Metallurgical technology with multiple closed cycles for tungsten mineral raw materials

A mineral raw material and process technology, applied in the field of tungsten smelting, can solve the problems of non-recycling, difficult continuous production, high production cost, etc., and achieve the effects of reducing energy consumption and cost, easy industrial application, and reducing processing costs

Active Publication Date: 2015-01-07
JIANGXI RARE EARTH & RARE METALS TUNGSTEN GRP HLDG CO LTD +1
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  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The existing technologies all have the following essential defects: they all adopt non-circulation or semi-circulation process systems, and do not realize all circulation processes
There are at least the following technical problems in the prior art: waste water discharge outlets must be installed, and the waste water pollution problem cannot be completely eradicated; most of the auxiliary materials are disposable consumables, and the leaching agent used in the leaching process is excessive. Either directly discharged, or need to use the corresponding acid or alkali to neutralize and then discharged, the consumption of auxiliary materials is high, and the production cost is high; part of the tungsten element is inevitably brought out in the wastewater, and the recovery rate of the tungsten element is low; the investment in equipment is large, The process is long, the productivity is low, and it is difficult to achieve continuous production
[0007] In such an APT preparation process, the consumption of auxiliary raw materials is relatively large, and a large amount of waste water is generated; a large amount of high-salt waste liquid is generated during the transformation of sodium tungstate solution, and ammonia nitrogen waste water is generated by evaporating the crystallization mother liquid
[0008] If the open-circuit process with waste water discharge is changed into a closed-circuit process without waste water discharge, it is not technically impossible, but the capital invested may even be greater than the profit. Therefore, enterprises have to choose to discharge, resulting in serious environmental pollution

Method used

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  • Metallurgical technology with multiple closed cycles for tungsten mineral raw materials
  • Metallurgical technology with multiple closed cycles for tungsten mineral raw materials
  • Metallurgical technology with multiple closed cycles for tungsten mineral raw materials

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0104] Embodiment 1: by CaO / WO 3 Molecular ratio is 3.3, a certain scheelite (WO 3 The mass percentage content is 49.53%, the Fe mass percentage content is 0.43%) and clinker leaching residue (the main component is CaCO 3 ) and mineralizer calcium fluoride are ground and mixed to obtain the raw meal, the addition of calcium fluoride is 5.2% (mass percentage) of the dry tungsten mineral raw material amount, and the particle size of the raw meal is ≤40 μm. Then, in the roasting furnace In the air atmosphere, the clinker was obtained by roasting at 800°C for 2.0h. After the clinker is cooled to room temperature, it is ground with a vibrating mill, and the clinker particle size is ≤45 μm. Weigh 5.0g of finely ground clinker and add it to the reaction kettle with ventilation and mechanical stirring device, and add 50g-(NH 4 ) 2 CO 3 / 100g-H 2 O ammonium carbonate solution 50mL and sealed, and then into CO 2 gas, control the absolute pressure of the reaction system to 2atm, a...

Embodiment 2

[0105] Embodiment 2: by (CaO+FeO) / WO 3 Molecular ratio is 4.5, a black and white tungsten mixed ore (WO 3 The mass percent content is 63.75%, the Fe mass percent content is 5.90%) and the clinker leaching slag are ground and mixed to obtain raw meal, the raw meal particle size is ≤45μm, and then, in the shaft furnace, the weak reducing atmosphere At 950°C for 3.0 hours, clinker was obtained. After the clinker is cooled to room temperature, it is ground with a ball mill, and the particle size of the clinker is ≤45 μm. Take by weighing 20.0g clinker and join in the reaction kettle of band ventilation and mechanical stirring device, add 35g-(NH 4 ) 2 CO 3 / 100g-H 2 O ammonium carbonate solution 100mL and sealed, and then into CO 2 Gas, control the absolute pressure of the reaction system to 2atm, and react at 70°C for 4h. After the reaction, the leached pulp is vacuum filtered, and the filter cake is washed three times with pure water. The leaching rate of tungsten in cli...

Embodiment 3

[0106] Embodiment 3: press (CaO+FeO+MnO) / WO 3 Molecular ratio is 3.4, a wolframite (WO 3 The mass percentage content is 62.40%, the Fe mass percentage content is 14.08%, the Mn mass percentage content is 2.25%) and the clinker leaching residue and calcium fluoride are ground and mixed to obtain the raw meal, and the calcium fluoride The amount of addition is 7% (mass percentage) of the dry tungsten mineral raw material, and the particle size of the raw material is ≤40 μm. Then, in a tubular roaster, under a neutral atmosphere, roast at 800°C for 6.0 hours to obtain clinker, and the clinker is cooled After reaching room temperature, use a rod mill to grind finely, the clinker particle size is ≤45μm; the leaching equipment selects a ball mill leaching device with a built-in ammonium carbonate saturated solution, and adds ammonium bicarbonate according to 1.0 times the theoretical amount; put the clinker into the leaching equipment, Reaction at 80°C for 4h. After the reaction, ...

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Abstract

The invention discloses a metallurgical technology for tungsten mineral raw materials. The technology comprises the following steps: proportioning the mineral raw materials and ingredients to obtain raw materials; roasting the raw materials to enable the raw materials to be transformed into clinker; using a weak alkali solution to leach the clinker, and recovering solutions fed back from all the links; performing solid-liquid separation on leached slurry, washing leached residues, feeding back washing liquid to a clinker leaching link (a first closed cycle), and feeding back at least part of the leached residues to a raw material preparing link (a second closed cycle) as the ingredients; performing purification and residue-removing on crude solutions; evaporating and crystallizing the purified solutions; returning released gases to the clinker leaching step (a third closed cycle), and feeding back evaporated water to a solid-liquid separation link (a fourth closed cycle) of leaching the slurry; performing the solid-liquid separation on the crystallized slurry, washing a solid phase through water and / or an ammonium salt solution, and drying the washed solid phase to obtain a final product containing W elements; returning crystallized mother liquid to the clinker leaching step (a fifth closed cycle). Therefore, the technology disclosed by the invention comprises the multiple closed cycles, and the situation of zero waste water discharge in the whole process is realized.

Description

technical field [0001] The invention relates to a method for preparing APT from tungsten mineral raw materials, belonging to the technical field of tungsten smelting. [0002] The term "raw meal" refers to tungsten mineral raw materials and ingredients, which are mixed in proportion and ground to a certain fineness. [0003] The term "clinker" refers to tungsten mineral raw materials and ingredients that are ground, mixed into raw materials, and then roasted at high temperature. [0004] The term "mineralizer" refers to a substance that can accelerate the reaction between tungsten mineral raw materials and ingredients or reduce the roasting temperature during the roasting process of raw meal. Background technique [0005] In the prior art, the industrial method for preparing APT mainly includes the following steps: decompose tungsten mineral raw material by caustic soda or soda to obtain crude sodium tungstate solution; transform by solution purification-ion exchange or sol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B34/36C22B3/14C22B1/02
CPCY02P10/20
Inventor 李小斌崔源发周秋生李建圃齐天贵徐双刘桂华林国荣彭志宏李继红徐向明童潇依
Owner JIANGXI RARE EARTH & RARE METALS TUNGSTEN GRP HLDG CO LTD
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