Method for preparing high-purity ammonium paratungstate

A technology of pure ammonium paratungstate and ammonium paratungstate, which is applied in the field of preparing high-purity ammonium paratungstate, can solve the problems of high pressure of wastewater treatment, many equipment required, and large liquid volume.

Pending Publication Date: 2020-08-11
XIAMEN TUNGSTEN
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  • Claims
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Problems solved by technology

[0002] Due to the development of science and technology, in order to obtain high-quality follow-up products containing tungsten, higher and higher requirements are put forward for the chemical composition of ammonium paratungstate (APT). The ammonium paratungstate products produced by the existing ion exchange method and extraction method cannot meet the production requirements The needs of tungsten deep processing products
At present, the production methods of high-purity ammonium paratungstate in China are mainly divided into two categories: one is the use of ion exchange method, sodium tungstate solution is diluted with water to a certain extent, and then the ion exchange resin is used to adsorb tungsten. Washing steps, or use saturated adsorption secondary ion exchange method for purification, because the ion exchange method is widely used in industry, this method has the advantages of simple operat

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  • Method for preparing high-purity ammonium paratungstate

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Example Embodiment

[0044] Example 1

[0045] 1. The raw material is national standard 0 level APT, and the total content of impurities detected is 165.4ppm. Add 12m to the mixing tank 3 Ammonia water, the concentration of ammonia water is 140g / l, and 3428.6kg of raw materials are slowly poured into the slurry during the stirring process.

[0046] 2. After the feeding is completed, the autoclave is turned on and stirred, and the material liquid is added to 15m 3 In the autoclave, the jacket is heated by steam and heated to a temperature of 140°C, and the pressure is 0.6MPa at this time. After the temperature is reached, the temperature is maintained and the pressure is maintained for 3 hours.

[0047] 3. After the heat preservation and pressure retention, open the steam exhaust valve of the autoclave for pressure relief and deamination, adjust the opening of the steam valve to control the pressure relief time for 1 hour, and then cool to 60°C to stop cooling and filter, and filter to obtain wet ammonium...

Example Embodiment

[0050] Example 2

[0051] 1. The raw material is the unqualified APT in the production process, and the total content of impurities detected is 300ppm. Add 12m to the mixing tank 3 Ammonia water, the concentration of ammonia water is 115g / l, and 3000kg of raw materials are slowly poured into the slurry during the stirring process.

[0052] 2. After the feeding is completed, the autoclave is turned on and stirred, and the material liquid is added to 15m 3 In the autoclave, the jacket is heated with steam and heated to a temperature of 125°C, at which time the pressure is 0.51MPa. After the temperature is reached, the temperature is maintained and the pressure is maintained for 1 hour.

[0053] 3. After the heat preservation and pressure keeping, open the steam exhaust valve of the autoclave for pressure relief and deammification, adjust the opening of the steam valve to control the pressure relief time for 2h, then cool to 50℃, stop cooling and filter, and filter to obtain wet ammoniu...

Example Embodiment

[0056] Example 3

[0057] 1. The raw material is unqualified APT in the production process, and the total content of impurities detected is 233.8ppm. Add 12m to the mixing tank 3 Ammonia water, the concentration of ammonia water is 90g / l, and 3200kg of raw materials are slowly poured into the slurry during the stirring process.

[0058] 2. After the feeding is completed, the autoclave is turned on and stirred, and the material liquid is added to 15m 3 In the autoclave, the jacket is heated with steam and heated to a temperature of 110°C, at which time the pressure is 0.4 MPa. After the temperature is reached, the temperature is maintained and the pressure is maintained for 2 hours.

[0059] 3. After heat preservation and pressure keeping, open the steam exhaust valve of the autoclave for pressure relief and deamination, adjust the opening of the steam valve to control the pressure relief time for 1.5h, then cool to 55℃ to stop cooling and filter, and filter to obtain wet ammonium par...

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Abstract

The invention provides a method for preparing high-purity ammonium paratungstate. The method comprises the following steps: (1) carrying out size mixing on an ammonium paratungstate crude product by using ammonia water to obtain slurry; (2) introducing the slurry into an autoclave for high-temperature and high-pressure dissolution so as to obtain an ammonium tungstate solution; (3) carrying out pressure relief deamination crystallization on the ammonium tungstate solution to obtain wet ammonium paratungstate crystals; and (4) drying the wet ammonium paratungstate crystal so as to obtain the high-purity ammonium paratungstate. The method effectively utilizes the advantages of high temperature and high pressure of the autoclave and the characteristics of high temperature and high pressure dissolution and pressure relief deamination of the ammonium paratungstate to separate out crystals, and effectively realizes efficient purification of the ammonium paratungstate crude product, and the total content of impurities in the finally obtained high-purity ammonium paratungstate is less than or equal to 65ppm. Therefore, the method has the advantages of short process, low cost, high efficiency, high yield, high purification and the like.

Description

technical field [0001] The invention belongs to the field of chemical industry, in particular, the invention relates to a method for preparing high-purity ammonium paratungstate. Background technique [0002] Due to the development of science and technology, in order to obtain high-quality follow-up products containing tungsten, higher and higher requirements are put forward for the chemical composition of ammonium paratungstate (APT). The ammonium paratungstate products produced by the existing ion exchange method and extraction method cannot meet the production requirements The needs of tungsten deep processing products. At present, the production methods of high-purity ammonium paratungstate in China are mainly divided into two categories: one is the use of ion exchange method, sodium tungstate solution is diluted with water to a certain extent, and then the ion exchange resin is used to adsorb tungsten. Washing steps, or use saturated adsorption secondary ion exchange m...

Claims

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Application Information

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IPC IPC(8): C01G41/00
CPCC01G41/00C01P2006/80
Inventor 曾微微陈杰王海军
Owner XIAMEN TUNGSTEN
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