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Method for comprehensively recovering tungsten and fluorine from minerals

A mineral and leaching technology, applied in the direction of halide silicon compound, fluorine/hydrogen fluoride, process efficiency improvement, etc., can solve the problem of sulfuric acid consumption, etc., achieve the effect of reducing waste water discharge, ensuring decomposition rate, and avoiding incomplete decomposition

Inactive Publication Date: 2012-07-18
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existence of calcite is mainly caused by the consumption of sulfuric acid, and the by-product CO 2 Can escape without affecting the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Containing fluorite, SiO described in the present invention 2 , scheelite, apatite and calcite and other complex minerals (including CaF 2 95.4%, WO 3 1.7%, SiO 2 0.8%) 1kg to prepare a mixed solution of phosphoric acid and sulfuric acid, P 2 o 5 The content is 20%, the sulfuric acid concentration is controlled at 500g / L, the liquid-solid ratio is 5:1, the reaction temperature is 90°C, and the reaction time is 4h. Under these experimental conditions, CaF 2 The decomposition rate is 99.5%, and the decomposition residue contains WO 3 0.09%. Immediately filter after the decomposition is completed, add the consumed sulfuric acid and lost phosphoric acid to the filtrate, and then return to a new round of leaching of fluorite ore powder. Further distillation is used to prepare hydrofluoric acid. When using the above conditions to circulate leaching fluorite ore powder, the WO in the filtrate 3 When the concentration gradually accumulates to 156.9g / L, the filtrate ...

Embodiment 2

[0047] Containing fluorite, SiO described in the present invention 2 , scheelite, apatite and calcite and other complex minerals (including CaF 2 95.4%, WO 3 1.7%, SiO 2 0.8%) 1kg to prepare a mixed solution of phosphoric acid and sulfuric acid, P 2 o 5 The content is 5%, the sulfuric acid concentration is controlled at 350g / L, the liquid-solid ratio is 10:1, the reaction temperature is 100°C, and the reaction time is 8h. Under these experimental conditions, CaF 2 The decomposition rate is 99.2%, and the decomposition residue contains WO 3 was 0.21%. Immediately filter after the decomposition is completed, add the consumed sulfuric acid and lost phosphoric acid to the filtrate, and then return to a new round of leaching of fluorite ore powder. Further distillation is used to produce hydrofluoric acid. When using the above conditions to circulate leaching fluorite ore powder, the WO in the filtrate 3 When the concentration gradually accumulates to 172.1g / L, the filt...

Embodiment 3

[0049] Low-grade tungsten ore tailings after flotation (containing CaF 2 68.4%, WO 3 10.5%, SiO 2 1.2%, and apatite and calcite, etc.) 1kg to prepare a mixed solution of phosphoric acid and sulfuric acid, P 2 o 5 The content is 15%, the sulfuric acid concentration is controlled at 500g / L, the liquid-solid ratio is 3:1, the reaction temperature is 100°C, and the reaction time is 1h. Under these experimental conditions, CaF 2 The decomposition rate is 98.3%, and the decomposition residue contains WO 3 was 0.31%. Immediately filter after the decomposition is completed, add the consumed sulfuric acid and lost phosphoric acid to the filtrate, and then return to a new round of leaching of fluorite ore powder. Further distillation is used to produce hydrofluoric acid. When using the above conditions to circulate leaching fluorite ore powder, the WO in the filtrate 3 When the concentration gradually accumulates to 143.1g / L, the filtrate is cooled to 30°C by cooling and crys...

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Abstract

The invention provides a method for comprehensively recovering tungsten and fluorine from minerals, namely a mixed acid of phosphoric acid and sulfuric acid is adopted for decomposing complex calcium-containing minerals containing fluorite, scheelite, apatite, and calcite, wherein the fluorite is decomposed to fluorine hydride or silicon tetrafluoride to escape, and absorption treatment is performed for preparing hydrofluoric acid or a fluoride salt; and the scheelite is transformed to phosphotungstic acid to enter into a solution, and filtrate after filtration is supplemented into the consumed sulfuric acid and the phosphoric acid after extraction of the tungsten and returned to the new-round mineral leaching. The method disclosed by the invention has the advantages of comprehensively recovering the fluorine and the tungsten from the minerals, reducing the requirements on the fluorite or the tungsten ore raw material, reducing the pressure on a mineral dressing link, improving the comprehensive recovery rate and simultaneously ensuring the decomposition rate of the fluorite and the scheelite, wherein the decomposition rate of the fluorite is above 98%, and WO3 contained in decomposition slag is reduced to below 0.5%; furthermore, a leaching agent can be recycled, so that leaching cost and wastewater emission are greatly reduced; and the method also has the advantages of simple leaching equipment, convenience in operation and easiness in realization of industrialization.

Description

technical field [0001] The invention is a method for comprehensively recovering fluorine and tungsten in minerals. Background technique [0002] In the skarn tungsten deposit, black and scheelite coexist, and scheelite also coexists with calcium gangue minerals such as fluorite, calcite, apatite and garnet. [0003] The selectivity of scheelite and wolframite is quite different, but the buoyancy of scheelite and calcium gangue minerals is similar. Therefore, the flotation separation of scheelite and calcium gangue minerals, such as fluorite, has always been a mineral processing technology. problem. [0004] According to the existing technical ideas, it is necessary to strongly suppress calcium-containing minerals such as fluorite during the scheelite flotation process. On the one hand, such inhibition also affects the recovery rate of scheelite, which is also a calcium mineral. On the other hand, it also makes it difficult to recover fluorite due to poor buoyancy. Hundreds...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B34/36C22B3/08C22B3/06C01B33/107C01B33/12C01B7/19
CPCY02P10/20
Inventor 赵中伟李江涛
Owner CENT SOUTH UNIV
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