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A method for preparing tungsten products from crude sodium tungstate solution

A technology of sodium tungstate and solution, which is applied in the preparation of tungsten compounds, chemical instruments and methods, tungsten oxide/tungsten hydroxide, etc. It can solve the problems of complexity and high content of impurities, difficult products, and no tungstic acid purity detection. , to achieve the effect of increasing product added value and reducing environmental protection costs

Active Publication Date: 2020-07-31
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, for the crude sodium tungstate solution obtained by industrially decomposing tungsten ore, the complexity and content of impurities are much higher than those recorded in patent 201510698722.3. This technical method is difficult to process to obtain qualified products.
[0005] In addition, Jiang Anren and others prepared tungstic acid by adding a certain amount of hydrogen peroxide to sodium tungstate solution, adjusting the acidity of the solution, and then decomposing peroxytungstate, but did not test the purity of tungstic acid

Method used

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  • A method for preparing tungsten products from crude sodium tungstate solution

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Effect test

Embodiment 1

[0050] A method for preparing tungsten products from crude sodium tungstate, comprising the steps of:

[0051] (1) Add 100g / L sulfuric acid to WO 3 In the sodium tungstate solution (scheelite alkali pressure cooking) with a concentration of 152g / L, the pH value of the solution is controlled at -0.5, the reaction temperature is 90°C, and the reaction time is 0.5 hours. After the reaction is completed, tungstic acid precipitate and Filtrate; the precipitation rate of tungsten was detected to be 98.5%;

[0052] (2) Contact the filtrate with D301 resin for 1 hour to absorb the tungsten in it, and control the reaction temperature to 50°C; add sulfuric acid to the solution after the adsorption and return to step (1) to precipitate tungsten from the sodium tungstate solution;

[0053] (3) after the tungstic acid precipitation that step (1) obtains is washed, then be the hydrogen peroxide solution dissolving of 30% with mass concentration, the mol ratio of the add-on of hydrogen pero...

Embodiment 2

[0058] A method for preparing tungsten products from crude sodium tungstate, comprising the steps of:

[0059] (1) Add 150g / L hydrochloric acid to WO 3 In the sodium tungstate solution with a concentration of 258g / L ( wolframite alkali pressure cooking), the pH value of the solution is controlled at 0.1, the reaction temperature is 85°C, and the reaction time is 2 hours. After the reaction is completed, it is filtered to obtain tungstic acid precipitate and filtrate ; The precipitation rate of tungsten was detected to be 99.2%

[0060] (2) Contact the filtrate with "30% N235 + 10% TBP + kerosene" at a water-to-oil ratio of 1:1 for 10 minutes to extract the tungsten, and control the extraction temperature to 50°C; add hydrochloric acid to the raffinate and return to step (1) Used to precipitate tungsten from sodium tungstate solution;

[0061] Alternatively, contact the filtrate with D301 resin for 1 hour to absorb the tungsten in it, and control the reaction temperature to 5...

Embodiment 3

[0067] A method for preparing tungsten products from crude sodium tungstate, comprising the steps of:

[0068] (1) Add 150g / L nitric acid to WO 3 In the sodium tungstate solution with a concentration of 300g / L (scheelite soda pressure cooking), add solid tungstic acid with 10% of the mass of tungsten in the sodium tungstate solution as a seed crystal at the same time, control the pH value of the solution to 1.1, and the reaction temperature is 100°C, the reaction time is 2 hours, after the reaction is completed, the tungstic acid precipitate and filtrate are obtained by filtration; the precipitation rate of tungsten is 99.7% after testing

[0069] (2) Contact the filtrate with "40% TBP + 10% 2-octanol + kerosene" at a water-to-oil ratio of 2:1 to extract the tungsten in it for 15 minutes, and control the extraction temperature to 50°C; add nitric acid to the raffinate and return to the step (1) Used to precipitate tungsten from sodium tungstate solution;

[0070] Alternative...

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Abstract

The invention relates to a method of producing a tungsten product from a crude sodium tungstate solution. The method includes steps of: adding a proper amount of acid to the crude sodium tungstate solution to generate precipitate, and filtering the solution to obtain crude tungstic acid and a filtrate; recycling tungsten from the filtrate through a weak-alkaline anion exchange resin or with an extraction agent; extracting the crude tungstic acid with H2O2, and heating a peroxytungstic acid solution or feeding SO2 to prepare tungstic acid; repeating the step for several times until preparing pure tungstic acid; preparing WO3 or tungsten powder from the pure tungstic acid; dissolving the tungstic acid in H2O2 solution to obtain the peroxytungstic acid solution; and performing ultrasonic spray pyrolysis to obtain tungsten oxide powder or tungsten powder. The method has great separation effect, is simple and controllable in operation process, and is easy to promote and apply in industry.

Description

technical field [0001] The invention relates to the technical field of rare metal metallurgy, in particular to a method for preparing tungsten products from crude sodium tungstate solution. Background technique [0002] At present, the mainstream process of tungsten smelting in industry is to first prepare crude sodium tungstate solution by boiling tungsten ore with alkali pressure. The obtained crude sodium tungstate solution has a high concentration. In order to adapt to the ion exchange process, it is necessary to add water Diluted to about 25g / L, then adsorbed by ion exchange resin, and then desorbed with ammonium chloride to obtain ammonium tungstate solution. This process will also produce a large amount of harmful components containing low concentrations of phosphorus, arsenic, silicon, ammonia nitrogen and alkali. The exchanged solution cannot be properly disposed of, which seriously pollutes the environment. In addition, the solvent extraction method is used to ext...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G41/00C01G41/02C01B15/055B22F9/30
CPCB22F9/30C01B15/055C01G41/00C01G41/003C01G41/02C01P2004/32
Inventor 陈星宇赵中伟
Owner CENT SOUTH UNIV
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