A method for decomposing wolframite under pressure and countercurrent with sulfur-phosphorus mixed acid

A technology of sulfur-phosphorus mixed acid and wolframite, applied in the field of hydrometallurgy, can solve the problem of inability to decompose directly, and achieve the effect of low decomposition cost, speeding up the reaction speed, and realizing the effect of recycling.

Active Publication Date: 2020-05-26
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is a problem that it cannot be directly decomposed when decomposing minerals containing black tungsten

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] This embodiment relates to a method for decomposing wolframite under pressure and countercurrent with sulfur-phosphorus mixed acid, including the following steps:

[0046] 1) will WO 3 Wolframite powder with a content of 65% is mixed with a mixed acid of phosphoric acid and sulfuric acid at a mass volume ratio of 1:6, wherein the concentration of phosphoric acid is 120g / L, and the concentration of sulfuric acid is 160g / L. By pressurizing the reaction system to 1.85 MPa, control the reaction temperature at 200°C, react for 3.0 hours, extract tungsten from wolframite, filter the system after the reaction is completed, and obtain the filtrate;

[0047] 2) Mix fresh wolframite powder with the filtrate again at a mass volume ratio of 1:6, and extract according to the same conditions as described in step 1), to obtain qualified leachate and incompletely leached decomposition slag;

[0048]3) Use 30% TBP + 10% 2-octanol + kerosene as the organic phase to extract the tungsten ...

Embodiment 2

[0053] This embodiment relates to a method for decomposing wolframite under pressure and countercurrent with sulfur-phosphorus mixed acid, including the following steps:

[0054] 1) will WO 3 Wolframite powder with a content of 51% is mixed with a mixed acid of phosphoric acid and sulfuric acid at a mass volume ratio of 1:4, wherein the concentration of phosphoric acid is 130g / L, and the concentration of sulfuric acid is 180g / L. By pressurizing the reaction system to 1.25 MPa, control the reaction temperature at 180°C, react for 2.0 hours, extract the tungsten in wolframite, filter the system after the reaction is completed, and obtain the filtrate;

[0055] 2) Mix fresh wolframite powder with the filtrate described in step 1) again with a mass volume ratio of 1:4, and extract under the same conditions as described in step 1), to obtain qualified leachate and incomplete leaching decomposition slag;

[0056] 3) Use 20% TBP+10% 2-octanol+kerosene as the organic phase to extrac...

Embodiment 3

[0061] This embodiment relates to a method for decomposing wolframite under pressure and countercurrent with sulfur-phosphorus mixed acid, including the following steps:

[0062] 1) will WO 3 Wolframite powder with a content of 35% is mixed with a mixed acid of phosphoric acid and sulfuric acid at a mass volume ratio of 1:10, wherein the concentration of phosphoric acid is 100g / L, and the concentration of sulfuric acid is 200g / L. By pressurizing the reaction system to 0.75 MPa, control the reaction temperature at 160°C, react for 4.0 hours, extract tungsten from wolframite, filter the system after the reaction is completed, and obtain the filtrate;

[0063] 2) Mix fresh wolframite powder with the filtrate again in a mass volume ratio of 1:10, and extract according to the same conditions as described in step 1), to obtain qualified leachate and incompletely leached decomposition slag;

[0064] 3) using 40% sec-octanol+kerosene as the organic phase to extract the tungsten in th...

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Abstract

The invention relates to a method for carrying out pressurization and reverse-flow decomposition on wolframite with mixed acid of phosphoric acid and sulfuric acid. According to the method, the main improvements are that a reaction system is pressurized and the temperature is controlled to be higher than 100 DEG C in the process of extracting tungsten from wolframite powder with the mixed acid ofphosphoric acid and sulfuric acid, and a reverse-flow decomposition method is adopted in the operation process. According to the method, by pressurizing, calcium-containing compounds do not need to beadded to conduct conversion on the wolframite in the extracting process of the tungsten, the tungsten can be directly extracted from the high-tin wolframite or a high-tin black and white tungsten mixed ore, so that the production process is simplified, and the production cost is reduced; and through the process of reverse-flow decomposition, the mixed acid can be recycled, and the production costis further reduced.

Description

technical field [0001] The invention belongs to the extraction of metal tungsten in the field of hydrometallurgy, and in particular relates to a method for decomposing wolframite by pressurization. Background technique [0002] China's tungsten resource reserves rank first in the world, of which scheelite accounts for more than 2 / 3 of the tungsten resource reserves. Chinese invention patents 201010605095.1, 201010605107.0, 201010605103.2, 201010605110.2 and 201010605094.7 propose a new method of synergistically decomposing tungsten ore with sulfuric acid-phosphoric acid. Realized the decomposition of scheelite, and provided a new smelting process for scheelite. [0003] However, when wolframite, which accounts for 1 / 3 of my country's tungsten resource reserves, is directly leached using sulfuric acid-phosphoric acid synergistic decomposition technology, the leaching rate of tungsten is difficult to achieve the decomposition effect of scheelite. This is mainly because wolfra...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B3/08C22B3/06C22B34/36
CPCC22B3/06C22B3/08C22B34/36
Inventor 陈星宇赵中伟
Owner CENT SOUTH UNIV
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