Method for deep purification and lead removal of ammonium perrhenate solution

An ammonium perrhenate and deep purification technology, applied in the field of divalent cations, can solve problems such as high difficulty, low product qualification rate, and long process flow, and achieve the goal of reducing the loss of rhenium, high product pass rate, and short process flow Effect

Active Publication Date: 2020-07-03
ANHUI UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to solve the problem that the Pb impurity in ammonium perrhenate is difficult to remove in the existing technology, and it is difficult to prepare high-purity ammonium perrhenate, and a method for deep purification of ammonium perrhenate solution to remove lead is provided
The present invention selects a crown ether resin of a special size as the Pb ion adsorbent, and forms a stable host-guest complex action mechanism according to the dipole-ion interaction between the host molecule and the guest molecule of the crown ether ligand, It achieves the purpose of having obvious selective recognition ability for the complexation of different metal ions, so that it can efficiently and selectively remove Pb deeply, and solve the problem of the difficulty in removing Pb with ammonium perrhenate, 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 Pb 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

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0032] Step 1, the preparation of ammonium perrhenate solution

[0033] Dissolve the crude ammonium perrhenate with lead exceeding the standard in high-purity water to prepare ammonium perrhenate solution with metal rhenium content of 5-30g / L, adjust the pH value of the solution to alkaline by adding alkali, and vacuum filter with precision filter cloth Solution, remove the fine particles of solid impurities to get the filtrate for use, the size of the precision filter cloth is not less than 2000 mesh, it is worth noting that the smaller filter cloth pore size is conducive to the removal of more fine particles of impurities in the solution, but it will Increase the difficulty of filtering the solution.

[0034] The crude ammonium perrhenate whose lead content exceeds the standard in the above step 1 is 99.0% qualified product ammonium perrhenate or 99.90% first-class ammonium perrhenate, or ammonium perrhenate after the ammonium perrhenate solution is evaporated and crystalliz...

Embodiment 1

[0048] Step 1, the preparation of ammonium perrhenate solution

[0049] Get 74g lead content and be that 99.0% thick ammonium perrhenate of 78ppm is dissolved in 5L high-purity water and prepare ammonium perrhenate solution, adjust the pH value of the ammonium perrhenate solution that is prepared to 8 with ultra-pure ammonia, then use 2000 Use a precision filter cloth to vacuum filter the solution to remove fine particles of solid impurities to obtain the filtrate for use.

[0050] Step 2, the selective deep adsorption and removal of Pb in the ammonium perrhenate solution

[0051] First synthesize a new type of molecular recognition cationic resin capable of adsorbing Pb, add 100ml of the synthesized resin into a 500ml beaker, add 150ml of high-purity water to fully swell for 2 hours, then use a 60-mesh 316L sieve to filter and wash, and then filter the filtered resin with high-grade pure The dilute ammonia water with a concentration of 8% prepared by ammonia water is subject...

Embodiment 2

[0056] Step 1, the preparation of ammonium perrhenate solution

[0057] Get 99.0% thick ammonium perrhenate solution with lead content of 32ppm and dissolve it in 5L high-purity water to prepare ammonium perrhenate solution, adjust the pH value of the prepared ammonium perrhenate solution to 9 with high-grade pure ammonia water, and then use 5000 Use a precision filter cloth to vacuum filter the solution to remove fine particles of solid impurities to obtain the filtrate for use.

[0058] Step 2, the selective deep adsorption and removal of Pb in the ammonium perrhenate solution

[0059] First synthesize a new type of molecular recognition cationic resin capable of adsorbing Pb, add 100ml of the synthesized resin to a 500ml beaker, add 200ml of high-purity water to fully swell for 4 hours, then use a 60-mesh 316L sieve to filter and wash, and then filter the filtered resin with high-grade pure Dilute ammonia water with a concentration of 4% prepared by ammonia water was subje...

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PUM

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Abstract

The invention discloses a method for deep purification and lead removal of an ammonium perrhenate solution, and belongs to the field of separation and purification of scattered metals. The method comprises the following steps: preparing a ammonium perrhenate solution, selectively and deeply adsorbing and removing Pb in the ammonium perrhenate solution, and evaporating and crystallizing the adsorbed and purified solution to obtain high-purity ammonium perrhenate. According to the invention, special crown ether resin is synthesized for lead ions and is used as a lead ion adsorbent to adsorb andremove lead ions in the ammonium perrhenate solution, the specific lead removal process and parameters are optimally designed, therefore, lead can be efficiently and selectively adsorbed and removed,it is guaranteed that the solution obtained after lead removal can be subjected to evaporative crystallization to produce 99.99% or higher grade ammonium perrhenate, the loss of valuable element rhenium is reduced, the requirement for low impurity content of ammonium perrhenate in various industries is met, the technological process is short, the product percent of pass is high, and the productioncost is low.

Description

technical field [0001] The invention belongs to the field of separation and purification of scattered metals, more specifically, it relates to the synthesis of a novel molecular recognition cationic resin, which can deeply purify divalent cations in ammonium perrhenate solution, and is used for producing high-purity ammonium perrhenate above 99.99% new method. Background technique [0002] Rhenium is one of the seven rare metals with a high melting point second only to tungsten. When rhenium is added to a variety of transition metal elements to form an alloy, it can produce a functional material with excellent "rhenium effect", making it suitable for use in aero-engine turbine blades. It has special applications in manufacturing, nuclear reactor alloys, missile high-temperature components, special crucibles, and super-temperature materials. At the same time, because rhenium has an unsaturated 4d electron shell and is easy to donate 5 electrons, rhenium and its compounds hav...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G47/00C22B3/24B01D15/10
CPCC01G47/00C22B3/24B01D15/10C01P2006/80Y02P10/20
Inventor 张福元赵卓
Owner ANHUI UNIVERSITY OF TECHNOLOGY
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