CN102228827A - Method for preparing Mg2<+>-doped ZnO nano-photochemical catalyst - Google Patents
Method for preparing Mg2<+>-doped ZnO nano-photochemical catalyst Download PDFInfo
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- CN102228827A CN102228827A CN2011101002829A CN201110100282A CN102228827A CN 102228827 A CN102228827 A CN 102228827A CN 2011101002829 A CN2011101002829 A CN 2011101002829A CN 201110100282 A CN201110100282 A CN 201110100282A CN 102228827 A CN102228827 A CN 102228827A
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- photochemical catalyst
- zinc oxide
- oxide nanometer
- nitrate hexahydrate
- magnesium sulfate
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Abstract
The invention relates to a method for preparing a Mg2<+>-doped ZnO nano-photochemical catalyst, which is characterized by comprising the following steps: taking phenylcarbinol as a solvent; and reacting zinc nitrate hexahydrate, an anhydrous magnesium sulfate solution with the concentration being 0.01mol/L with a sodium hydroxide water solution with the concentration being 1mol/L for 24 hours, wherein the mole ratio of the zinc nitrate hexahydrate to the anhydrous magnesium sulfate to the sodium hydroxide is 1: (0.01-0.04): (0.5-1.5). The method is simple in operation, and the degradation rate of the catalyst prepared by the method to catalyze and degrade rhodamine B is higher than that of a pure ZnO nano-photochemical catalyst.
Description
Technical field
The invention belongs to the material technology field, be specifically related to photochemical catalyst and preparation method thereof.
Background technology
At present, metal oxide semiconductor and sulfide is as photochemical catalyst, for example TiO
2, ZnO, CdS, WO
3Deng, caused that people pay close attention to widely.In these catalyst, ZnO is as the semiconductor material with wide forbidden band of direct band gap, and energy gap is 3.37eV under the room temperature, is a kind of extremely important catalyst.ZnO was studied by a lot of people as the photocatalyst for degrading organic pollution.Yet, as light-catalyst ZnO himself shortcoming is arranged also, for example, its catalytic efficiency is not very high, can not satisfy commercial the application.Thereby, just there is a lot of research work research to improve the photocatalysis efficiency of ZnO, generally speaking, select for use suitable surface vacancy or trapping agent to catch the room or electronics can make recombination process be suppressed, and then just can improve its photocatalysis efficiency.At present, can obviously suppress the electron-hole pair composite methods and mainly comprise compound, the surface sensitizing between the size that reduces semiconductor particle, the semiconductor, the doping of metal ion and surface deposition of noble metal etc., wherein the doping of metal ion is a kind of effectively way.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of simple to operate, Mg that gained catalyst photocatalysis efficiency is high
2+The preparation method of doping zinc oxide nanometer photochemical catalyst.
Solving the problems of the technologies described above the technical scheme that is adopted is: be solvent with the phenmethylol, under 180 ℃ of conditions, the anhydrous magnesium sulfate aqueous solution of zinc nitrate hexahydrate, 0.01mol/L, the reaction of the sodium hydrate aqueous solution of 1mol/L 24 hours, the mol ratio of zinc nitrate hexahydrate and anhydrous magnesium sulfate, NaOH is 1: 0.01～0.04: 0.5～1.5, cooling, spend deionised water and use absolute ethanol washing 3 times for 3 times again, remove solvent and accessory substance, product after the washing is put into baking oven, 70 ℃ of dryings 12 hours are prepared into Mg
2+The doping zinc oxide nanometer photochemical catalyst.
The optimum mole ratio of zinc nitrate hexahydrate and anhydrous magnesium sulfate, NaOH is 1: 0.01: 1 among the present invention.
Adopt the Mg of the inventive method preparation
2+The doping zinc oxide nanometer photochemical catalyst, the degradation rate of catalytic degradation rhodamine B is higher than pure ZnO nano-photocatalyst under UV-irradiation.
Description of drawings
Fig. 1 is the Mg of zinc nitrate hexahydrate and the preparation of anhydrous magnesium sulfate different mol ratio
2+The X-ray diffraction spectrogram of doping zinc oxide nanometer photochemical catalyst.
Fig. 2 is the Mg of zinc nitrate hexahydrate and the preparation of NaOH different mol ratio
2+The X-ray diffraction spectrogram of doping zinc oxide nanometer photochemical catalyst.
Fig. 3 is the Mg of embodiment 1 preparation
2+The scanning electron microscope diagram of doping zinc oxide nanometer photochemical catalyst.
