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High-purity ultra-coarse particle ammonium paratungstate and preparation method thereof

A technology of ammonium paratungstate and coarse particles, applied in the field of high-purity ultra-coarse particle ammonium paratungstate and its preparation, can solve problems such as poor fluidity

Pending Publication Date: 2021-02-02
江钨世泰科钨品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most researchers mainly consider using batch evaporation and crystallization equipment to prepare ammonium paratungstate. By adding seed crystals and adding ammonium tungstate solution to make the particle size of APT thicker, the Fsss particle size of coarse-grained APT products currently developed can only reach 40~ 50μm, poor fluidity

Method used

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  • High-purity ultra-coarse particle ammonium paratungstate and preparation method thereof
  • High-purity ultra-coarse particle ammonium paratungstate and preparation method thereof
  • High-purity ultra-coarse particle ammonium paratungstate and preparation method thereof

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preparation example Construction

[0017] The invention provides a method for preparing high-purity ultra-coarse particle ammonium paratungstate. The method uses ammonium tungstate solution produced by an extraction process as a raw material. Preferably, WO in the ammonium tungstate solution 3 Concentration is 180~260g / L, more preferably, WO 3 The concentration is 200-240g / L. Add the ammonium tungstate solution into continuous evaporation crystallization equipment such as a continuous crystallizer, use a circulation pump to circulate the slurry, stir at a stirring speed of 1000-1400r / min, control the crystallization temperature at 90-100°C, vacuum degree of 0-10KPa, and steam pressure of 0.1 ~0.4MPa, the discharge interval time (the interval time for the crystallized material to be discharged from the crystallization equipment) is 4~10h, more preferably, the crystallization temperature is controlled at 95~99°C, the vacuum degree is 0~5KPa, and the steam pressure is 0.2 ~0.3MPa, evaporation crystallization time...

Embodiment 1

[0021] Ammonium tungstate solution produced by extraction method, its composition is WO 3 220g / L, Mo 0.015g / L, Na 0.011g / L, P 0.007g / L, As 0.003g / L, SiO2 0.12g / L. Add the ammonium tungstate solution into continuous evaporation and crystallization equipment such as a continuous crystallizer, stirring speed 1100r / min, crystallization temperature 94°C, vacuum degree 6KPa, steam pressure 0.4MPa, feeding interval 6h, to generate wet ammonium paratungstate, and wet ammonium paratungstate through Wash, dry and sieve to obtain ammonium paratungstate.

Embodiment 2

[0023] Ammonium tungstate solution produced by extraction method, its composition is WO 3 200g / L, Mo 0.011g / L, Na 0.011g / L, P 0.007g / L, As 0.003g / L, SiO 2 0.12g / L. Add the ammonium tungstate solution into the continuous crystallizer to evaporate, the crystallization temperature is 94.8°C, the stirring speed is 1200r / min, the vacuum degree is 5KPa, the steam pressure is 0.3MPa, and the feeding interval is 6h, to generate wet ammonium paratungstate, and the wet ammonium paratungstate is washed and dried , and sieved to obtain ammonium paratungstate.

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Abstract

The invention discloses high-purity ultra-coarse particle ammonium paratungstate, and relates to the technical field of ammonium paratungstate, the total content of impurities is less than or equal to0.007%, the Fisher particle size is greater than 60 mu m, and the proportion of the Fisher particle size greater than 75 mu m in particle size distribution is greater than 70%; the invention also discloses a preparation method of the high-purity ultra-coarse particle ammonium paratungstate. The method comprises the following steps: by using the ammonium paratungstate solution produced by the extraction technique as the raw material, adding the ammonium paratungstate solution into continuous evaporative crystallization equipment, stirring at 1000-1400 r / min, and carrying out evaporative crystallization while controlling the crystallization temperature at 90-100 DEG C, vacuum degree at 0-10 KPa and steam pressure at 0.1-0.4 MPa. The method has the beneficial effects that a continuous evaporative crystallization method is adopted, the total content of 23 impurity elements required by the national standard of the prepared ammonium paratungstate is smaller than 0.007%, the Fsss particle size is larger than 60 microns, the proportion of the impurity elements larger than 75 microns in particle size distribution exceeds 70%, the apparent density is 2.4-2.6 g / cm < 3 >, and the fluidity issmaller than 35 s / 50 g.

Description

technical field [0001] The invention relates to the technical field of ammonium paratungstate production, in particular to a high-purity ultra-coarse granular ammonium paratungstate and a preparation method thereof. Background technique [0002] Tungsten metallurgical process The preparation of ammonium paratungstate from sodium tungstate solution mainly goes through two steps, the preparation of pure ammonium tungstate solution and the crystallization of ammonium paratungstate. Among them, there are three main methods for the preparation of pure ammonium tungstate: 1) ion exchange method, through ion exchange, the tungstate in sodium tungstate solution is separated from impurities and converted into ammonium tungstate solution; 2) solvent extraction method, mainly Transform sodium tungstate solution into ammonium tungstate; 3) Classical method, the purified sodium tungstate solution is transformed into ammonium tungstate solution through steps such as precipitation to synth...

Claims

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Application Information

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IPC IPC(8): C01G41/00
CPCC01G41/00C01P2004/61
Inventor 陈亿徐双谢中华李继红余春荣黄亮胡祖辉张威
Owner 江钨世泰科钨品有限公司
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