Preparation method of multistage-structured flower-shaped molybdenum dioxide

A molybdenum dioxide and flower-like technology is applied in the field of preparation of molybdenum dioxide, which can solve the problems of poor sensitivity of molybdenum trioxide and poor gas sensitivity of triethylamine gas, and achieve the effects of good monodispersity and good gas sensitivity characteristics.

Active Publication Date: 2013-01-16
HEILONGJIANG UNIV
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Problems solved by technology

[0003] In order to solve the technical problems of poor sensitivity of flower-shaped molybdenum trioxide prepared by the existing method and poor gas sensitivity to triethylamine gas, the present invention provides a method for preparing flower-shaped molybdenum dioxide with a multi-level structure

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  • Preparation method of multistage-structured flower-shaped molybdenum dioxide
  • Preparation method of multistage-structured flower-shaped molybdenum dioxide
  • Preparation method of multistage-structured flower-shaped molybdenum dioxide

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specific Embodiment approach 1

[0016] Specific embodiment one: the preparation method of multi-level structure flower-shaped molybdenum dioxide of this embodiment is carried out according to the following steps:

[0017] 1. According to the volume ratio of 1:0.59~2.5, add hydrogen peroxide dropwise into the methanol solution of oxymolybdenum acetylacetonate, stir for 30 minutes to obtain a light yellow transparent solution, and transfer it to a 50mL reaction kettle, and heat it at 140~200°C Solvothermal reaction for 24h to obtain a black precursor;

[0018] 2. The precursor obtained in step 1 is washed with absolute ethanol and then vacuum-dried at 60-70° C. for 8-15 hours to obtain multi-level flower-like molybdenum dioxide with a vacuum degree of 0.05 MPa-0.07 MPa.

[0019] Wherein the mass concentration of hydrogen peroxide in the step 1 is 30%; the concentration of the methanol solution of oxymolybdenum acetylacetonate is 0.016mol / L-0.035mol / L.

specific Embodiment approach 2

[0020] Embodiment 2: This embodiment differs from Embodiment 1 in that in step 1, hydrogen peroxide is added dropwise to the methanol solution of oxymolybdenum acetylacetonate at a volume ratio of 1:0.59. Others are the same as in the first embodiment.

specific Embodiment approach 3

[0021] Embodiment 3: The difference between this embodiment and Embodiment 1 is that in step 1, hydrogen peroxide is added dropwise to the methanol solution of oxymolybdenum acetylacetonate at a volume ratio of 1:0.6. Others are the same as in the first embodiment.

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Abstract

The invention provides a preparation method of multistage-structured flower-shaped molybdenum dioxide, and relates to a preparation method of molybdenum dioxide. The invention solves the technical problems that flower-shaped molybdenum trioxide prepared by the existing method is poor in sensitivity and the triethylamine gas sensitivity is poor. The method comprises the following steps: 1, dropwisely adding hydrogen peroxide into a molybdenyl acetylacetonate methanol solution, stirring, transferring into a reaction kettle, and performing thermal reaction to obtain a black precursor; and 2, washing the precursor obtained in the step 1 with anhydrous alcohol, and performing vacuum drying at 60-70 DEG C for 8-15 hours to obtain the multistage-structured flower-shaped molybdenum dioxide. According to the invention, the multistage-structured flower-shaped molybdenum dioxide of different sizes can be obtained by regulating the ratio of the reactants through the simple hydrothermal method without subsequent thermal treatment, the monodispersity of the multistage-structured flower is satisfactory, and the obtained multistage-structured flower-shaped molybdenum dioxide material has favorable triethylamine gas sensitivity characteristic.

Description

technical field [0001] The invention relates to a preparation method of molybdenum dioxide. Background technique [0002] In recent years, due to the good performance of molybdenum oxide and its use in catalysis, sensors, battery materials, magnetic recording materials, etc., people have prepared molybdenum oxide powders with different particle sizes by various methods, and prepared molybdenum oxide nanowires. Nanoribbons, hollow fibers, and mesoporous molybdenum oxide in mixed valence states. The preparation of flower-like multi-level structure oxide materials mainly focuses on zinc oxide, titanium dioxide, tungsten oxide, iron oxide, etc., while the preparation of molybdenum oxide flowers is relatively small and all of them are molybdenum trioxide flower-shaped, and the flower-shaped morphology is three Molybdenum oxide has poor sensitivity and poor gas sensitivity to triethylamine gas, and the preparation of flower-like molybdenum dioxide with multi-level structure has n...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/02B82Y30/00B82Y40/00
Inventor 程晓丽霍丽华宋肖肖徐英明张现发高山赵辉
Owner HEILONGJIANG UNIV
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