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A method for extracting tungsten and molybdenum from high-molybdenum scheelite

A technology of scheelite, tungsten and molybdenum, applied in the direction of improving process efficiency, etc., can solve problems such as high price, environmental pollution, hydrogen sulfide harmful production and environment, etc.

Active Publication Date: 2020-09-01
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 2,000 yuan / ton of environmental protection tax on the hazardous waste alkali cooking slag, which greatly increases the cost of tungsten smelting; third, in order to separate the associated molybdenum in scheelite, it is necessary to add sulfide to separate molybdenum by sulfide , the process will produce toxic gas hydrogen sulfide that will endanger production and the environment; fourth, in order to produce tungsten products with qualified impurity content, ammonia water or ammonium chloride and other ammonia reagents must be used as transformation reagents in the current tungsten smelting process , so the production process will inevitably produce a large amount of ammonia nitrogen wastewater, 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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  • A method for extracting tungsten and molybdenum from high-molybdenum scheelite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0091] Raw material of high molybdenum scheelite used in this embodiment: WO 3 The grade is 40%, the Mo grade is 5%, and the particle size is 120 μm.

[0092] A method for extracting tungsten and molybdenum from high-molybdenum scheelite, comprising the steps of:

[0093] (1) Leaching reaction: Add high-molybdenum scheelite into a sulfuric acid solution with a concentration of 150g / L. The liquid-solid ratio of the system is 5:1. The leaching reaction is carried out at 150°C and 0.5Mpa for 3 hours; 99.5% Tungsten is converted into tungstic acid, 10.5% of molybdenum is converted into molybdenum acid, and the leaching rate of molybdenum is 89.1%;

[0094] (2) extracting molybdenum in the leachate: filter the reaction product obtained in step (1) to obtain decomposition residue and leachate; add extractant (30% N235+10%TBP+kerosene) to the gained leachate to control the volume of the organic phase and the water phase The ratio is 1:1, mixed, and extracted at 40°C for 10 minutes ...

Embodiment 2

[0102] Raw material of high molybdenum scheelite used in this embodiment: WO 3 The grade is 30%, the Mo grade is 25%, and the particle size is 50 μm.

[0103] A method for extracting tungsten and molybdenum from high-molybdenum scheelite, comprising the steps of:

[0104] (1) Leaching reaction: Add high-molybdenum scheelite into a sulfuric acid solution with a concentration of 300g / L, and at the same time add calcium sulfate with 5% tungsten ore mass. The liquid-solid ratio of the system is 5:1. At 200°C, 1.85 The leaching reaction was carried out under the condition of Mpa for 3 hours; 99.5% of tungsten was converted into tungstic acid, 8.5% of molybdenum was converted into molybdenum acid, and the leaching rate of molybdenum was 91.2%;

[0105] (2) Extract molybdenum in the leachate: filter the reaction product obtained in step (1) to obtain decomposition slag and leachate; add extractant (40% P204+kerosene) to the gained leachate, and control the organic phase to water pha...

Embodiment 3

[0113] Raw material of high molybdenum scheelite used in this embodiment: WO 3 The grade is 55%, the Mo grade is 2.5%, and the particle size is 150 μm.

[0114] A method for extracting tungsten and molybdenum from high-molybdenum scheelite, comprising the steps of:

[0115] (1) Leaching reaction: Add high-molybdenum scheelite into sulfuric acid solution with a concentration of 200g / L, and at the same time add tungstic acid with 10% tungsten ore mass. The liquid-solid ratio of the system is 7:1. Carry out leaching reaction for 4 hours; 99.3% of tungsten is converted into tungstic acid, 1.2% of molybdenum is converted into molybdenum acid, and the leaching rate of molybdenum is 98.2%;

[0116] (2) Molybdenum extraction in the leachate: filter the reaction product gained in step (1) to obtain decomposition slag and leachate; add extractant (35% LIX63+kerosene) to the gained leachate, control the volume ratio of the organic phase to the water phase to be 1: 1. Mix, carry out mol...

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Abstract

The invention relates to a method for extracting tungsten and molybdenum from high-molybdenum scheelite, comprising: leaching high-molybdenum scheelite with sulfuric acid solution, extracting molybdenum from the leaching solution; extracting leaching slag with hydrogen peroxide to obtain peroxide-containing Solution of tungstic acid and peroxymolybdic acid, heating or passing through SO 2 , to obtain tungstic acid and a solution containing peroxymolybdic acid; dissolve tungstic acid with hydrogen peroxide, and heat the resulting solution or pass through SO 2 , to obtain tungstic acid and a solution containing peroxymolybdic acid; repeat several times until pure tungstic acid is obtained; prepare tungsten trioxide or tungsten powder from pure tungstic acid; heat the solution containing peroxymolybdic acid or pass through SO 2 , dissolving the obtained molybdenum acid with hydrogen peroxide solution to obtain a peroxymolybdenum acid solution, and ultrasonic spray pyrolysis to prepare molybdenum trioxide powder or molybdenum powder. The method has good separation effect, simple and easy-to-control operation process, and easy industrial popularization and application.

Description

technical field [0001] The invention relates to the technical field of rare metal metallurgy, in particular to a method for extracting tungsten and molybdenum from high-molybdenum scheelite. Background technique [0002] At present, the mainstream technology for processing high-molybdenum scheelite in the industry is to first use alkaline reagents such as sodium hydroxide or sodium carbonate to obtain crude sodium tungstate solution and alkali boiling residue by pressure cooking. The crude sodium tungstate solution contains a certain amount of molybdenum, which needs to be vulcanized first, and then acidified to precipitate and separate molybdenum in the form of molybdenum trisulfide. This process will inevitably produce a large amount of toxic gas hydrogen sulfide. The acidified solution adopts a weakly basic extractant or a weakly basic ion exchange resin to absorb tungsten in it, and then back-extracts or desorbs with ammonia water to obtain an ammonium tungstate solutio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B3/08C22B3/26C22B34/34C22B34/36
CPCC22B3/08C22B34/34C22B34/36C22B3/26Y02P10/20
Inventor 陈星宇赵中伟
Owner CENT SOUTH UNIV
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