A kind of preparation method of high-purity ammonium rhenate

A high-purity technology of ammonium rhenate, applied in chemical instruments and methods, rhenium compounds, inorganic chemistry, etc., can solve the problems of heavy processing burden and unsuitability for industrial scale production, and achieve low pollution, accelerated crystallization, and simple methods Effect

Active Publication Date: 2018-01-16
江苏杰之砂新材料有限公司
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  • Abstract
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AI Technical Summary

Problems solved by technology

The method of washing with sodium hydroxide produces a large amount of alkaline wastewater, and the post-treatment burden of wastewater is heavy, which is not suitable for industrial scale production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Embodiment 1: 10% ammoniacal liquor is added in the thick ammonium rhenate of 5 g / L and carry out evaporation concentration, the rhenium concentration after concentration is 20g / L; 0.5g ammonium rhenate seed crystal is joined in the concentrated solution, at 500rmp rotating speed The solution was subjected to high-speed centrifugation for 5 minutes; the centrifuged ammonium rhenate solution was put into the crystallizer, and 2 m 2 The above-mentioned glass beads were left to stand at room temperature for 24h; the above solution was separated from the solid and liquid to obtain the ammonium rhenate product; the above process was repeated twice to obtain a high-purity ammonium rhenate with a purity of 99.99%. shown in the table below.

[0016] Table 1: Concentrations of K ions and Na ions before and after crystallization

[0017] name

Embodiment 2

[0018] Embodiment 2: the ammoniacal liquor of 15% is joined in the thick ammonium rhenate of 10g / L and carry out evaporation concentration, the rhenium concentration after concentration is 25g / L; 1g ammonium rhenate seed crystal is joined in the concentrated solution; Under 1000rmp rotating speed, to The solution was subjected to high-speed centrifugation for 10 minutes; the centrifuged ammonium rhenate solution was put into the crystallizer, and 5 m 2 The glass beads were left at room temperature for 24 hours; the above solution was separated from solid and liquid to obtain ammonium rhenate product; the above process was repeated 3 times to obtain high-purity ammonium rhenate with a purity of 99.99%.

Embodiment 3

[0019] Embodiment 3: 20% ammoniacal liquor is added in the thick ammonium rhenate of 7g / L and carry out evaporation concentration, the rhenium concentration after concentration is 20g / L; 3g ammonium rhenate seed crystal is joined in the concentrated solution; Under 1000rmp rotating speed, to The solution was subjected to high-speed centrifugation for 10 minutes; the centrifuged ammonium rhenate solution was put into the crystallizer, and 3 m 2 The glass beads were left at room temperature for 24 hours; the above solution was separated from solid and liquid to obtain ammonium rhenate product; the above process was repeated 3 times to obtain high-purity ammonium rhenate with a purity of 99.99%.

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Abstract

The invention relates to a preparation method of high-purity ammonium rhenate. The preparation method comprises the steps of adding 5-20% of ammonia water into crude ammonium rhenate, and carrying out evaporation and concentration, wherein after the concentration is finished, the rhenium concentration is 15-25g / L; adding 0.5-5g of ammonium rhenate seed crystals into the concentrated solution, carrying out high-speed centrifugal treatment on the solution under the condition that the rotating speed is 500-2000rmp, putting the ammonium rhenate solution, subjected to the centrifugal treatment, into a crystallizer and adding 0.5-5m<2> of glass beads into the crystallizer at the same time, and standing for 20-30h at room temperature; carrying out solid-liquid separation on the solution to obtain an ammonium rhenate product; repeating the previous processes for 2-3 times to obtain the product. The preparation method of the high-purity ammonium rhenate can effectively control a crystallization process and reduce the entrainment of impurities, especially the entrainment of K ions, Na ions and the like, thus improving the purity of the ammonium rhenate; therefore, the high-purity ammonium rhenate with the purity of 99.99% can be prepared.

Description

technical field [0001] The invention relates to a preparation method of high-purity ammonium rhenate. Background technique [0002] Ammonium rhenate is an important raw material for the preparation of rhenium metal, and its purity has a decisive influence on the purity of rhenium metal. In order to obtain high-purity rhenium metal, it is first necessary to obtain high-purity ammonium rhenate. The currently widely used ammonium rhenate purification technology is simple recrystallization treatment. The ammonium rhenate obtained has problems such as poor chroma, poor appearance quality, low purity, and high impurity elements such as K and Na. . [0003] CN201110267640.5 discloses a crystallization method of ammonium rhenate solution, the technical solution of which is: comprising the following method steps: a) placing the ammonium rhenate solution having a temperature of 30°C to 90°C and a concentration of ≥15g / L after evaporation and concentration In an open container; b) a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G47/00
CPCC01G47/00C01P2006/80
Inventor 邓丽周亦胄侯桂臣田爱平孙毓泽
Owner 江苏杰之砂新材料有限公司
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