CN105561965A - Preparation method of flower shaped ZnO/graphene composite microsphere - Google Patents
Preparation method of flower shaped ZnO/graphene composite microsphere Download PDFInfo
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- CN105561965A CN105561965A CN201511033046.4A CN201511033046A CN105561965A CN 105561965 A CN105561965 A CN 105561965A CN 201511033046 A CN201511033046 A CN 201511033046A CN 105561965 A CN105561965 A CN 105561965A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 73
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 50
- 239000004005 microsphere Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000002131 composite material Substances 0.000 title abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 8
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000004246 zinc acetate Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 24
- 239000010439 graphite Substances 0.000 claims description 24
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- 239000007864 aqueous solution Substances 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 9
- -1 polytetrafluoroethylene Polymers 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- 230000001699 photocatalysis Effects 0.000 abstract description 14
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 abstract description 12
- 229940012189 methyl orange Drugs 0.000 abstract description 12
- 239000000463 material Substances 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 239000011941 photocatalyst Substances 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 4
- 239000007795 chemical reaction product Substances 0.000 abstract 2
- 238000001816 cooling Methods 0.000 abstract 2
- 239000002253 acid Substances 0.000 abstract 1
- 230000007794 irritation Effects 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 88
- 239000011787 zinc oxide Substances 0.000 description 44
- 238000007146 photocatalysis Methods 0.000 description 9
- 150000001875 compounds Chemical class 0.000 description 8
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 8
- 238000000034 method Methods 0.000 description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 4
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000004043 dyeing Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 244000145845 chattering Species 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 1
- 230000036962 time dependent Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
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Abstract
The invention discloses a preparation method of a flower shaped ZnO/graphene composite microsphere. The preparation method comprises the following steps: mixing zinc acetate and critic acid, sequentially adding deionized water and anhydrous ethanol into the mixture, evenly mixing, slowly adding sodium hydroxide; transferring the solution to a reactor, drying the reactor, naturally cooling to the room temperature, washing the reaction product by deionized water and anhydrous ethanol, drying the obtained sample overnight in vacuum; transferring the solution to a reactor, drying the reactor, naturally cooling to the room temperature, washing the reaction product by deionized water and anhydrous ethanol, and drying the obtained sample overnight in vacuum. By combining ZnO and graphene, the separation of electron and cavity is promoted, the combination of electron and cavity is inhibited, thus a photocatalyst material having the advantages of high catalytic efficiency and low cost can be obtained, and under the irritation of ultraviolet rays, the methyl orange can be degraded in the presence of the flower shaped ZnO/graphene composite microsphere. Through the graphene doping, the transferring of photo-generated electron is promoted, the electron-cavity combination is inhibited, and thus the photocatalytic performance is enhanced.
Description
Technical field
The present invention relates to a kind of ZnO photocatalyst, in particular a kind of preparation method of flower-shaped ZnO/ Graphene complex microsphere.
Background technology
Along with the development of society, the growth of dyeing, the sewage produced of printing and dyeing makes great impact to environment.Because the high chroma of waste water from dyestuff, organic principle are complicated, be difficult to decompose, have a strong impact on the various features such as water quality environment, be a great problem in Industrial Wastewater Treatment always.The sewage solution produced for printing and dyeing is mainly divided into physical method and chemical method.Utilize the organic pollution in photocatalytic degradation water, owing to having non-secondary pollution, low cost and other advantages, receives and pays close attention to more and more widely.
Advantages such as ZnO is because having stable chemical nature, nontoxic, pollution-free and by fields such as wide variety of user photocatalysis, gas sensor and lithium batteries.In photocatalytic applications field, have that particle dispersion is poor, quantum efficiency is on the low side due to ZnO and the shortcoming such as electron-hole compound is serious, restrict its industrialized development.Some achievements in research show: carry out compound by ZnO, effectively can inhibit the compound of electron-hole, improve photocatalysis efficiency.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of preparation method of flower-shaped ZnO/ Graphene complex microsphere, by water heat transfer ZnO/ graphene complex, improve photocatalysis performance.
