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Method for preparing tungsten products through acid decomposition of wolframite and scheelite mixed ore

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: 2018-09-21
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
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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

Method used

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  • Method for preparing tungsten products through acid decomposition of wolframite and scheelite mixed ore

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Embodiment 1

[0038] This embodiment provides a method for preparing tungsten products by acid decomposition of black and white tungsten mixed ore. The raw material used in the method is a 40% grade of black and white tungsten mixed ore with a particle size of 120 μm. The method is specifically:

[0039] (1) Leaching reaction: adding black and white tungsten mixed ore to a sulfuric acid solution with a concentration of 200g / L, the liquid-to-solid ratio of the system is 6:1, and the leaching reaction is carried out for 3 hours under the conditions of 150℃ and 0.5Mpa, 99.2% tungsten Converted into tungstic acid;

[0040] (2) Filtering and washing: filtering the reaction product obtained in step (1) to obtain decomposition residue and leachate; add sulfuric acid to the leachate and return to step (1) as a raw material for leaching reaction;

[0041] (3) Hydrogen peroxide extraction-decomposition extraction of tungsten: the decomposition residue obtained in step (2) is washed and mixed with a hydrogen...

Embodiment 2

[0045] This embodiment provides a method for preparing tungsten products by acid decomposing black and white tungsten mixed ore. The raw material used in the method is 52% black and white tungsten mixed ore with a particle size of 50 μm. The method is specifically:

[0046] (1) Leaching reaction: adding black and white tungsten mixed ore to a sulfuric acid solution with a concentration of 400g / L, and then adding calcium sulfate accounting for 5% of the mass of the black and white tungsten mixed ore. The liquid-to-solid ratio of the system is 10:1, The leaching reaction was carried out under the conditions of ℃ and 1.85Mpa for 1 hour, and 99.3% of the tungsten was converted into tungstic acid;

[0047] (2) Filtering and washing: filtering the reaction product obtained in step (1) to obtain decomposition residue and leachate; add sulfuric acid to the leachate and return to step (1) as a raw material for leaching reaction;

[0048] (3) Hydrogen peroxide extraction-decomposition extracti...

Embodiment 3

[0052] This embodiment provides a method for preparing tungsten products by acid decomposition of black and white tungsten mixed ore. The raw material used in the method is 55% black and white tungsten mixed ore with a particle size of 100 μm. The method is specifically:

[0053] (1) Leaching reaction: adding black and white tungsten mixed ore into a sulfuric acid solution with a concentration of 250g / L, and oxygen, the liquid-solid ratio of the system is 3:1, and the leaching reaction is carried out at 180°C and 2.5Mpa for 4 hours. 99.3% of tungsten is converted into tungstic acid;

[0054] (2) Filtering and washing: filtering the reaction product obtained in step (1) to obtain decomposition residue and leachate; add sulfuric acid to the leachate and return to step (1) as a raw material for leaching reaction;

[0055] (3) Hydrogen peroxide extraction-decomposition extraction of tungsten: the decomposition residue obtained in step (2) is washed and mixed with a 5% mass concentration ...

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Abstract

The invention relates to a method for preparing tungsten products through acid decomposition of wolframite and scheelite mixed ore. The wolframite and scheelite mixed ore serves as a raw material in the method, the method comprises the following steps that firstly, the leaching reaction is conducted; secondly, filtering and washing are conducted; thirdly, hydrogen peroxide extraction-decompositionare conducted for tungsten extraction; fourthly, multi-time hydrogen peroxide dissolving-decomposition are conducted for tungstic acid purification; fifthly, tungsten trioxide is prepared through pure tungstic acid roasting; and sixthly, a peroxotungstic acid solution is subjected to spray pyrolysis, and tungsten oxide and tungsten powder are prepared. According to the method, only the cheap sulfuric acid easy to obtain is consumed, and the wolframite and scheelite mixed ore decomposition cost is greatly reduced; the sulfuric acid is adopted for decomposition, decomposition slag is gypsum andcan be used as building materials, dangerous waste alkali boiling slag is not generated, and the enterprise producing and operating cost is greatly reduced; hydrogen peroxide is adopted as an extraction agent for tungstic acid, ammonia-nitrogen waste water is not produced, an ammonia-nitrogen waste water production technology used for many years for tungsten smelting is removed, and the environment protection cost is greatly reduced; and various tungsten terminal products and tungsten powder are directly produced, and the product added value of the tungsten smelting enterprise is improved.

Description

Technical field [0001] The invention relates to the field of chemical production, in particular to a method for preparing tungsten products by acid decomposition of black and white tungsten mixed ore. Background technique [0002] At present, the mainstream technology for processing black and white tungsten mixed ore in industry is to first use sodium hydroxide to pressure cook to obtain crude sodium tungstate solution and alkaline cooking residue. After the crude sodium tungstate solution is diluted by adding a large amount of water, it is transformed into an ammonium tungstate solution by ion exchange technology, or transformed into an ammonium tungstate solution by solvent extraction. This mainstream technology currently faces several serious problems: First, alkaline pressure cooking needs to consume alkalis such as sodium hydroxide or sodium carbonate. These reagents are currently expensive to reach, especially sodium hydroxide reaching 5000-6000 yuan / ton. The decomposition...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B3/08C22B3/04C22B3/44C22B34/36
CPCC22B3/04C22B3/08C22B3/44C22B34/36Y02P10/20
Inventor 陈星宇赵中伟
Owner CENT SOUTH UNIV
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