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Method for preparing ultra-pure ammonium rhenate crystals with controllable particle sizes

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

Active Publication Date: 2019-12-03
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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  • Method for preparing ultra-pure ammonium rhenate crystals with controllable particle sizes
  • Method for preparing ultra-pure ammonium rhenate crystals with controllable particle sizes
  • Method for preparing ultra-pure ammonium rhenate crystals with controllable particle sizes

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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, first cool the ammonium rhenate solution obtained through step (1) to 40° C. in 1 hour, and then carry out suction filtration after crystallization for 3 hours 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 the ultra-pure ammonium rhenate crystals with the controllable particle sizes, and belongs to the technical field of hydrometallurgy. According to the invention, the recrystallization treatment is carried out on an aqueous solution of the ammonium rhenate crude product by using a multi-step crystallization method, meanwhile, the crystallization temperature nodes are controlled to be 35-45 DEG C, 0-5 DEG C and 20-40 DEG C, so that the ultra-pure ammonium rhenate crystal with the purity being greater than or equal to 99.999% can be prepared, and theyield of the ultra-pure ammonium rhenate crystal can reach 90% or above. Meanwhile, the consistency of the particle sizes of the obtained ultra-pure ammonium rhenate crystals is ensured, and the grainsize of the crystal can be adjusted by adjusting the crystallization concentration, temperature, time, crystallization times and the like of the ammonium rhenate solution, so that the requirements ofdifferent purposes on the flowability of the ammonium rhenate crystal can be met. The method is suitable for the industrial continuous production, and can realize the high-efficiency and low-energy-consumption large-scale production of the ammonium rhenate crystals with ultrahigh purity and controllable particle sizes.

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 Applications(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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