The present invention is achieved by the following technical solutions, the present invention includes following steps:
(1) making ZnO
(11) by zinc acetate and citric acid mixing, in mixture, add deionized water successively and absolute ethyl alcohol mixes, under the condition stirred, slowly add NaOH;
(12) above-mentioned solution is transferred in reactor, reactor is dried 20 ~ 28h at 100 ~ 150 DEG C, and naturally cool to room temperature, then use deionized water and absolute ethanol washing, the ZnO sample obtained is 50 ~ 70 DEG C of vacuum dried overnight, stand-by;
(2) preparation of ZnO/ Graphene
Get in the aqueous solution that the ZnO prepared joins containing graphite oxide, then solution is transferred in reactor, reactor is dried 2 ~ 4h at 100 ~ 150 DEG C, naturally cool to room temperature, use deionized water and absolute ethanol washing again, the ZnO/ Graphene complex microsphere sample obtained is 50 ~ 70 DEG C of vacuum dried overnight, stand-by.
In described step (11), get 0.6 ~ 1.0g zinc acetate and the mixing of 0.5 ~ 0.8g citric acid, in mixture, add 50mL deionized water successively and 10mL absolute ethyl alcohol mixes, under the condition stirred, slowly add the NaOH of 18 ~ 25mL1mol/L.
In described step (2), in the ZnO/ Graphene complex microsphere prepared, the mass content of graphite oxide is 0 ~ 10%.
In described step (2), get the ZnO that 0.2g prepares and join in the graphite oxide aqueous solution 30mL of different quality, wherein graphite oxide content is respectively 0g, 0.002g, 0.004g, 0.006g, 0.012g, 0.02g.
In described step (12), reactor is the autoclave of inner liner polytetrafluoroethylene.
The ZnO/ Graphene complex microsphere that a kind of described preparation method obtains.
The present invention has the following advantages compared to existing technology: the present invention is by ZnO and Graphene compound, being separated of electronics and hole can be promoted, suppress its compound, the catalysis material that catalytic efficiency is high, cost is low can be obtained, adopt a kind of composite of simple and effective water heat transfer ZnO/ Graphene, as photochemical catalyst.Under UV-irradiation, photo-catalytic degradation of methyl-orange.Pass through, the doping of Graphene, composite advantageous, in the transfer of light induced electron, suppresses electron-hole compound, thus improves photocatalysis performance.
Accompanying drawing explanation
Fig. 1 is that SEM of the present invention schemes;
Fig. 2 is the XRD figure of ZnO and ZnO/ Graphene;
Fig. 3 is the Raman collection of illustrative plates of ZG-3, ZnO and Graphene;
Fig. 4 be methyl orange under the effect of ZnO/ Graphene with photocatalytic process under UV-irradiation ultraviolet-visible light spectrogram;
Fig. 5 is under UV-irradiation, and ZnO, ZG-1, ZG-2, ZG-3, ZG-4 and ZG-5 are to the efficiency schematic diagram of Photocatalytic Degradation of Methyl Orange.
Detailed description of the invention
Elaborate to embodiments of the invention below, the present embodiment is implemented under premised on technical solution of the present invention, give detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
The reagent of the present embodiment: potassium permanganate, NaOH, 30% (w) hydrogen peroxide, citric acid, zinc acetate, hydrochloric acid, sulfuric acid, nitric acid, absolute ethyl alcohol, methyl orange are to be analyzed pure, and graphite is all purchased from Chemical Reagent Co., Ltd., Sinopharm Group; Use for laboratory water is all from redistilled water.
UV-3310 ultraviolet-uisible spectrophotometer (HIT), DX-2600X x ray diffractometer x (Dandong Fangyuan Instrument Co., Ltd.), HATICH-1510 electron microscope (Jeol Ltd.).
