CN103408059A - Method for synthesizing chain-like nano-ZnO by adopting homogeneous precipitation method - Google Patents
Method for synthesizing chain-like nano-ZnO by adopting homogeneous precipitation method Download PDFInfo
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- CN103408059A CN103408059A CN2013101694566A CN201310169456A CN103408059A CN 103408059 A CN103408059 A CN 103408059A CN 2013101694566 A CN2013101694566 A CN 2013101694566A CN 201310169456 A CN201310169456 A CN 201310169456A CN 103408059 A CN103408059 A CN 103408059A
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Abstract
The invention discloses a method for synthesizing chain-like nano-ZnO and specifically relates to the method for synthesizing the chain-like nano-ZnO by adopting a homogeneous precipitation method. The method comprises the following steps of: firstly uniformly mixing 0.1-0.5M of zinc acetate solution with 1.0-1.5M of urea under magnetic stirring condition at room temperature then adding PEG (polyethylene glycol) 6000 and stirring for 20min, wherein the adding quantity of the PEG 6000 is 0-10wt%; and then heating and boiling for 2h, filtering, washing and drying to get a precursor; and burning the precursor at the temperature of 400-600 DEG C to get a chain-like nano-ZnO product. The prepared chain-like nano-ZnO can be used for photocatalytic degradation of methyl orange, and the degradation rate can reach 98.5%. The synthesis method is simple and easy to operate, and the photocatalytic activity is high, and therefore the obtained product can be widely applied to the field of environment pollution control.
Description
Technical field
The present invention relates to a kind of method of synthesizing chain-like nano-ZnO, particularly a kind of employing sluggish precipitation, take the method for PEG6000 as dispersion agent synthesizing chain-like nano-ZnO.
Background technology
Along with developing rapidly of chemical industry, problem of environmental pollution, especially organic pollution is on the rise, very urgent to the improvement of organic pollutant.Photocatalytic degradation is a kind of method of very effective improvement organic pollutant, compares with treatment processs such as traditional absorption, filtration, sedimentations, and Photocatalytic Degradation Process does not need complicated postprocessing working procedures, greatly reduces the running cost in actual application.Therefore, with ZnO and TiO
2Deng conductor oxidate, be the photocatalysis technology of photocatalyst material because efficiency is high, energy consumption is low, reaction conditions is gentle, can reduce the advantages such as secondary pollution, more and more cause people's attention.
ZnO is a kind of semiconductor material of direct band gap, under room temperature, energy gap is 3.37eV, and have the exciton bind energy up to 60meV, have broad application prospects at numerous areas such as photodiode, ultraviolet light detector, gas sensor, photochemical catalysis, piezoelectric device, biological fluorescent labelling and solar cells.Due to nano material, be subjected to the impact of small-size effect, surface effects, quantum size effect and macroscopic quantum tunneling effect, make nano material have the character such as unique light, electricity, sound, thermal and magnetic.If the ZnO that adopts nanoscale is as photocatalyst, light induced electron and photohole can be easy to move to the surface of catalyzer so, and this has just greatly reduced the compound of light induced electron and photohole, has effectively improved photocatalysis efficiency; Moreover, with general body phase material, comparing, the ZnO of nanoscale has high specific surface area, can on its surface, provide more reaction active site, and this also can significantly improve the activity of photocatalysis to degrade organic matter.People adopt a large amount of nano material technologies of preparing at present, prepared and much had 0 dimension (quantum dot, nanoparticle etc.), one dimension (nano wire, nanometer rod, nano belt etc.), two dimension (nanometer sheet, nanometer film), the nano ZnO material of three-dimensional structure, and studied its application in the catalyzed degradation organic dye.Yet, as these common nanotopographies such as nanometer rod, nanometer ball, nanometer sheet, in process of growth or in the light-catalyzed reaction process, be easy to assemble, cause the overall specific surface area of catalyzer to descend, make the raising of photocatalytic activity limited.Therefore how to realize the regulation and control to structure and the performance of ZnO nano material, prepare the nano-ZnO with high dispersive and high-specific surface area thereof and have important theory value and practical significance.
Summary of the invention
The object of the invention is to adopt the method for precipitation from homogeneous solution, the PEG6000 of take is dispersion agent, and zinc acetate is zinc salt, and urea is precipitation agent, under mild conditions, has synthesized the chain nano-ZnO with polymolecularity, makes it can be widely used in the environmental pollution field.
