A method for preparing tungsten oxide and tungsten powder from scheelite

A technology of scheelite and tungsten oxide, which is applied in the field of chemical production, can solve the problems of high price, increased tungsten smelting cost, and environmental pollution, so as to reduce production and operation costs, increase product added value, and reduce environmental protection costs. Effect

Active Publication Date: 2020-07-14
CENT SOUTH UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This mainstream technology is currently facing several serious problems: First, alkaline pressure cooking needs to consume alkali such as sodium hydroxide or sodium carbonate. The cost of scheelite decomposition is very high; secondly, alkali pressure cooking will produce alkali cooking slag, which has been listed in the national hazardous waste catalogue, and tungsten smelting enterprises are not allowed to dispose of it at will, and must be handed over to qualified enterprises for paid treatment, and The state also charges an environmental protection tax of 2,000 yuan / ton for the hazardous waste alkali cooking slag, which greatly increases the cost of tungsten smelting; third, in order to produce tungsten products with qualified impurity content, the current tungsten smelting process must also Ammonium reagents such as ammonia water or ammonium chloride are used as transformation reagents, so a large amount of ammonia nitrogen wastewater will inevitably be generated during the production process, resulting in environmental pollution
Moreover, the main purpose of its invention is to separate tungsten and molybdenum according to the stability difference between peroxytungstic acid and peroxymolybdic acid in acidic solution, and does not involve the purification method of tungsten

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  • A method for preparing tungsten oxide and tungsten powder from scheelite

Examples

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Embodiment 1

[0039] This example provides a method for preparing tungsten oxide and tungsten powder from scheelite. The raw material used in this method is scheelite with a grade of 40% and a particle size of 100 μm. The method is specifically as follows:

[0040] (1) Leaching reaction: Add scheelite to sulfuric acid solution with a concentration of 250g / L, and then add calcium sulfate accounting for 5% of the mass of scheelite. The liquid-solid ratio of the system is 6:1. The leaching reaction was carried out under the condition of 0.5Mpa for 3 hours, and 99.4% of tungsten was converted into tungstic acid;

[0041] (2) Filtration and washing: filter the reaction product obtained in step (1) to obtain decomposition residue and leaching solution; add sulfuric acid to the leaching solution and return to step (1) as a raw material for leaching reaction;

[0042] (3) hydrogen peroxide extraction-decomposition and extraction of tungsten: wash the decomposed slag obtained in step (2) and mix it ...

Embodiment 2

[0046] This example provides a method for preparing tungsten oxide and tungsten powder from scheelite. The raw material used in this method is scheelite with a grade of 10% and a particle size of 200 μm. The method is specifically as follows:

[0047] (1) Leaching reaction: Add scheelite to a sulfuric acid solution with a concentration of 50g / L. The liquid-solid ratio of the system is 10:1. The leaching reaction is carried out at 90°C and 0Mpa for 4 hours, and 99.2% of tungsten is converted into Tungstic acid;

[0048] (2) Filtration and washing: filter the reaction product obtained in step (1) to obtain decomposition residue and leaching solution; add sulfuric acid to the leaching solution and return to step (1) as a raw material for leaching reaction;

[0049] (3) hydrogen peroxide extraction-decomposition and extraction of tungsten: wash the decomposed slag obtained in step (2) and mix it with a hydrogen peroxide solution with a mass concentration of 30%, the molar ratio of...

Embodiment 3

[0054] This example provides a method for preparing tungsten oxide and tungsten powder from scheelite. The raw material used in this method is scheelite with a grade of 65% and a particle size of 50 μm. The method is specifically as follows:

[0055] (1) Leaching reaction: Add scheelite to sulfuric acid solution with a concentration of 300g / L, and then add solid tungstic acid accounting for 10% of the mass of scheelite. The liquid-solid ratio of the system is 4:1. , Under the condition of 0.65Mpa, the leaching reaction was carried out for 4 hours, and 99.1% of the tungsten was converted into tungstic acid;

[0056] (2) Filtration and washing: filter the reaction product obtained in step (1) to obtain decomposition residue and leaching solution; add sulfuric acid to the leaching solution and return to step (1) as a raw material for leaching reaction;

[0057] (3) hydrogen peroxide extraction-decomposition and extraction of tungsten: wash the decomposed slag obtained in step (2)...

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Abstract

The present invention relates to a method for preparing tungsten oxide and tungsten powder from scheelite. The method uses the scheelite as a raw material and comprises the following steps: (1) conducting leaching reaction; (2) conducting filtering and washing; (3) conducting hydrogen peroxide extraction-decomposition to extract tungsten; (4) conducting hydrogen peroxide multiple dissolution-decomposition to purify tungstic acid; (5) pure tungstic acid calcination to prepare tungsten trioxide; and (6) conducting peroxotungstic acid solution spraying pyrolysis to prepare tungsten oxide and tungsten powder. The method only consumes cheap and easily available sulfuric acid, greatly reduces the decomposition cost of the scheelite and uses sulfuric acid to decompose; decomposed residues are gypsum; the gypsum can be used as building materials; the method does not produce dangerous waste alkali cooking residues, greatly reduces production and operation costs of enterprises, uses hydrogen peroxide as an extractant of tungstic acid, does not produce ammonia nitrogen wastewater, eliminates the technology of producing the ammonia nitrogen wastewater for many years in tungsten smelting, greatly reduces environmental protection costs, directly produces various tungsten end products and tungsten powder, and improves added value of products of the tungsten smelting enterprises.

Description

technical field [0001] The invention relates to the field of chemical production, in particular to a method for preparing tungsten oxide and tungsten powder from scheelite. Background technique [0002] At present, the mainstream technology for processing scheelite in industry is to first use alkaline reagents such as sodium hydroxide or sodium carbonate to obtain crude sodium tungstate solution and alkali cooking residue by pressure cooking. Crude sodium tungstate solution is converted into ammonium tungstate solution by ion exchange technology after being diluted with a large amount of water, and is also transformed into ammonium tungstate solution by solvent extraction. This mainstream technology is currently facing several serious problems: First, alkaline pressure cooking needs to consume alkali such as sodium hydroxide or sodium carbonate. The cost of scheelite decomposition is very high; secondly, alkali pressure cooking will produce alkali cooking slag, which has be...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G41/02C22B3/08C22B3/44C22B34/36
CPCC01G41/02C22B3/08C22B3/44C22B34/36Y02P10/20
Inventor 陈星宇刘旭恒李江涛何利华赵中伟
Owner CENT SOUTH UNIV
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