CN103818959A

CN103818959A - Low-temperature hydrothermal preparation method of molybdenum trioxide nanorod material

Info

Publication number: CN103818959A
Application number: CN201410022412.5A
Authority: CN
Inventors: 孙晓红; 秦茜茜; 武梦姣; 杨以娜; 张思敏; 关东齐来; 郑春明
Original assignee: Tianjin University
Current assignee: Tianjin University
Priority date: 2014-01-17
Filing date: 2014-01-17
Publication date: 2014-05-28

Abstract

The invention relates to a low-temperature hydrothermal preparation method of a molybdenum trioxide nanorod material, which comprises the steps of slowly pouring 65% concentrated nitric acid into distilled water to form an acid solution at a concentration of 20-55mol/L, adding ammonium molybdate with a molybdenum element concentration of 0.1-2mol/L for stirring and dissolving, then adding n-butyl alcohol at a concentration of 0.5-4mol/L for stirring, transferring the solution to a hydrothermal reaction kettle for reaction for 1-10h at a temperature of 90-110 DEG C, cooling at a room temperature, then opening the kettle, performing suction filtration and separation, and drying at 50-90 DEG C to form the molybdenum trioxide nanorod material. The morphology and the structure of the material are the same as those of a material prepared by a high-temperature preparation method, the reaction temperature is low, equipment is simple, and the energy consumption is low. A molybdenum trioxide nanorod product which is approximately 3-7 micrometers in length, 80-300nm in width and 60-100nm in thickness is obtained. The material has the same application effect as a nano molybdenum trioxide material prepared by a high-temperature hydrothermal method.

Description

A kind of low-temperature hydrothermal is prepared the method for molybdenum trioxide nano bar material

Technical field

The invention belongs to inorganic nano material Application Areas.Relate in particular a kind of method of utilizing hydrothermal reaction at low temperature to prepare molybdenum trioxide nano rod.

Background technology

Molybdenum trioxide nano material is by material supply section scholar broad research, because it has a wide range of applications field, comprises electrochromism, photochromic, gas sensing, photochemical catalysis, photovoltaic device, electrical condenser and lithium ion battery etc.And a lot of synthetic methods are also applied to the preparation of molybdenum trioxide nano material, comprise the precipitator method, chemical Vapor deposition process, high-temperature sintering process, radio-frequency magnetron sputter method, infrared radiation method, sol-gel method, hydrothermal method etc.Wherein, owing to having, product purity is high, the reaction times is short, uniform product appearance, be easy to the advantages such as realization and adopted by increasing investigator for hydrothermal method.Nanometer molybdenum trioxide material prepared by conventional hydrothermal method generally carries out between higher than 120 ℃ to 200 ℃, as shown in Figure 1, high temperature causes preparation process power consumption better, limit its extensive popularization at industrial circle, therefore sought a kind ofly can guarantee that product structure pattern homogeneous can realize again the synthetic hydro-thermal of low temperature simultaneously and prepare the method for nanometer molybdenum trioxide material and become problem demanding prompt solution.

Summary of the invention

The object of the invention is to overcome in the preparation of existing molybdenum trioxide nano bar material hydro-thermal temperature high, the high problem that consumes energy, provides a kind of low-temperature hydrothermal to prepare the method for molybdenum trioxide nano bar material.

Technical scheme of the present invention is as follows:

Low-temperature hydrothermal is prepared a method for molybdenum trioxide nano bar material, by adding the auxiliary nitric acid aqueous solution hot acid ammonium molybdate of propyl carbinol, then through washing, the dry molybdenum trioxide nano bar material that obtains.

The concrete steps that the present invention relates to preparation method comprise:

A. 65% concentrated nitric acid is slowly poured in distilled water, forms acid solution, concentration of nitric acid is 20-55mol/L;

B. to the ammonium molybdate stirring and dissolving adding in above-mentioned solution, the concentration of molybdenum element is 0.1-2mol/L;

C. the propyl carbinol adding again stirs, and the concentration of propyl carbinol is 0.5-4mol/L;

D. above-mentioned solution is transferred in hydrothermal reaction kettle, at 90 ℃ of-110 ℃ of temperature, reacted 1-10h;

E. after cooling under room temperature, drive still, suction filtration separates, the dry high-crystallinity molybdenum trioxide nano bar material that obtains at 50-90 ℃.

