CN102266764A - Expanded graphite/zinc oxide composite photocatalyst and preparation method thereof - Google Patents
Expanded graphite/zinc oxide composite photocatalyst and preparation method thereof Download PDFInfo
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- CN102266764A CN102266764A CN 201110164917 CN201110164917A CN102266764A CN 102266764 A CN102266764 A CN 102266764A CN 201110164917 CN201110164917 CN 201110164917 CN 201110164917 A CN201110164917 A CN 201110164917A CN 102266764 A CN102266764 A CN 102266764A
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Abstract
The invention relates to an expanded graphite/zinc oxide composite photocatalyst and a preparation method thereof. The composite photocatalyst comprises the following components in percentage by weight: 10%-99% of expanded graphite and 1%-90% of zinc oxide. The preparation method comprises the following steps: (1) adding expanded graphite into sodium hydroxide solution according to a mass-to-volume ratio of 1-2g:100ml, stirring at the room temperature for 0.5-3 hours to obtain reaction solution; and (2) adding zinc acetate into the reaction solution, wherein the molar ratio of zinc acetate to sodium hydroxide is 1:(0.1-5); reacting at 50-90 DEG C for 2-6 hours, performing vacuum filtration on the mixed solution, and drying filter residues at 60-120 DEG C to obtain the photocatalyst. By adopting the preparation method, the agglomeration of own particles can be avoided and the re-accumulation of the expanded graphite lamella can be effectively prevented; and the preparation method has the advantages of common and accessible raw materials, low cost and good application prospects.
Description
Technical field
The invention belongs to zinc oxide composite photo-catalyst and preparation field thereof, particularly a kind of expanded graphite/zinc oxide composite photo-catalyst and preparation method thereof.
Background technology
Photochemical catalytic oxidation elimination at present and degradation of contaminant have become active research direction of environmental area.Compare with the physical method in the traditional water treatment technology, photocatalysis oxidation technique has the efficient height, energy consumption is low, easy and simple to handle, reaction condition is gentle, applied widely, outstanding feature such as degradation of contaminant is thorough, enjoys people's favor aspect environmental improvement.Compare with titanium dioxide optical catalyst commonly used, zinc oxide can not only absorb the ultraviolet light in the sunshine, and it is simple to absorb a large amount of visible lights and preparation technology.Therefore, zinc oxide has bigger actual application value as photochemical catalyst, utilizes the environmentally friendly photochemical catalyst of nano zine oxide as sewage disposal, has become worldwide research focus.At present, preparation method and the application study thereof about zinc oxide has more report both at home and abroad.
Wet chemical method is the main method of preparation nano material, it have equipment simple, can react by stoichiometry, characteristics such as products obtained therefrom purity height, controllable granularity.Nano zine oxide can directly obtain by one step of hydro-thermal method, but it is to react under HTHP, and equipment and technology is had relatively high expectations, and was unfavorable for large-scale industrialization production.Removing hydro-thermal method, can directly to obtain oxide powder and zinc external, and other wet chemical method as chemical precipitation method etc., all need at first obtain predecessor, obtains nano zine oxide by predecessor again through thermal decomposition process.This method process system complexity, and, cause equipment investment to increase owing to increased thermal decomposition process, energy consumption raises, and product cost strengthens.
The nano zinc oxide photocatalysis reaction unit comprises fluid bed, stator, recycle column, membrane reactor, but the less precipitate and separate that is difficult to of zinc oxide particle diameter.A kind of solution is exactly that nano zine oxide is fixed on the suitable solid carrier, is convenient to the practical application of zinc oxide photocatalysis process.Nano granular of zinc oxide can be fixed on pottery by different technology, glass, and plastics are on the pvc coating fabric.But oxidation operation need be adsorbed onto zinc oxide surface efficiently, because photocatalytic process takes place on the surface.Expanded graphite is as novel sorbing material, and specific area is bigger, is 50-200m
2/ g, there are many netted holes its inside, is a kind of good sorbing material, and its adsorbance is apparently higher than active carbon.Therefore expanded graphite can be used as the combination of the photocatalysis performance of the carrier of zinc oxide and strong absorption property that expanded graphite/zinc oxide composite can be realized expanded graphite and zinc oxide, for the pollutant in disposing of sewage provides a kind of novel, practical environment-friendly materials.
Summary of the invention
Technical problem to be solved by this invention provides a kind of expanded graphite/zinc oxide composite photo-catalyst and preparation method thereof, and this catalyst had both been avoided the reunion of self particle, has also effectively prevented the heavily accumulation of expanded graphite lamella; Preparation method's raw material is common to be easy to get, with low cost.
