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Method for preparing APT (Ammonium Paratungstate) from tungsten mineral raw material with zero waste water discharge

A technology of mineral raw materials and raw materials, applied in the field of tungsten smelting, can solve the problems of non-circulation, 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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  • Abstract
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  • Claims
  • 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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  • Method for preparing APT (Ammonium Paratungstate) from tungsten mineral raw material with zero waste water discharge
  • Method for preparing APT (Ammonium Paratungstate) from tungsten mineral raw material with zero waste water discharge
  • Method for preparing APT (Ammonium Paratungstate) from tungsten mineral raw material with zero waste water discharge

Examples

Experimental program
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Effect test

Embodiment 1

[0103] Embodiment 1: certain scheelite (WO 3 The mass percent composition is 49.53%, and the Fe mass percent composition is 0.43%) by generating Ca 3 WO 6 1.1 times the theoretical amount, mixed with clinker leaching slag (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...

Embodiment 2

[0104] Embodiment 2: a certain black and white tungsten mixed ore (WO 3 The mass percent composition is 63.75%, and the Fe mass percent composition is 5.90%) by generating Ca 3 WO 6 and Ca 2 FeWO 6 1.5 times the theoretical amount, mixed with clinker leaching slag for grinding and mixing to obtain raw meal, raw meal particle size ≤ 45μm, and then roasted at 950°C for 3.0h in a shaft furnace under a weak reducing atmosphere to obtain cooked material. 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 thre...

Embodiment 3

[0105] Embodiment 3: certain wolframite (WO 3 The mass percent composition is 62.40%, the Fe mass percent composition is 14.08%, and the Mn mass percent composition is 2.25%) by generating Ca 3 WO 6 and Ca 2 FeWO 6 and Ca 2 MnO 6 1.13 times the theoretical amount, mixed with clinker leaching slag and calcium fluoride for grinding and mixing to obtain raw meal, the amount of calcium fluoride added is 7% (mass percentage) of the dry tungsten mineral raw material amount, the raw meal particle size ≤40μm, then, in a tube-type roasting furnace, under a neutral atmosphere, roast at 800°C for 6.0h to obtain clinker, after the clinker is cooled to room temperature, grind it with a rod mill, the clinker particle size is ≤45μm; leaching equipment Choose a ball mill leaching device with a built-in saturated ammonium carbonate solution, and add ammonium bicarbonate according to 1.0 times the theoretical amount; put the clinker into the leaching equipment, and react at 80°C for 4 hour...

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Abstract

The invention discloses a metallurgical process for a tungsten mineral raw material. A weakly basic leaching agent which is conductive to forming a local process cycle is adopted; a leaching solution of the weakly basic leaching agent generates two or more gases in the evaporating and crystallizing process; various gases can participate in the synthesis of the leaching agent again; the crystallized separating washing solution can be also used as the leaching agent for recycling; the tungsten mineral raw material and a certain amount of calcium-containing substances and mineralizer are ground and uniformly mixed to obtain raw materials; when the raw materials are prepared, the addition of the calcium-containing substance is at least 1.0 time of the theoretical amount of Ca3WO6, Ca2FeWO6 and / or Ca2MnWO6 which are generated by tungsten in the tungsten mineral raw material, preferably 1.1-1.5 times and more preferably 1.1-1.2 times; a transformation ingredient is adopted to be subjected to a chemical reaction with the tungsten mineral raw material, so that tungsten elements are changed to be contained in an intermediate substance which is easily dissolved by the leaching agent; leaching slag also contains ingredient elements, so that at least part of leaching slag can be used as the ingredient for recycling. Therefore, the process contains multiple closed loops; waste water is not discharged in the whole process.

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申雷霆
Owner JIANGXI RARE EARTH & RARE METALS TUNGSTEN GRP HLDG CO LTD
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