CN103896323A - Method for preparing nanometer zinc oxide with micro-emulsion - Google Patents
Method for preparing nanometer zinc oxide with micro-emulsion Download PDFInfo
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- CN103896323A CN103896323A CN201410088035.5A CN201410088035A CN103896323A CN 103896323 A CN103896323 A CN 103896323A CN 201410088035 A CN201410088035 A CN 201410088035A CN 103896323 A CN103896323 A CN 103896323A
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- hexanaphthene
- pentyl alcohol
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Abstract
The invention relates to a method for preparing nanometer zinc oxide with micro-emulsion. According to the method, SDS/n-amyl alcohol-cyclohexane-NaOH micro-emulsion is dripped into a flask with SDS/n-amyl alcohol-cyclohexane-zinc nitrate in a constant-temperature tank of 30-70 DEG C by using a constant-pressure funnel and then mixed to obtain an ivory liquid; the ivory liquid is centrifuged to separate ultrafine particles from micro-emulsion, the ultrafine particles are sequentially washed with anhydrous alcohol for three times, then washed with water for three times and washed with anhydrous alcohol once during centrifuging, and finally are vacuum-dried at a temperature of 30 DEG C to obtain nanometer zinc oxide. According to the method, the DS/n-amyl alcohol-cyclohexane-zinc nitrate solution and the SDS/n-amyl alcohol-cyclohexane-NaOH micro-emulsion are used as raw materials, nanometer zinc oxide can be prepared in water-in-oil micro-emulsion water droplets by using the two materials, the operation is simple, the experimental conditions are mild, and the cost is low.
Description
Technical field
The invention belongs to nano material preparing technical field, be specifically related to a kind of method that microemulsion is prepared nano zine oxide.
Background technology
Nano-ZnO is a kind of material with many properties such as non-migrating, fluorescence, piezoelectricity, antisepsis and anti-inflammation, uvioresistants.It is applied to the fields such as rubber, weaving, coating, magneticsubstance, gas sensor, image recording material.Purposes is very extensive.Constantly strengthening and deepening in the research of nano-ZnO preparation and Application Areas both at home and abroad.What the preparation of nano-ZnO was conventional have solid phase method-first generate ZnCO
3precursor again pyrolytic decomposition generates nano-ZnO particulate, microemulsion method, although these methods can obtain nano-ZnO particulate, its preparation process is more, and experiment condition is gentle not, and cost is low not.Existing zinc nitrate and sodium hydroxide solution direct reaction method, the bad control of particle size were and uniformity coefficient and consume energy more.
Summary of the invention
The object of this invention is to provide a kind of microemulsion and prepare the method for nano zine oxide, solved the problem that preparation method's experiment condition is gentle not, cost is high of existing nano zine oxide.
The technical solution adopted in the present invention is that a kind of microemulsion is prepared the method for nano zine oxide, specifically implements according to following steps:
Step 1: SDS/ Pentyl alcohol-hexanaphthene-zinc nitrate solution is placed in to flask, flask is put into water bath with thermostatic control, and add whipping appts, SDS/ Pentyl alcohol-hexanaphthene-NaOH microemulsion is splashed in 30～70 ℃ of thermostatic baths and is equipped with in the flask of SDS/ Pentyl alcohol-hexanaphthene-zinc nitrate solution by constant pressure funnel, after titration, stir 10～15 minutes, obtain milky white liquid;
Step 2: the milky white liquid that step 1 is obtained carries out the centrifugal ultra-fine grain that makes and separates with microemulsion, washes 3 times successively in centrifugal process with dehydrated alcohol, washes 3 times, and dehydrated alcohol is washed once again, finally at 30 ℃ at vacuum-drying 4h, obtain nano zine oxide.
Feature of the present invention is also,
In step 1, the volume ratio of SDS/ Pentyl alcohol-hexanaphthene-zinc nitrate solution and SDS/ Pentyl alcohol-hexanaphthene-NaOH microemulsion is 1～3:1～3.
The compound method of SDS/ Pentyl alcohol-hexanaphthene-zinc nitrate microemulsion is: Pentyl alcohol is joined in sodium laurylsulfonate SDS and stirred, then drip hexanaphthene, stir evenly, then drip 0.2-0.4mol/l zinc nitrate solution, obtain, the ratio of SDS and Pentyl alcohol is 2:3.
