CN103896323B - A kind of microemulsion prepares the method for nano zine oxide - Google Patents

Abstract

Microemulsion prepares a method for nano zine oxide, by constant pressure funnel, SDS/ Pentyl alcohol-hexanaphthene-NaOH microemulsion instillation 30-70 DEG C of thermostatic bath is obtained milky white liquid built with rear stirring in the flask of SDS/ Pentyl alcohol-hexanaphthene-zinc nitrate solution; Milky white liquid is carried out the centrifugal ultra-fine grain that makes to be separated with microemulsion, in centrifugal process, wash 3 times successively with dehydrated alcohol, wash 3 times, dehydrated alcohol is washed once again, in vacuum-drying at last 30 DEG C, to obtain final product.The present invention for raw material, can prepare nano-ZnO with SDS/ Pentyl alcohol-hexanaphthene-zinc nitrate solution and SDS/ Pentyl alcohol-hexanaphthene-NaOH microemulsion in water-in-oil microemulsion water core, simple to operate, and the gentle cost of experiment condition is low.

Description

A kind of method that microemulsion prepares nano zinc oxide

technical field

The invention belongs to the technical field of nanometer material preparation, and in particular relates to a method for preparing nanometer zinc oxide by microemulsion.

Background technique

Nano-ZnO is a material with many special properties such as non-migration, fluorescence, piezoelectricity, antibacterial and anti-inflammatory, and anti-ultraviolet. It is used in rubber, textiles, coatings, magnetic materials, gas sensors, image recording materials and other fields. It has a wide range of uses. The researches in the field of preparation and application of nano-ZnO at home and abroad are constantly being strengthened and deepened. The commonly used methods for the preparation of nano-ZnO are solid-phase methods—that is, first generate ZnCO ₃ precursors and then pyrolyze to generate nano-ZnO particles, and microemulsion methods. Although these methods can obtain nano-ZnO particles, there are many preparation steps and the experimental conditions are not mild enough. , the cost is not low enough. In the existing direct reaction method of zinc nitrate and sodium hydroxide solution, the particle size and uniformity of the product are difficult to control and consume a lot of energy.

Contents of the invention

The purpose of the present invention is to provide a method for preparing nano-zinc oxide by microemulsion, which solves the problems that the experimental conditions of the existing nano-zinc oxide preparation method are not mild enough and the cost is high.

The technical scheme adopted in the present invention is, a kind of method for microemulsion preparation nano-zinc oxide, specifically implement according to the following steps:

Step 1: Put the SDS/n-pentanol-cyclohexane-zinc nitrate solution in a flask, put the flask in a constant temperature water bath, and add a stirring device, and use a constant pressure funnel to mix the SDS/n-pentanol-cyclohexane -NaOH microemulsion was dropped into the flask containing SDS/n-pentanol-cyclohexane-zinc nitrate solution in a constant temperature tank at 30-70°C, and stirred for 10-15 minutes after the titration was completed to obtain a milky white liquid;

Step 2: Centrifuge the milky white liquid obtained in step 1 to separate the ultrafine particles from the microemulsion. During the centrifugation process, wash with absolute ethanol for 3 times, water for 3 times, and absolute ethanol for one more time. Dry in vacuum for 4 hours to obtain nanometer zinc oxide.

The present invention is also characterized in that,

In step 1, the volume ratio of SDS/n-pentanol-cyclohexane-zinc nitrate solution and SDS/n-pentanol-cyclohexane-NaOH microemulsion is 1-3:1-3.

The preparation method of SDS/n-pentanol-cyclohexane-zinc nitrate microemulsion is as follows: add n-pentanol to sodium dodecylsulfonate SDS and stir evenly, then add cyclohexane dropwise, stir well, and then add dropwise 0.2-0.4mol/l zinc nitrate solution, that is, the ratio of SDS and n-pentanol is 2:3.

The preparation method of SDS/n-pentanol-cyclohexane-NaOH microemulsion is as follows: add n-pentanol to sodium dodecylsulfonate SDS and stir evenly, then dropwise add cyclohexane, stir well, and then dropwise add 0.6 -0.8mol/l NaOH solution, that is, the ratio of SDS and n-pentanol is 2:3.

The beneficial effect of the present invention is, the method for preparing nano-zinc oxide by microemulsion of the present invention, with SDS/n-pentanol-cyclohexane-(0.2-0.4)mol/l zinc nitrate solution and SDS/n-pentanol-cyclohexane -(0.6-0.8) mol/lNaOH microemulsion as raw material enables it to prepare nano-ZnO in water-in-oil (W/O) microemulsion water core, with uniform particles, high purity, simple operation, mild experimental conditions and low cost Low.

