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Crystallization method of ammonium paratungstate

A technology of ammonium paratungstate and ammonium paratungstate, applied in the field of ammonium paratungstate crystallization, can solve the problems such as unseen research on ammonium paratungstate crystallization, inability to obtain large particles of ammonium paratungstate, uneven distribution, etc., to achieve coarse particles, controllable particle size, simple and easy process Effect

Inactive Publication Date: 2008-05-21
JINDUICHENG MOLYBDENUM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Scholars at home and abroad have used adding seeds or ammonium tungstate solution (NH 4 ) 2 WO 4 Methods Some experiments were carried out: by adding seed crystal method, large particles of ammonium paratungstate could be obtained, but the distribution was uneven and the crystal morphology was poor; adding ammonium tungstate solution (NH 4 ) 2 WO 4 The method can modify the crystal form, but cannot obtain large particles of ammonium paratungstate
At present, there is no research and report on the use of seed crystals and dilute ammonia water to control the crystallization of ammonium paratungstate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Preparation density 1.25g / cm 3 , ammonium tungstate solution with a volume of 1.01 and a pH value of 8.0 was added to a 3l three-necked flask and heated by an electric heating mantle. When boiling reaches a supersaturated state, or when tiny grains appear, or when the density reaches 1.38g / cm 3 20 g of ammonium paratungstate seed crystals with a Fischer particle size of 30 μm were added to the solution. Keep the temperature at 95°C, return to the boiling state after 40 minutes, then add dilute ammonia water (pH value 11) dropwise to adjust the pH value of the ammonium tungstate solution, and keep the pH value of the solution at 8.0. Evaporate until the mother liquor density is 1.08g / cm 3 time, discharge, filter, wash once with dilute ammonia water, wash twice with deionized water, and finally dry at 90°C.

[0014] The produced ammonium paratungstate product has a Fischer particle size > 45 μm, normal distribution, intact crystal form and smooth surface.

Embodiment 2

[0016] Preparation density 1.28g / cm 3 , ammonium tungstate solution with a volume of 1.01 and a pH value of 8.5 was added to a 31 three-necked flask and heated by an electric heating mantle. When boiling reaches a supersaturated state, or when tiny grains appear, or when the density reaches 1.38g / cm 3 10 g of ammonium paratungstate seed crystals with a Fischer particle size of 35 μm were added to the solution. Keep the temperature at 93°C, return to the boiling state after 30 minutes, then add dilute ammonia water (pH value 12) dropwise to adjust the pH value of the ammonium tungstate solution, and keep the pH value of the solution at 8.5. Evaporate until the mother liquor density is 1.10g / cm 3 time, discharge, filter, wash twice with dilute ammonia water, then wash twice with deionized water, and finally dry at 90°C.

[0017] The produced ammonium paratungstate product has a Fischer particle size > 45 μm, normal distribution, intact crystal form and smooth surface.

Embodiment 3

[0019] Industrial production

[0020] (1) Make the density 1.30g / cm 3 , volume 3.5m 3 , the ammonium tungstate solution with a pH value of 9.0 is pumped into the evaporative crystallization kettle;

[0021] (2) Start stirring, slowly open the steam valve, after the solution boils, adjust the steam valve, and evaporate to boiling;

[0022] (3) When it reaches the supersaturated state, or when tiny grains appear, or the density reaches 1.38g / cm 3 , add 15 kg of ammonium paratungstate seed crystals with a particle size of 40 μm, and keep the solution temperature at 90 ° C for 20 min;

[0023] (4) Open the dilute ammonia water pipeline in the head tank, add ammonia water (pH value 13) to the solution, and adjust the pH value of the ammonium tungstate solution to 8.0;

[0024] (5) Evaporate until the density of the mother liquor is 1.09g / cm 3 , discharge, filter, wash 2 times with dilute ammonia water, then wash 3 times with deionized water;

[0025] (6) Dry at 90°C.

[0026...

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Abstract

The invention discloses a crystallization method of ammonium paratungstate and relates to a production method of ammonium tungstate by adopting hydrometallurgy. The method is characterized in that the invention has a crystallization process that ammonium paratungstate crystal seeds are added into ammonium tungstate solution when the solution is evaporated and concentrated to appear microcrystalline particles for isothermal crystallization under the solution temperature of 90-95 DEG C for 20-40mins; the solution is then heated up to boil and added with weak aqua ammonia to adjust the pH value of the ammonium tungstate solution to 8.0-8.5 and then treated with feeding and filtering when the density of mother liquor reaches 10.8 to 1.10 g / cm <3>; the solution is again washed with the weak aqua ammonia and deionized water and dried to obtain the ammonium paratungstate crystals with large particle size and uniform distribution. The method of the invention effectively controls the crystallization of the ammonium paratungstate through the measures of removing fine crystals through the weak aqua ammonia, adding the crystal seeds, controlling the evaporation speed, etc.; in addition, the produced ammonium paratungstate crystals with large and controllable particle size are uniform and smooth; and the technology is simple and easy to be operated.

Description

technical field [0001] A method for crystallizing ammonium paratungstate relates to a method for producing ammonium tungstate by adopting a hydrometallurgical method. Background technique [0002] With the continuous development of new types of cemented carbide and tungsten wire for lamps, more and more stringent requirements are put forward for the chemical composition, Fischer particle size, particle size distribution and crystal morphology of ammonium paratungstate as raw material. Some users require The particles are fine, reaching the micron or even nanometer level; some users require coarse particles and perfect crystal morphology, and this patent mainly solves the latter problem. [0003] At present, the production methods of ammonium paratungstate mainly include neutralization method, evaporation method, ion exchange and extraction method. Evaporation method is often used in industrial production, but when preparing ammonium paratungstate by evaporation method, it is...

Claims

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Application Information

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IPC IPC(8): C01G41/00C01C1/00
Inventor 唐军利
Owner JINDUICHENG MOLYBDENUM CO LTD
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