CN104001498B - The preparation method of a kind of zinc molybdate/Graphene composite visible light catalyst - Google Patents
The preparation method of a kind of zinc molybdate/Graphene composite visible light catalyst Download PDFInfo
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- CN104001498B CN104001498B CN201410247440.7A CN201410247440A CN104001498B CN 104001498 B CN104001498 B CN 104001498B CN 201410247440 A CN201410247440 A CN 201410247440A CN 104001498 B CN104001498 B CN 104001498B
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Abstract
Does the present invention disclose the preparation method of a kind of zinc molybdate/Graphene composite visible light catalyst, comprises the following steps: (1) is by 2mmol? Na2MoO4Join in graphene oxide water solution, ultrasonic dissolution 30min obtained solution X; (2) by 2mmol? Zn (CH3COO)2��2H2O stirring and dissolving, in 40mL water, obtains transparent settled solution Y; (3) dropwise joining in solution X by solution Y under ultrasonication, ultrasonic 120min adds hydrazine hydrate, stirs and is reduced to polymerization precipitation in 80 DEG C of water-baths after evenly, and solution becomes clarification; (4) after reaction terminates, solution naturally cools to room temperature, filters, and water and ethanol respectively wash three times, then in 80 DEG C of dry 5h i.e. obtained zinc molybdate/Graphene composite visible light catalyst in thermostatic drying chamber. Zinc molybdate prepared by the present invention/Graphene composite visible light catalyst can improve light absorption, there is absorption spectrum ranges width, stable performance, nontoxic, efficiently cheap, the degraded that can be applied to difficult for biological degradation organic pollutant, has stronger market application foreground.
Description
Technical field
The invention belongs to visible light catalytic material technical field, be specifically related to a kind of can the preparation method of zinc molybdate/Graphene composite visible light catalyst of efficient degradation rhdamine B waste water.
Background technology
Waste water from dyestuff is one of typical difficult for biological degradation organic waste water, a large amount of basicity height, the dyestuff that color and luster is dark, stink is big are being produced and are being entered environment in use, what wherein have also contains the carcinogenic substances such as phenyl ring, amido, azo group, serious environment pollution, adopts conventional biological treatment removal effect not ideal enough. Nanosecond science and technology be progressively grow up in late 1980s forward position, intercrossing new branch of science, it has tremendous potential in new production technique, new material and new product etc. creating. Nano semiconductor photocatalysis oxidation technique is paid close attention to increasingly, especially shows good application prospect in the removal of difficult for biological degradation pollutent, has become domestic and international research focus. The single-phase semiconductor nano photocatalyst powder suspension system being widely studied at present, also exist that nanoparticle is easily condensed, easy in inactivation, utilising efficiency are low, difficult separation and recycling and the defect such as absorption spectrum ranges is narrow, seriously limit the industrial applications of nano photo catalyzed oxidation. Therefore the compound nanometer photocatalyst of loading type, high reactivity becomes research focus now. For above-mentioned defect, the novel nano photocatalyst of improvement need to meet the condition of three aspects: (1) can effectively stop the compound in light induced electron and hole; (2) pollutent is had good adsorptive power by catalyzer;(3) catalyst cupport on suitable carrier to avoid particle agglomeration.
Owing to Graphene has excellent electroconductibility so that it is easily catch light induced electron and serve as the medium of transfer transport, greatly strengthen the transhipment rate of electric charge, thus can effectively stop the compound of current carrier; Secondly Graphene specific surface area is relatively big, is about 2600m2��g-1, the aromatic structure of its inside can form ��-��conjugation with pollutent, thus shows the adsorption that pollutent is strong; Moreover Graphene has higher physical strength, for the deposition of catalyzer provides a two-dimentional face structure; Graphene is a kind of energy gap simultaneously is the semi-metal of zero, adjust its energy gap by modification, not only can realize the photoabsorption of wide band, and electric charge can also be made more to mate with catalyzer in transfer process, improve its photocatalysis performance, so Graphene becomes the desirable material of load.
Summary of the invention
The technical problem that the present invention solves there is provided one can the preparation method of the effective zinc molybdate/Graphene composite visible light catalyst of rhodamine B degradation (RhB) waste water from dyestuff.