Fig. 4 is the Mg of embodiment 2 preparations
2+The scanning electron microscope diagram of doping zinc oxide nanometer photochemical catalyst.
Fig. 5 is the Mg of embodiment 3 preparations
2+The scanning electron microscope diagram of doping zinc oxide nanometer photochemical catalyst.
Fig. 6 is the Mg of embodiment 4 preparations
2+The scanning electron microscope diagram of doping zinc oxide nanometer photochemical catalyst.
Fig. 7 is the Mg of embodiment 5 preparations
2+The scanning electron microscope diagram of doping zinc oxide nanometer photochemical catalyst.
Fig. 8 is the scanning electron microscope diagram of the ZnO nano-photocatalyst for preparing of comparative example.
Fig. 9 is the Mg of zinc nitrate hexahydrate and the preparation of anhydrous magnesium sulfate different mol ratio
2+The ultraviolet-visible absorption spectroscopy figure of doping zinc oxide nanometer photochemical catalyst catalytic degradation rhodamine B different time.
Figure 10 is the Mg of zinc nitrate hexahydrate and the preparation of NaOH different mol ratio
2+The ultraviolet-visible absorption spectroscopy figure of doping zinc oxide nanometer photochemical catalyst catalytic degradation rhodamine B different time.
The specific embodiment
The present invention is described in more detail below in conjunction with drawings and Examples, but the invention is not restricted to these embodiment.
With zinc nitrate hexahydrate 0.595g (0.002mol), 0.01mol/L anhydrous magnesium sulfate aqueous solution 2mL (0.00002mol), sodium hydrate aqueous solution 2mL (0.002mol) adding of 1mol/L fills in the reactor of 30mL phenmethylol, make the solid dissolving, be heated to 180 ℃, isothermal reaction 24 hours, after having reacted, naturally cool to room temperature, 4000 rev/mins of centrifugations of gained white precipitate 5 minutes, spend deionised water earlier and use absolute ethanol washing 3 times for 3 times again, remove solvent and accessory substance, product after the washing is put into baking oven, and 70 ℃ of dryings 12 hours are prepared into Mg
2+The doping zinc oxide nanometer photochemical catalyst.
The sodium hydrate aqueous solution 2mL (0.002mol) of anhydrous magnesium sulfate aqueous solution 4mL (0.00004mol), the 1mol/L of zinc nitrate hexahydrate 0.595g (0.002mol), 0.01mol/L added fill in the reactor of 30mL phenmethylol, make the solid dissolving, be heated to 180 ℃, isothermal reaction 24 hours, after having reacted, naturally cool to room temperature, 4000 rev/mins of centrifugations of gained white precipitate 5 minutes, with deionized water and absolute ethyl alcohol cyclic washing, remove solvent and accessory substance, product after the washing is put into baking oven, and 70 ℃ of dryings 12 hours are prepared into Mg
2+The doping zinc oxide nanometer photochemical catalyst.
The sodium hydrate aqueous solution 2mL (0.002mol) of anhydrous magnesium sulfate aqueous solution 8mL (0.00008mol), the 1mol/L of zinc nitrate hexahydrate 0.595g (0.002mol), 0.01mol/L added fill in the reactor of 30mL phenmethylol, make the solid dissolving, be heated to 180 ℃, isothermal reaction 24 hours, after having reacted, naturally cool to room temperature, 4000 rev/mins of centrifugations of gained white precipitate 5 minutes, with deionized water and absolute ethyl alcohol cyclic washing, remove solvent and accessory substance, product after the washing is put into baking oven, and 70 ℃ of dryings 12 hours are prepared into Mg
2+The doping zinc oxide nanometer photochemical catalyst.
With zinc nitrate hexahydrate 0.595g (0.002mol), 0.01mol/L anhydrous magnesium sulfate aqueous solution 2mL (0.00002mol), sodium hydrate aqueous solution 1mL (0.001mol) adding of 1mol/L fills in the reactor of 30mL phenmethylol, make the solid dissolving, be heated to 180 ℃, isothermal reaction 24 hours, after having reacted, naturally cool to room temperature, 4000 rev/mins of centrifugations of gained white precipitate 5 minutes, spend deionised water earlier and use absolute ethanol washing 3 times for 3 times again, remove solvent and accessory substance, product after the washing is put into baking oven, and 70 ℃ of dryings 12 hours are prepared into Mg
2+The doping zinc oxide nanometer photochemical catalyst.
