CN102941080A - Graphene/ bismuth oxide compound light catalyst and preparation method thereof - Google Patents
Graphene/ bismuth oxide compound light catalyst and preparation method thereof Download PDFInfo
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- CN102941080A CN102941080A CN2012104721541A CN201210472154A CN102941080A CN 102941080 A CN102941080 A CN 102941080A CN 2012104721541 A CN2012104721541 A CN 2012104721541A CN 201210472154 A CN201210472154 A CN 201210472154A CN 102941080 A CN102941080 A CN 102941080A
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Abstract
The invention discloses a graphene/bismuth oxide compound light catalyst and a preparation method thereof. The graphene/bismuth oxide compound light catalyst is characterized in that a photoproduction electron-hole of a bismuth oxide light catalyst is prone to recombine so that the photocatalytic activity is reduced, by means of modification effect of graphene on the surface of the bismuth oxide light catalyst, the separation of the photoproduction electron-hole can be remarkably improved, and thereby the photocatalysis performance of the bismuth oxide light catalyst is improved. The preparation method includes that step one, preparing the graphene oxide; step two, subjecting graphene oxide obtained in the step one to ultrasonic dispersion in an alcoholic solution to prepare a graphene oxide dispersing liquid; and step three, preparing the graphene/bismuth oxide compound light catalyst. The preparation method is simple in process and low in cost, and the prepared compound light catalyst has high visible light catalytic activity.
Description
Technical field
The invention belongs to photocatalysis technology, relate to and adopt the standby graphene oxide of improvement Hummers legal system, utilize ultrasonic dispersion to obtain the graphene oxide dispersion liquid, recycling hydro-thermal method redox graphene, the compound Graphene/bismuth oxide composite photo-catalyst that obtains of original position.
Background technology
The seriousness of at present environmental pollution has become one and has directly threatened human survival, needs the focal issue of solution badly.Photocatalysis technology is at the energy and environmental area the green technology of important application prospect to be arranged from what twentieth century progressively grew up the seventies.This technology can make the organic pollution generation oxidative decomposition in the environment, finally is degraded to CO
2, the small-molecule substance such as water and inorganic ions, so non-secondary pollution, the high at present the most promising pollution treatment method that is considered to of palliating degradation degree.
Bismuth based semiconductor photochemical catalyst can be had good photocatalytic activity by excited by visible light, and degradable organic pollutant has good development prospect effectively.Their common feature and significant advantage have absorption exactly in visible-range, have good photocatalysis performance.Yet bismuth based semiconductor photochemical catalyst is Bi particularly
2O
3There is the easily again combination of light induced electron-hole in photochemical catalyst, to problems such as visible Optical Absorption limiteds, has limited greatly its large-scale application.Therefore, must take certain measure to improve the light induced electron transport efficiency, effectively limit again combination of electron-hole.
In recent years, more about the synthetic aspect research of bismuth oxide photocatalyst, if any report polyalcohol medium method and the standby Bi of ammonia precipitation process legal system
2O
3The photocatalytic activity of nano particle all is higher than commodity Bi
2O
3Nano particle.And for Bi
2O
3Study on the modification still be in the junior stage, Graphene has unique conductive characteristic, with itself and Bi
2O
3Compound, will be to Bi
2O
3Photocatalysis performance produce significant impact, at present in this respect research there is not yet report.The reason that Graphene can improve the bismuth oxide photocatalysis performance can be summarized as: at first Graphene can improve Bi
2O
3The separative efficiency in the light induced electron-hole of photochemical catalyst; Secondly, Graphene can improve Bi
2O
3To visible Optical Absorption.Based on above-mentioned analysis, try to explore Graphene and Bi
2O
3The preparation and property research of composite photo-catalyst be significant.
Summary of the invention
The object of the present invention is to provide a kind of Graphene/bismuth oxide composite photo-catalyst and preparation method thereof, the method technique is simple, with low cost, and synthetic composite photo-catalyst photocatalytic degradation effect is better.
The invention provides Graphene for degradable organic pollutant/bismuth oxide composite photo-catalyst, it is characterized in that: be that 1: 1000～1: 10 Graphene and bismuth oxide original position is composited by mass ratio, utilize the special electric action of Graphene, significantly improve the visible light photocatalysis performance of bismuth oxide.Preparation method's step of Graphene/bismuth oxide composite photo-catalyst is as follows:
(1) preparation graphene oxide: with the standby graphene oxide of improvement Hummers legal system, 10g graphite, the mixing of 100～300mL98% concentrated sulfuric acid are placed ice bath, stir 30min, it is fully mixed, take by weighing 30～50g KMnO
4Add after above-mentioned mixed liquor continues to stir 1h, continue stirring 30min in the tepidarium in moving into 30～50 ℃; Add an amount of 5～20%H after with distilled water reactant liquor (control temperature below 100 ℃) being diluted to 800～1000mL
2O
2, filter while hot, fully wash to approaching neutrality with 1～10%HCl and distilled water, filter at last, wash, 60 ℃ of lower oven dry, obtain the graphene oxide sample.
