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A method and device for producing ammonium tungstate from tungsten-containing waste

A technology of ammonium tungstate and tungsten waste, applied in the direction of improving process efficiency, etc., can solve problems such as low tungsten recovery rate and equipment corrosion, achieve high tungsten recovery rate and improve production efficiency

Active Publication Date: 2020-10-30
XIAMEN TUNGSTEN +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to overcome the limitation of the existing tungsten-containing waste recovery technology on the cobalt content of the raw material, the phenomenon of sintering in the roasting equipment, the low recovery rate of tungsten and the corrosion of the equipment, and to provide a method that does not reduce the cobalt content of the raw material. A method and device for producing ammonium tungstate from tungsten-containing waste materials with restrictions, no sintering phenomenon in roasting equipment, high tungsten recovery rate and no corrosion to equipment

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  • A method and device for producing ammonium tungstate from tungsten-containing waste

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Experimental program
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Effect test

Embodiment 1

[0044] S1, get tungsten-containing waste (in WO 3 The mass content of tungsten is 40%, with Co 3 o 4 The mass content of cobalt calculated is 20%) 200g, add calcium carbonate, Ca / WO 3 The mol ratio is controlled at 4.5:1, mixes evenly, obtains compound;

[0045] S2. Calcining the mixed material at a temperature of 800° C. for 4 hours to obtain a roasted material;

[0046] S3, add ammonium carbonate in the roasting material, then the gained mixture is placed in airtight container and react, the addition of ammonium carbonate is to make the calcium in the roasting material be converted into 1.2 times of the amount (theoretical amount) of calcium carbonate, reaction temperature The temperature is 60°C, the reaction time is 4h, and the solid-liquid ratio is 1:6. After that, the obtained solid-liquid mixture is filtered, and the filter residue is washed three times with heated anhydrous salt water (50°C, the same below), and the filtrate is combined with the washed water phase t...

Embodiment 2

[0048] S1, get tungsten-containing waste (in WO 3 The mass content of tungsten is 95%, with Co 3 o 4 The mass content of cobalt is 0.1%) 150g, add calcium hydroxide, Ca / WO 3 The mol ratio is controlled at 4.8:1, mixes homogeneously, obtains compound;

[0049] S2. Calcining the mixed material at a temperature of 750° C. for 3 hours to obtain a roasted material;

[0050] S3, adding ammonium bicarbonate to the roasting material, then the resulting mixture is placed in a closed container for reaction, the amount of ammonium bicarbonate added is 1.4 times the amount (theoretical amount) that makes the calcium in the roasting material convert into calcium carbonate, The reaction temperature is 75°C, the reaction time is 3 hours, and the solid-to-liquid ratio is 1:5. Afterwards, the obtained solid-liquid mixture is filtered, and the filter residue is washed three times with heated anhydrous salt water. The combined and washed water phase of the filtrate is ammonium tungstate solut...

Embodiment 3

[0052] S1, get tungsten-containing waste (in WO 3 The mass content of tungsten is 65%, with Co 3 o 4 The mass content of cobalt is 10%) 100g, add calcium oxide, Ca / WO 3 The mol ratio of the mixture is controlled at 6:1, and the mixture is homogeneously obtained to obtain a mixture;

[0053] S2. Calcining the mixed material at a temperature of 780° C. for 4 hours to obtain a roasted material;

[0054] S3, add ammonium phosphate in roasting material, then place gained mixture in airtight container and react, the addition of ammonium phosphate is to make the calcium in roasting material be converted into 1.5 times of the amount (theoretical amount) of calcium phosphate, reaction temperature The temperature is 55°C, the reaction time is 5h, and the solid-liquid ratio is 1:8. After that, the obtained solid-liquid mixture is filtered, and the filter residue is washed three times with heated anhydrous salt water. was 97.5%.

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Abstract

The invention belongs to the field of tungsten secondary resource recycling and particularly relates to a method and a device for producing ammonium tungstate from tungstenic waste. The method for producing ammonium tungstate from tungstenic waste comprises the steps that firstly, tungstenic waste and a calcic compound are mixed, the appending proportion of the calcic compound is controlled so that the molar ratio of Ca / WO3 is (4.5-9): 1, and a mixed material is acquired; secondly, the mixed material is roasted at the temperature of equal to or higher than 500 DEG C, and a roasted material isacquired; and thirdly, an ammonium salt is added to the roasted material, the mixture acquired is placed in a sealed container to react so that tricalcium tungstate in the roasted material is transformed into ammonium tungstate and an insoluble calcium salt, and then reaction products acquired are filtrated, and a ammonium tungstate solution and filter residues are acquired. The method provided is applicable to recycling processing of various tungstenic waste; the tungsten recycling rate is high; moreover, universal mixing equipment and sintering equipment is adopted in the whole process; clotted slag does not form in the equipment; besides, corrosion to the equipment does not exist; and the method has great popularization significance.

Description

technical field [0001] The invention belongs to the field of recovery of tungsten secondary resources, and in particular relates to a method and a device for producing ammonium tungstate from waste materials containing tungsten. Background technique [0002] Tungsten is an important strategic resource, known as "industrial teeth". With the increasing mining of tungsten ore, the reserves of tungsten ore resources are shrinking day by day, and the recovery of tungsten secondary resources is particularly important. However, due to the complex and diverse components of tungsten-containing waste, the existence state of tungsten is difficult to determine and the treatment is difficult. The methods for recycling tungsten-containing waste in the prior art mainly include "zinc melting method", "saltpeter smelting method" and "roasting alkali leaching method". [0003] These recycling methods suffer from various drawbacks. For example, the "zinc fusion method" is based on the fact ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B1/02C22B7/00C22B34/36
CPCC22B1/02C22B7/006C22B34/36Y02P10/20
Inventor 王世良胡庆民
Owner XIAMEN TUNGSTEN