Embodiment 5
With zinc nitrate hexahydrate 0.595g (0.002mol), 0.01mol/L anhydrous magnesium sulfate aqueous solution 2mL (0.00002mol), sodium hydrate aqueous solution 3mL (0.003mol) adding of 1mol/L fills in the reactor of 30mL phenmethylol, make the solid dissolving, be heated to 180 ℃, isothermal reaction 24 hours, after having reacted, naturally cool to room temperature, 4000 rev/mins of centrifugations of gained white precipitate 5 minutes, spend deionised water earlier and use absolute ethanol washing 3 times for 3 times again, remove solvent and accessory substance, product after the washing is put into baking oven, and 70 ℃ of dryings 12 hours are prepared into Mg
2+The doping zinc oxide nanometer photochemical catalyst.
The comparative example
Sodium hydrate aqueous solution 2mL (0.002mol) adding of zinc nitrate hexahydrate 0.595g (0.002mol), 1mol/L is filled in the reactor of 30mL phenmethylol, make the solid dissolving, be heated to 180 ℃, isothermal reaction 24 hours, after having reacted, naturally cool to room temperature, 4000 rev/mins of centrifugations of gained white precipitate 5 minutes, with deionized water and absolute ethyl alcohol cyclic washing, remove solvent and accessory substance, product after the washing is put into baking oven, and 70 ℃ of dryings 12 hours are prepared into the ZnO nano-photocatalyst.
The inventor is with the Mg of zinc nitrate hexahydrate among the embodiment 1～3 and the preparation of anhydrous magnesium sulfate different mol ratio
2+The Mg of zinc nitrate hexahydrate and NaOH different mol ratio preparation among doping zinc oxide nanometer photochemical catalyst, embodiment 1 and the embodiment 4～5
2+The ZnO nano-photocatalyst of doping zinc oxide nanometer photochemical catalyst, comparative example's preparation adopts D/Max-3c type x-ray diffractometer, Quanta 200 type transmission electron microscopes to characterize respectively, the results are shown in Figure 1～8.Fig. 1 is the Mg of zinc nitrate hexahydrate and the preparation of anhydrous magnesium sulfate different mol ratio
2+The X-ray diffraction spectrogram of doping zinc oxide nanometer photochemical catalyst, wherein curve a is the X-ray diffraction spectrogram of the ZnO nano-photocatalyst for preparing of comparative example, curve b, c, d are the Mg of embodiment 1, embodiment 2, embodiment 3 preparations successively
2+The X-ray diffraction spectrogram of doping zinc oxide nanometer photochemical catalyst; Fig. 2 is the Mg of zinc nitrate hexahydrate and the preparation of NaOH different mol ratio
2+The X-ray diffraction spectrogram of doping zinc oxide nanometer photochemical catalyst, wherein curve a, b, c are the Mg of embodiment 1, embodiment 4, embodiment 5 preparations successively
2+The X-ray diffraction spectrogram of doping zinc oxide nanometer photochemical catalyst; Fig. 3 is the Mg of embodiment 1 preparation
2+The scanning electron microscope diagram of doping zinc oxide nanometer photochemical catalyst; Fig. 4 is the Mg of embodiment 2 preparations
2+The scanning electron microscope diagram of doping zinc oxide nanometer photochemical catalyst; Fig. 5 is the Mg of embodiment 3 preparations
2+The scanning electron microscope diagram of doping zinc oxide nanometer photochemical catalyst; Fig. 6 is the Mg of embodiment 4 preparations
2+The scanning electron microscope diagram of doping zinc oxide nanometer photochemical catalyst; Fig. 7 is the Mg of embodiment 5 preparations
2+The scanning electron microscope diagram of doping zinc oxide nanometer photochemical catalyst; Fig. 8 is the scanning electron microscope diagram of the ZnO nano-photocatalyst for preparing of comparative example.
By Fig. 1 and Fig. 2 as seen, the Mg of zinc nitrate hexahydrate and anhydrous magnesium sulfate different mol ratio preparation among the embodiment 1～3
2+The Mg of zinc nitrate hexahydrate and NaOH different mol ratio preparation among doping zinc oxide nanometer photochemical catalyst, embodiment 1 and the embodiment 4～5
2+The diffraction maximum data of the ZnO nano-photocatalyst of doping zinc oxide nanometer photochemical catalyst and comparative example preparation and six sides are buergerite ZnO standard spectrum (a=0.3249nm mutually, c=0.52nm, JCPDSNo.36-1451) data are corresponding one by one, diffraction maximum is all narrow and the peak is very sharp-pointed, the crystallinity that ZnO is described is fine, in addition, do not have the existence at other dephasign peaks in the diffraction maximum, Mg is described
2+Being doped in the ZnO lattice of success.
