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A method for low-temperature synthesis of h-moo3 microrods

A technology of h-moo3 and microrods, applied in the direction of molybdenum oxide/molybdenum hydroxide, etc., can solve the problems of side reactions, difficult reactions, high reaction temperature, etc., and achieve the effect of short reaction cycle, low cost and high purity

Active Publication Date: 2015-08-19
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Synthesis of h-MoO due to hydrothermal method 3 Nanocrystals have disadvantages such as relatively high reaction temperature and long reaction time, while sonochemical synthesis of h-MoO 3 Nanocrystals have the disadvantages that the reaction is not easy to control and side reactions occur, so we are looking for a low-temperature, easy-to-control, and rapid synthesis of h-MoO 3 The method of micro- and nanocrystals is of great significance

Method used

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  • A method for low-temperature synthesis of h-moo3 microrods
  • A method for low-temperature synthesis of h-moo3 microrods

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] 1) Analytical pure ammonium molybdate ((NH 4 ) 6 Mo 7 o 24 4H 2 O) join in deionized water and stir to make the concentration of ammonium molybdate is the solution A of 0.01mol / L;

[0018] 2) After stirring and dissolving solution A evenly, use 4mol / L HNO 3 The solution adjusts the pH value of solution A to 1.0 to obtain solution B;

[0019] 3) Pour solution B into a four-necked round-bottomed flask, put the equipped four-necked round-bottomed flask into a UWave-1000 microwave-ultraviolet-ultrasonic trinity synthesis extraction reaction apparatus, and fix it;

[0020] 4) Adopt the microwave synthesis mode, adopt the direct temperature measurement method, select the temperature-time working mode, set the reaction temperature to 60°C, the holding time to 120min, and the heating time to 10min. The output power of the microwave during the holding process is 24W, and the reaction is over After cooling to room temperature naturally;

[0021] 5) Turn on the UWave-1000 m...

Embodiment 2

[0023] 1) Analytical pure ammonium molybdate ((NH 4 ) 6 Mo 7 o 24 4H 2 O) join in deionized water and stir to make the concentration of ammonium molybdate is the solution A of 0.02mol / L;

[0024] 2) After stirring and dissolving solution A evenly, use 5mol / L HNO 3 The solution adjusts the pH value of solution A to 2.0 to obtain solution B;

[0025] 3) Pour solution B into a four-necked round-bottomed flask, put the equipped four-necked round-bottomed flask into a UWave-1000 microwave-ultraviolet-ultrasonic trinity synthesis extraction reaction apparatus, and fix it;

[0026] 4) Adopt the microwave synthesis mode, adopt the direct temperature measurement method, select the temperature-time working mode, set the reaction temperature to 90°C, the holding time to 150min, and the heating time to 10min. During the holding process, the microwave output power is 24W, and the reaction is over. After cooling to room temperature naturally;

[0027] 5) Turn on the UWave-1000 microw...

Embodiment 3

[0029] 1) Analytical pure ammonium molybdate ((NH 4 ) 6 Mo 7 o 24 4H 2 O) adding to deionized water and stirring to make the concentration of ammonium molybdate is solution A of 0.04mol / L;

[0030]2) After stirring and dissolving solution A evenly, use 3mol / L HNO 3 The solution adjusts the pH of solution A to be 1.5 to obtain solution B;

[0031] 3) Pour solution B into a four-necked round-bottomed flask, put the equipped four-necked round-bottomed flask into a UWave-1000 microwave-ultraviolet-ultrasonic trinity synthesis extraction reaction apparatus, and fix it;

[0032] 4) Adopt the microwave synthesis mode, adopt the direct temperature measurement method, select the temperature-time working mode, set the reaction temperature to 100°C, the holding time to 120min, the heating time to 10min, the output power of the microwave during the holding process is 24W, and the reaction is over After cooling to room temperature naturally;

[0033] 5) Turn on the UWave-1000 microw...

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Abstract

The invention relates to a method for synthetizing h-MoO3 at low temperature. The method comprises the following steps of adding (NH4)6Mo7O24.4H2O into deionized water and stirring so as to prepare a solution A; regulating the pH value of the solution A to be 0.5-3.0 so as to obtain a solution B; pouring the solution B into a four-neck round-bottom flask and putting the flask into a synthetizing extraction reactor integrating functions of microwave, ultraviolet and ultrasonic, after reaction, naturally cooling to room temperature, opening the synthetizing extraction reactor integrating functions of microwave, ultraviolet and ultrasonic, taking out the product, after washing by deionized water and absolute ethyl alcohol sequentially, drying in an electric heating vacuum drying oven so as to obtain the h-MoO3 micrometer crystal. According to the method, the synthetizing technology range of the h-MoO3 micrometer crystal is enlarged, the prepared h-MoO3 micrometer crystal has simple technology, the raw material is easy to obtain, the yield is high, the reaction period is short, and the cost is low; the obtained h-MoO3 micrometer rods grow completely, have high purity and good crystallinity, and are distributed uniformly; the method can be used for synthetizing h-MoO3 micrometer crystal on a large scale.

Description

technical field [0001] The present invention relates to a kind of preparation h-MoO 3 Microcrystalline method, in particular related to a low-temperature synthesis of h-MoO 3 Microrod method. Background technique [0002] MoO 3 As an important functional inorganic material, it is the core material of electrochromic, photochromic, gasochromic, gas sensing, intelligent camouflage and other devices. Industry, military and other fields have great application prospects. MoO 3 There are three common crystal structures: thermodynamically stable orthorhombic α-MoO 3 , monoclinic β-MoO with a thermodynamically metastable structure 3 and hexagonal h-MoO 3 . Hexagonal h-MoO 3 Nanocrystals have attracted more and more attention from researchers because of their newer and more superior physical and chemical activities. Looking for h-MoO 3 Simple, effective and rapid synthesis of nanocrystals, exploring h-MoO 3 The theory and application of nanocrystals in optics, electricity ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G39/02
Inventor 曹丽云马凤兰黄剑锋吴建鹏费杰卢靖李翠艳
Owner SHAANXI UNIV OF SCI & TECH
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