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Preparation method of ammonium paratungstate

A technology of ammonium paratungstate and sodium tungstate, which is applied in the field of tungsten metallurgy, can solve the problems of small exchange volume of resin work, increase production cost, and low concentration of sodium chloride, and achieve the effects of low cost, easy processing, and short process flow

Active Publication Date: 2018-09-21
CENT SOUTH UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the ion exchange process is widely used in the industry to produce ammonium paratungstate, but the existing ion exchange technology has the following problems: (1) It can only adapt to the feed liquid with low tungsten concentration, and a large amount of dilution water needs to be added to the high concentration sodium tungstate solution , which not only wastes a large amount of water resources, but also has a low concentration of sodium chloride in the ion exchange liquid obtained after extracting tungsten, which is not easy to further recycle; (2) the unit treatment capacity of the basic ion exchange resin used is not high, and the resin The amount of work exchange is small; (3) The amount of waste water is large, and the treatment is difficult, which increases the production cost

Method used

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  • Preparation method of ammonium paratungstate

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Effect test

Embodiment 1

[0038] The invention provides a kind of preparation method of ammonium paratungstate, as figure 1 shown, including the following steps:

[0039] (1) Take 1000mL of 100g / L (WO 3 concentration) sodium tungstate solution, adjust the pH of the feed solution to 6.0 with a mass concentration of 35% hydrochloric acid, and then add solid NH 4 Cl (sodium tungstate and NH 4 The molar ratio of Cl is 1:4), stirred and reacted at 90°C for 0.5h and kept warm for 2h, obtained ammonium paratungstate-sodium double salt and filtrate I after solid-liquid separation, and the precipitation rate of ammonium paratungstate-sodium double salt was 98.3%;

[0040] (2) Take ammonium paratungstate-sodium double salt product as raw material, take 100g of the double salt product in a beaker, and then add 400mL of 28% NH 4Cl solution, converted at a constant temperature of 85°C for 20min, filtered to obtain crude ammonium paratungstate and filtrate II, with 3% NH 4 The crude ammonium paratungstate is was...

Embodiment 2

[0045] The invention provides a kind of preparation method of ammonium paratungstate, as figure 1 shown, including the following steps:

[0046] (1) Take 1000mL of 300g / L (WO 3 concentration) sodium tungstate solution, adjust the pH of the feed solution to 7.2 with a mass concentration of 30% hydrochloric acid, and then add solid NH 4 Cl (sodium tungstate and NH 4 The molar ratio of Cl is 1:3), stirred and reacted at 60°C for 1.0h and kept warm for 4h, and obtained ammonium paratungstate-sodium double salt and filtrate I after solid-liquid separation, and the precipitation rate of ammonium paratungstate-sodium double salt was 98.8%;

[0047] (2) Take ammonium paratungstate-sodium double salt product as raw material, take 100g of the double salt product in a beaker, and then add 600mL of 15% NH 4 Cl solution, converted at a constant temperature of 95°C for 40min, and filtered to obtain crude ammonium paratungstate and filtrate II, with 5% NH 4 The crude ammonium paratungsta...

Embodiment 3

[0052] The invention provides a kind of preparation method of ammonium paratungstate, as figure 1 shown, including the following steps:

[0053] (1) Take 1000mL of 500g / L (WO 3 concentration) sodium tungstate solution, adjust the pH of the feed solution to 7.5 with a mass concentration of 20% hydrochloric acid, and then add solid NH 4 Cl (sodium tungstate and NH 4 The molar ratio of Cl is 1:1.6), stirred and reacted at 95°C for 2.0 hours and kept warm for 8 hours, and obtained ammonium paratungstate-sodium double salt and filtrate I after solid-liquid separation, and the precipitation rate of ammonium paratungstate-sodium double salt was 97.6%;

[0054] (2) Using ammonium paratungstate-sodium double salt product as raw material, take 100g of the double salt product in a beaker, and then add 500mL of 25% NH 4 Cl solution, converted at a constant temperature of 90°C for 30min, and filtered to obtain crude ammonium paratungstate and filtrate II, with 5% NH 4 The crude ammoniu...

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Abstract

The invention discloses a preparation method of ammonium paratungstate and belongs to the technical field of tungsten metallurgy. The ammonium paratungstate is prepared by taking high-concentration sodium tungstate solutions as raw material, WO3 concentration in the sodium tungstate solutions can reach 100-500g / L, a great deal of dilute water is reduced as compared with that in a traditional ion exchange method, and salt bearing liquid waste obtained in preparation of the ammonium paratungstate is small in size, high in concentration and convenient in treatment. By setting up a plurality of processes of 'internal microcirculation' to treat wastewater effluent, ammonium chloride and sodium chloride are separated and recycled through 'evaporative crystallization-hot filtration', sodium chloride is converted into ammonium chloride cyclically used in the production process and sodium carbonate used for high pressure leaching of sodium carbonate from tungsten minerals by introducing a 'Hou's process for soda production', preparation of the ammonium paratungstate directly by high-concentration sodium tungstate solutions is realized, the salt bearing liquid waste generated during the process is effectively reclaimed, pollution of the wastewater and waste salt on environment is removed, waste is turned into wealth, and cleaning production is realized.

Description

technical field [0001] The invention belongs to the technical field of tungsten metallurgy, and in particular relates to a preparation method of ammonium paratungstate. Background technique [0002] Ammonium paratungstate (APT) is an important raw material in the production of tungsten industry, and is widely used in the preparation of tungsten products such as cemented carbide, tungsten plate, and tungsten wire. Since the morphology and impurities of ammonium paratungstate have "genetic characteristics" for subsequent products, it is very important to prepare qualified ammonium paratungstate. At present, the ion exchange process is widely used in the industry to produce ammonium paratungstate, but the existing ion exchange technology has the following problems: (1) It can only adapt to the feed liquid with low tungsten concentration, and a large amount of dilution water needs to be added to the high concentration sodium tungstate solution , which not only wastes a large am...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G41/00C01D3/14C01C1/16
CPCC01C1/164C01D3/14C01G41/00
Inventor 霍广生赵晨阳王新强
Owner CENT SOUTH UNIV
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