By Fig. 3～8 as seen, the ZnO nano-photocatalyst of comparative example preparation is that the nano particle of 500nm left and right sides regular morphology is formed the Mg that zinc nitrate hexahydrate and anhydrous magnesium sulfate different mol ratio prepare among the embodiment 1～3 by particle diameter
2+The doping zinc oxide nanometer photochemical catalyst is that the nano particle of 500nm left and right sides regular morphology is formed by particle diameter also, shows Mg
2+Be doped among the ZnO and do not change pattern and the size of ZnO.And the Mg of embodiment 4～5 preparations
2+The doping zinc oxide nanometer photochemical catalyst is made up of the hollow bowl-shape nanocrystal and the rhombus nanometer sheet of 500nm left and right sides regular morphology respectively, shows that NaOH is to prepared Mg
2+The pattern influence of doping zinc oxide nanometer photochemical catalyst is bigger.
In order to determine beneficial effect of the present invention, the inventor adopts the Mg that zinc nitrate hexahydrate and anhydrous magnesium sulfate different mol ratio prepare among the embodiment 1～3
2+The Mg of zinc nitrate hexahydrate and NaOH different mol ratio preparation among doping zinc oxide nanometer photochemical catalyst, embodiment 1 and the embodiment 4～5
2+The ZnO nano-photocatalyst of doping zinc oxide nanometer photochemical catalyst and comparative example's preparation, the light degradation rhodamine B aqueous solution (rhodamine B by new fine chemistry industry development centre, sky, Tianjin sell) under ultraviolet light respectively, compare its photocatalytic activity, concrete test situation is as follows:
In 6 100mL beakers, add the nano-photocatalyst of 0.006g embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5, comparative example's preparation respectively, in 6 beakers, all add 60mL1.25 * 10 again
-5The rhodamine B aqueous solution of mol/L, magnetic agitation is 1 hour in the darkroom.
Will be in the darkroom solution of magnetic agitation after 1 hour place under the uviol lamp of 30W (distance between beaker mouth and ultraviolet lamp tube is 10cm), radiation wavelength be 254nm, intensity of illumination be under the 1.875lux condition irradiation (all tests are all at room temperature carried out, temperature is 20 ± 2 ℃), solution in the 5mL beaker was got at every interval in 1 hour, adopt ultraviolet-uisible spectrophotometer detect respectively the solution of getting at the maximum absorption band at 553nm place, testing result is seen Fig. 9 and Figure 10.Fig. 9 is the Mg of zinc nitrate hexahydrate and the preparation of anhydrous magnesium sulfate different mol ratio
2+The ultraviolet-visible absorption spectroscopy figure of doping zinc oxide nanometer photochemical catalyst catalytic degradation rhodamine B different time, wherein curve a, b, c are the Mg of embodiment 1, embodiment 2, embodiment 3 preparations successively
2+The ultraviolet-visible absorption spectroscopy figure of doping zinc oxide nanometer photochemical catalyst catalytic degradation different time, curve d are the ultraviolet-visible absorption spectroscopy figure of the ZnO nano-photocatalyst catalytic degradation rhodamine B different time for preparing of comparative example; Figure 10 is the Mg of zinc nitrate hexahydrate and the preparation of NaOH different mol ratio
2+The ultraviolet-visible absorption spectroscopy figure of doping zinc oxide nanometer photochemical catalyst catalytic degradation rhodamine B different time, wherein curve a, b, c are the Mg of embodiment 1, embodiment 4, embodiment 5 preparations successively
2+The ultraviolet-visible absorption spectroscopy figure of doping zinc oxide nanometer photochemical catalyst catalytic degradation different time.