The present invention includes following three steps:
(1) preparation of presoma
At room temperature, the zinc acetate solution of 0.1～0.5M is mixed with the urea soln of 1.0～1.5M under magnetic agitation, then add the PEG6000 of different amounts to stir 20min, heated and boiled 2h, obtain presoma by filtration, washing, drying.
(2) preparation of chain nano-ZnO
Presoma is obtained to chain nano-ZnO product 400～600 ℃ of lower calcinations.
(3) photo-catalytic degradation of methyl-orange
A certain amount of chain nano-ZnO is joined in the methyl orange solution of 20mg/L, after in dark place, stirring 1 hour, mixing solutions is used to ultra violet lamp 1 hour under the state stirred, at interval of 5min, get a sample, to take out liquid and after centrifugation, survey its absorbancy under the twin-beam ultraviolet-visible spectrophotometer
The degradation effect of tropeolin-D means with degradation rate (D),
D＝[(A
0-A)/A
0]*100％
Wherein, A
0For the absorbancy of the maximum absorption band of methyl orange aqueous solution before light-catalyzed reaction, A is the absorbancy of the maximum absorption band of methyl orange aqueous solution after light-catalyzed reaction.
Advance of the present invention is:
Adopt sluggish precipitation, the PEG6000 of take is dispersion agent, under mild conditions, has synthesized the chain nano-ZnO, makes it can be widely used in administering the Organic pollutants in environment.
The accompanying drawing explanation:
In accompanying drawing 1, showed the X-ray powder diffraction figure of the obtained ZnO sample of embodiment mono-, by reference standard XRD figure spectrum, find: gained ZnO is attributed to wurtzite phase (PDF#01-1136), there is no other dephasign.
In accompanying drawing 2, be respectively the SEM figure of embodiment mono-～embodiment tri-prepared samples, as can be seen from the figure, prepared product is the nano-ZnO of chain, and along with the increase of PEG6000 add-on, the dispersiveness of chain ZnO improves, and particle diameter diminishes.
In accompanying drawing 3, showed the absorbancy curve of the photo-catalytic degradation of methyl-orange of ZnO sample prepared by embodiment tetra-.As can be seen from the figure, along with the prolongation of light application time, the absorbancy of tropeolin-D reduces, while to light application time, being 60min, the absorbancy of tropeolin-D is down to 0.097, and the degradation rate of tropeolin-D reaches 98.5%, and therefore the chain nano-ZnO of preparation has good photocatalytic activity.
The invention will be further described below in conjunction with embodiment:
Embodiment mono-:
(1) preparation of presoma
At room temperature, the zinc acetate solution of 0.3M is mixed with the urea soln of 1.2M under magnetic agitation, heated and boiled 2h, obtain presoma by filtration, washing, drying.
(2) preparation of chain nano-ZnO
Presoma is obtained to chain nano-ZnO product 500 ℃ of lower calcinations.
Embodiment bis-:
(1) preparation of presoma
At room temperature, the zinc acetate solution of 0.3M is mixed with the urea soln of 1.2M under magnetic agitation, the amount that then adds PEG6000 is 3wt.%, stirs 20min, and heated and boiled 2h, obtain presoma by filtration, washing, drying.
(2) preparation of chain nano-ZnO
Presoma is obtained to chain nano-ZnO product 500 ℃ of lower calcinations.
Embodiment tri-:
(1) preparation of presoma
At room temperature, the zinc acetate solution of 0.3M is mixed with the urea soln of 1.2M under magnetic agitation, the amount that then adds PEG6000 is 10wt.%, stirs 20min, and heated and boiled 2h, obtain presoma by filtration, washing, drying.
(2) preparation of chain nano-ZnO
Presoma is obtained to chain nano-ZnO product 500 ℃ of lower calcinations.
Embodiment tetra-:
(1) preparation of presoma
At room temperature, the zinc acetate solution of 0.5M is mixed with the urea soln of 1.5M under magnetic agitation, the amount that then adds PEG6000 is 3wt.%, stirs 20min, and heated and boiled 2h, obtain presoma by filtration, washing, drying.
(2) preparation of chain nano-ZnO
Presoma is obtained to chain nano-ZnO product 500 ℃ of lower calcinations.
