CN104888751A - Biomimetic synthetic method of morphology-controllable zinc oxide photocatalyst - Google Patents
Biomimetic synthetic method of morphology-controllable zinc oxide photocatalyst Download PDFInfo
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- CN104888751A CN104888751A CN201510260395.3A CN201510260395A CN104888751A CN 104888751 A CN104888751 A CN 104888751A CN 201510260395 A CN201510260395 A CN 201510260395A CN 104888751 A CN104888751 A CN 104888751A
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Abstract
The invention discloses a biomimetic synthetic method of a morphology-controllable zinc oxide photocatalyst. The method comprises the following steps: (1) dissolving ascorbic acid in water and performing stirring and mixing to obtain a uniform solution; (2) adding zinc sulfate heptahydrate into the uniform solution obtained from step (1), wherein the mol ratio of ascorbic acid and zinc sulfate heptahydrate is 1:5, performing stirring to uniformly mix the solution, adjusting the pH value of the solution to 13 with a sodium hydroxide solution having a mol concentration of 1 mol/L, and continuing performing stirring; and (3) performing reaction for 12-120h at a room temperature while the obtained solution is standing, performing centrifugal separation, performing washing, performing vacuum drying for 12h at 60 DEG C, and performing calcination for 1-5h at a temperature of 300-600 DEG C to obtain the zinc oxide photocatalyst with different micro-morphologies. According to the invention, the method is simple in equipment, mild in condition, easy and simple to operate, and easily available in raw material, and the prepared zinc oxide photocatalyst with different micro-morphologies is special in morphology and has relatively high photocatalytic activity.
Description
Technical field
The invention belongs to the synthesis technical field of photocatalyst of zinc oxide, be specifically related to a kind of biomimetic synthesis method of photocatalyst of zinc oxide of morphology controllable.
Background technology
Photocatalytic pollutant degradation, as a high-level oxidation technology, has application prospect for environment remediation, have also been obtained increasing concern.And photochemical catalyst is the core of this technology, in numerous semiconductor light-catalysts, ZnO due to its chemical stability and Heat stability is good, biological safety is high, reaction condition is gentle, to the advantage such as the selective little and photocatalysis performance of system is good, receive and pay attention to widely in the process of Recalcitrant chemicals.
Under UV-irradiation, ZnO shows high photocatalytic activity, organic pollutants of can degrading rapidly.The crystal phase structure, appearance and size etc. of photochemical catalyst are the principal elements affecting its ultraviolet catalytic activity, and these have inseparable relation with its synthetic method and preparation condition.The ZnO of nanoscale, because its size is little, specific area large, have the features such as obvious surface and interface effect, thus shows more excellent performance in photochemical catalyst field.The method of making ZnO is a lot, and conventional method has hydro-thermal method, sol-gel process and solid phase method etc., and the ZnO photocatalyst that diverse ways obtains has different structures, pattern and size, and photocatalytic activity is widely different.For improving the photocatalytic activity of ZnO, people often adopt some technological means to change physical dimension and the pattern of ZnO, such as synthesize ZnO in organic solvent or adopt its pattern of inducing action modulation of chemical organic reagent, but these measures not only increase preparation cost, but also bring pressure to environment.Therefore, find a kind of simple, easy to operate and eco-friendly synthetic method to prepare and there is morphology controllable and active high ZnO is significant.
Summary of the invention
The technical problem that the present invention solves there is provided a kind of biomimetic synthesis method of photocatalyst of zinc oxide of morphology controllable, and this synthetic method mild condition, simple and environmental friendliness, products obtained therefrom morphology controllable also has higher photocatalytic activity.
The present invention adopts following technical scheme for solving the problems of the technologies described above, and the biomimetic synthesis method of the photocatalyst of zinc oxide of morphology controllable, is characterized in that comprising the steps: that soluble in water for ascorbic acid being uniformly mixed is obtained uniform solution by (1); (2) add Zinc vitriol in the uniform solution obtained to step (1), wherein the mol ratio of ascorbic acid and Zinc vitriol is 1:5, is uniformly mixed, then is 13 by the sodium hydroxide solution adjust ph that molar concentration is 1mol/L, continues to stir; (3) reaction 12-120h is left standstill in room temperature, centrifugation, washing, 60 DEG C of vacuum drying 12h, then in 300-600 DEG C of calcining 1-5h, the photocatalyst of zinc oxide of obtained diverse microcosmic appearance;
In step (1) by soluble in water for ascorbic acid be uniformly mixed the uniform solution obtaining 0.083mol/L time set of nanowires that to obtain by average diameter the be 80nm fishnet shape photocatalyst of zinc oxide dressed up;
In step (1) by soluble in water for ascorbic acid be uniformly mixed the uniform solution obtaining 0.042mol/L time nanometer sheet that to obtain by average thickness the be 50nm flower-shaped photocatalyst of zinc oxide of tree peony that is assembled into;
In step (1) by soluble in water for ascorbic acid be uniformly mixed the uniform solution obtaining 0.021mol/L time groups of grains that to obtain by average diameter the be 15nm Crassulaceae sky chapter dressed up belong to succulent sky Pingyue County shape photocatalyst of zinc oxide;
In step (1) by soluble in water for ascorbic acid be uniformly mixed the uniform solution obtaining 0.010mol/L time obtain Crassulaceae thick leaf grass and belong to succulent peach beauty shape photocatalyst of zinc oxide;
In step (1) by soluble in water for ascorbic acid be uniformly mixed the uniform solution obtaining 0.005mol/L time average diameter that to obtain by average diameter be the particle packing of 31nm be the porous cauliflower-shaped photocatalyst of zinc oxide of 900nm.