As seen from Figure 9, the Mg of zinc nitrate hexahydrate and anhydrous magnesium sulfate different mol ratio preparation among the embodiment 1～3
2+The speed of doping zinc oxide nanometer photochemical catalyst catalytic degradation rhodamine B will be compared more faster than the speed of the ZnO nano-photocatalyst catalytic degradation rhodamine B of embodiment preparation, and the Mg of embodiment 1 preparation
2+The speed of doping zinc oxide nanometer photochemical catalyst catalytic degradation rhodamine B is the fastest, because the pattern of embodiment 1～3 photochemical catalyst all is the square nano particle about 500nm, illustrate that pattern can ignore to the influence of photocatalysis efficiency, thereby can prove not being both of photocatalysis efficiency because Mg
2+Doping different caused, the mol ratio that can determine best zinc nitrate hexahydrate and anhydrous magnesium sulfate, NaOH is 1: 0.01: 1
As seen from Figure 10, the Mg of embodiment 1, embodiment 4 and 5 preparations
2+The speed of doping zinc oxide nanometer photochemical catalyst catalytic degradation rhodamine B is all very fast, and the Mg of embodiment 1 preparation wherein
2+The speed of doping zinc oxide nanometer photochemical catalyst catalytic degradation rhodamine B is the fastest.Because embodiment 1 prepared photochemical catalyst is the square nano particle about 500nm, embodiment 4 is the hollow bowl-shape nanocrystal about 500nm, embodiment 5 is the rhombus nanometer sheet about 500nm, illustrate that different NaOH concentration is very big to the pattern influence of photochemical catalyst, and then influence its photocatalytic speed, wherein the photochemical catalyst efficient of square nano particle is best, and the mol ratio that can determine best zinc nitrate hexahydrate and anhydrous magnesium sulfate, NaOH is 1: 0.01: 1
Comprehensive above-mentioned result of the test, the mol ratio of zinc nitrate hexahydrate and anhydrous magnesium sulfate, NaOH are the Mg of 1: 0.01～0.04: 0.5～1.5 preparations
2+The photocatalysis performance of doping zinc oxide nanometer photochemical catalyst is all better, and wherein the mol ratio of zinc nitrate hexahydrate and anhydrous magnesium sulfate, NaOH is 1: 0.01: 1 o'clock, the Mg of preparation
2+The photocatalysis performance of doping zinc oxide nanometer photochemical catalyst is best.
Claims (2)
1. Mg
2+The preparation method of doping zinc oxide nanometer photochemical catalyst, it is characterized in that: be solvent with the phenmethylol, under 180 ℃ of conditions, the anhydrous magnesium sulfate aqueous solution of zinc nitrate hexahydrate, 0.01mol/L, the reaction of the sodium hydrate aqueous solution of 1mol/L 24 hours, the mol ratio of zinc nitrate hexahydrate and anhydrous magnesium sulfate, NaOH is 1: 0.01～0.04: 0.5～1.5, cooling, washing, drying are prepared into Mg
2+The doping zinc oxide nanometer photochemical catalyst.
2. Mg according to claim 1
2+The preparation method of doping zinc oxide nanometer photochemical catalyst is characterized in that: the mol ratio of described zinc nitrate hexahydrate and anhydrous magnesium sulfate, NaOH is 1: 0.01: 1.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103204538A (en) * | 2013-04-26 | 2013-07-17 | 通化师范学院 | Preparation method of porous ZnO and ZnO/Ag nanometer free-standing film |
| CN108906025A (en) * | 2018-08-01 | 2018-11-30 | 安徽锦华氧化锌有限公司 | A kind of preparation method of rare earth doped modified nano zinc oxide-graphene composite photocatalyst material |
| CN110560031A (en) * | 2019-09-10 | 2019-12-13 | 安徽锦华氧化锌有限公司 | Method for improving photocatalytic activity of zinc oxide |
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| CN101445961A (en) * | 2008-12-15 | 2009-06-03 | 浙江大学 | Superfine Mg-doped ZnO nano wire and synthetic method thereof |
| CN101565611A (en) * | 2009-06-04 | 2009-10-28 | 复旦大学 | Mg<2+> doped zinc oxide luminescent nanoparticle and the preparation method thereof |
| US20090297626A1 (en) * | 2006-11-03 | 2009-12-03 | The Trustees Of Columbia University In The City Of New York | Methods for preparing metal oxides |
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2011
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| US20090297626A1 (en) * | 2006-11-03 | 2009-12-03 | The Trustees Of Columbia University In The City Of New York | Methods for preparing metal oxides |
| CN101445961A (en) * | 2008-12-15 | 2009-06-03 | 浙江大学 | Superfine Mg-doped ZnO nano wire and synthetic method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103204538A (en) * | 2013-04-26 | 2013-07-17 | 通化师范学院 | Preparation method of porous ZnO and ZnO/Ag nanometer free-standing film |
| CN103204538B (en) * | 2013-04-26 | 2014-11-26 | 通化师范学院 | Preparation method of porous ZnO and ZnO/Ag nanometer free-standing film |
| CN108906025A (en) * | 2018-08-01 | 2018-11-30 | 安徽锦华氧化锌有限公司 | A kind of preparation method of rare earth doped modified nano zinc oxide-graphene composite photocatalyst material |
| CN110560031A (en) * | 2019-09-10 | 2019-12-13 | 安徽锦华氧化锌有限公司 | Method for improving photocatalytic activity of zinc oxide |
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Application publication date: 20111102 |