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Method for comprehensively recovering fluorine and tungsten from tungsten-containing fluorite mineral

A mineral and fluorite technology, which is applied in the field of tungsten and fluorine comprehensive recovery, can solve the problems of increasing leaching costs, difficulty in dissolving, and low decomposition rate, and achieves the effects of convenient operation, high comprehensive utilization rate, and simple equipment

Active Publication Date: 2013-02-13
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

Since there is excess sulfuric acid in tungsten-containing fluorine gypsum slag, if NaOH or Na 2 CO 3 If the existing tungsten mineral decomposition technology is used, it will inevitably consume a large amount of leaching agent, which will greatly increase the cost of leaching, and the decomposition rate is not high, and the slag contains WO 3 Difficult to reduce to less than 0.5%; and use phosphoric acid and sulfuric acid leaching system to decompose the fluorine gypsum slag, because most of the tungsten in the fluorine gypsum slag is solid tungstic acid (or WO 3 ) exists in the form, it is difficult to dissolve in the system and cannot be effectively recovered

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Using sulfuric acid and phosphoric acid to decompose 1kg of tungsten-containing fluorite concentrate (containing CaF 2 95.6%, WO 3 2.7%). The molar ratio of the sulfuric acid dosage of 98% to the calcium content in the mineral is 1.2, the phosphoric acid dosage and the WO in the mineral 3 The molar ratio of the content is 1.0, the roasting temperature is 250°C, and the roasting time is 6h. The HF gas generated during the roasting process is absorbed and used to prepare hydrofluoric acid, CaF 2 The decomposition rate is 96.2%. The fluorine gypsum obtained after the sintering process is treated with H 3 PO 4 The solution with a concentration of 100g / L was leached for 4 hours, the liquid-solid ratio was 5:1, the leaching temperature was 80°C, the leaching rate of tungsten was 96.5%, and the slag contained WO 3 is 0.056%. The filtrate obtained after the leaching process can be returned to a new round of leaching of tungsten-containing fluorogypsum. The tungsten in th...

Embodiment 2

[0031] Using sulfuric acid and phosphoric acid to decompose 1kg of tungsten-containing fluorite concentrate (containing CaF 2 95.6%, WO 3 2.7%). The concentration is that the molar ratio of the sulfuric acid dosage of 95% to the calcium content in the mineral is 1.05, the phosphoric acid dosage and the WO in the mineral 3 The molar ratio of the content is 1.5, the roasting temperature is 220°C, and the roasting time is 4h. The HF gas generated during the roasting process is absorbed and used to prepare hydrofluoric acid, CaF 2 The decomposition rate is 95.1%. The fluorine gypsum obtained after the sintering process is treated with H 3 PO 4 The solution with a concentration of 20g / L was leached for 6 hours, the liquid-solid ratio was 1:1, the leaching temperature was 100°C, the leaching rate of tungsten was 97.3%, and the slag contained WO 3 is 0.043%. The filtrate obtained after the leaching process can be returned to a new round of leaching of tungsten-containing fluor...

Embodiment 3

[0033] Using sulfuric acid and phosphoric acid to decompose 1kg of tungsten-containing fluorite concentrate (containing CaF 2 98.4%, WO 3 0.9%). The molar ratio of the amount of sulfuric acid with a concentration of 90% to the calcium content in the mineral is 1.5, and the amount of phosphoric acid and the WO in the mineral are 3 The molar ratio of the content is 2.0, the roasting temperature is 200°C, and the roasting time is 8h. The HF gas generated during the roasting process is absorbed and used to prepare hydrofluoric acid, CaF 2 The decomposition rate is 95.2%. The fluorine gypsum obtained after the sintering process was leached with water for 1 hour, the liquid-solid ratio was 10:1, the leaching temperature was 100°C, the leaching rate of tungsten was 94.5%, and the slag contained WO 3 is 0.029%. The filtrate obtained after the leaching process can be returned to a new round of leaching of tungsten-containing fluorogypsum. The tungsten in the leach solution is ads...

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Abstract

The invention provides a method for comprehensively recovering fluorine and tungsten from tungsten-containing fluorite mineral. In the method, the tungsten-containing fluorite mineral is roasted by use of sulfuric acid and phosphoric acid (or phosphorite), and the HF gas generated by decomposing the fluorite by sulfuric acid is used for preparing hydrofluoric acid; and meanwhile, the tungsten-containing mineral reacts with the sulfuric acid and phosphoric acid to obtain soluble heteropoly acid which is left in fluorgypsum and can be recovered by a water leaching or acid leaching method. Through the invention, the tungsten in mineral can be efficiently recovered while preparing the hydrofluoric acid; the decomposition rate of fluorite is over 95%, the recovery rate of tungsten exceeds 90%, and the content of WO3 in the fluorgypsum is reduced to below 0.1%; a leaching reagent can be recycled, thus the cost and the waste water discharge are greatly reduced; and the equipment is simple, the operation is convenient, and the industrialization is easy to realize.

Description

technical field [0001] The invention is a method for comprehensively recovering fluorine and tungsten from tungsten-containing fluorite minerals. Background technique [0002] Fluorite is the most important mineral in fluoride. It has unique physical and chemical properties and is widely used. It plays a pivotal role in industrial development and is closely related to the development of the national economy. my country is recognized as a fluorite resource country, producer and exporter in the world. Its resource reserves, mining volume and export volume all rank first in the world. [0003] However, the reserves of single-type fluorite deposits in my country are small, and the CaF 2 The rich ore with a grade of more than 65% is less than 23% of my country's fluorite resource reserves, and most of the fluorite resources are associated ores (Zhong Jiangchun. Utilization of fluorite resources in my country and its development trend. Chemical Industry, 2011, 29; Xu Xiaotian. D...

Claims

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Application Information

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IPC IPC(8): C22B1/06C22B34/36C01B7/19
CPCY02P10/20
Inventor 赵中伟李江涛张文娟刘旭恒陈星宇何利华
Owner CENT SOUTH UNIV
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