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Preparation method of spherical nanoscale niobium pentaoxide powder

A nano-scale technology of niobium pentoxide, which is applied in the field of preparation of spherical nano-scale niobium pentoxide powder, can solve problems such as difficulty in preparing uniform nano-niobium oxide, difficulty in ensuring safety, and harsh process conditions, etc., to achieve Light agglomeration, safe process and good dispersion

Active Publication Date: 2010-05-05
CHINA AUTOMOTIVE BATTERY RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The niobium alcohol hydrolysis method uses niobium alkoxide as raw material, which is not only expensive, but also has very harsh process conditions; HF is used in the process of ammonia water precipitation after dissolving commercial niobium hydroxide, which seriously corrodes the equipment and safety in production Difficult to guarantee
In addition, these methods are difficult to prepare nano-niobium oxide with uniform particles, especially the electronic ceramic grade niobium pentoxide is required to have the characteristics of small particle size, narrow particle size distribution, less particle agglomeration and good dispersion.

Method used

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  • Preparation method of spherical nanoscale niobium pentaoxide powder
  • Preparation method of spherical nanoscale niobium pentaoxide powder
  • Preparation method of spherical nanoscale niobium pentaoxide powder

Examples

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Embodiment 1

[0040] Preparation of niobium oxalate solution: heating and boiling niobium hydroxide and oxalic acid in distilled water for 1 hour, stirring constantly, stirring at a speed of 450 revolutions per minute, and then using a common funnel to filter under normal pressure. The clear liquid obtained is the niobium oxalate solution; The mass ratio of niobium hydroxide and oxalic acid is 1:3, the mass ratio of niobium hydroxide and distilled water is 1:300; the concentration of niobium oxalate expressed as niobium pentoxide is 10.45mg (Nb 2 O 5 ) / ml.

[0041] The concentration of niobium oxalate expressed as niobium pentoxide is calculated according to the following method:

[0042] Take 5ml, 10ml, and 20ml niobium oxalate solution respectively, volatilize the water between 70~80℃ to obtain white crystals, then place the white crystals in a muffle furnace at 800℃ and calcinate for 2 hours, after cooling to obtain white powder (this The white powder is tested as niobium pentoxide), weigh th...

Embodiment 2

[0048] Preparing niobium oxalate solution: heating and boiling niobium hydroxide and oxalic acid in distilled water for 2 hours, stirring constantly, stirring at a speed of 400 revolutions per minute, and then filtering with an ordinary funnel under normal pressure, and the clear liquid obtained is the niobium oxalate solution; The mass ratio of niobium hydroxide and oxalic acid is 1:4, the mass ratio of niobium hydroxide and distilled water is 1:400; the concentration of niobium oxalate expressed as niobium pentoxide is 12.18mg (Nb 2 O 5 ) / ml. The calculation method of the concentration of niobium oxalate expressed as niobium pentoxide is the same as in Example 1.

[0049] First, the carbon black is boiled for 2 hours with a 2mol / l sodium hydroxide solution, and then vacuum filtered and dried; 4 grams of carbon black, 82.1ml of niobium oxalate solution and 206.2ml of ethylene glycol (pentoxide The loading of niobium is 20%), and the pH value is adjusted to 8.5 with ammonia water...

Embodiment 3

[0054] Preparing the niobium oxalate solution: heating and boiling niobium hydroxide and oxalic acid in distilled water for 3 hours, stirring constantly at a stirring speed of 350 revolutions per minute, and then using a common funnel to filter under normal pressure, and the clear liquid obtained is the niobium oxalate solution; The mass ratio of niobium hydroxide and oxalic acid is 1:5, the mass ratio of niobium hydroxide and distilled water is 1:500; the concentration of niobium oxalate expressed as niobium pentoxide is 15.37mg (Nb 2 O 5 ) / ml. The calculation method of the concentration of niobium oxalate expressed as niobium pentoxide is the same as in Example 1.

[0055] First, the carbon black is boiled for 2 hours with a 2mol / l sodium hydroxide solution, and then vacuum filtered and dried; 4 grams of carbon black, 110.6ml of niobium oxalate solution and 221.2ml of ethylene glycol are mixed (pentoxide The loading of niobium is 30%), and the pH value is adjusted to 8 with amm...

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Abstract

The invention relates to a preparation method of spherical nanoscale niobium pentaoxide powder, comprising the following steps: niobium hydroxide and oxalic acid are heated and boiled in distilled water to prepare niobium oxalate solution; carbon black, the niobium oxalate solution and ethanediol are mixed according to proportion, the mass ratio of the niobium pentaoxide and the carbon black is 1:2-1:9, and the volume ratio of the niobium oxalate solution and the ethanediol is 1:2-1:3; pH value is adjusted to be 8-9 by ammonia water; the mixture is stirred, and the temperature is kept to be 60-70 DEG C for 8-15 minutes, and then cooling, water filling, placing still, filtering and drying are carried out; the dries product is calcined in a muffle furnace, so as to obtain the spherical nanoscale niobium pentaoxide powder. The prepared spherical nanoscale niobium pentaoxide powder has small grain diameter, particles are uniform and spherical and the dispersity is good; the purity of the product can reach more than 99.99 percent; the whole technological process is simple, the raw material source is wide, the price is low, the process is safe, and the method is beneficial to realizing industrialization.

Description

Technical field [0001] The invention relates to a method for preparing spherical nano-level niobium pentoxide powder, which can be used to prepare ceramic materials, nano materials and catalyst materials, and belongs to the field of nano materials and catalysts. Background technique [0002] As a new catalytic material, niobium oxide has attracted wide attention from scholars at home and abroad due to its unique catalytic performance. They can be used as active components, assistants or carriers of catalysts, and their catalytic effects are mainly derived from their unique catalytic properties. Acidity and redox properties, showing good catalytic performance in many reactions such as hydrocarbon conversion, selective oxidation, esterification, condensation, hydrolysis, hydration, hydrogenation / dehydrogenation. Not only that, niobium pentoxide is also widely used in ceramic capacitors, piezoelectric ceramics, new thermal materials, dielectric materials, magnetic materials and opti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G33/00
Inventor 张向军李伟伟卢世刚
Owner CHINA AUTOMOTIVE BATTERY RES INST CO LTD
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