A method for preparing ultra-high-purity ammonium rhenate crystals with controllable particle size

A technology of ammonium rhenate and crystals, which is applied in the field of purification parameters of ultra-high-purity ammonium rhenate crystals and control of crystal growth process, which can solve the problems of cumbersome process flow, long time period, and no control of crystal growth process, etc., and achieve low energy consumption , the effect of high efficiency energy consumption

Active Publication Date: 2021-06-11
昆明先导新材料科技有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This patent also discloses a method for preparing high-purity ammonium rhenate, but the process flow is cumbersome and the time period is long, and the crystal growth process is not controlled

Method used

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  • A method for preparing ultra-high-purity ammonium rhenate crystals with controllable particle size
  • A method for preparing ultra-high-purity ammonium rhenate crystals with controllable particle size
  • A method for preparing ultra-high-purity ammonium rhenate crystals with controllable particle size

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Embodiment 1

[0032] A kind of embodiment of the method for the ultra-high-purity ammonium rhenate crystal that the present invention prepares particle size controllable, it comprises the following steps:

[0033] (1) Dissolving: the ammonium rhenate crude product (which meets the specified standard required in Table 1) with a purity of 99.99% (4N) is mixed with water, heated to 70° C. to dissolve it completely, and to obtain a mass concentration of 15%. Ammonium rhenate solution;

[0034] (2) Crystallization 1: under stirring conditions, the ammonium rhenate solution obtained by the treatment in step (1) was first cooled to 40° C. in 1 h, and then suction filtered after 3 h of crystallization to obtain crystal A and mother liquor A;

[0035] (3) Crystallization 2: under the condition of stirring, the temperature of the mother liquor A is lowered to 5° C. in 1 hour, and then suction filtration is carried out after 3 hours of crystallization to obtain the crystal B and the mother liquor B; ...

Embodiment 2

[0045] A kind of embodiment of the method for the ultra-high-purity ammonium rhenate crystal that the present invention prepares particle size controllable, it comprises the following steps:

[0046] (1) Dissolving: the ammonium rhenate crude product (which meets the specified standard required in Table 1) with a purity of 99.99% (4N) is mixed with water, heated to 80° C. to dissolve it completely, and to obtain a mass concentration of 20%. Ammonium rhenate solution;

[0047] (2) Crystallization 1: under stirring conditions, first cool the ammonium rhenate solution obtained through step (1) to 40° C. in 4 hours, and then carry out suction filtration after crystallization for 6 hours to obtain crystal A and mother liquor A;

[0048] (3) Crystallization 2: under the condition of stirring, the temperature of the mother liquor A was lowered to 5° C. in 4 hours, and then suction filtration was carried out after 6 hours of crystallization to obtain the crystal B and the mother liquo...

Embodiment 3

[0054] A kind of embodiment of the method for the ultra-high-purity ammonium rhenate crystal that the present invention prepares particle size controllable, it comprises the following steps:

[0055] (1) Dissolving: the ammonium rhenate crude product (which meets the specified standard required in Table 1) with a purity of 99.99% (4N) is mixed with water, heated to 60° C. to dissolve it completely, and to obtain a mass concentration of 15%. Ammonium rhenate solution;

[0056] (2) Crystallization 1: under stirring conditions, the ammonium rhenate solution obtained through the treatment of step (1) was first cooled to 40° C. in 2 hours, and then suction filtered after crystallization for 5 hours to obtain crystal A and mother liquor A;

[0057] (3) Crystallization 2: under the condition of stirring, the temperature of the mother liquor A was lowered to 5°C in 2 hours, and then suction filtration was performed after the crystallization was separated for 5 hours to obtain the crys...

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Abstract

The invention provides a method for preparing ultra-high-purity ammonium rhenate crystals with controllable particle size, which belongs to the technical field of hydrometallurgy. The present invention adopts multiple fractional crystallization methods to recrystallize the aqueous solution of ammonium rhenate crude product, and at the same time controls the crystallization temperature nodes to be 35-45°C, 0-5°C and 20-40°C, not only can obtain the purity ≥ 99.999% Ultra-high-purity ammonium rhenate crystals, and the yield of ultra-high-purity ammonium rhenate crystals can reach more than 90%; at the same time, it ensures the consistency of the obtained ultra-high-purity ammonium rhenate crystals; The crystallization concentration, temperature, time and number of crystallization of the ammonium solution are used to adjust the crystal particle size, which can meet the fluidity requirements of ammonium rhenate crystals for different purposes; it is suitable for industrial continuous production, and can realize large-scale production with high efficiency and low energy consumption. Ammonium rhenate crystals with high purity and controlled particle size.

Description

technical field [0001] The invention belongs to the technical field of hydrometallurgy, and relates to a process for producing ammonium rhenate by wet technology, in particular to purification parameters and crystal growth control process of ultra-high-purity ammonium rhenate crystals. Background technique [0002] Ultra-high purity ammonium rhenate (NH 4 ReO 4 , with a purity of 99.999% or above) is the raw material for the production of high-purity rhenium metal. With the increasing demand for metal rhenium by high-tech, the R&D and production of ultra-high-purity ammonium rhenate has also attracted extensive attention from the industry. At present, the purification of ammonium rhenate mainly adopts recrystallization method and ion exchange-crystallization method. However, most of the patented technologies lack the process research on the production of ultra-high-purity ammonium rhenate and the control research on the crystallization process of ammonium rhenate. [0003...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B61/00C22B3/22
CPCC22B3/22C22B61/00Y02P10/20
Inventor 王权朱刘李永鹏秦婷婷
Owner 昆明先导新材料科技有限责任公司
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