Description of drawings

Fig. 1 is the TEM figure of the nano zinc oxide prepared by the inventive method;

Fig. 2 is the electron diffraction figure of the nanometer zinc oxide that the inventive method prepares;

Fig. 3 is the XRD collection of illustrative plates of the nano-zinc oxide prepared by the inventive method;

Fig. 4 is the XRD analysis figure of the nano-zinc oxide prepared by the method of the present invention.

Detailed ways

The present invention will be described in detail below in conjunction with the accompanying drawings and specific embodiments.

Microemulsion of the present invention prepares the method for nano-zinc oxide, specifically implements according to the following steps:

Step 1, add n-pentanol to SDS and stir evenly, then dropwise add cyclohexane, stir well, then add dropwise 0.2-0.4mol/l zinc nitrate solution to obtain SDS/n-pentanol-cyclohexane-zinc nitrate Solution, the volume ratio of SDS and n-pentanol is 2:3;

Step 2, add n-pentanol to SDS and stir evenly, then dropwise add cyclohexane, stir well, then add dropwise 0.6-0.8mol/l NaOH solution to obtain SDS/n-pentanol-cyclohexane-NaOH microemulsion, The volume ratio of SDS and n-pentanol is 2:3;

Step 3, SDS/n-pentanol-cyclohexane-zinc nitrate solution and SDS/n-pentanol-cyclohexane-NaOH microemulsion respectively according to the volume ratio of 1~3:1~3, SDS/n-pentanol- Put the cyclohexane-zinc nitrate solution in a flask, put the flask in a constant temperature water bath, and add a stirring device, use a constant pressure funnel to drop the SDS/n-pentanol-cyclohexane-NaOH microemulsion into the 30-70℃ In the flask equipped with SDS/n-pentanol-cyclohexane-zinc nitrate solution in the constant temperature tank, stir for 10-15 minutes after the titration is completed to obtain a milky white liquid;

Step 4, centrifuge the milky white liquid obtained in step 3 to separate the ultrafine particles from the microemulsion. During the centrifugation process, wash with absolute ethanol for 3 times, water for 3 times, and absolute ethanol for one more time. Dry in vacuum for 4 hours to obtain nanometer zinc oxide.

Fig. 1 is the TEM picture of the nano-zinc oxide prepared by the method of the present invention, as can be seen from Fig. 1, the prepared nano-zinc oxide material is spherical, and diameter is between 50-100nm, and particle is uniform. Fig. 2 is the electron diffraction figure of the nano-zinc oxide prepared by the method of the present invention, as can be seen from Fig. 2, the prepared material is a polycrystalline structure. Fig. 3 and Fig. 4 are the XRD spectrum and the XRD analysis figure of the nano-zinc oxide prepared by the inventive method, as can be seen from the figure, the prepared material XRD spectrum is consistent with the XRD standard spectrum of zinc oxide, illustrates that the prepared material It is zinc oxide.

The present invention is described below from the principle aspect:

Preparation method of the present invention mainly passes through following two reaction processes:

Zn(NO ₃ ) ₂ +2NaOH=Zn(OH) ₂ +2HNO ₃

Zn(OH) ₂ =ZnO+H ₂ O

Compared with the existing method, the present invention is different in that it uses SDS/n-pentanol-cyclohexane-(0.6-0.8) mol/lNaOH microemulsion and SDS/n-pentanol-cyclohexane-(0.2-0.4 ) mol/l zinc nitrate solution mixed to prepare nano zinc oxide method. This method is low cost and simple to operate.

Among the present invention, the SDS/n-pentanol-cyclohexane-(0.2-0.4) mol/l zinc nitrate solution and the SDS/n-pentanol-cyclohexane-(0.6- 0.8) mol/lNaOH microemulsion, the advantage of using these two reagents is that nano ZnO can be prepared in the W/O microemulsion water core. The volume ratio is 1-3:1-3, and the quality of nano-zinc oxide prepared above or below this range is not good enough, and causes waste of reagents.