(2) preparation graphene oxide dispersion liquid: the graphene oxide of a certain amount of step (1) gained is carried out ultrasonic dispersion in the certain volume alcoholic solution, preparation graphene oxide dispersion liquid.
(3) preparation Graphene/bismuth oxide composite photo-catalyst: take by weighing in the nitric acid or hydrochloric acid solution that a certain amount of bismuth salt is dissolved in dilution, this solution is slowly added in the graphene oxide dispersion liquid of step (2) gained, fully stir, then add certain density alkaline solution and regulate pH to 10～14, continue to stir 30～60 minutes, then solution is put in the hydrothermal reaction kettle, 100～220 ℃ of lower reaction 5～20h, naturally cool to room temperature, with deionized water and absolute ethyl alcohol with product centrifuge washing 3～4 times, to remove unnecessary ion and impurity, 60 ℃ of oven dry obtain Graphene/bismuth oxide composite photo-catalyst in drying box, the method technique is simple, and is with low cost, and the composite photo-catalyst of preparation has higher visible light catalysis activity.
The present invention compared with prior art has remarkable advantage:
(1) the present invention adopts hydro-thermal method to synthesize Graphene/bismuth oxide composite photo-catalyst, the method is when realizing the graphene oxide reduction, the original position that has realized bismuth oxide photocatalyst is synthetic, thereby utilize one step of water-heat process to realize the preparation of Graphene/bismuth oxide composite photo-catalyst, method is simple, and is easy to operate.
(2) Graphene of the present invention has significantly increased bismuth oxide photocatalyst to visible Optical Absorption in the modification on bismuth oxide surface, accelerates the separation in light induced electron-hole, and the bismuth oxide photocatalyst visible light catalysis activity significantly improves.
Description of drawings
The scanning electron microscopy picture of Fig. 1 Graphene/bismuth oxide composite photo-catalyst;
The X-ray diffraction spectrogram of the compound front and back of Fig. 2 Graphene bismuth oxide photocatalyst;
The UV-Vis DRS spectrum of the compound front and back of Fig. 3 Graphene bismuth oxide photocatalyst: (a) Graphene compound before, (b) Graphene compound after;
The photocatalysis performance of the Graphene of the different Graphene content of Fig. 4/bismuth oxide composite photo-catalyst.
The specific embodiment
(1) preparation graphene oxide: with the standby graphene oxide of improvement Hummers legal system, 10g graphite, the mixing of 100～300mL98% concentrated sulfuric acid are placed ice bath, stir 30min, it is fully mixed, take by weighing 30～50g KMnO
4Add after above-mentioned mixed liquor continues to stir 1h, continue stirring 30min in the tepidarium in moving into 30～50 ℃; Add an amount of 5～20%H after with distilled water reactant liquor (control temperature below 100 ℃) being diluted to 800～1000mL
2O
2, filter while hot, fully wash to approaching neutrality with 1～10%HCl and distilled water, filter at last, wash, 60 ℃ of lower oven dry, obtain the graphene oxide sample.
(2) preparation graphene oxide dispersion liquid: the graphene oxide of a certain amount of step (1) gained is carried out ultrasonic dispersion in the certain volume alcoholic solution, preparation graphene oxide dispersion liquid.
(3) preparation Graphene/bismuth oxide composite photo-catalyst: take by weighing in the nitric acid or hydrochloric acid solution that a certain amount of bismuth salt is dissolved in dilution, this solution is slowly added in the graphene oxide dispersion liquid of step (2) gained, fully stir, then add certain density alkaline solution and regulate pH to 10～14, continue to stir 30～60 minutes, then solution is put in the hydrothermal reaction kettle, 100～220 ℃ of lower reaction 5～20h, naturally cool to room temperature, with deionized water and absolute ethyl alcohol with product centrifuge washing 3～4 times, to remove unnecessary ion and impurity, 60 ℃ of oven dry obtain Graphene/bismuth oxide composite photo-catalyst in drying box, the method technique is simple, and is with low cost, and the composite photo-catalyst of preparation is the degradating organic dye better performances under visible light.
For a better understanding of the present invention, further illustrate content of the present invention below in conjunction with example, but content of the present invention is not limited to following given example.
