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Method for preparing pyrochlore-type tungsten oxide directly from ammonium tungstate solution

A technology of ammonium tungstate and pyrochlore is applied in the field of tungsten smelting to achieve the effect of reducing production cost, wide application range and high tungsten crystallization rate

Active Publication Date: 2017-10-10
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] All tungsten smelting processes generally include the preparation of ammonium tungstate solution. If the pyrochlore-type tungsten oxide can be directly and cost-effectively prepared from the ammonium tungstate solution system, the preparation and application of pyrochlore-type tungsten oxide powder will be promoted. However, , there is no such technology in the existing technology

Method used

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  • Method for preparing pyrochlore-type tungsten oxide directly from ammonium tungstate solution
  • Method for preparing pyrochlore-type tungsten oxide directly from ammonium tungstate solution
  • Method for preparing pyrochlore-type tungsten oxide directly from ammonium tungstate solution

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Effect test

Embodiment 1

[0058] Embodiment 1: get 50g L -1 Ammonium tungstate solution 50ml, add pyrochlore-type tungsten oxide to the ammonium tungstate solution according to the seed crystal coefficient of 2, and at the same time according to 450g L -1 The concentration of ammonium carbonate is added as solid, and steel balls are added as a stirring medium. Put it into the reaction kettle for hydrothermal reaction, set the temperature of the low-pressure kettle to 120°C, and after 24 hours of reaction, take it out and cool it, then use vacuum filtration, wash the filter cake with pure water three times and then dry it. recycle and re-use. The concentration of tungsten in the filtrate was analyzed, and the decomposition rate of the ammonium tungstate solution was calculated to be 75.7%. X-ray diffraction analysis confirmed that pure pyrochlore-type tungsten oxide was obtained.

Embodiment 2

[0059] Embodiment 2: get 200g L -1 Ammonium tungstate solution 50ml, add pyrochlore-type tungsten oxide to the ammonium tungstate solution according to the seed crystal coefficient of 3, and at the same time, according to 450g L -1 Ammonium carbonate and ammonium sulfate solids are added at a concentration of 100%, and steel balls are added as a stirring medium. Put it into the reaction kettle for hydrothermal reaction, set the temperature of the low-pressure kettle to 130°C, after 24 hours of reaction, take it out and cool it, then use vacuum filtration, wash the filter cake with pure water three times and then dry it, part of it is returned as a seed crystal, and the filtrate is recycle and re-use. The concentration of tungsten in the filtrate was analyzed, and the decomposition rate of the ammonium tungstate solution was calculated to be 76.87%. X-ray diffraction analysis confirmed that pure pyrochlore-type tungsten oxide was obtained.

Embodiment 3

[0060] Embodiment 3: get 300g L -1 Ammonium tungstate solution 50ml, add pyrochlore-type tungsten oxide to the ammonium tungstate solution according to the seed crystal coefficient of 2, and at the same time -1 Add solid ammonium carbonate, ammonia water, and steel balls as the stirring medium. Put it into the reaction kettle for hydrothermal reaction, set the temperature of the low-pressure kettle to 130°C, after 24 hours of reaction, take it out and cool it, then use vacuum filtration, wash the filter cake with pure water three times and then dry it, part of it is returned as a seed crystal, and the filtrate is recycle and re-use. The concentration of tungsten in the filtrate was analyzed, and the decomposition rate of the ammonium tungstate solution was calculated to be 77.86%. X-ray diffraction analysis confirmed that pure pyrochlore-type tungsten oxide was obtained.

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Abstract

The invention discloses a method for directly preparing pyrochlore type tungsten oxide from an ammonium tungstate solution. The method comprises the following steps: 1) adding pyrochlore type tungsten oxide seed crystal into the ammonium tungstate solution to obtain ammonium tungstate slurry; 2) putting the obtained ammonium tungstate solution into a reaction kettle, sealing, and performing hydrothermal reaction; 3) cooling the slurry obtained through hydrothermal reaction, performing solid-liquid separation, washing and drying the obtained solid, and feeding back a part of the solid as the seed crystal in the step 1), thereby obtaining the residual part, namely, a pyrochlore type tungsten oxide product. The method is high in production efficiency, low in production cost, convenient to operate and control and free of environment pollution.

Description

technical field [0001] The invention relates to a method for directly preparing pyrochlore-type tungsten oxide from an ammonium tungstate solution, and belongs to the technical field of tungsten smelting. Background technique [0002] As an important form of tungsten compound, pyrochlore-type tungsten oxide may be used in the fields of aerochromism, electrochromism, photochromism, catalysis, and battery materials. [0003] The preparation method of pyrochlore-type tungsten oxide generally adopts soft chemical synthesis method and hydrothermal synthesis method. [0004] The soft chemical synthesis method uses APT as a precursor, in an acidic ethylene glycol solution, heating to reflux, so as to obtain [(NH 4 ) 2 O]W 2 o 6 (x≈0.5), the product is dehydrated by ion exchange and heating to obtain pyrochlore-type tungsten oxide. The soft chemical synthesis method is an early method for preparing pyrochlore-type tungsten oxide, but its reaction efficiency is low and it is not...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G41/02
CPCC01G41/02C01P2002/72C01P2004/03
Inventor 李小斌崔源发周秋生罗建新齐天贵李建圃刘桂华徐双彭志宏江海浪
Owner CENT SOUTH UNIV
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