The present invention and adopting compared with the ZnO photocatalyst prepared of other method has the following advantages: (1) avoids in organic solvent or synthesizes in the mixed solvent of organic reagent and water, it also avoid simultaneously and use poisonous and hazardous chemical organic reagent to carry out the pattern of modulation product, because of but a kind of eco-friendly synthetic method; (2) simple, the mild condition of equipment, easy and simple to handle and raw material are easy to get; (3) the photocatalyst of zinc oxide pattern of the diverse microcosmic appearance prepared is unique and have higher photocatalytic activity.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the photocatalyst of zinc oxide that the embodiment of the present invention 1 obtains, Fig. 2 is the SEM figure of the photocatalyst of zinc oxide that the embodiment of the present invention 2 obtains, Fig. 3 is the FESEM figure of the photocatalyst of zinc oxide that the embodiment of the present invention 3 obtains, Fig. 4 is the FESEM figure of the photocatalyst of zinc oxide that the embodiment of the present invention 4 obtains, the photocatalyst of zinc oxide 2 of Fig. 5 to be the FESEM figure of the obtained photocatalyst of zinc oxide of the embodiment of the present invention 5, Fig. 6 the be embodiment of the present invention 2 bio-mimetic syntheses and the ZnO of ordinary precipitation process synthesis are to the correlation curve of rhodamine B degradation rate.
Detailed description of the invention
Be described in further details foregoing of the present invention by the following examples, but this should be interpreted as that 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 scope of the present invention.
Embodiment 1
Getting 4mmol ascorbic acid is dissolved in 48mL water, stirs 0.5h and obtains uniform solution; In uniform solution, add 20mmol Zinc vitriol, stir 2h, then be 13 by the sodium hydroxide solution adjust ph of 1mol/L, continue to stir 0.5h; Then leave standstill reaction 120h in room temperature, centrifugation, washing, 60 DEG C of vacuum drying 12h, then in 400 DEG C of calcining 5h, the fishnet shape photocatalyst of zinc oxide 1 that the set of nanowires that to obtain by average diameter be 80nm is dressed up, its pattern as shown in Figure 1.
Embodiment 2
Getting 2mmol ascorbic acid is dissolved in 48mL water, stirs 0.5h and obtains uniform solution; In uniform solution, add 10mmol Zinc vitriol, stir 2h, then be 13 by the sodium hydroxide solution adjust ph of 1mol/L, continue to stir 0.5h; Then leave standstill reaction 120h in room temperature, centrifugation, washing, 60 DEG C of vacuum drying 12h, then in 300 DEG C of calcining 2h, the flower-shaped photocatalyst of zinc oxide 2 of tree peony that the nanometer sheet that to obtain by average thickness be 50nm is assembled into, its pattern as shown in Figure 2.
Embodiment 3
Getting 1mmol ascorbic acid is dissolved in 48mL water, stirs 0.5h and obtains uniform solution; In uniform solution, add 5mmol Zinc vitriol, stir 2h, then be 13 by the sodium hydroxide solution adjust ph of 1mol/L, continue to stir 0.5h; Then reaction 12h is left standstill in room temperature, centrifugation, washing, 60 DEG C of vacuum drying 12h, again in 600 DEG C of calcining 1h, the Crassulaceae sky chapter that the groups of grains that to obtain by average diameter be 15nm is dressed up belongs to succulent sky Pingyue County shape photocatalyst of zinc oxide 3, and its pattern as shown in Figure 3.
Embodiment 4
Getting 0.5mmol ascorbic acid is dissolved in 48mL water, stirs 0.5h and obtains uniform solution; In uniform solution, add 2.5mmol Zinc vitriol, stir 2h, then be 13 by the sodium hydroxide solution adjust ph of 1mol/L, continue to stir 0.5h; Then reaction 72h is left standstill in room temperature, centrifugation, washing, 60 DEG C of vacuum drying 12h, again in 450 DEG C of calcining 3h, obtain the thick leaf grass of Crassulaceae and belong to succulent peach beauty shape photocatalyst of zinc oxide 4, the particle that its porous hollow " petal " is 31nm by average diameter assembles, and pattern as shown in Figure 4.