The compound method of SDS/ Pentyl alcohol-hexanaphthene-NaOH microemulsion is: Pentyl alcohol is joined in sodium laurylsulfonate SDS and stirred, then drip hexanaphthene, stir evenly, then drip 0.6-0.8mol/lNaOH solution, to obtain final product, the ratio of SDS and Pentyl alcohol is 2:3.
The invention has the beneficial effects as follows, microemulsion of the present invention is prepared the method for nano zine oxide, take the mol/lNaOH microemulsion of the mol/l zinc nitrate solution of SDS/ Pentyl alcohol-hexanaphthene-(0.2-0.4) and SDS/ Pentyl alcohol-hexanaphthene-(0.6-0.8) as raw material, can in water-in-oil (W/O) microemulsion water core, prepare nano-ZnO, its uniform particles, purity is high, and simple to operate, and the gentle cost of experiment condition is low.
Accompanying drawing explanation
Fig. 1 is the TEM figure of the nano zine oxide prepared of the inventive method;
Fig. 2 is the electron-diffraction diagram of the nano zine oxide prepared of the inventive method;
Fig. 3 is the XRD figure spectrum of the nano zine oxide prepared of the inventive method;
Fig. 4 is the XRD analysis figure of the nano zine oxide prepared of the inventive method.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Microemulsion of the present invention is prepared the method for nano zine oxide, specifically implements according to following steps:
Step 1, joins Pentyl alcohol in SDS and stirs, and then drips hexanaphthene, stirs evenly, then drips 0.2-0.4mol/l zinc nitrate solution, obtains SDS/ Pentyl alcohol-hexanaphthene-zinc nitrate solution, and the volume ratio of SDS and Pentyl alcohol is 2:3;
Step 2, joins Pentyl alcohol in SDS and stirs, and then drips hexanaphthene, stirs evenly, then drips 0.6-0.8mol/lNaOH solution, obtains SDS/ Pentyl alcohol-hexanaphthene-NaOH microemulsion, and the volume ratio of SDS and Pentyl alcohol is 2:3;
Step 3, be 1～3:1～3 SDS/ Pentyl alcohol-hexanaphthene-zinc nitrate solution and SDS/ Pentyl alcohol-hexanaphthene-NaOH microemulsions respectively by volume, SDS/ Pentyl alcohol-hexanaphthene-zinc nitrate solution is placed in to flask, flask is put into water bath with thermostatic control, and add whipping appts, SDS/ Pentyl alcohol-hexanaphthene-NaOH microemulsion is splashed in 30-70 ℃ of thermostatic bath and is equipped with in the flask of SDS/ Pentyl alcohol-hexanaphthene-zinc nitrate solution by constant pressure funnel, after titration, stir 10-15 minute, obtain milky white liquid;
Step 4, the milky white liquid that step 3 is obtained carries out the centrifugal ultra-fine grain that makes and separates with microemulsion, in centrifugal process, washes 3 times successively with dehydrated alcohol, washes 3 times, dehydrated alcohol is washed once again, finally at 30 ℃ at vacuum-drying 4h, obtain nano zine oxide.
Fig. 1 is the TEM figure of the nano zine oxide prepared of the inventive method, and as can be seen from Figure 1, prepared nano zinc oxide material is spherical, and diameter is between 50-100nm, uniform particles.Fig. 2 is the electron-diffraction diagram of the nano zine oxide prepared of the inventive method, and as can be seen from Figure 2, prepared material is polycrystalline structure.Fig. 3 and Fig. 4 are XRD spectrum and the XRD analysis figure of the nano zine oxide prepared of the inventive method, and as can be seen from the figure, prepared material XRD spectra is consistent with the XRD standard spectrogram of zinc oxide, illustrate that the material of preparing is zinc oxide.
From principle aspect, the present invention will be described below:
Preparation method of the present invention mainly passes through following two reaction process:
Zn（NO
3）
2+2NaOH=Zn（OH）
2+2HNO
3
Zn（OH）
2=ZnO+H
2O
The present invention compares with existing method, and difference is, has used the mol/lNaOH microemulsion of SDS/ Pentyl alcohol-hexanaphthene-(0.6-0.8) and SDS/ Pentyl alcohol-hexanaphthene-(0.2-0.4) mol/l zinc nitrate solution is mixed with the method for nano zine oxide.This method cost is low, simple to operate.