(3) photo-catalytic degradation of methyl-orange
50mg gained chain nano-ZnO is joined in the methyl orange solution of 20mg/L, after in dark place, stirring 1 hour, mixing solutions is used to ultra violet lamp 1 hour under the state stirred, at interval of 5min, get a sample, to take out liquid and after centrifugation, survey its absorbancy under the twin-beam ultraviolet-visible spectrophotometer
The degradation effect of tropeolin-D means with degradation rate (D),
D＝[(A
0-A)/A
0]*100％
Wherein, A
0For the absorbancy of the maximum absorption band of methyl orange aqueous solution before light-catalyzed reaction, A is the absorbancy of the maximum absorption band of methyl orange aqueous solution after light-catalyzed reaction.
Claims (4)
1. the method for a synthesizing chain-like nano-ZnO, it is characterized in that: concrete steps are as follows:
(1) preparation of presoma
At ambient temperature, the zinc acetate solution of 0.1～0.5M is mixed with the urea soln of 1.0～1.5M under the magnetic agitation condition, then add the PEG6000 of different amounts to stir 20min, heated and boiled 2h, obtain presoma by filtration, washing, drying;
(2) preparation of chain nano-ZnO
Presoma is obtained to chain nano-ZnO product 400～600 ℃ of lower calcinations;
(3) photo-catalytic degradation of methyl-orange
A certain amount of chain nano-ZnO is joined in the methyl orange solution of 20mg/L, after in dark place, stirring 1 hour, mixing solutions is used to ultra violet lamp 1 hour under the state stirred, at interval of 5min, get a sample, to take out liquid and after centrifugation, survey its absorbancy under the twin-beam ultraviolet-visible spectrophotometer
The degradation effect of tropeolin-D means with degradation rate (D),
D＝[(A
0-A)/A
0]*100％
Wherein, A
0For the absorbancy of the maximum absorption band of methyl orange aqueous solution before light-catalyzed reaction, A is the absorbancy of the maximum absorption band of methyl orange aqueous solution after light-catalyzed reaction.
2. the method for claim 1, it is characterized in that: the add-on of PEG6000 is 0～10wt.%.
3. the method for claim 1, it is characterized in that: the zinc salt of employing is zinc acetate, its concentration range is 0.1～0.5M.
4. the method for claim 1, it is characterized in that: the amount that joins ZnO in methyl orange solution is 20～60mg.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107117643A (en) * | 2017-05-27 | 2017-09-01 | 安徽锦华氧化锌有限公司 | A kind of preparation method of high yield nano zine oxide |
| CN108145822A (en) * | 2018-01-04 | 2018-06-12 | 浙江农林大学 | A kind of preparation method of mould proof bamboo fibreboard |
| CN108145813A (en) * | 2018-01-04 | 2018-06-12 | 浙江农林大学 | A kind of preparation method of the mould proof bamboo wood of Chinese medicine |
| CN112408459A (en) * | 2020-11-19 | 2021-02-26 | 昆明理工大学 | Recycling treatment method for hot galvanizing pickling waste liquid |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001163619A (en) * | 1999-12-08 | 2001-06-19 | Tosoh Corp | Production process of powdery zinc oxide and intermediate for producing the same |
| US20110300061A1 (en) * | 2010-06-04 | 2011-12-08 | Indian Institute Of Technology Bombay | Polymer-mediated synthesis of ZnO nanostructures |
-
2013
- 2013-05-10 CN CN2013101694566A patent/CN103408059A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001163619A (en) * | 1999-12-08 | 2001-06-19 | Tosoh Corp | Production process of powdery zinc oxide and intermediate for producing the same |
| US20110300061A1 (en) * | 2010-06-04 | 2011-12-08 | Indian Institute Of Technology Bombay | Polymer-mediated synthesis of ZnO nanostructures |
Non-Patent Citations (2)
| Title |
|---|
| 刘琳等: ""纳米氧化锌的均匀沉淀法制备工艺研究"", 《粉末冶金工业》 * |
| 王赛: ""纳米ZnO的制备", 《中国优秀博硕士学文论文全文数据库工程科技I辑》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107117643A (en) * | 2017-05-27 | 2017-09-01 | 安徽锦华氧化锌有限公司 | A kind of preparation method of high yield nano zine oxide |
| CN108145822A (en) * | 2018-01-04 | 2018-06-12 | 浙江农林大学 | A kind of preparation method of mould proof bamboo fibreboard |
| CN108145813A (en) * | 2018-01-04 | 2018-06-12 | 浙江农林大学 | A kind of preparation method of the mould proof bamboo wood of Chinese medicine |
| CN112408459A (en) * | 2020-11-19 | 2021-02-26 | 昆明理工大学 | Recycling treatment method for hot galvanizing pickling waste liquid |
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Application publication date: 20131127 |