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Method for carrying out acid decomposition on wolframite-scheelite mixed ore to prepare tungsten oxide and tungsten powder

A technology of black and white tungsten and mixed ore, applied in the direction of improving process efficiency, etc., 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 decomposition cost effect

Active Publication Date: 2018-08-24
CENT SOUTH UNIV
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  • Summary
  • 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 decomposition cost of black and white tungsten mixed ore is very high; second, alkali pressure cooking will produce alkali cooking slag, which has been listed in the national hazardous waste catalog, and tungsten smelting enterprises are not allowed to dispose of it at will, and must be handed over to qualified enterprises for paid treatment. Moreover, the country 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 still requires Ammonium reagents such as ammonia water or ammonium chloride must be 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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  • Method for carrying out acid decomposition on wolframite-scheelite mixed ore to prepare tungsten oxide and tungsten powder

Examples

Experimental program
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Effect test

Embodiment 1

[0038] This example provides a method for acid-decomposing black and white tungsten mixed ore to prepare tungsten oxide and tungsten powder. The raw material used in this method is black and white tungsten mixed ore with a grade of 40% and a particle size of 150 μm. The method is specifically as follows:

[0039] (1) Leaching reaction: Add black and white tungsten mixed ore to hydrochloric acid solution with a concentration of 200g / L. The liquid-solid ratio of the system is 6:1. The leaching reaction is carried out at 150°C and 5Mpa for 3 hours, and 99.4% of the tungsten is converted. into tungstic acid;

[0040] (2) Filtration and washing: the reaction product obtained in step (1) is filtered to obtain decomposition residue and leachate;

[0041] Add sulfuric acid to the leaching solution, the molar ratio of the amount of sulfuric acid to the content of calcium ions in the leaching solution is 1:1, perform conversion reaction at 45°C for 1 hour to generate gypsum; the acid so...

Embodiment 2

[0047] This example provides a method for acid-decomposing black and white tungsten ore to prepare tungsten oxide and tungsten powder. The raw material used in this method is black and white tungsten ore with a grade of 55% and a particle size of 80 μm. The method is specifically as follows:

[0048] (1) Leaching reaction: Add black and white tungsten mixed ore to hydrochloric acid solution with a concentration of 150g / L, the liquid-solid ratio of the system is 6:1, and at the same time, oxygen is introduced at 200°C and 10Mpa for leaching reaction for 2 hours, 99.2 % of tungsten converted into tungstic acid;

[0049] (2) Filtration and washing: the reaction product obtained in step (1) is filtered to obtain decomposition residue and leachate;

[0050] Add sulfuric acid to the leaching solution, the molar ratio of the amount of sulfuric acid to the content of calcium ions in the leaching solution is 1:1, and carry out conversion reaction at 60°C for 0.5h to generate gypsum; th...

Embodiment 3

[0055] This example provides a method for acid-decomposing black and white tungsten mixed ore to prepare tungsten oxide and tungsten powder. The raw material used in this method is black and white tungsten mixed ore with a grade of 65% and a particle size of 50 μm. The method is specifically as follows:

[0056] (1) Leaching reaction: Add black and white tungsten mixed ore to the nitric acid solution with a concentration of 100g / L, then add solid tungstic acid accounting for 10% of the black and white tungsten mixed ore, the liquid-solid ratio of the system is 3:1, in The leaching reaction was carried out at 80°C and 0Mpa for 6 hours, and 99.1% of tungsten was converted into tungstic acid;

[0057] (2) Filtration and washing: the reaction product obtained in step (1) is filtered to obtain decomposition residue and leachate;

[0058] Add sulfuric acid to the leaching solution, the molar ratio of the amount of sulfuric acid to the calcium ion content in the leaching solution is ...

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Abstract

The invention relates to a method for carrying out acid decomposition on wolframite-scheelite mixed ore to prepare tungsten oxide and tungsten powder. According to the method, the wolframite-scheelitemixed ore is taken as a raw material, and the method comprises the following steps: (1) carrying out a leaching reaction; (2) carrying out filtering and washing; (3) carrying out extraction-decomposition through hydrogen peroxide to extract tungsten; (4) carrying out dissolution-decomposition through hydrogen peroxide for many times to purify tungsten acid; (5) calcining the pure tungsten acid toprepare tungsten trioxide; and (6) carrying out spray pyrolysis on peroxotungstic acid solution to prepare tungsten oxide and tungsten powder. According to the method disclosed by the invention, onlycheap and easily-available sulfuric acid is consumed actually, so that the decomposition cost for the wolframite-scheelite mixed ore is greatly lowered; the acid is used for decomposition, the decomposition slag is gypsum and can be used as a building material, and hazardous waste soda-boiling slag is not generated, so that the production and operation costs of an enterprise are greatly lowered;the hydrogen peroxide is used as an extraction agent for the tungsten acid, ammonia-nitrogen wastewater is not generated, and the process generating ammonia-nitrogen wastewater, which is used for manyyears, in tungsten smelting, is abolished, so that the environmental protection cost is greatly lowered; and the various terminal products of tungsten, and the tungsten powder are directly produced,so that the added value of products in the tungsten smelting enterprise is increased.

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 by acid-decomposing black and white tungsten mixed ore. Background technique [0002] At present, the mainstream technology for processing black and white tungsten mixed ore in the industry is to first use sodium hydroxide to pressure cook to obtain crude sodium tungstate solution and alkali cooking residue. 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 decomposition cost of black and white tungsten mixed ore is very high; second, alkali pressure cooking wil...

Claims

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Application Information

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IPC IPC(8): C22B3/06C22B3/10C22B3/44C22B34/36B22F9/22
CPCB22F9/22C22B3/065C22B3/10C22B3/44C22B34/36Y02P10/20
Inventor 陈星宇赵中伟
Owner CENT SOUTH UNIV
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