A kind of expanded graphite of the present invention/zinc oxide composite photo-catalyst, its composition comprises: by weight percentage, 10%～99% expanded graphite and 1%～90% zinc oxide, nano zine oxide load in the part hole on expanded graphite surface uniformly.
The composition of described composite photo-catalyst comprises: by weight percentage, and 50%～90% expanded graphite and 10%～50% zinc oxide.
Described Zinc oxide particles is a nanoscale, and particle diameter is 10～100nm.
The preparation method of a kind of expanded graphite of the present invention/zinc oxide composite photo-catalyst comprises:
(1) in sodium hydroxide solution, presses mass volume ratio 1～2g: 100ml and add expanded graphite, stirred under the room temperature 0.5～3 hour, get reactant liquor;
(2) will be that 1: 0.1～5 acetic acid zinc solution adds in the above-mentioned reactant liquor with the NaOH mol ratio, 50 ℃～90 ℃ reactions 2～6 hours down, with the mixed liquor vacuum filtration, oven dry be promptly down at 60 ℃～120 ℃ for filter residue.
Concentration of sodium hydroxide solution in the described step (1) is 0.1～1mol/L.
Acetic acid zinc solution concentration in the described step (2) is 0.1～0.5mol/L.
Preferable reaction temperature in the described step (2) is 60 ℃, and the preferred reaction time is 3 hours.
Preferred bake out temperature in the described step (2) is 60 ℃～80 ℃.
Beneficial effect
(1) Zinc oxide particles of the present invention can be dispersed in the expanded graphite surface, stronger active force is arranged between the two, both avoided the reunion of self particle, also effectively prevented the heavily accumulation of expanded graphite lamella, structural advantage makes the photocatalysis performance double action of its adsorption function with expanded graphite and zinc oxide;
(2) common being easy to get of preparation method's raw material of the present invention, with low cost, preparation process is simple and safe, has a good application prospect in field of waste water treatment.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
To 100mL concentration is the expanded graphite that adds 0.1g in the sodium hydroxide solution of 1mol/L, stirs 3 hours under the room temperature; Configuration concentration is the acetic acid zinc solution 100mL of 0.5mol/L, slowly is added drop-wise in the above-mentioned solution, stirs 2 hours down at 60 ℃; With the mixed liquor vacuum filtration, filter residue is dried down at 60 ℃ and is obtained expanded graphite/zinc oxide composite photo-catalyst (25% expanded graphite, 75% zinc oxide), and the Zinc oxide particles particle diameter is 30nm.Afterwards under ultra violet lamp with this composite photocatalyst for degrading methyl orange simulated wastewater, survey absorbance before and after the methyl orange degradation with ultraviolet specrophotometer, the degradation rate that obtains methyl orange is 58.12%.
Embodiment 2
To 100ml concentration is the expanded graphite that adds 0.5g in the sodium hydroxide solution of 0.7mol/L, stirs 0.5 hour under the room temperature; Configuration concentration is the acetic acid zinc solution 100mL of 0.3mol/L, slowly is added drop-wise in the above-mentioned solution, stirs 3 hours down at 50 ℃; With the mixed liquor vacuum filtration, filter residue is dried down at 70 ℃ and is obtained expanded graphite/zinc oxide composite photo-catalyst (45% expanded graphite, 55% zinc oxide), and the Zinc oxide particles particle diameter is 10nm.Afterwards under ultra violet lamp with this composite photocatalyst for degrading methyl orange simulated wastewater, survey absorbance before and after the methyl orange degradation with ultraviolet specrophotometer, the degradation rate that obtains methyl orange is 78.93%.
Embodiment 3
To 100mL concentration is the expanded graphite that adds 1.0g in the sodium hydroxide solution of 0.5mol/L, stirs 0.5 hour under the room temperature; Configuration concentration is the acetic acid zinc solution 100mL of 0.2mol/L, slowly is added drop-wise in the above-mentioned solution, stirs 4 hours down at 80 ℃; With the mixed liquor vacuum filtration, filter residue is dried down at 80 ℃ and is obtained expanded graphite/zinc oxide composite photo-catalyst (60% expanded graphite, 40% zinc oxide), and the Zinc oxide particles particle diameter is 70nm.Afterwards under ultra violet lamp with this composite photocatalyst for degrading methyl orange simulated wastewater, survey absorbance before and after the methyl orange degradation with ultraviolet specrophotometer, the degradation rate that obtains methyl orange is 86.84%.
