/mL ~ 1.0mg/mL; Two, the concentration that iodide is added step 1 preparation is in the graphene oxide dispersion liquid of 0.1mg/mL ~ 1.0mg/mL, and low whipping speed is to stir 10min ~ 50min under 200r/min ~ 900r/min, adds Bi (NO again
3)
35H
2O, and to continue low whipping speed be mix and blend 10min ~ 60min under 200r/min ~ 900r/min, makes suspension; Three, be that 60 ℃ ~ 90 ℃, supersonic frequency are that 40Hz ~ 250Hz and mixing speed are that the suspension that under 200r/min ~ 900r/min condition step 2 is obtained carries out ultrasonic processing at bath temperature, the ultrasonic processing time is 1h ~ 3h, then filter, the brick-red precipitation that filtration obtains adopts deionized water washing 2 ~ 6 times, then be 40 ℃ ~ 80 ℃ dry 12h ~ 36h in temperature, namely obtain bismuthyl iodide/graphene oxide composite visible light catalysis material; The iodide that add described in the step 2 and the mass ratio of the graphite oxide described in the step 1 are (50 ~ 200): 1; I in the iodide that add described in the step 2
-With Bi (NO
3)
35H
2Bi among the O
3+Mol ratio be (0.9 ~ 1.1): 1.
2. the preparation method of a kind of bismuthyl iodide according to claim 1/graphene oxide composite visible light catalysis material, it is characterized in that in the step 1 in supersonic frequency being under 80Hz ~ 200Hz graphite oxide to be scattered in the deionized water, ultrasonic jitter time is 1.5h ~ 2.5h, and namely obtaining concentration is the graphene oxide dispersion liquid of 0.1mg/mL ~ 1.0mg/mL.
3. the preparation method of a kind of bismuthyl iodide according to claim 2/graphene oxide composite visible light catalysis material is characterized in that the iodide that add described in the step 2 and the mass ratio of the graphite oxide described in the step 1 are (80 ~ 150): 1.
4. the preparation method of a kind of bismuthyl iodide according to claim 1/graphene oxide composite visible light catalysis material is characterized in that the iodide described in the step 2 are KI or NaI.
5. the preparation method of a kind of bismuthyl iodide according to claim 1/graphene oxide composite visible light catalysis material is characterized in that low whipping speed is to stir 20min ~ 40min under 300r/min ~ 700r/min in the step 2, adds Bi (NO again
3)
35H
2O, and to continue low whipping speed be mix and blend 20min ~ 50min under 300r/min ~ 700r/min, makes suspension.
6. the preparation method of a kind of bismuthyl iodide according to claim 1/graphene oxide composite visible light catalysis material, it is characterized in that in the step 3 at bath temperature being 70 ℃ ~ 80 ℃, supersonic frequency is that 80Hz ~ 200Hz and mixing speed are that the suspension that under 300r/min ~ 700r/min condition step 2 is obtained carries out ultrasonic processing, the ultrasonic agitation time is 1.5h ~ 2.5h, then filter, the brick-red precipitation that filtration obtains adopts deionized water washing 3 ~ 5 times, and then temperature is 50 ℃ ~ 70 ℃ dry 18h ~ 30h, namely obtains bismuthyl iodide/graphene oxide composite visible light catalysis material.
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| CN103861621A (en) * | 2014-02-27 | 2014-06-18 | 上海大学 | Bi7O9I3/graphene complex visible-light-induced photocatalyst and preparation method thereof |
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| CN104148094A (en) * | 2014-07-14 | 2014-11-19 | 河南师范大学 | Preparation method of bismuth oxyfluoride/ grapheme composite visible-light-induced photocatalyst |
| CN105642316A (en) * | 2015-12-22 | 2016-06-08 | 江苏大学 | Method for preparing BiOI / CdWO4 heterojunction photocatalyst |
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| CN106732681A (en) * | 2016-12-07 | 2017-05-31 | 湖北工业大学 | The preparation method of three-dimensional foam shape reduced graphene bismuth oxyiodide composite photo-catalyst |
| CN106732681B (en) * | 2016-12-07 | 2019-04-02 | 湖北工业大学 | The preparation method of three-dimensional foam shape reduced graphene bismuth oxyiodide composite photo-catalyst |
| CN108359272A (en) * | 2018-03-20 | 2018-08-03 | 常州大学 | It is a kind of using graphene as the preparation method and application of the conductive pearl powder of base material |
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