The side's of enforcement example 1: the preparation method of a kind of Graphene of the present invention/bismuth oxide composite photo-catalyst may further comprise the steps:
(1) preparation graphene oxide: adopt the standby graphene oxide of improvement Hummers legal system, 10g graphite, the 230mL98% concentrated sulfuric acid are mixed placing ice bath, stir 30min, it is fully mixed, take by weighing 40g KMnO
4Add after above-mentioned mixed liquor continues to stir 1h, continue stirring 30min in the tepidarium in moving into 40 ℃; Add an amount of 5%H after with distilled water reactant liquor (control temperature below 100 ℃) being diluted to 800mL
2O
2, filter while hot, fully wash to approaching neutrality with 5%HCl and distilled water, filter at last, wash, 60 ℃ of lower oven dry, obtain the graphene oxide sample.
(2) preparation graphene oxide dispersion liquid: carry out ultrasonic dispersion, preparation graphene oxide dispersion liquid in the graphene oxide adding 10mL butanol solution with 0.01g step (1) gained.
(3) preparation Graphene/bismuth oxide composite photo-catalyst: the bismuth nitrate that takes by weighing 1g is dissolved in the 2M salpeter solution of dilution, this solution is slowly added in the graphene oxide dispersion liquid of step (2) gained, fully stir, then the NaOH solution that adds 2M is regulated pH to 14, continue to stir 30 minutes, then solution is put in the hydrothermal reaction kettle, 180 ℃ of lower reaction 12h, naturally cool to room temperature, with deionized water and absolute ethyl alcohol with product centrifuge washing 3 times, to remove unnecessary ion and impurity, 60 ℃ of oven dry obtain Graphene/bismuth oxide composite photo-catalyst in drying box.
Characterize through the pattern of SEM to Graphene/bismuth oxide composite photo-catalyst, from Fig. 1, can be clearly seen that the existence of graphene film, illustrate that Graphene and bismuth oxide have well carried out compound.Phase to Graphene/bismuth oxide composite photo-catalyst characterizes, and as shown in Figure 2, the phase of the compound front and back of Graphene bismuth oxide does not change.Utilize ultraviolet-diffuse reflection spectrum that the absorbing state of the compound front and back of Graphene bismuth oxide to visible light is characterized, as shown in Figure 3, the compound rear oxidation bismuth of Graphene significantly strengthens the absorption of visible region.Under radiation of visible light, studied the Graphene of different Graphene content/bismuth oxide composite photo-catalyst to the degraded situation of rhodamine B, as shown in Figure 4, the composite photo-catalyst photocatalysis effect of 3% content is best.
The side's of enforcement example 2: the preparation method of a kind of Graphene of the present invention/bismuth oxide composite photo-catalyst may further comprise the steps:
(1) preparation graphene oxide: adopt the standby graphene oxide of improvement Hummers legal system, 10g graphite, the 250mL98% concentrated sulfuric acid are mixed placing ice bath, stir 30min, it is fully mixed, take by weighing 40g KMnO
4Add after above-mentioned mixed liquor continues to stir 1h, continue stirring 30min in the tepidarium in moving into 45 ℃; Add an amount of 5%H after with distilled water reactant liquor (control temperature below 100 ℃) being diluted to 1000mL
2O
2, filter while hot, fully wash to approaching neutrality with 5%HCl and distilled water, filter at last, wash, 60 ℃ of lower oven dry, obtain the graphene oxide sample.
(2) preparation graphene oxide dispersion liquid: carry out ultrasonic dispersion, preparation graphene oxide dispersion liquid in the graphene oxide adding 15mL normal propyl alcohol solution with 0.03g step (1) gained.
(3) preparation Graphene/bismuth oxide composite photo-catalyst: the bismuth nitrate that takes by weighing 1g is dissolved in the 2M salpeter solution of dilution, this solution is slowly added in the graphene oxide dispersion liquid of step (2) gained, fully stir, then the KOH solution that adds 2M is regulated pH to 13, continue to stir 30 minutes, then solution is put in the hydrothermal reaction kettle, 200 ℃ of lower reaction 8h, naturally cool to room temperature, with deionized water and absolute ethyl alcohol with product centrifuge washing 3 times, to remove unnecessary ion and impurity, 60 ℃ of oven dry obtain Graphene/bismuth oxide composite photo-catalyst in drying box.