In the present invention, adopting volume ratio is SDS/ Pentyl alcohol-hexanaphthene-(0.2-0.4) mol/l zinc nitrate solution and SDS/ Pentyl alcohol-hexanaphthene-(0.6-0.8) mol/lNaOH microemulsion of 1-3:1-3, and the benefit that adopts these two kinds of reagent is in W/O microemulsion water core, to prepare nano-ZnO.Volume ratio is 1-3:1-3, and the quality that is greater than or less than the nano zine oxide that this scope prepares is good not, and causes reagent waste.
Embodiment 1
Step 1: be 1:1 SDS/ Pentyl alcohol-hexanaphthene-0.2mol/l zinc nitrate solution and SDS/ Pentyl alcohol-hexanaphthene-0.6mol/lNaOH microemulsion respectively by volume, SDS/ Pentyl alcohol-hexanaphthene-0.2mol/l zinc nitrate solution is placed in to flask, flask is put into water bath with thermostatic control, and add whipping appts, SDS/ Pentyl alcohol-hexanaphthene-0.6mol/lNaOH microemulsion is splashed in 30 ℃ of thermostatic baths and is equipped with in the flask of SDS/ Pentyl alcohol-hexanaphthene-0.2mol/l zinc nitrate solution by constant pressure funnel, after titration, stir 15 minutes, obtain milky white liquid;
Step 2: the milky white liquid that step 1 is obtained carries out the centrifugal ultra-fine grain that makes and separates with microemulsion, washes 3 times successively in centrifugal process with dehydrated alcohol, washes 3 times, and dehydrated alcohol is washed once again, finally at 30 ℃ at vacuum-drying 4h, obtain nano zine oxide.
Embodiment 2
Step 1: be 2:3 SDS/ Pentyl alcohol-hexanaphthene-0.3mol/l zinc nitrate solution and SDS/ Pentyl alcohol-hexanaphthene-0.7mol/lNaOH microemulsion respectively by volume, SDS/ Pentyl alcohol-hexanaphthene-0.3mol/l zinc nitrate solution is placed in to flask, flask is put into water bath with thermostatic control, and add whipping appts, SDS/ Pentyl alcohol-hexanaphthene-0.7mol/lNaOH microemulsion is splashed in 70 ℃ of thermostatic baths and is equipped with in the flask of SDS/ Pentyl alcohol-hexanaphthene-0.3mol/l zinc nitrate solution by constant pressure funnel, after titration, stir 10 minutes, obtain milky white liquid;
Step 2: the milky white liquid that step 1 is obtained carries out the centrifugal ultra-fine grain that makes and separates with microemulsion, washes 3 times successively in centrifugal process with dehydrated alcohol, washes 3 times, and dehydrated alcohol is washed once again, finally at 30 ℃ at vacuum-drying 4h, obtain nano zine oxide.
Embodiment 3
Step 1: be 3:2 SDS/ Pentyl alcohol-hexanaphthene-0.4mol/l zinc nitrate solution and SDS/ Pentyl alcohol-hexanaphthene-0.8mol/lNaOH microemulsion respectively by volume, SDS/ Pentyl alcohol-hexanaphthene-0.4mol/l zinc nitrate solution is placed in to flask, flask is put into water bath with thermostatic control, and add whipping appts, SDS/ Pentyl alcohol-hexanaphthene-0.8mol/lNaOH microemulsion is splashed in 60 ℃ of thermostatic baths and is equipped with in the flask of SDS/ Pentyl alcohol-hexanaphthene-0.4mol/l zinc nitrate solution by constant pressure funnel, after titration, stir 12 minutes, obtain milky white liquid;
Step 2: the milky white liquid that step 1 is obtained carries out the centrifugal ultra-fine grain that makes and separates with microemulsion, washes 3 times successively in centrifugal process with dehydrated alcohol, washes 3 times, and dehydrated alcohol is washed once again, finally at 30 ℃ at vacuum-drying 4h, obtain nano zine oxide.
