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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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  • Abstract
  • Description
  • Claims
  • Application Information

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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 operation and high degree of automation, but due to the large volume of liquid after the adsorption process, the pressure of wastewater treatment Larger, at the same time, in order to obtain high-purity ammonium tungstate solution on the basis of conventional product production, the direct recovery rate is low, and the amount of waste water generated increases
One is to calcinate the APT obtained by the general method into tungsten trioxide, and then carry out conventional evaporation and crystallization of the ammonium tungstate solution obtained. The high-purity APT obtained by this method has low impurity content, and the process does not increase additional waste water, but the process is lengthy , the overall direct recovery rate is low, more equipment is required, high energy consumption, mechanical pollution is easy to be introduced in the material operation process, and process protection is difficult

Method used

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  • Method for preparing high-purity ammonium paratungstate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] 1. The raw material is national standard 0 grade APT, and the total content of detected impurities 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 put into the mixing process for slurry mixing.

[0046] 2. After the feeding is completed, the pressure cooker is turned on and stirred, and the feed liquid is added to the 15m 3 In the pressure cooker, the jacket is heated with steam until the temperature is 140° C., and the pressure is 0.6 MPa at this time. After the temperature is reached, the heat preservation and pressure are kept for 3 hours.

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

Embodiment 2

[0051] 1. The raw material is 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 put into the slurry during the stirring process.

[0052] 2. After the feeding is completed, the pressure cooker is turned on and stirred, and the feed liquid is added to the 15m 3 In the autoclave, the jacket is heated with steam until the temperature is 125°C, and the pressure is 0.51MPa at this time. After the temperature is reached, the reaction is carried out with heat preservation and pressure for 1 hour.

[0053] 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 exhaust valve to control the pressure relief time for 2 hours, and then cool to 50°C to stop cooling and filter to obtain wet ammonium paratungs...

Embodiment 3

[0057] 1. The raw material is unqualified APT in the production process, and the total detected impurity content 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 put into the slurry during the stirring process.

[0058] 2. After the feeding is completed, the pressure cooker is turned on and stirred, and the feed liquid is added to the 15m 3 In the autoclave, the jacket is heated with steam until the temperature is 110° C. and the pressure is 0.4 MPa at this time. After the temperature is reached, the heat preservation and pressure are kept for 2 hours.

[0059] 3. After heat preservation and pressure keeping, open the steam exhaust valve of the pressure cooker for pressure relief and deamination, adjust the opening of the steam exhaust valve to control the pressure relief time for 1.5 hours, and then cool to 55°C to stop cooling and filter to obtain wet ammonium paratungstate crystals ...

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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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