A kind of method for deep purification and potassium removal of ammonium perrhenate solution

A technology of ammonium perrhenate and deep purification, applied in chemical instruments and methods, rhenium compounds, inorganic chemistry, etc., can solve the problems of high production cost, difficulty in potassium removal, long process flow, etc., and achieve the effect of large saturation capacity

Active Publication Date: 2022-08-02
ANHUI UNIVERSITY OF TECHNOLOGY
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  • Description
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Problems solved by technology

[0007] The purpose of the present invention is to solve the problem that the potassium impurity in ammonium perrhenate is difficult to remove in the existing technology, and it is difficult to prepare high-purity ammonium perrhenate, and provides a method for deep purification and removal of potassium in ammonium perrhenate solution
The present invention selects a crown ether resin of a special size as the potassium ion adsorbent, thereby being able to efficiently and selectively remove potassium in depth, and solve the problems of difficulty in removing potassium from ammonium perrhenate in the existing process, long process flow, low product qualification rate, and production problems. Problems such as high cost and high loss of valuable element rhenium enable the solution after potassium removal to evaporate and crystallize to produce 99.99% or higher ammonium perrhenate, which meets the requirements of various industries, especially aerospace materials, for ammonium perrhenate with low impurities Require

Method used

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Examples

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preparation example Construction

[0038] Step 1. Preparation of ammonium perrhenate solution

[0039] The thick ammonium perrhenate product is dissolved in high-purity water to form an ammonium perrhenate solution, and an alkaline substance is used to adjust the pH value of the ammonium perrhenate solution to be alkaline, and the alkaline substance is not easy to use NaOH, KOH, Ca( OH) and other alkalis that are easy to introduce metal ions, preferably high-grade pure ammonia water or high-purity ammonia gas, to avoid the secondary introduction of impurity metal ions, and the pH value of the ammonium perrhenate solution is preferably adjusted to 8-11. The pH of the ammonium perrhenate is easy to cause the volatilization of ammonia to deteriorate the working environment, and the lower pH is easy to increase the loss of rhenium in the evaporation and crystallization process of ammonium perrhenate after purification. The size of the precision filter cloth is not less than 2000 mesh. It is worth noting that the sm...

Embodiment 1

[0054] Step 1. Preparation of ammonium perrhenate solution

[0055] Dissolve 30 grams of 99.0% qualified crude ammonium perrhenate product in 4L of high-purity water to form an ammonium perrhenate solution, adjust the pH of the ammonium perrhenate solution to about 8 with high-grade pure ammonia water, and then use a 2000-mesh precision filter cloth The solution is vacuum filtered to remove fine particulate solid impurities, and the obtained filtrate is used for the next step to remove potassium ion impurities.

[0056] Step 2. Selective deep adsorption and removal of potassium ions in ammonium perrhenate solution

[0057] First add 100ml of the new molecular recognition cationic resin into a 500ml beaker, add 100ml of high-purity water to fully swell for 2 hours, filter and wash with a 60-mesh 316L sieve after the swelling is completed, and then filter the resin with 10% dilute ammonia water prepared with high-grade pure ammonia water Alkali leaching transformation for 48 hour...

Embodiment 2

[0064] Step 1. Preparation of ammonium perrhenate solution

[0065] Dissolve 100 grams of 99.0% first-grade ammonium perrhenate in 2.5L of high-purity water to form an ammonium perrhenate solution, and use high-purity ammonia gas to adjust the pH of the ammonium perrhenate solution to about 11 through an air distributor, and then use 8000 The solution is vacuum filtered with a mesh precision filter cloth to remove fine particulate solid impurities, and the obtained filtrate is used for the next step to remove potassium ion impurities.

[0066] Step 2. Selective deep adsorption and removal of potassium ions in ammonium perrhenate solution

[0067] First add 50ml of the new molecular recognition cationic resin into a 200ml beaker, add 100ml of high-purity water to fully swell for 10h, filter and wash with a 60-mesh 316L sieve after the swelling, and then filter the resin with 8% dilute ammonia water prepared with high-grade pure ammonia water Alkali leaching transformation for ...

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Abstract

The invention discloses a method for deeply purifying and removing potassium from an ammonium perrhenate solution, which belongs to the field of separation and purification of scattered metals. The method for deep purification and removal of potassium from ammonium perrhenate solution of the present invention includes preparation of ammonium perrhenate solution, selective deep adsorption and removal of potassium ions in ammonium perrhenate solution, regeneration of novel molecular recognition cation resin, and adsorption and purification Liquid evaporation and crystallization of high-purity ammonium perrhenate in four steps. By using special crown ether resin as potassium ion adsorbent, and optimizing the design of potassium removal process and parameters for deep purification of ammonium perrhenate solution, it can efficiently select depth Potassium removal solves the current problems of difficult potassium removal with ammonium perrhenate, long process flow, low product qualification rate, high production cost, and high loss of valuable element rhenium, ensuring that the solution after potassium removal can be evaporated and crystallized to produce 99.99% or more High-grade ammonium perrhenate meets the requirements of various industries for low impurities in ammonium perrhenate.

Description

technical field [0001] The invention belongs to the field of separation and purification of scattered metals, and more particularly relates to the synthesis of a new type of molecular recognition cation resin, which deeply purifies monovalent cations in ammonium perrhenate solution, and is used for producing more than 99.99% high-purity ammonium perrhenate. new method. Background technique [0002] Rhenium is one of the seven rare metals, with a high melting point second only to tungsten. After rhenium is added to various transition metal elements to form alloys, it can produce functional materials with excellent "rhenium effect" performance, making it suitable for aero-engine turbine blades. It has special and critical applications in manufacturing, nuclear reactor alloys, missile high temperature components, special crucibles, ultra-high temperature materials, etc. At the same time, because rhenium has an unsaturated 4d electron layer, it is easy to give 5 electrons and h...

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 张福元赵卓
Owner ANHUI UNIVERSITY OF TECHNOLOGY
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