The invention provides a kind of low-temperature hydro-thermal synthesis of preparing molybdenum trioxide nano material.Relatively-high temperature hydrothermal preparing process, the appearance structure of material is suitable with high temperature preparation method, and temperature of reaction low (90-110 ℃), and equipment is simple, and energy consumption is low.Obtain and be about 3-7 μ m, wide 80-300nm, the molybdenum trioxide nano rod product of thickness 60-100nm.The nanometer molybdenum trioxide material standby with high temperature hydro-thermal legal system has equal effect.

Accompanying drawing explanation

Nanometer molybdenum trioxide material electromicroscopic photograph figure prepared by the hydrothermal method of Fig. 1 prior art.

Fig. 2 is the stereoscan photograph of the prepared molybdenum trioxide nano rod of embodiment 1, illustrates that prepared product has the pattern of homogeneous.

Fig. 3 is the stereoscan photograph of the prepared molybdenum trioxide nano rod of embodiment 2, illustrates that prepared product has the pattern of homogeneous.

Fig. 4 is the X-ray diffractogram of the prepared molybdenum trioxide nano rod of embodiment 2, illustrates that prepared product is molybdenum trioxide material.

Fig. 5 is the stereoscan photograph of the prepared molybdenum trioxide nano rod of embodiment 3, illustrates that prepared product has the pattern of homogeneous.

Embodiment

Embodiment 1:

65% the concentrated nitric acid of 19.4mL is slowly poured in 10mL distilled water, form acid solution, concentration of nitric acid is 20mol/L, add the ammonium molybdate stirring and dissolving of 0.18g, the concentration of molybdenum element is 0.1mol/L, add again the propyl carbinol of 0.37g to stir, the concentration of propyl carbinol is 0.5mol/L, above-mentioned solution is transferred in reactor, hydrothermal crystallizing reaction 1h at 90 ℃ of temperature, drives still after cooling under room temperature, and suction filtration separates, at 50 ℃, be dried and obtain product, the stereoscan photograph of prepared molybdenum trioxide nano bar material as shown in Figure 2.

Embodiment 2:

65% the concentrated nitric acid of 194mL is slowly poured in 50mL distilled water, form acid solution, concentration of nitric acid is 40mol/L, add the ammonium molybdate stirring and dissolving of 9g, the concentration of molybdenum element is 1mol/L, add again the propyl carbinol of 9.25g to stir, the concentration of propyl carbinol is 2.5mol/L, above-mentioned solution is transferred in reactor, hydrothermal crystallizing reaction 4h at 105 ℃ of temperature, after cooling under room temperature, drive still, suction filtration separates, the dry product that obtains at 70 ℃, the stereoscan photograph of prepared molybdenum trioxide nano bar material as shown in Figure 3, Fig. 4 is the X-ray diffractogram of the prepared molybdenum trioxide nano rod of embodiment 2, illustrate that prepared product is molybdenum trioxide material.

Embodiment 3:

65% the concentrated nitric acid of 133.4mL is slowly poured in 25mL distilled water, form acid solution, concentration of nitric acid is 55mol/L, add the ammonium molybdate stirring and dissolving of 9g, the concentration of molybdenum element is 2mol/L, add again the propyl carbinol of 7.4g to stir, the concentration of propyl carbinol is 4mol/L, above-mentioned solution is transferred in reactor, hydrothermal crystallizing reaction 10h at 110 ℃ of temperature, drives still after cooling under room temperature, and suction filtration separates, at 90 ℃, be dried and obtain product, the stereoscan photograph of prepared molybdenum trioxide nano bar material as shown in Figure 5.

To sum up the accompanying drawing of implementation column also can clearly be found out, the prepared product of the present invention has the pattern of homogeneous, and the pattern of the molybdenum trioxide material prepared with high temperature hydrothermal method (Fig. 1) is identical.

Claims

1. low-temperature hydrothermal is prepared a method for molybdenum trioxide nano bar material, it is characterized in that step is as follows:

1). 65% concentrated nitric acid is slowly poured in distilled water, forms acid solution, concentration of nitric acid is 20-55mol/L;

2). in above-mentioned solution, add ammonium molybdate stirring and dissolving, the concentration of molybdenum element is 0.1-2mol/L;

3). add propyl carbinol to stir, the concentration of propyl carbinol is 0.5-4mol/L again;

4). above-mentioned solution is transferred in hydrothermal reaction kettle, at 90 ℃ of-110 ℃ of temperature, reacted 1-10h;

5). after cooling under room temperature, drive still, suction filtration separates, the dry high-crystallinity molybdenum trioxide nano bar material that obtains at 50-90 ℃.