The preparation method of the present embodiment comprises the following steps:
The citric acid of the zinc acetate of 0.8g and 0.6g is mixed, adds 50mL deionized water to the inside, then add 10mL absolute ethyl alcohol and mix, under the condition stirred, slowly add the NaOH of 20mL1mol/L.Then above-mentioned solution is transferred in the autoclave of 100mL inner liner polytetrafluoroethylene, take out after reactor being put into 120 DEG C of baking oven 24h, naturally cool to room temperature, then use deionized water and absolute ethanol washing, the sample obtained is 60 DEG C of vacuum dried overnight, stand-by.
By Hummers legal system for graphite oxide.Get in the 30mL aqueous solution that 0.2gZnO joins containing graphite oxide, then solution is transferred in the autoclave of 100mL inner liner polytetrafluoroethylene, take out after reactor being put into 120 DEG C of baking oven 3h, naturally cool to room temperature, use deionized water and absolute ethanol washing again,, the sample obtained is 60 DEG C of vacuum dried overnight, stand-by.
In the present embodiment, in the aqueous solution of graphite oxide, the content of graphite oxide is 0g, is designated as ZG-0.
Embodiment 2
In the present embodiment, in the aqueous solution of graphite oxide, the content of graphite oxide is 0.002g, is designated as ZG-1.Other embodiments are identical with embodiment 1.
Embodiment 3
In the present embodiment, in the aqueous solution of graphite oxide, the content of graphite oxide is 0.004g, is designated as ZG-2.Other embodiments are identical with embodiment 1.
Embodiment 4
In the present embodiment, in the aqueous solution of graphite oxide, the content of graphite oxide is 0.006g, is designated as ZG-3.Other embodiments are identical with embodiment 1.
Embodiment 5
In the present embodiment, in the aqueous solution of graphite oxide, the content of graphite oxide is 0.012g, is designated as ZG-4.Other embodiments are identical with embodiment 1.
Embodiment 6
In the present embodiment, in the aqueous solution of graphite oxide, the content of graphite oxide is 0.02g, is designated as ZG-5.Other embodiments are identical with embodiment 1.
In embodiment 1 ~ 6, in ZnO/ Graphene, the content of graphite oxide is respectively 0,1%, 2%, 3%, 6% and 10% (mass fraction).
As shown in Figure 1, in Fig. 1, a, b are the SEM pictures preparing pure zinc oxide, and as can be seen from the figure zinc oxide is flower-shaped, and specific area is larger.That c, d show is the SEM of Graphene, therefrom can find out that Graphene is fold and curling transparent membrane.E, f are the SEM pictures of ZnO/ graphene complex, and as can be seen from the figure fold, transparent graphene are entrained in ZnO flower-like microsphere.
As shown in Figure 2, in 2 θ=32.1,34.6,36.4,47.7,56.7,63.1,66.6,68.2, the diffraction maximum at 69.2 places correspond to (100), (002), (101), (102), (110), (103), (200), (112), (201) face respectively, consistent with the standard diagram (JCPDS36-1451) of ZnO.Do not have unnecessary peak to occur after doping, show: the doping through Graphene does not have other material to generate.But, the diffraction maximum of ZnO/ Graphene and the same of ZnO, be due to doping after sample in Graphene content less, do not demonstrate the characteristic peak of Graphene.
As shown in Figure 3, Graphene has 2 Raman peaks, lays respectively at 1352cm
-1and 1586cm
-1place, corresponding to D peak and G peak.ZnO is at 435cm
-1there is a strong Raman peaks at place, and corresponding to the E2 in ZnO, contrast ZnO, ZG-3 is many at 1349cm
-1the D peak at place and 1591cm
-1g peak.G peak is due at sp
2c-C key chattering causes, and D peak is caused by the hexagon Graphene of symmetry.