Embodiment 4
To 100ml concentration is the expanded graphite that adds 1.5g in the 0.5mol/L sodium hydroxide solution, stirs 0.5 hour under the room temperature; Configuration concentration is the acetic acid zinc solution 100mL of 0.1mol/L, slowly is added drop-wise in the above-mentioned solution, stirs 3 hours down at 60 ℃; With the mixed liquor vacuum filtration, filter residue is dried down at 60 ℃ and is obtained expanded graphite/zinc oxide composite photo-catalyst (80% expanded graphite, 20% zinc oxide), and the Zinc oxide particles particle diameter is 60nm.Afterwards under ultra violet lamp with this composite photocatalyst for degrading methyl orange simulated wastewater, survey absorbance before and after the methyl orange degradation with ultraviolet specrophotometer, the degradation rate that obtains methyl orange is 90.87%.
Embodiment 5
To 100ml concentration is the expanded graphite that adds 2.0g in the sodium hydroxide solution of 0.3mol/L, stirs 0.5 hour under the room temperature; Configuration concentration is the acetic acid zinc solution 100mL of 0.2mol, slowly is added drop-wise in the above-mentioned solution, stirs 3 hours down at 80 ℃; With the mixed liquor vacuum filtration, filter residue is dried down at 80 ℃ and is obtained expanded graphite/zinc oxide composite photo-catalyst (75% expanded graphite, 25% zinc oxide), and the Zinc oxide particles particle diameter is 80nm.Afterwards under ultra violet lamp with this composite photocatalyst for degrading methyl orange simulated wastewater, survey absorbance before and after the methyl orange degradation with ultraviolet specrophotometer, the degradation rate that obtains methyl orange is 92.11%.
Embodiment 6
To 100ml concentration is the expanded graphite that adds 1.5g in the sodium hydroxide solution of 0.5mol/L, stirs 0.5 hour under the room temperature; Configuration concentration is the acetic acid zinc solution 100mL of 0.1mol, slowly is added drop-wise in the above-mentioned solution, stirs 3 hours down at 60 ℃; With the mixed liquor vacuum filtration, filter residue is dried down at 60 ℃ and is obtained expanded graphite/zinc oxide composite photo-catalyst (85% expanded graphite, 15% zinc oxide), and the Zinc oxide particles particle diameter is 70nm.Afterwards under ultra violet lamp with this composite photocatalyst for degrading methyl orange simulated wastewater, survey absorbance before and after the methyl orange degradation with ultraviolet specrophotometer, the degradation rate that obtains methyl orange is 97.46%.
Embodiment 7
To 100mL concentration is to add 2.0 expanded graphite in the sodium hydroxide solution of 0.5mol/L, stirs 0.5 hour under the room temperature; Configuration concentration is the acetic acid zinc solution 100mL of 0.1mol, slowly is added drop-wise in the above-mentioned solution, stirs 3 hours down at 60 ℃; With the mixed liquor vacuum filtration, filter residue is dried down at 60 ℃ and is obtained expanded graphite/zinc oxide composite photo-catalyst (90% expanded graphite, 10% zinc oxide), and the Zinc oxide particles particle diameter is 50nm.Afterwards under ultra violet lamp with this composite photocatalyst for degrading methyl orange simulated wastewater, survey absorbance before and after the methyl orange degradation with ultraviolet specrophotometer, the degradation rate that obtains methyl orange is 97.72%.
Claims (8)
1. expanded graphite/zinc oxide composite photo-catalyst, its composition comprises: by weight percentage, 10%～99% expanded graphite and 1%～90% zinc oxide, nano zine oxide load in the part hole on expanded graphite surface uniformly.
2. a kind of expanded graphite according to claim 1/zinc oxide composite photo-catalyst, it is characterized in that: the composition of described composite photo-catalyst comprises: by weight percentage, 50%～90% expanded graphite and 10%～50% zinc oxide.
3. a kind of expanded graphite according to claim 1/zinc oxide composite photo-catalyst is characterized in that: described Zinc oxide particles is a nanoscale, and particle diameter is 10～100nm.