The side's of enforcement example 3: the preparation method of a kind of Graphene of the present invention/bismuth oxide composite photo-catalyst may further comprise the steps:
(1) preparation graphene oxide: adopt the standby graphene oxide of improvement Hummers legal system, 10g graphite, the 230mL98% concentrated sulfuric acid are mixed placing ice bath, stir 30min, it is fully mixed, take by weighing 40g KMnO
4Add after above-mentioned mixed liquor continues to stir 1h, continue stirring 30min in the tepidarium in moving into 50 ℃; Add an amount of 10%H after with distilled water reactant liquor (control temperature below 100 ℃) being diluted to 1000mL
2O
2, filter while hot, fully wash to approaching neutrality with 5%HCl and distilled water, filter at last, wash, 60 ℃ of lower oven dry, obtain the graphene oxide sample.
(2) preparation graphene oxide dispersion liquid: carry out ultrasonic dispersion, preparation graphene oxide dispersion liquid in the graphene oxide adding 20mL butanol solution with 0.05g step (1) gained.
(3) preparation Graphene/bismuth oxide composite photo-catalyst: the bismuth nitrate that takes by weighing 1g is dissolved in the 2M salpeter solution of dilution, this solution is slowly added in the graphene oxide dispersion liquid of step (2) gained, fully stir, then add ammonia spirit and regulate pH to 12, continue to stir 40 minutes, then solution is put in the hydrothermal reaction kettle, 160 ℃ of lower reaction 15h, naturally cool to room temperature, with deionized water and absolute ethyl alcohol with product centrifuge washing 3 times, to remove unnecessary ion and impurity, 60 ℃ of oven dry obtain Graphene/bismuth oxide composite photo-catalyst in drying box.
Claims (3)
1. Graphene/bismuth oxide composite photo-catalyst, it is characterized in that: be that 1: 1000～1: 10 Graphene and bismuth oxide original position is composited by mass ratio, utilize the special electric action of Graphene, can significantly improve the right separating power in light induced electron-hole of bismuth oxide photocatalyst, thereby significantly improve the photocatalysis performance of bismuth oxide.
2. the preparation method of Graphene/bismuth oxide composite photo-catalyst is characterized in that, comprises the steps:
(1) preparation graphene oxide: with the standby graphene oxide of improvement Hummers legal system, 10g graphite, the mixing of 100～300mL98% concentrated sulfuric acid are placed ice bath, stir 30min, it is fully mixed, take by weighing 30～50g KMnO
4Add after above-mentioned mixed liquor continues to stir 1h, continue stirring 30min in the tepidarium in moving into 30～50 ℃; Add an amount of 5～20%H after with distilled water reactant liquor (control temperature below 100 ℃) being diluted to 800～1000mL
2O
2, filter while hot, fully wash to approaching neutrality with 1～10%HCl and distilled water, filter at last, wash, 60 ℃ of lower oven dry, obtain the graphene oxide sample.
(2) preparation graphene oxide dispersion liquid: the graphene oxide of a certain amount of step (1) gained is carried out ultrasonic dispersion in the certain volume alcoholic solution, preparation graphene oxide dispersion liquid.
(3) preparation Graphene/bismuth oxide composite photo-catalyst: take by weighing in the nitric acid or hydrochloric acid solution that a certain amount of bismuth salt is dissolved in dilution, this solution is slowly added in the graphene oxide dispersion liquid of step (2) gained, fully stir, then add certain density alkaline solution and regulate pH to 10～14, continue to stir 30～60 minutes, then solution is put in the hydrothermal reaction kettle, 100～220 ℃ of lower reaction 5～20h, naturally cool to room temperature, with deionized water and absolute ethyl alcohol with product centrifuge washing 3～4 times, to remove unnecessary ion and impurity, 60 ℃ of oven dry obtain Graphene/bismuth oxide composite photo-catalyst in drying box, the method technique is simple, and is with low cost, and the composite photo-catalyst of preparation has higher visible light catalysis activity.
3. the preparation method of Graphene according to claim 2/bismuth oxide composite photo-catalyst is characterized in that the certain volume alcohol described in the step (2) is any in ethanol, normal propyl alcohol or the n-butanol of 5～20mL.