Example 1

Step 1: SDS/n-pentanol-cyclohexane-0.2mol/l zinc nitrate solution and SDS/n-pentanol-cyclohexane-0.6mol/lNaOH microemulsion respectively according to the volume ratio of 1:1. Pentanol-cyclohexane-0.2mol/l zinc nitrate solution is placed in a flask, the flask is placed in a constant temperature water bath, and a stirring device is added, and the SDS/n-pentanol-cyclohexane-0.6mol is mixed with a constant pressure funnel /lNaOH microemulsion was dripped into the flask equipped with SDS/n-pentanol-cyclohexane-0.2mol/l zinc nitrate solution in a 30°C constant temperature tank, and stirred for 15 minutes after the titration was completed to obtain a milky white liquid;

Step 2: Centrifuge the milky white liquid obtained in step 1 to separate the ultrafine particles from the microemulsion. During the centrifugation process, wash with absolute ethanol for 3 times, water for 3 times, and absolute ethanol for one more time. Dry in vacuum for 4 hours to obtain nanometer zinc oxide.

Example 2

Step 1: SDS/n-pentanol-cyclohexane-0.3mol/l zinc nitrate solution and SDS/n-pentanol-cyclohexane-0.7mol/lNaOH microemulsion respectively according to the volume ratio of 2:3, the SDS/n- Pentanol-cyclohexane-0.3mol/l zinc nitrate solution is placed in a flask, the flask is placed in a constant temperature water bath, and a stirring device is added, and the SDS/n-pentanol-cyclohexane-0.7mol is mixed with a constant pressure funnel /lNaOH microemulsion was dropped into the flask equipped with SDS/n-pentanol-cyclohexane-0.3mol/l zinc nitrate solution in a 70°C constant temperature tank, and stirred for 10 minutes after the titration was completed to obtain a milky white liquid;

Step 2: Centrifuge the milky white liquid obtained in step 1 to separate the ultrafine particles from the microemulsion. During the centrifugation process, wash with absolute ethanol for 3 times, water for 3 times, and absolute ethanol for one more time. Dry in vacuum for 4 hours to obtain nanometer zinc oxide.

Example 3

Step 1: SDS/n-pentanol-cyclohexane-0.4mol/l zinc nitrate solution and SDS/n-pentanol-cyclohexane-0.8mol/lNaOH microemulsion respectively according to the volume ratio of 3:2, the SDS/n- Pentanol-cyclohexane-0.4mol/l zinc nitrate solution is placed in a flask, the flask is placed in a constant temperature water bath, and a stirring device is added, and the SDS/n-pentanol-cyclohexane-0.8mol is mixed with a constant pressure funnel /lNaOH microemulsion was dripped into a flask equipped with SDS/n-pentanol-cyclohexane-0.4mol/l zinc nitrate solution in a 60°C constant temperature tank, and stirred for 12 minutes after the titration was completed to obtain a milky white liquid;

Step 2: Centrifuge the milky white liquid obtained in step 1 to separate the ultrafine particles from the microemulsion. During the centrifugation process, wash with absolute ethanol for 3 times, water for 3 times, and absolute ethanol for one more time. Dry in vacuum for 4 hours to obtain nanometer zinc oxide.

Claims (3)

1. microemulsion prepares 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 flask, flask is put into water bath with thermostatic control, and add whipping appts, by constant pressure funnel by the SDS/ Pentyl alcohol-flask of hexanaphthene-NaOH microemulsion instillation 30 ~ 70 DEG C of thermostatic baths built with SDS/ Pentyl alcohol-hexanaphthene-zinc nitrate solution, stir 10 ~ 15 minutes after titration, obtain milky white liquid;

Step 2: milky white liquid step 1 obtained carries out the centrifugal ultra-fine grain that makes and is separated with microemulsion, washes 3 times successively in centrifugal process with dehydrated alcohol, wash 3 times, dehydrated alcohol is washed once again, finally at 30 DEG C at vacuum-drying 4h, obtain nano zine oxide;

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.

2. microemulsion according to claim 1 prepares the method for nano zine oxide, it is characterized in that, the compound method of SDS/ Pentyl alcohol-hexanaphthene-zinc nitrate microemulsion is: joined in SDS by Pentyl alcohol and stir, then hexanaphthene is dripped, 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.

3. microemulsion according to claim 1 prepares the method for nano zine oxide, it is characterized in that, the compound method of SDS/ Pentyl alcohol-hexanaphthene-NaOH microemulsion is: joined in SDS by Pentyl alcohol and stir, then hexanaphthene is dripped, stir evenly, drip 0.6-0.8mol/lNaOH solution again, to obtain final product, the ratio of SDS and Pentyl alcohol is 2:3.