4. the preparation method of expanded graphite/zinc oxide composite photo-catalyst comprises:
(1) in sodium hydroxide solution, presses mass volume ratio 1～2g: 100ml and add expanded graphite, stirred under the room temperature 0.5～3 hour, get reactant liquor;
(2) will be that 1: 0.1～5 acetic acid zinc solution adds in the above-mentioned reactant liquor with the NaOH mol ratio, 50 ℃～90 ℃ reactions 2～6 hours down, with the mixed liquor vacuum filtration, oven dry be promptly down at 60 ℃～120 ℃ for filter residue.
5. the preparation method of a kind of expanded graphite according to claim 1/zinc oxide composite photo-catalyst is characterized in that: the concentration of sodium hydroxide solution in the described step (1) is 0.1～1mol/L.
6. the preparation method of a kind of expanded graphite according to claim 1/zinc oxide composite photo-catalyst is characterized in that: the acetic acid zinc solution concentration in the described step (2) is 0.1～0.5mol/L.
7. the preparation method of a kind of expanded graphite according to claim 1/zinc oxide composite photo-catalyst is characterized in that: the reaction temperature in the described step (2) is 60 ℃, and the reaction time is 3 hours.
8. the preparation method of a kind of expanded graphite according to claim 1/zinc oxide composite photo-catalyst is characterized in that: the bake out temperature in the described step (2) is 60 ℃～80 ℃.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102580715A (en) * | 2012-01-10 | 2012-07-18 | 黑龙江大学 | Method for preparing zinc oxide/graphene composite from expanded graphite by stripping |
| CN103071498A (en) * | 2013-01-14 | 2013-05-01 | 杜亚丽 | Preparation method of Cu2O compound photocatalyst |
| CN104475076A (en) * | 2014-12-11 | 2015-04-01 | 上海烟草集团有限责任公司 | Preparation method of graphene-nano zinc oxide composite photocatalytical material for adsorbing and degrading nitrosamine |
| CN104667902A (en) * | 2015-03-02 | 2015-06-03 | 哈尔滨理工大学 | Method for preparing ZnO-expanded graphite composite with sol method |
| CN105001443A (en) * | 2015-08-04 | 2015-10-28 | 北京化工大学 | Polyurethane sponge compositely modified through expanded graphite and zinc oxide and preparing method thereof |
| CN106565620A (en) * | 2016-11-18 | 2017-04-19 | 盐城工学院 | Method for preparing tetrazole compound |
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| JPS5288290A (en) * | 1976-01-19 | 1977-07-23 | Nippon Pillar Packing | Rust preventing method of swell graphite |
| CN101214433A (en) * | 2008-01-04 | 2008-07-09 | 昆明理工大学 | Preparation method of active carbon supported with zinc oxide |
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2011
- 2011-06-17 CN CN 201110164917 patent/CN102266764A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5288290A (en) * | 1976-01-19 | 1977-07-23 | Nippon Pillar Packing | Rust preventing method of swell graphite |
| CN101214433A (en) * | 2008-01-04 | 2008-07-09 | 昆明理工大学 | Preparation method of active carbon supported with zinc oxide |
Non-Patent Citations (2)
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| 《化工环保》 20071231 王文颖 等 膨胀石墨- ZnO复合材料的制备及其光催化降解原油的性能 第367-370页 1-8 第27卷, 第4期 * |
| 《燕山大学学报》 20090731 岳学庆 等 使用膨胀石墨/ZnO 复合材料去除水中甲基橙 第299-303页 1-8 第33卷, 第4期 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102580715A (en) * | 2012-01-10 | 2012-07-18 | 黑龙江大学 | Method for preparing zinc oxide/graphene composite from expanded graphite by stripping |
| CN103071498A (en) * | 2013-01-14 | 2013-05-01 | 杜亚丽 | Preparation method of Cu2O compound photocatalyst |
| CN103071498B (en) * | 2013-01-14 | 2015-04-22 | 杜亚丽 | Preparation method of Cu2O compound photocatalyst |
| CN104475076A (en) * | 2014-12-11 | 2015-04-01 | 上海烟草集团有限责任公司 | Preparation method of graphene-nano zinc oxide composite photocatalytical material for adsorbing and degrading nitrosamine |
| CN104667902A (en) * | 2015-03-02 | 2015-06-03 | 哈尔滨理工大学 | Method for preparing ZnO-expanded graphite composite with sol method |
| CN105001443A (en) * | 2015-08-04 | 2015-10-28 | 北京化工大学 | Polyurethane sponge compositely modified through expanded graphite and zinc oxide and preparing method thereof |
| CN106565620A (en) * | 2016-11-18 | 2017-04-19 | 盐城工学院 | Method for preparing tetrazole compound |
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Application publication date: 20111207 |