The technical scheme of the present invention is: the preparation method of a kind of zinc molybdate/Graphene composite visible light catalyst, it is characterized in that comprising the following steps: the graphene oxide of 4.8-43.2mg is joined in 40mL water by (1), ultrasonic disperse 60min forms graphene oxide water solution, then by 2mmolNa2MoO4Join in graphene oxide water solution, continue ultrasonic dissolution 30min obtained solution X; (2) by 2mmolZn (CH3COO)2��2H2O stirring and dissolving, in 40mL water, obtains transparent settled solution Y; (3) under ultrasonication, solution Y is dropwise joined in solution X, continue ultrasonic 120min, add hydrazine hydrate, stir and be reduced to polymerization precipitation in 80 DEG C of water-baths after evenly, solution becomes clarification, and the quality wherein often adding the corresponding graphene oxide of 1mL hydrazine hydrate is 48mg; (4) after reaction terminates, solution naturally cools to room temperature, filters, and water and ethanol respectively wash three times, then in 80 DEG C of dry 5h i.e. obtained zinc molybdate/Graphene composite visible light catalyst in thermostatic drying chamber.
The zinc molybdate that the present invention obtains/Graphene composite visible light catalyst has brilliant type and absorbing properties preferably, and there is visible light-responded photocatalysis performance, there is the performance of efficient degradation rhdamine B waste water under sunlight, there is absorption spectrum ranges width, stable performance, nontoxic, efficiently cheap, it is possible to be applied to the degraded of difficult for biological degradation organic pollutant, there is stronger market application foreground.
Embodiment
Being described in further details by the foregoing of the present invention by the following examples, but this should not being interpreted as, the scope of the above-mentioned theme of the present invention is only limitted to following embodiment, all technology realized based on foregoing of the present invention all belong to the scope of the present invention.
Embodiment 1
By 2mmolNa2MoO4Joining in 40mL water, ultrasonic dissolution 30min obtains settled solution, is designated as solution X. Meanwhile, by 2mmolZn (CH3COO)2��2H2O stirring and dissolving, in 40mL water, obtains transparent settled solution, is designated as solution Y. Then ultrasonic lower by solution Y dropwise (about 2mL/min) join in solution X, continue ultrasonic 120min. After reaction terminates, filtering, water and ethanol respectively wash three times, then 80 DEG C of dry 5h in thermostatic drying chamber, i.e. obtained pure zinc molybdate photocatalyst. The RhB clearance of rhdamine B waste water 10h of degrading under nature sunlight is 28.4%.
Embodiment 2
0.0048g graphene oxide (GO) is joined in 40mL water, ultrasonic disperse 60min. Then by 2mmolNa2MoO4Join in graphene oxide water solution, continue ultrasonic dissolution 30min, be designated as solution X. Meanwhile, by 2mmolZn (CH3COO)2��2H2O stirring and dissolving, in 40mL water, obtains transparent settled solution, is designated as solution Y. Then ultrasonic lower by solution Y dropwise (about 2mL/min) join in solution X, continue ultrasonic 120min. Then adding 0.1mL hydrazine hydrate, stir after evenly, proceed in thermostat water bath, 80 DEG C of water-bath reduction reactions are to being polymerized precipitation, and solution becomes clarification. After reaction terminates, solution naturally cools to room temperature, filters, and water and ethanol respectively wash three times, then 80 DEG C of dry 5h in thermostatic drying chamber, i.e. obtained zinc molybdate/Graphene composite visible light catalyst containing 1wt% Graphene. The RhB clearance of rhdamine B waste water 10h of degrading under nature sunlight is 77.2%.
Embodiment 3
0.0144g graphene oxide is joined in 40mL water, ultrasonic disperse 60min. Then by 2mmolNa2MoO4Join in graphene oxide water solution, continue ultrasonic dissolution 30min, be designated as solution X. Meanwhile, by 2mmolZn (CH3COO)2��2H2O stirring and dissolving, in 40mL water, obtains transparent settled solution, is designated as solution Y. Then ultrasonic lower by solution Y dropwise (about 2mL/min) join in solution X, continue ultrasonic 120min. Then adding 0.3mL hydrazine hydrate, stir after evenly, proceed in thermostat water bath, 80 DEG C of water-bath reduction reactions are to being polymerized precipitation, and solution becomes clarification. After reaction terminates, solution naturally cools to room temperature, filters, and water and ethanol respectively wash three times, then 80 DEG C of dry 5h in thermostatic drying chamber, i.e. obtained zinc molybdate/Graphene composite visible light catalyst containing 3wt% Graphene. The RhB clearance of rhdamine B waste water 10h of degrading under nature sunlight is 96.5%.
