CN102218316A - Preparation method of nanometer zinc oxide photochemical catalyst with visible light photocatalytic activity - Google Patents
Preparation method of nanometer zinc oxide photochemical catalyst with visible light photocatalytic activity Download PDFInfo
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- CN102218316A CN102218316A CN2010101502492A CN201010150249A CN102218316A CN 102218316 A CN102218316 A CN 102218316A CN 2010101502492 A CN2010101502492 A CN 2010101502492A CN 201010150249 A CN201010150249 A CN 201010150249A CN 102218316 A CN102218316 A CN 102218316A
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Abstract
The invention provides a preparation method of an iron-doped nanometer zinc oxide crystal, aiming at overcoming the shortcoming of the traditional photocatalytic property and particularly solving the problem that the photocatalytic activity is hardly available in a visible light region. The preparation method has the advantages of simplicity, low cost and rapid reaction speed; and the nanometer zinc oxide prepared by the invention has very good photocatalysis capability in the visible light and the grain size of 5 nanometers to 50 nanometers and can be used for preparing high-performance materials related to solar energy.
Description
[technical field]
The present invention relates to a kind of semi-conducting material technology and environmental area, specifically is a kind of preparation method with visible light photocatalysis active nano zinc oxide photocatalyst.
[background technology]
Zinc oxide is a kind of novel broad stopband (being about 3.3eV) semi-conducting material with many superior functions, also is the novel environment friendly material that is widely studied at present, and, low cost and other advantages nontoxic because of it are widely used in photocatalysis field.It can destroy various organic pollutions by the effect of light auxiliary catalysis; The organic matter of difficult degradation finally is oxidized to inorganic matters such as carbon dioxide and water; Nearly all organic pollution in the energy oxidation removal water.Studies show that, the reaction speed of nano zinc oxide particles is 100～1000 times of common zinc oxide particle, and compare with ordinary particle, it causes scattering of light hardly, and have being with of bigger specific area and broad, therefore be considered to one of high activity catalysis material that has application prospect, and be able to extensive use, the method for preparing nano zinc oxide material has sol-gel process, hydro-thermal method, spray pyrolysis, sedimentation etc., and hydro-thermal method has characteristics such as reaction speed is fast, product property is superior.Energy gap with zinc oxide of catalysis characteristics is 3.3eV, and its photocatalysis characteristic only limits to ultraviolet band, has caused it directly to utilize sunshine to carry out the efficient lower (less than 3%) of photocatalysis Decomposition; In addition, because h+ is easy and e-is compound, thereby greatly reduce the light decomposition efficiency.Therefore, reduce h+ and e-recombination probability, prolong its disengaging time, the utilization rate that improves sunshine is the key of enhancing nano zinc oxide photocatalysis activity.Method by surface modification can reach this purpose.At present, the method for modification is mainly metal ion mixing, surperficial noble metal loading, surface light sensitization or adopts composite semiconductor.
[summary of the invention]
The objective of the invention is to overcome the deficiency of existing photocatalysis performance, particularly almost do not have photocatalytic activity that a kind of preparation method of iron doped zinc oxide nano crystalline substance is provided at visible region.Production method of the present invention is simple, and is cheap, and reaction speed is fast; The nano zine oxide of the present invention's preparation has good photo-catalysis capability under visible light.
The present invention realizes by following preparation method:
Nano zine oxide visible-light photocatalyst production technology involved in the present invention comprises the steps:
Step 1 accurately takes by weighing a certain amount of FeCl with balance
36H
2O places beaker, and adds a certain amount of hydrochloric acid solution in beaker;
Step 2 adds a certain amount of distilled water diluting to 10mmol/L in the solution of step 1 gained;
Step 3 takes by weighing a certain amount of two water acetic acid zinc and is dissolved in the absolute ethyl alcohol, places;
Step 4 takes by weighing an a certain amount of hydronium(ion) oxidation lithium and is dissolved in the absolute ethyl alcohol, places;
Step 5, cooling, stirring slowly are added drop-wise to the solution of a certain amount of step 2 gained in the solution of step 3 gained down;
Step 6 adds the solution of step 4 gained in the solution of step 5 gained, and heating is concentrated into certain volume;
Step 7 adds the PEG400 solution of certain volume 0.05mol/l, and mixes in step 6 solution;
Step 8 with step 7 gained solution hydro-thermal certain hour at a certain temperature, is cooled to room temperature and centrifugation and obtains precipitation;
Step 9, the washing of precipitate drying that step 8 is obtained had both got product.
In the step 1, the hydrochloric acid solution of described adding is about 1ml.
In the step 6, described concentrated volume is controlled at 60ml-100ml.
In the step 7, the volume of described solution is 3ml-5ml.
In the step 8, described hydrothermal temperature is at 100 ℃-140 ℃.
In the step 8, the described hydro-thermal time is 24～48h.
The present invention has following beneficial effect: its nano zine oxide particle diameter is 5 nanometers-50 nanometers, and technology of the present invention has been saved the energy, has simplified step, has improved photocatalysis efficiency and safer.
[specific embodiment]
The invention will be further described below in conjunction with embodiment.Production technology of the present invention is to implement easily to this professional people.Present embodiment has provided detailed embodiment and process being to implement under the prerequisite with the technical solution of the present invention, but protection scope of the present invention is not limited to following embodiment.The experimental technique of unreceipted actual conditions in the following example, usually according to normal condition, or the condition of advising according to manufacturer.
Embodiment
Take by weighing 0.27g FeCI
36H
2O puts in the beaker, adds 1mL HCI solution, the storing solution that 250mL 10mmol/L is joined in the adding distil water dilution.
