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Method of preparing superfine APT

An alcohol-based solvent, ammonium paratungstate technology, applied in chemical instruments and methods, tungsten compounds, inorganic chemistry, etc., can solve the problems of low crystallization rate, high energy consumption, long production cycle, etc.

Inactive Publication Date: 2017-04-19
CHONGYI ZHANGYUAN TUNGSTEN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the evaporative crystallization method takes a long time, consumes a lot of energy, and has a long production cycle, and if the product is required to have high purity, the crystallization rate must be controlled to be low, and the particle size of the ammonium paratungstate crystals prepared by this method is 25-60 μm. It is difficult to meet the needs of production

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  • Method of preparing superfine APT
  • Method of preparing superfine APT
  • Method of preparing superfine APT

Examples

Experimental program
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Effect test

experiment example 1

[0051] Mix ammonium paratungstate concentrate (concentration of ammonium paratungstate concentrate is 100-400g / L in terms of tungsten trioxide) and ethanol to obtain a mixed solution containing ultrafine ammonium paratungstate and crystal mother liquor, wherein the volume ratio of ethanol to ammonium paratungstate concentrate=4: 1. The mixing temperature is 30 degrees Celsius, the mixing and stirring speed is 200r / min, the adding speed of ammonium paratungstate concentrate is 17cm / min, the mixing time is 5, 10, 15, 20, 25, 30 and 40 minutes respectively, and then the superfine The mixture of ammonium paratungstate and crystallization mother liquor is filtered to obtain superfine ammonium paratungstate and crystallization mother liquor respectively, and then the crystallization mother liquor is distilled and separated to obtain ethanol, ammonia gas and water vapor, and the ethanol is returned to mix with the ammonium paratungstate concentrate, and the filtered Ultrafine ammonium...

experiment example 2

[0055] Mix ammonium paratungstate concentrate (concentration of ammonium paratungstate concentrate is 100-400g / L in terms of tungsten trioxide) and ethanol to obtain a mixed solution containing ultrafine ammonium paratungstate and crystal mother liquor, wherein the volume ratio of ethanol to ammonium paratungstate concentrate=4: 1. The mixing time is 10 minutes, the mixing and stirring speed is 200r / min, the adding speed of ammonium paratungstate concentrate is 17cm / min, the mixing temperature is 25, 30, 35, 40, 45 and 50 degrees Celsius respectively, and then the superfine ammonium paratungstate and The mixed solution of crystallization mother liquor is filtered to obtain superfine ammonium paratungstate and crystallization mother liquor, and then the crystallization mother liquor is distilled and separated to obtain ethanol, ammonia gas and water vapor, and the ethanol is returned to mix with ammonium paratungstate concentrate, and the ultrafine ammonium paratungstate obtained b...

experiment example 3

[0059] Mix ammonium paratungstate concentrate (concentration of ammonium paratungstate concentrate is 100-400g / L in terms of tungsten trioxide) and ethanol to obtain a mixed solution containing ultrafine ammonium paratungstate and crystal mother liquor, wherein the volume ratio of ethanol to ammonium paratungstate concentrate=4: 1. The mixing time is 10 minutes, the mixing temperature is 25 degrees Celsius, the adding speed of ammonium paratungstate concentrate is 17cm / min, the mixing and stirring speed is 100, 200, 300, 400 and 500r / min respectively, and then the ultrafine ammonium paratungstate and crystallization mother liquor The mixed solution is filtered to obtain ultrafine ammonium paratungstate crystals and crystallization mother liquor, and then the crystallization mother liquor is distilled and separated to obtain ethanol, ammonia gas and water vapor, and the ethanol is returned to mix with ammonium paratungstate concentrate, and the ultrafine ammonium paratungstate ob...

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Abstract

The invention discloses a method of preparing superfine APT. The method comprises the following steps: (1) an ammonium paratungstate concentrated material is mixed with an alcohol type solvent, and mixed liquor containing superfine APT and crystallization mother liquor is obtained; and (2) the mixed liquor containing superfine APT and the crystallization mother liquor is filtered, and superfine APT and the crystallization mother liquor are obtained respectively. With the adoption of the method, a crystallization rate (greater than 95%) of superfine ammonium paratungstate can be raised significantly, particularly the BET mean particle size of obtained superfine ammonium paratungstate is not higher than 0.5 micrometer, thus the requirements on high-quality tungstenic subsequent products can be met. The method is easy and simple to handle and is low in energy consumption.

Description

technical field [0001] The invention belongs to the field of tungsten concentrate smelting, in particular, the invention relates to a method for preparing ultrafine APT. Background technique [0002] The molecular formula of ammonium paratungstate (APT) crystal is 5(NH 4 ) 2 O·12WO 3 ·nH 2 O(n=5,7,11), the solubility in water is very small, and it increases slightly as the temperature rises. It is the main intermediate product for the preparation of tungsten products such as blue tungsten oxide, ammonium tungsten bronze, and tungsten powder. The morphological structure of tungsten products largely affects the morphology and properties of tungsten products. The particle size and bulk density of tungsten products are dependent on the raw material ammonium paratungstate. Due to the development of science and technology, in order to obtain high-quality follow-up products containing tungsten, the quality requirements for APT, the intermediate product of tungsten, are becomin...

Claims

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Application Information

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IPC IPC(8): C01G41/00
CPCC01G41/00C01P2004/03C01P2004/62
Inventor 黄泽辉邓登飞邓声华
Owner CHONGYI ZHANGYUAN TUNGSTEN