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Cited By (11)
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|---|---|---|---|---|
| CN104001495A (en) * | 2014-06-06 | 2014-08-27 | 河南师范大学 | Preparation method of bismuth oxychloride/graphene composite visible light catalyst |
| CN104014325A (en) * | 2014-06-13 | 2014-09-03 | 张家港市山牧新材料技术开发有限公司 | Visible light reaction nanometer titania catalyst |
| CN106311256A (en) * | 2016-07-06 | 2017-01-11 | 重庆大学 | Preparation method of graphene/beta-Bi2O3/SrFe12O19 ternary composite magnetic photocatalyst |
| CN106964334A (en) * | 2017-05-05 | 2017-07-21 | 国家纳米科学中心 | A kind of full spectral response type catalyst material and its production and use |
| CN107398265A (en) * | 2017-08-09 | 2017-11-28 | 张家港市汇鼎新材料科技有限公司 | A kind of preparation method based on graphene oxide catalysis material |
| CN109399616A (en) * | 2018-12-11 | 2019-03-01 | 四川省安德盖姆石墨烯科技有限公司 | A kind of graphene organic material and its application in gas sensor |
| CN110336022A (en) * | 2019-07-25 | 2019-10-15 | 广东工业大学 | A kind of preparation method of bismuth compound sulphur combination electrode material |
| CN110918104A (en) * | 2019-11-22 | 2020-03-27 | 西北矿冶研究院 | Ternary heterojunction graphene-bismuth oxide/bismuth oxyhalide visible light photocatalyst and preparation method thereof |
| CN111229268A (en) * | 2020-02-13 | 2020-06-05 | 中国石油大学(华东) | Full-spectrum response bismuth oxide/silver phosphate/carbon nanotube sponge composite photocatalyst for well drilling waste liquid treatment, and preparation method and application thereof |
| CN111359603A (en) * | 2020-03-12 | 2020-07-03 | 辽宁大学 | Bismuth-based self-supporting electrocatalyst, preparation method thereof and application of bismuth-based self-supporting electrocatalyst in ammonia production by nitrogen reduction |
| CN112495364A (en) * | 2020-12-15 | 2021-03-16 | 陕西科技大学 | Bi12SiO20-Bi2O2SiO3Preparation method of/rGO photocatalyst |
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| CN104001495B (en) * | 2014-06-06 | 2016-09-21 | 河南师范大学 | A kind of preparation method of bismuth oxychloride/Graphene composite visible light catalyst |
| CN104001495A (en) * | 2014-06-06 | 2014-08-27 | 河南师范大学 | Preparation method of bismuth oxychloride/graphene composite visible light catalyst |
| CN104014325A (en) * | 2014-06-13 | 2014-09-03 | 张家港市山牧新材料技术开发有限公司 | Visible light reaction nanometer titania catalyst |
| CN106311256A (en) * | 2016-07-06 | 2017-01-11 | 重庆大学 | Preparation method of graphene/beta-Bi2O3/SrFe12O19 ternary composite magnetic photocatalyst |
| CN106311256B (en) * | 2016-07-06 | 2019-06-14 | 重庆大学 | A kind of graphene/β-Bi2O3/SrFe12O19The preparation method of tri compound magnetic photocatalyst |
| CN106964334B (en) * | 2017-05-05 | 2019-08-20 | 国家纳米科学中心 | A kind of full spectral response type catalyst material and its preparation method and application |
| CN106964334A (en) * | 2017-05-05 | 2017-07-21 | 国家纳米科学中心 | A kind of full spectral response type catalyst material and its production and use |
| CN107398265A (en) * | 2017-08-09 | 2017-11-28 | 张家港市汇鼎新材料科技有限公司 | A kind of preparation method based on graphene oxide catalysis material |
| CN109399616A (en) * | 2018-12-11 | 2019-03-01 | 四川省安德盖姆石墨烯科技有限公司 | A kind of graphene organic material and its application in gas sensor |
| CN110336022A (en) * | 2019-07-25 | 2019-10-15 | 广东工业大学 | A kind of preparation method of bismuth compound sulphur combination electrode material |
| CN110918104A (en) * | 2019-11-22 | 2020-03-27 | 西北矿冶研究院 | Ternary heterojunction graphene-bismuth oxide/bismuth oxyhalide visible light photocatalyst and preparation method thereof |
| CN111229268A (en) * | 2020-02-13 | 2020-06-05 | 中国石油大学(华东) | Full-spectrum response bismuth oxide/silver phosphate/carbon nanotube sponge composite photocatalyst for well drilling waste liquid treatment, and preparation method and application thereof |
| CN111229268B (en) * | 2020-02-13 | 2021-06-08 | 中国石油大学(华东) | Full-spectrum response bismuth oxide/silver phosphate/carbon nanotube sponge composite photocatalyst for well drilling waste liquid treatment, and preparation method and application thereof |
| CN111359603A (en) * | 2020-03-12 | 2020-07-03 | 辽宁大学 | Bismuth-based self-supporting electrocatalyst, preparation method thereof and application of bismuth-based self-supporting electrocatalyst in ammonia production by nitrogen reduction |
| CN112495364A (en) * | 2020-12-15 | 2021-03-16 | 陕西科技大学 | Bi12SiO20-Bi2O2SiO3Preparation method of/rGO photocatalyst |
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Application publication date: 20130227 |