Take by weighing 1.1g Zn (Ac)
22H
2O and 0.3g LiOHH
2O is dissolved in respectively in the absolute ethyl alcohol, and cooling, stirring slowly are added drop-wise to Zn (Ac) with the iron chloride storing solution of 5mL earlier down
2Solution slowly is added drop-wise to LiOH solution Zn (Ac) again
2In the solution, heating is concentrated into 80mL, adds the PEG400 solution of 4.0mL 0.05mol/L then, and is evenly mixed.
Steady temperature is 120 ℃ in the drying box, keeps 24h, naturally cool to room temperature after, centrifugation obtains precipitation.
With the ultrasonic eccentric cleaning several of deionized water, 60 ℃ of dryings, finally obtain the Zinc oxide powder sample of doped F e ¨.
The nanometer Zinc oxide powder crystalline size that present embodiment obtains is between 10nm-20nm.
Utilize said method can prepare iron nanometer doped zinc oxide powder, and reach its distinctive visible light photocatalysis effect.
Claims (7)
1. the present invention is a kind of preparation method with visible light photocatalysis active nano zinc oxide photocatalyst.Zinc oxide product of the present invention has good photocatalytic, and its nano zine oxide particle diameter is 5 nanometers-50 nanometers.
2. a kind of preparation method with visible light photocatalysis active nano zinc oxide photocatalyst according to claim 1 comprises the steps:
Step 1 accurately takes by weighing a certain amount of FeCl with balance
36H
2O places beaker, and adds a certain amount of hydrochloric acid solution in beaker;
Step 2 adds a certain amount of distilled water diluting to 10mmol/L in the solution of step 1 gained;
Step 3 takes by weighing a certain amount of two water acetic acid zinc and is dissolved in the absolute ethyl alcohol, places;
Step 4 takes by weighing an a certain amount of hydronium(ion) oxidation lithium and is dissolved in the absolute ethyl alcohol, places;
Step 5, cooling, stirring slowly are added drop-wise to the solution of a certain amount of step 2 gained in the solution of step 3 gained down;
Step 6 adds the solution of step 4 gained in the solution of step 5 gained, and heating is concentrated into certain volume;
Step 7 adds the PEG400 solution of certain volume 0.05mol/l, and mixes in step 6 solution;
Step 8 with step 7 gained solution hydro-thermal certain hour at a certain temperature, is cooled to room temperature and centrifugation and obtains precipitation;
Step 9, the washing of precipitate drying that step 8 is obtained had both got product.
3. a kind of preparation method with visible light photocatalysis active nano zinc oxide photocatalyst according to claim 2 is characterized in that in the step 1 that the hydrochloric acid solution of described adding is about 1ml.
4. a kind of preparation method with visible light photocatalysis active nano zinc oxide photocatalyst according to claim 2 is characterized in that in the step 6 that described concentrated volume is controlled at 60ml-100ml.
5. a kind of preparation method with visible light photocatalysis active nano zinc oxide photocatalyst according to claim 2 is characterized in that in the step 7 that the volume of described solution is 3ml-5ml.
6. a kind of preparation method with visible light photocatalysis active nano zinc oxide photocatalyst according to claim 2 is characterized in that in the step 8, and described hydrothermal temperature is at 100 ℃-140 ℃.
7. a kind of preparation method with visible light photocatalysis active nano zinc oxide photocatalyst according to claim 2 is characterized in that in the step 8 that the described hydro-thermal time is 24～48h.
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| CN2010101502492A CN102218316A (en) | 2010-04-16 | 2010-04-16 | Preparation method of nanometer zinc oxide photochemical catalyst with visible light photocatalytic activity |
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| CN2010101502492A CN102218316A (en) | 2010-04-16 | 2010-04-16 | Preparation method of nanometer zinc oxide photochemical catalyst with visible light photocatalytic activity |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102513074A (en) * | 2011-10-27 | 2012-06-27 | 云南大学 | Nanoparticle photocatalysis board, its preparation method and application thereof |
| CN105062262A (en) * | 2015-08-05 | 2015-11-18 | 天长市开林化工有限公司 | Building interior wall special-purpose antibacterial mildew-resistant emulsion paint |
| CN105062338A (en) * | 2015-08-05 | 2015-11-18 | 天长市开林化工有限公司 | Weatherproof aqueous alkyd resin/epoxy resin coating |
| CN106540703A (en) * | 2016-12-06 | 2017-03-29 | 沈阳化工大学 | A kind of preparation method of Fe doping zinc oxide nanometers photocatalyst |
| CN112691675A (en) * | 2019-10-22 | 2021-04-23 | 江苏康润净化科技有限公司 | GO and Fe3+Doped ZnO visible light catalyst fabric |
-
2010
- 2010-04-16 CN CN2010101502492A patent/CN102218316A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102513074A (en) * | 2011-10-27 | 2012-06-27 | 云南大学 | Nanoparticle photocatalysis board, its preparation method and application thereof |
| CN105062262A (en) * | 2015-08-05 | 2015-11-18 | 天长市开林化工有限公司 | Building interior wall special-purpose antibacterial mildew-resistant emulsion paint |
| CN105062338A (en) * | 2015-08-05 | 2015-11-18 | 天长市开林化工有限公司 | Weatherproof aqueous alkyd resin/epoxy resin coating |
| CN106540703A (en) * | 2016-12-06 | 2017-03-29 | 沈阳化工大学 | A kind of preparation method of Fe doping zinc oxide nanometers photocatalyst |
| CN112691675A (en) * | 2019-10-22 | 2021-04-23 | 江苏康润净化科技有限公司 | GO and Fe3+Doped ZnO visible light catalyst fabric |
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Application publication date: 20111019 |