Preparation method of submicron-level vanadium trioxide powder

A vanadium trioxide, submicron technology, applied in vanadium oxide and other directions, can solve the problems of high reaction equipment and operation control requirements, potential explosion safety hazards, difficult to obtain precursors, etc. High and easy industrial production effect

Active Publication Date: 2016-10-26
有研资源环境技术研究院(北京)有限公司
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  • Abstract
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Problems solved by technology

[0004] V 2 o 3 The powder is prepared by mixing graphite or carbon with vanadium pentoxide and reducing it at high temperature to obtain vanadium trioxide powder. However, the obtained powder has coarse particles and impure phases, and other low-valent vanadium oxide phases are easily formed. ; also in H 2 Reduction of V in atmosphere or other reducing atmosphere 2 o 5 Powder or decomposed vanadium precursor NH 4 VO 3 、VOCl 2 , vanadyl (IV) basic ammonium carbonate to prepare vanadium trioxide powder, but when using reducing gas such as hydrogen as the reducing agent, there is a potential safety hazard of explosion, and the requirements for reaction equipment and operation control are relatively high; in N 2 10-40μm V can be obtained by thermally decomposing hydrazine-containing vanadium salt at 700℃ 2 o 3 Powder, this method has mild reaction conditions, but the precursor is difficult to obtain

Method used

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  • Preparation method of submicron-level vanadium trioxide powder
  • Preparation method of submicron-level vanadium trioxide powder
  • Preparation method of submicron-level vanadium trioxide powder

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Use analytically pure oxalic acid and deionized water to prepare 1L of 5mol / L oxalic acid solution, heat it to 70°C, add 100g of vanadium pentoxide powder (purity 4N), stir and react to dissolve it completely; filter the solution after cooling to remove insoluble Impurities; 10wt% ammonia water was added to the filtrate to produce precipitation until pH = 8-9; the precipitate was filtered and dried in an oven at 100°C for 36h, and the obtained highly active precursor was roasted at 800°C for 1h in an argon atmosphere. Cool down to room temperature under an argon atmosphere to obtain a black vanadium trioxide powder product, the particles are spherical, uniform in size, and the particle size is less than 1 μm, at the submicron level. The purity of the product analyzed by ICP-AES was greater than 99.8%.

Embodiment 2

[0031] Use chemically pure oxalic acid and deionized water to prepare 1L of 8mol / L oxalic acid solution, heat it to 80°C, add 200g of vanadium pentoxide powder (purity 4N), stir and react to dissolve it completely; filter the solution after cooling to remove insoluble Impurities; 15wt% ammonia water was added to the filtrate to precipitate to about pH=9; the precipitate was filtered and dried in an oven at 120°C for 48h, and the obtained precursor was roasted at 900°C for 1.5h in an argon atmosphere, Cool down to room temperature to obtain a black vanadium trioxide powder product, the particles are spherical, uniform in size, and the particle size is less than 1 μm, at the submicron level. The purity of the product analyzed by ICP-AES is greater than 99.5%.

Embodiment 3

[0033] Prepare 2L of 10mol / L oxalic acid solution with high-grade pure oxalic acid and deionized water, heat to 90°C, add 400g of vanadium pentoxide powder (purity 4N), stir and react to dissolve it completely; filter the solution after cooling, remove Insoluble impurities; 20wt% ammonia water was added to the filtrate to precipitate to about pH=10; the precipitate was filtered and dried in an oven at 120°C for 72h, and the obtained precursor was roasted at 950°C for 2h in an argon atmosphere. Lower the temperature and cool to room temperature to obtain a black vanadium trioxide powder product. The purity of the product analyzed by ICP-AES is greater than 99.9%. The XRD spectrum of the powder is as follows figure 2 As shown, the diffraction peaks are sharp and there are no impurity peaks. The scanning electron microscope photograph of the powder is as image 3 As shown, the particles are spherical, uniform in size, and the particle size is less than 1 μm, at the submicron ...

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Abstract

The invention relates to a preparation method of submicron-level vanadium trioxide powder. The preparation method comprises 1, preparing an oxalic acid solution, 2, heating the oxalic acid solution, adding vanadium pentoxide powder into the oxalic acid solution, and carrying out a stirring reaction process until complete dissolution to obtain a vanadyl oxalate solution, 3, slowly adding ammonium hydroxide into the vanadyl oxalate solution and carrying out stirring for a reaction to obtain precipitates, 4, filtering the precipitates and carrying out drying to obtain a high-activity precursor and 5, roasting the high-activity precursor in an inert atmosphere to obtain submicron-level vanadium trioxide powder. The submicron-level vanadium trioxide powder has high product purity and a single phase, contains submicron-level spherical particles with the uniform sizes less than 1 microns and high particle surface activity and is conducive to further processing and use. The preparation method has simple processes, can be operated easily, has a low cost, is free of hydrogen or other reducing atmospheres, has high safety and a low three waste treating capacity and can be easily industrialized.

Description

technical field [0001] The invention belongs to the technical field of chemical materials, in particular to a preparation method of submicron vanadium trioxide powder. Background technique [0002] V 2 o 3 There are two temperature-dependent phase transitions. A first-order phase transition from low-temperature antiferromagnetic insulating phase (AFI) to high-temperature paramagnetic metallic phase (PM) occurs at about 160K, and the resistivity change shows a negative temperature coefficient (NTC) characteristic, and the single crystal resistivity mutation reaches 7 orders of magnitude. In the range of about 350K to 540K, a secondary phase transition from a low-temperature paramagnetic metallic phase (PM) to a high-temperature paramagnetic metallic phase (PM) occurs, and the resistivity change exhibits a positive temperature coefficient (PTC) characteristic. At the same time, the magnetic susceptibility, light transmittance and The reflectivity is also mutated. [0003] ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/02
CPCC01G31/02C01P2002/72C01P2004/03C01P2004/32C01P2004/62C01P2006/80
Inventor 彭程王星明张碧田段华英孙静石志霞何芬
Owner 有研资源环境技术研究院(北京)有限公司
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