The time dependent rule of methyl orange characteristic absorption peak intensity is detected with ultraviolet-uisible spectrophotometer.In the ordinary course of things, methyl orange solution is very stable, and characteristic absorption peak is at 460nm place.Fig. 4 be methyl orange under the effect of ZnO/ Graphene with photocatalytic process under UV-irradiation ultraviolet-visible light spectrogram.Along with the increase of time, methyl orange declines gradually at the absworption peak at 460nm place, shows that catalyst is under the irradiation of ultraviolet light, has decomposed methyl orange gradually.
Under UV-irradiation, carried out the experiment of ZnO, ZG-1, ZG-2, ZG-3, ZG-4 and ZG-5 photo-catalytic degradation of methyl-orange, result as shown in Figure 5.As can be seen from the figure, under UV-irradiation, when not using photochemical catalyst, methyl orange can not be reduced.In addition, ZnO/ graphene complex presents the photocatalysis performance more excellent than pure ZnO.In ZnO after doped graphene, when the photocatalysis time is 140min, ZG-3 photocatalysis efficiency reaches maximum, and maximal efficiency is 90%.This shows that Graphene has played important effect when ZnO/ graphene complex photo catalytic reduction degraded methyl orange.After doped graphene, compound light absorption strengthens and decreases electron-hole compound, thus improves photocatalysis performance.
But when the content of Graphene exceeds certain value, its photocatalysis efficiency reduces, may be formed due to following two reasons: (1) zinc oxide and Graphene compete mutually absorption ultraviolet light; (2) too much Graphene as complex centre, for electronics transmission provides unnecessary path, can increase the probability of electron-hole compound.
By experimental result, infer and possible experiment mechanism: UV-irradiation on zinc oxide, is sent to after the electronics in valence band is stimulated on conduction band, the electronics on conduction band and combination with oxygen soluble in water produce O
2*, the hole in zinc oxide valence band is transferred in Graphene valence band, and UV-irradiation is in Graphene valence band, valence band is transmitted electronically on conduction band, the hydroxide ion of the hole stayed in water is combined, and generate OH*, electronics unnecessary on conduction band can be sent to zinc oxide again.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (6)
1. a preparation method for flower-shaped ZnO/ Graphene complex microsphere, is characterized in that, comprise the following steps:
(1) making ZnO
(11) by zinc acetate and citric acid mixing, in mixture, add deionized water successively and absolute ethyl alcohol mixes, under the condition stirred, slowly add NaOH;
(12) above-mentioned solution is transferred in reactor, reactor is dried 20 ~ 28h at 100 ~ 150 DEG C, and naturally cool to room temperature, then use deionized water and absolute ethanol washing, the ZnO sample obtained is 50 ~ 70 DEG C of vacuum dried overnight, stand-by;
(2) preparation of ZnO/ Graphene
Get in the aqueous solution that the ZnO prepared joins containing graphite oxide, then solution is transferred in reactor, reactor is dried 2 ~ 4h at 100 ~ 150 DEG C, naturally cool to room temperature, use deionized water and absolute ethanol washing again, the ZnO/ Graphene complex microsphere sample obtained is 50 ~ 70 DEG C of vacuum dried overnight, stand-by.
2. the preparation method of a kind of flower-shaped ZnO/ Graphene complex microsphere according to claim 1, it is characterized in that, in described step (11), get 0.6 ~ 1.0g zinc acetate and the mixing of 0.5 ~ 0.8g citric acid, 50mL deionized water is added successively and 10mL absolute ethyl alcohol mixes in mixture, under the condition stirred, slowly add the NaOH of 18 ~ 25mL1mol/L.
3. the preparation method of a kind of flower-shaped ZnO/ Graphene complex microsphere according to claim 1, is characterized in that, in described step (2), in the ZnO/ Graphene complex microsphere prepared, the mass content of graphite oxide is 0 ~ 10%.
4. the preparation method of a kind of flower-shaped ZnO/ Graphene complex microsphere according to claim 1, it is characterized in that, in described step (2), get the ZnO that 0.2g prepares to join in the graphite oxide aqueous solution 30mL of different quality, wherein graphite oxide content is respectively 0g, 0.002g, 0.004g, 0.006g, 0.012g, 0.02g.
