Ammonium paratungstate deep purification and impurity removal method

An advanced technology of ammonium paratungstate, applied in the field of tungsten smelting, can solve the problem of inability to remove potassium and sodium, and achieve the effect of obvious impurity removal, easy removal and good volatility.

Active Publication Date: 2017-01-04
CNMC GUANGXI PGMA
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

Relevant literature reports and patents: The two-step ion exchange method discussed in the patent CN86108390A prepares high-purity ammonium paratungstate, both times use alkaline anion exchange resin to purify and remove impurities, and have a certain purification effect on phosphorus, arsenic, silicon, etc. in the product , but cannot remove the potassium and sodium in the product; a process technology for producing high-purity ammonium paratungstate mentioned in the patent CN101643245B, the method is to adjust the ion exchange process, and carry out deep impurity removal through enhanced adsorption and subsequent filtration, but this technology The method cannot deeply purify and remove active metal impurities such as potassium and sodium

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  • Ammonium paratungstate deep purification and impurity removal method

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example 1

[0031] The zero-grade product of ammonium paratungstate conforming to the GBT10116-2007 standard is deeply purified to remove impurities to prepare high-purity ammonium paratungstate products.

[0032] Take the standard sample APT-0 product: WO 3 The content of the main metal impurities in the product is 89%, as shown in the following table:

[0033] Element K Na Mg Ga Cu Al content (in WO 3 as the base ppm) 10 9.8 5 8.5 3 4

[0034] The ammonium paratungstate product is converted into a tungstic acid solution for use through acidification-filtration-dissolution, among which H 2 WO 4 WO in solution 3The concentration is 230g / L. Activate the K6-4 resin with hydrochloric acid 1.8 times the volume of the resin, and the concentration of hydrochloric acid is 3mol / L. Use a pump to send the tungstic acid solution into the ion exchange column at a flow rate of 20-30ml / s. The specifications of the exchange column are: 10cm in diameter and 200cm i...

example 2

[0039] The zero-grade product of ammonium paratungstate conforming to the GBT10116-2007 standard is deeply purified to remove impurities to prepare high-purity ammonium paratungstate products.

[0040] Take the standard sample APT-1 product: WO 3 Content of 88.5%, the content of main metal impurities in the product is shown in the table below:

[0041] Element K Na Mg Ga Cu Al content (in WO 3 as the base ppm) 15 14.7 6.8 9.8 5.0 6.2

[0042] The ammonium paratungstate product is converted into a tungstic acid solution for use through acidification-filtration-dissolution, among which H 2 WO 4 WO in solution 3 The concentration is 240g / L. Activate the K6-4 resin with hydrochloric acid 1.8 times the volume of the resin, and the concentration of hydrochloric acid is 3mol / L. Use a pump to send the tungstic acid solution into the ion exchange column at a flow rate of 20-30ml / s. The specifications of the exchange column are: 10cm in diameter a...

example 3

[0047] The zero-grade product of ammonium paratungstate conforming to the GBT10116-2007 standard is deeply purified to remove impurities to prepare high-purity ammonium paratungstate products.

[0048] Take the standard sample APT-1 product: WO 3 Content of 88.5%, the content of main metal impurities in the product is shown in the table below:

[0049] Element K Na Mg Ga Cu Al content (in WO 3 as the base ppm) 15 14.7 6.8 9.8 5.0 6.2

[0050] The ammonium paratungstate product is converted into a tungstic acid solution for use through acidification-filtration-dissolution, among which H 2 WO 4 WO in solution 3 The concentration is 240g / L. Activate the K6-4 resin with hydrochloric acid 1.8 times the volume of the resin, and the concentration of hydrochloric acid is 3mol / L. Use a pump to send the tungstic acid solution into the ion exchange column at a flow rate of 20-30ml / s. The specifications of the exchange column are: 10cm in diameter a...

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Abstract

The invention discloses a method for removing impurities by deeply purifying ammonium paratungstate. The method comprises the following steps of dissolving international zero-grade or first-grade ammonium paratungstate to prepare a to-be-treated solution; sequentially adsorbing the to-be-treated solution with cation exchange resin and anion exchange resin; then analyzing wolframate radical ions adsorbed by the anion exchange resin by using an analytical agent to obtain a analyzed solution; performing evaporation crystallization on the analyzed solution to obtain high-purity ammonium paratungstate. The method disclosed by the invention has the advantages of simple process, easiness in realization and wide application; in addition, the obtained ammonium paratungstate is high in purity.

Description

technical field [0001] The invention relates to the technical field of tungsten smelting, in particular to a method for deep purification and impurity removal of ammonium paratungstate. Background technique [0002] The improvement of the integration level of large-scale integrated circuits in microelectronics technology has put forward higher requirements for materials, and traditional Si-based devices are no longer applicable. High-purity tungsten or ultra-pure tungsten (5N or 6N) is widely used as gate electrode material, wiring material and shielding metal material for semiconductor large-scale integrated circuits due to its high electron migration resistance, high temperature stability and very high electron emission coefficient . High-purity metal tungsten target is one of the basic materials for manufacturing integrated circuits, and its market prospect is closely related to the development of integrated circuits; if the purity of tungsten targets is not high, the op...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G41/00
CPCC01G41/00C01P2006/80
Inventor 班双李敏
Owner CNMC GUANGXI PGMA
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