Claims (4)
1. microemulsion is prepared a method for nano zine oxide, it is characterized in that, specifically implements according to following steps:
Step 1: SDS/ Pentyl alcohol-hexanaphthene-zinc nitrate solution is placed in to flask, flask is put into water bath with thermostatic control, and add whipping appts, SDS/ Pentyl alcohol-hexanaphthene-NaOH microemulsion is splashed in 30～70 ℃ of thermostatic baths and is equipped with in the flask of SDS/ Pentyl alcohol-hexanaphthene-zinc nitrate solution by constant pressure funnel, after titration, stir 10～15 minutes, obtain milky white liquid;
Step 2: the milky white liquid that step 1 is obtained carries out the centrifugal ultra-fine grain that makes and separates with microemulsion, washes 3 times successively in centrifugal process with dehydrated alcohol, washes 3 times, and dehydrated alcohol is washed once again, finally at 30 ℃ at vacuum-drying 4h, obtain nano zine oxide.
2. microemulsion according to claim 1 is prepared the method for nano zine oxide, it is characterized in that, in step 1, the volume ratio of SDS/ Pentyl alcohol-hexanaphthene-zinc nitrate solution and SDS/ Pentyl alcohol-hexanaphthene-NaOH microemulsion is 1～3:1～3.
3. microemulsion according to claim 1 and 2 is prepared the method for nano zine oxide, it is characterized in that, the compound method of SDS/ Pentyl alcohol-hexanaphthene-zinc nitrate microemulsion is: Pentyl alcohol is joined in SDS and stirred, then drip hexanaphthene, stir evenly, drip 0.2-0.4mol/l zinc nitrate solution again, to obtain final product, the ratio of SDS and Pentyl alcohol is 2:3.
4. microemulsion according to claim 1 and 2 is prepared the method for nano zine oxide, it is characterized in that, the compound method of SDS/ Pentyl alcohol-hexanaphthene-NaOH microemulsion is: Pentyl alcohol is joined in SDS and stirred, then drip hexanaphthene, stir evenly, drip 0.6-0.8mol/lNaOH solution again, to obtain final product, the ratio of SDS and Pentyl alcohol is 2:3.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105086512A (en) * | 2015-08-18 | 2015-11-25 | 西安工程大学 | Preparation method of direct copper blue/ZnO core-shell-structure nano composite material |
| CN105111782A (en) * | 2015-08-18 | 2015-12-02 | 西安工程大学 | Method for preparing disperse red/ZnO core-shell structure composite nano-material |
| CN105111783A (en) * | 2015-08-18 | 2015-12-02 | 西安工程大学 | Direct violet/ZnO core-shell structured nano composite material preparation method |
| CN105924148A (en) * | 2016-04-13 | 2016-09-07 | 南方科技大学 | Forming method of ceramic powder |
| CN110803710A (en) * | 2019-11-15 | 2020-02-18 | 山东师范大学 | Method for preparing zinc oxide material based on surfactant-free microemulsion |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811726A (en) * | 2010-04-16 | 2010-08-25 | 广西民族大学 | Preparation method of windmill-shaped ZnO nanometer structure |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811726A (en) * | 2010-04-16 | 2010-08-25 | 广西民族大学 | Preparation method of windmill-shaped ZnO nanometer structure |
Non-Patent Citations (2)
| Title |
|---|
| 朱艳等: "SDS/正戊醇-二甲苯-水(盐水)拟三元体系相图和电导研究及纳米ZnO的制备", 《高等学校化学学报》 * |
| 朱艳等: "SDS/正戊醇-环己烷-水拟三元体系相图及温度对相图的影响", 《高等学校化学学报》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105086512A (en) * | 2015-08-18 | 2015-11-25 | 西安工程大学 | Preparation method of direct copper blue/ZnO core-shell-structure nano composite material |
| CN105111782A (en) * | 2015-08-18 | 2015-12-02 | 西安工程大学 | Method for preparing disperse red/ZnO core-shell structure composite nano-material |
| CN105111783A (en) * | 2015-08-18 | 2015-12-02 | 西安工程大学 | Direct violet/ZnO core-shell structured nano composite material preparation method |
| CN105924148A (en) * | 2016-04-13 | 2016-09-07 | 南方科技大学 | Forming method of ceramic powder |
| CN105924148B (en) * | 2016-04-13 | 2018-12-21 | 南方科技大学 | A kind of forming method of ceramic powders |
| CN110803710A (en) * | 2019-11-15 | 2020-02-18 | 山东师范大学 | Method for preparing zinc oxide material based on surfactant-free microemulsion |
| CN110803710B (en) * | 2019-11-15 | 2022-06-24 | 山东师范大学 | Method for preparing zinc oxide material based on surfactant-free microemulsion |
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