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Preparation method of vanadyl ethylene glycol and method for preparing M-phase vanadium dioxide powder from vanadyl ethylene glycol

A technology of vanadyl glycolate and vanadium dioxide, which is applied in the preparation of vanadyl glycolate and vanadium dioxide powder, and in the field of preparation of M-phase vanadium dioxide powder, which can solve the problem of difficult preparation of M-phase Vanadium, high synthesis cost and other problems, to achieve the effect of easy large-scale industrial production, low cost and high product purity

Inactive Publication Date: 2012-11-28
SOUTHWEST UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods require special equipment or long-time reaction, so the synthesis cost is very high, and it is also difficult to prepare pure M-phase vanadium dioxide

Method used

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  • Preparation method of vanadyl ethylene glycol and method for preparing M-phase vanadium dioxide powder from vanadyl ethylene glycol
  • Preparation method of vanadyl ethylene glycol and method for preparing M-phase vanadium dioxide powder from vanadyl ethylene glycol
  • Preparation method of vanadyl ethylene glycol and method for preparing M-phase vanadium dioxide powder from vanadyl ethylene glycol

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Example 1: 1 gram of ammonium metavanadate was added to 20 grams of ethylene glycol for ultrasonic dispersion treatment for 2 minutes, stirred in an oil bath at 160°C for 60 minutes, cooled to room temperature, and vacuum filtered to obtain a blue-purple precipitate of ethylene glycol vanadyl, The precipitate was washed with acetone until the filtrate was colorless, and the precipitate was put into a blast-type heating oven at 180° C., kept for 60 minutes, and taken out to obtain a blue-black M-phase vanadium dioxide powder.

Embodiment 2

[0035] Example 2: Add 1 gram of amorphous vanadium dioxide to 1 gram of ethylene glycol and 20 grams of benzyl alcohol for ultrasonic dispersion treatment for 3 minutes, stir in an oil bath at 200°C for 25 minutes; cool to room temperature, and vacuum filter to obtain ethylene glycol oxygen Vanadium blue-purple precipitates, the precipitate is washed with acetone until the filtrate is colorless, put the precipitate in a vacuum oven at 280°C, keep it warm for 5 minutes, and take it out to obtain blue-black M-phase vanadium dioxide powder.

Embodiment 3

[0036] Example 3: Add 1 gram of vanadyl acetylacetonate to 1000 grams of ethylene glycol and 50 grams of propylene glycol and glycerol for ultrasonic dispersion for 3 minutes, stir in an oil bath at 200°C for 5 minutes; cool to room temperature, and vacuum filter to obtain ethylene glycol The vanadyl alkoxide is precipitated, and the precipitate is washed with acetone until the filtrate is colorless. The precipitate is placed in a vacuum drying oven at 200° C., kept for 40 minutes and taken out to obtain a blue-black M-phase vanadium dioxide powder.

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Abstract

The invention relates to a preparation method of vanadyl ethylene glycol and a method for preparing M-phase vanadium dioxide powder from vanadyl ethylene glycol. The method comprises the following steps: adding a vanadium source into an ethylene glycol organic alcohol solvent, carrying out ultrasonic dispersion for 2-5 minutes, stirring in a 100-200 DEG C heating bath for 5-600 minutes, cooling to room temperature, and carrying out vacuum filtration to obtain the vanadyl ethylene glycol; and in a non-closed environment, carrying out heat treatment at 160-400 DEG C for 5-300 minutes to obtain the M-phase vanadium dioxide powder. The invention does not need special large-scale equipment or harsh medium atmosphere, and can obtain the M-phase vanadium dioxide powder by directly carrying out low-temperature heat treatment on the vanadyl ethylene glycol in a non-closed environment; the dopant is introduced to implement adjustable vanadium dioxide phase transition temperature within the range of 20-70 DEG C; and the compound filler is introduced to obtain the M-phase vanadium dioxide product which has different color tones and low emissivity. The M-phase vanadium dioxide prepared by the method provided by the invention has the advantages of high purity, simple preparation technique, low cost, safe and reliable production process and no pollutant emission, and can easily implement large-scale industrial production.

Description

technical field [0001] The invention relates to a method for preparing vanadyl glycolate and vanadium dioxide powder, in particular to a method for preparing vanadyl glycolate to obtain M-phase vanadium dioxide powder; it belongs to the field of functional materials. Background technique [0002] Vanadium dioxide (VO 2 ) with VO 2 (R), VO 2 (M), VO 2 (B) and VO 2 (A) Four polycrystalline structures, which are allotropes. M phase VO 2 Belongs to monoclinic crystal structure, semiconductor, has high transmittance to infrared light, R-phase VO 2 It belongs to rutile structure, conductor, and has high reflectivity to infrared light; M phase VO 2 Phase transition occurs at 68 °C, transforming into R-phase VO 2 , this phase transition is reversible. [0003] At the same time, M-phase vanadium dioxide has metal-insulator transition characteristics: when the temperature rises from low temperature to phase transition temperature, vanadium dioxide will transform from monoclin...

Claims

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Application Information

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IPC IPC(8): C07C31/28C07C29/70C01G31/02
Inventor 邹建
Owner SOUTHWEST UNIVERSITY
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