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Preparation method for monodisperse vanadium pentoxide solid microspheres

A vanadium pentoxide and monodisperse technology, which is applied in the field of preparation of vanadium pentoxide solid microspheres, can solve the problems of complex heat treatment process and many added species, and achieves the effects of simple heat treatment process, simple raw materials and reduced energy consumption.

Inactive Publication Date: 2012-08-01
HEILONGJIANG UNIV
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  • Summary
  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0003] The present invention aims to solve the problems that in the existing preparation method of vanadium pentoxide solid microspheres, more species are added in the low-temperature precipitation process and the heat treatment process is complicated, and the preparation method of monodisperse vanadium pentoxide solid microspheres provided

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  • Preparation method for monodisperse vanadium pentoxide solid microspheres
  • Preparation method for monodisperse vanadium pentoxide solid microspheres
  • Preparation method for monodisperse vanadium pentoxide solid microspheres

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specific Embodiment approach 1

[0012] Specific embodiment one: the preparation method of monodisperse vanadium pentoxide solid microsphere of this embodiment is carried out according to the following steps:

[0013] One, be 30% hydrogen peroxide by mass fraction: the volume ratio of distilled water=1: (1.5~4), preparation hydrogen peroxide aqueous solution; Preparation molar concentration is the methanol solution of the vanadium acetylacetonate of 0.015mol / L~0.033mol / L ;

[0014] Two, be 1: (4~8) ratio by volume ratio and take the aqueous hydrogen peroxide solution and the methanol solution of vanadium acetylacetonate prepared in step 1, join the methanol solution of vanadium acetylacetonate by hydrogen peroxide solution, stir After 1-2 hours, transfer to a reaction kettle, react at a temperature of 180-200°C for 4-24 hours, and obtain a vanadium oxide precursor;

[0015] 3. After washing the vanadium oxide precursor obtained in step 2 with ethanol, at a temperature of 60-70°C, vacuum-dry for 10-15 hours t...

specific Embodiment approach 2

[0018] Specific embodiment two: this embodiment is different from specific embodiment one: in step one, be 30% hydrogen peroxide by mass fraction: the volume ratio of distilled water=1: (2~3), prepare aqueous hydrogen peroxide solution. Others are the same as in the first embodiment.

specific Embodiment approach 3

[0019] Embodiment 3: The difference between this embodiment and Embodiment 1 or 2 is that in Step 1, a methanol solution of vanadium acetylacetonate with a molar concentration of 0.02 mol / L-0.03 mol / L is prepared. Others are the same as in the first or second embodiment.

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Abstract

The invention relates to a preparation method for vanadium pentoxide solid microspheres, in particular to a preparation method for monodisperse vanadium pentoxide solid microspheres, which aims to resolve the problem that in an existing preparation method for vanadium pentoxide solid microspheres, types of additives in a low-temperature precipitation process are excessive, and a heat treatment process is complex. The preparation method includes firstly, preparing aqueous hydrogen peroxide solution and methyl alcohol solution of vanadyl-acetylacetonate; secondly, weighing and mixing the aqueous hydrogen peroxide solution and the methyl alcohol solution of the vanadyl-acetylacetonate, transferring the aqueous hydrogen peroxide solution and the methyl alcohol solution of the vanadyl-acetylacetonate into a reactor after stirring, and reacting at the temperature ranging from 180 DEG C to 200 DEG C for 4-24 hours so as to obtain a vanadium oxide precursor; and thirdly, washing the precursor by ethanol, and performing heat treatment at the temperature ranging from 350 DEG C to 400 DEG C for 2-3 hours after vacuum drying so as to obtain the monodisperse vanadium pentoxide solid microspheres. Raw materials are simple and easy to obtain, a heat treatment process is simple, energy is saved, and energy consumption is reduced. The solid microspheres have an application potential in the fields of preparation of building formworks, air sensation, catalysis, chemical adsorption and the like.

Description

technical field [0001] The invention relates to a preparation method of vanadium pentoxide solid microspheres. Background technique [0002] The research on the preparation of oxide solid microspheres mainly focuses on ZnO, TiO 2 , Fe 2 o 3 , MnO 2 and Co 3 o 4 And other traditional semiconductor materials, most of the special morphology preparations of vanadium oxide series compounds are open layered structures, but there are few reports on the preparation of monodisperse vanadium pentoxide solid microspheres. It has been reported in the literature that vanadium pentoxide solid porous microspheres are prepared by low-temperature precipitation of an organic vanadium source (triisopropoxyvanadyl), then heat-treated at 400°C in a hydrogen atmosphere, and then heated at a temperature of 300°C. Obtained by oxidation. Although this method realizes the controllable preparation of vanadium pentoxide, more species are added in the low-temperature precipitation process, and th...

Claims

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Application Information

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IPC IPC(8): C01G31/02B82Y40/00
Inventor 程晓丽霍丽华武敏滋徐英明高山赵辉
Owner HEILONGJIANG UNIV
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