Embodiment 5
Getting 0.25mmol ascorbic acid is dissolved in 48mL water, stirs 0.5h and obtains uniform solution; In uniform solution, add 1.25mmol Zinc vitriol, stir 2h, then be 13 by the sodium hydroxide solution adjust ph of 1mol/L, continue to stir 0.5h; Then reaction 96h is left standstill in room temperature, centrifugation, washing, 60 DEG C of vacuum drying 12h, again in 500 DEG C of calcining 3h, the average diameter that to obtain by average diameter be the particle packing of 31nm is the porous cauliflower-shaped photocatalyst of zinc oxide 5 of 900nm, and its pattern as shown in Figure 5.
Embodiment 6
The photocatalyst of zinc oxide 2 of ZnO prepared by embodiment 2 that the present embodiment is used.In order to contrast, get the photocatalyst of zinc oxide 2 of equivalent (0.0500g) and the obtained ZnO of ordinary precipitation process respectively, join in rhodamine B (RhB) solution that 200mL mass concentration is 5mg/L, be transferred in light-catalyzed reaction glass reactor after ultrasonic 20min, 30min is stirred, to reach adsorption/desorption balance at lucifuge place.Adopt the high-pressure sodium lamp of 300W as light source, then pass into air with the speed of 80mL/min, turn on light and Keep agitation, at interval of certain hour sampling once, centrifugation, gets its supernatant measures rhodamine B residual concentration with 722 type ultraviolet-uisible spectrophotometers (λ=554nm).The ZnO of photocatalyst of zinc oxide 2 and ordinary precipitation process synthesis to the correlation curve of rhodamine B degradation rate as shown in Figure 6, as can be seen from this figure, in identical degradation time, the degradation speed of photocatalyst of zinc oxide 2 pairs of rhodamine Bs is apparently higher than the obtained ZnO of ordinary precipitation process.Equally, show through photocatalytic degradation experiment the ZnO photocatalyst that the photocatalyst of zinc oxide that other embodiment obtains obtains apparently higher than ordinary precipitation process the degradation rate of rhodamine B.Therefore, the ZnO photocatalyst that the photocatalytic activity of the photocatalyst of zinc oxide of diverse microcosmic appearance that prepared by the present invention is prepared higher than ordinary precipitation process.
Embodiment above describes general principle of the present invention, principal character and advantage; the technical staff of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and description just illustrates principle of the present invention; 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 biomimetic synthesis method of the photocatalyst of zinc oxide of morphology controllable, is characterized in that comprising the steps: that soluble in water for ascorbic acid being uniformly mixed is obtained uniform solution by (1); (2) add Zinc vitriol in the uniform solution obtained to step (1), wherein the mol ratio of ascorbic acid and Zinc vitriol is 1:5, is uniformly mixed, then is 13 by the sodium hydroxide solution adjust ph that molar concentration is 1mol/L, continues to stir; (3) reaction 12-120h is left standstill in room temperature, centrifugation, washing, 60 DEG C of vacuum drying 12h, then in 300-600 DEG C of calcining 1-5h, the photocatalyst of zinc oxide of obtained diverse microcosmic appearance;
The fishnet shape photocatalyst of zinc oxide that the set of nanowires that to obtain by average diameter when the molar concentration of ascorbic acid is 0.083mol/L in uniform solution in step (1) be 80nm is dressed up;
The flower-shaped photocatalyst of zinc oxide of tree peony that the nanometer sheet that to obtain by average thickness when the molar concentration of ascorbic acid is 0.042mol/L in uniform solution in step (1) be 50nm is assembled into;
The Crassulaceae sky chapter that the groups of grains that to obtain by average diameter when the molar concentration of ascorbic acid is 0.021mol/L in uniform solution in step (1) be 15nm is dressed up belongs to succulent sky Pingyue County shape photocatalyst of zinc oxide;
Obtain Crassulaceae thick leaf grass when the molar concentration of ascorbic acid is 0.010mol/L in uniform solution in step (1) and belong to succulent peach beauty shape photocatalyst of zinc oxide;
The average diameter that to obtain by average diameter when the molar concentration of ascorbic acid is 0.005mol/L in step (1) uniform solution be the particle packing of 31nm is the porous cauliflower-shaped photocatalyst of zinc oxide of 900nm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112517046A (en) * | 2020-12-29 | 2021-03-19 | 河南师范大学 | Universal preparation method of hierarchical-pore nitrogen-doped carbon-oxygen reduction catalyst based on double-pore-foaming agent synthesis |
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| US20090062109A1 (en) * | 2007-09-04 | 2009-03-05 | Boyd Joel E | Composite catalytic material and process for manufacture of such material |
| CN103400878A (en) * | 2013-07-30 | 2013-11-20 | 天津大学 | Zinc oxide nanopencil array electrode and preparation method and application thereof |
| CN103675026A (en) * | 2013-11-27 | 2014-03-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of classification self-assembly zinc oxide micro-nano structure for gas sensor |
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| CN112517046A (en) * | 2020-12-29 | 2021-03-19 | 河南师范大学 | Universal preparation method of hierarchical-pore nitrogen-doped carbon-oxygen reduction catalyst based on double-pore-foaming agent synthesis |
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