5. the preparation method of a kind of flower-shaped ZnO/ Graphene complex microsphere according to claim 1, it is characterized in that, in described step (12), reactor is the autoclave of inner liner polytetrafluoroethylene.
6. the ZnO/ Graphene complex microsphere that preparation method obtains as described in any one of Claims 1 to 5.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106268642A (en) * | 2016-09-09 | 2017-01-04 | 北京优碳环能科技有限公司 | Bobbles shape zinc oxide/graphene composite adsorbent and preparation method and application |
| CN108077250A (en) * | 2017-12-14 | 2018-05-29 | 安徽喜尔奇日用品有限公司 | Complex microsphere with efficient sterilizing performance |
| CN108579759A (en) * | 2018-03-30 | 2018-09-28 | 佛山市熙华科技有限公司 | A kind of preparation method of environment-friendly high-efficiency photocatalyst material |
| CN108993467A (en) * | 2018-08-15 | 2018-12-14 | 江苏仁净环保科技有限公司 | A kind of nano-photocatalyst and preparation method and application for sewage treatment |
| CN110227453A (en) * | 2019-04-17 | 2019-09-13 | 江苏省农业科学院 | A kind of preparation method of Ag/ZnO/GO composite visible light catalyst |
| CN111122006A (en) * | 2020-01-12 | 2020-05-08 | 哈尔滨理工大学 | Flower-shaped ZnO/graphene single-sphere micro-nano structure temperature sensor and manufacturing method thereof |
| CN113142743A (en) * | 2021-02-05 | 2021-07-23 | 宝峰时尚国际控股有限公司 | Application of composite photocatalytic material, sterilization and deodorization insole and shoe and preparation method |
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| CN104759282A (en) * | 2014-12-01 | 2015-07-08 | 青岛科技大学 | Novel method for microwave-assisted preparation of zinc oxide/graphene/silver nano-composite photocatalyst |
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| CN104759282A (en) * | 2014-12-01 | 2015-07-08 | 青岛科技大学 | Novel method for microwave-assisted preparation of zinc oxide/graphene/silver nano-composite photocatalyst |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106268642A (en) * | 2016-09-09 | 2017-01-04 | 北京优碳环能科技有限公司 | Bobbles shape zinc oxide/graphene composite adsorbent and preparation method and application |
| CN106268642B (en) * | 2016-09-09 | 2019-04-12 | 北京优碳环能科技有限公司 | Bobbles shape zinc oxide/graphene composite adsorbent and the preparation method and application thereof |
| CN108077250A (en) * | 2017-12-14 | 2018-05-29 | 安徽喜尔奇日用品有限公司 | Complex microsphere with efficient sterilizing performance |
| CN108579759A (en) * | 2018-03-30 | 2018-09-28 | 佛山市熙华科技有限公司 | A kind of preparation method of environment-friendly high-efficiency photocatalyst material |
| CN108993467A (en) * | 2018-08-15 | 2018-12-14 | 江苏仁净环保科技有限公司 | A kind of nano-photocatalyst and preparation method and application for sewage treatment |
| CN110227453A (en) * | 2019-04-17 | 2019-09-13 | 江苏省农业科学院 | A kind of preparation method of Ag/ZnO/GO composite visible light catalyst |
| CN110227453B (en) * | 2019-04-17 | 2022-03-25 | 江苏省农业科学院 | Preparation method of AgCl/ZnO/GO composite visible light catalyst |
| CN111122006A (en) * | 2020-01-12 | 2020-05-08 | 哈尔滨理工大学 | Flower-shaped ZnO/graphene single-sphere micro-nano structure temperature sensor and manufacturing method thereof |
| CN113142743A (en) * | 2021-02-05 | 2021-07-23 | 宝峰时尚国际控股有限公司 | Application of composite photocatalytic material, sterilization and deodorization insole and shoe and preparation method |
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