Embodiment 4
0.024g graphene oxide is joined in 40mL water, ultrasonic disperse 60min. Then by 2mmolNa2MoO4Join in graphene oxide water solution, continue ultrasonic dissolution 30min, be designated as solution X. Meanwhile, by 2mmolZn (CH3COO)2��2H2O stirring and dissolving, in 40mL water, obtains transparent settled solution, is designated as solution Y. Then ultrasonic lower by solution Y dropwise (about 2mL/min) join in solution X, continue ultrasonic 120min. Then adding 0.5mL hydrazine hydrate, stir after evenly, proceed in thermostat water bath, 80 DEG C of water-bath reduction reactions are to being polymerized precipitation, and solution becomes clarification. After reaction terminates, solution naturally cools to room temperature, filters, and water and ethanol respectively wash three times, then 80 DEG C of dry 5h in thermostatic drying chamber, i.e. obtained zinc molybdate/Graphene composite visible light catalyst containing 5wt% Graphene. The RhB clearance of rhdamine B waste water 10h of degrading under nature sunlight is 84.3%.
Embodiment 5
0.0336g graphene oxide is joined in 40mL water, ultrasonic disperse 60min. Then by 2mmolNa2MoO4Join in graphene oxide water solution, continue ultrasonic dissolution 30min, be designated as solution X. Meanwhile, by 2mmolZn (CH3COO)2��2H2O stirring and dissolving, in 40mL water, obtains transparent settled solution, is designated as solution Y. Then ultrasonic lower by solution Y dropwise (about 2mL/min) join in solution X, continue ultrasonic 120min. Then adding 0.7mL hydrazine hydrate, stir after evenly, proceed in thermostat water bath, 80 DEG C of water-bath reduction reactions are to being polymerized precipitation, and solution becomes clarification. After reaction terminates, solution naturally cools to room temperature, filters, and water and ethanol respectively wash three times, then 80 DEG C of dry 5h in thermostatic drying chamber, i.e. obtained zinc molybdate/Graphene composite visible light catalyst containing 7wt% Graphene.The RhB clearance of rhdamine B waste water 10h of degrading under nature sunlight is 80.3%.
Embodiment 6
0.0432g graphene oxide is joined in 40mL water, ultrasonic disperse 60min. Then by 2mmolNa2MoO4Join in graphene oxide water solution, continue ultrasonic dissolution 30min, be designated as solution X. Meanwhile, by 2mmolZn (CH3COO)2��2H2O stirring and dissolving, in 40mL water, obtains transparent settled solution, is designated as solution Y. Then ultrasonic lower by solution Y dropwise (about 2mL/min) join in solution X, continue ultrasonic 120min. Then adding 0.9mL hydrazine hydrate, stir after evenly, proceed in thermostat water bath, 80 DEG C of water-bath reduction reactions are to being polymerized precipitation, and solution becomes clarification. After reaction terminates, solution naturally cools to room temperature, filters, and water and ethanol respectively wash three times, then 80 DEG C of dry 5h in thermostatic drying chamber, i.e. obtained zinc molybdate/Graphene composite visible light catalyst containing 9wt% Graphene. The RhB clearance of rhdamine B waste water 10h of degrading under nature sunlight is 65%.
Embodiment above describes the ultimate principle of the present invention, main feature and advantage; the technician of the industry should understand; the present invention is not restricted to the described embodiments; the principle that the present invention is just described described in above-described embodiment and specification sheets; under the scope not departing from the principle of the invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the scope of protection of the invention.
Claims (1)
1. the preparation method of zinc molybdate/Graphene composite visible light catalyst, it is characterized in that comprising the following steps: the graphene oxide of 4.8-43.2mg is joined in 40mL water by (1), ultrasonic disperse 60min forms graphene oxide water solution, then by 2mmolNa2MoO4Join in graphene oxide water solution, continue ultrasonic dissolution 30min obtained solution X; (2) by 2mmolZn (CH3COO)2��2H2O stirring and dissolving, in 40mL water, obtains transparent settled solution Y; (3) under ultrasonication, solution Y is dropwise joined in solution X, continue ultrasonic 120min, add hydrazine hydrate, stir and be reduced to polymerization precipitation in 80 DEG C of water-baths after evenly, solution becomes clarification, and the quality wherein often adding the corresponding graphene oxide of 1mL hydrazine hydrate is 48mg; (4) after reaction terminates, solution naturally cools to room temperature, filters, and water and ethanol respectively wash three times, then in 80 DEG C of dry 5h i.e. obtained zinc molybdate/Graphene composite visible light catalyst in thermostatic drying chamber.
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| CN105591072A (en) * | 2016-02-29 | 2016-05-18 | 陕西科技大学 | Negative electrode piece of alpha-ZnMoO4 lithium ion battery and preparation method of negative electrode piece |
| CN112844368B (en) * | 2021-02-18 | 2023-09-15 | 辽宁大学 | ZnMoO with adjustable oxygen vacancy concentration 4 Photocatalyst, preparation method and application thereof |
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