A kind of method for deep purification of ammonium perrhenate solution for removing lead

An ammonium perrhenate, deep purification technology, applied in the field of divalent cations, can solve the problems of high difficulty, low product qualification rate, high production cost, etc., and achieve the effect of reducing the loss of rhenium, high product qualification rate, and large saturation capacity

Active Publication Date: 2022-08-02
ANHUI UNIVERSITY OF TECHNOLOGY
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  • Description
  • Claims
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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

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Effect test

preparation example Construction

[0032] Step 1. Preparation of ammonium perrhenate solution

[0033] Dissolve crude ammonium perrhenate with excess lead into high-purity water to prepare ammonium perrhenate solution with metal rhenium content of 5-30g / L, adjust the pH of the solution to alkaline by adding alkali, and use precision filter cloth for vacuum filtration The filtrate can be obtained by removing fine particles and solid impurities from the solution. The size of the precision filter cloth is not less than 2000 mesh. It is worth noting that the smaller pore size of the filter cloth is conducive to removing more fine particles in the solution. Increase the difficulty of filtration of the solution.

[0034] In the above-mentioned step 1, the crude ammonium perrhenate with excessive lead content is 99.0% qualified product ammonium perrhenate or 99.90% first-grade ammonium perrhenate, or the ammonium perrhenate solution is evaporated and crystallized. Products with a content of not less than 99.0% and a ...

Embodiment 1

[0048] Step 1. Preparation of ammonium perrhenate solution

[0049] Take 74g of 99.0% crude ammonium perrhenate with a lead content of 78ppm and dissolve it in 5L of high-purity water to prepare an ammonium perrhenate solution, adjust the pH of the prepared ammonium perrhenate solution to 8 with ultrapure ammonia, and then use 2000 The solution is vacuum filtered with a mesh precision filter cloth to remove fine particles and solid impurities to obtain a ready-to-use filtrate.

[0050] Step 2. Selective deep adsorption and removal of Pb in ammonium perrhenate solution

[0051] First synthesize a new 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, and then filter and wash it with a 60-mesh 316L sieve, and then filter the resin with superior grade pure water. The diluted ammonia water with a concentration of 8% prepared with ammonia water was subjecte...

Embodiment 2

[0056] Step 1. Preparation of ammonium perrhenate solution

[0057] Take 96g of 99.0% crude ammonium perrhenate with a lead content of 32ppm and dissolve it in 5L of high-purity water to prepare an ammonium perrhenate solution, adjust the pH of the prepared ammonium perrhenate solution to 9 with high-grade pure ammonia water, and then use 5000 The solution is vacuum filtered with a mesh precision filter cloth to remove fine particles and solid impurities to obtain a ready-to-use filtrate.

[0058] Step 2. Selective deep adsorption and removal of Pb in ammonium perrhenate solution

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

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Abstract

The invention discloses a method for deeply purifying and removing lead from an ammonium perrhenate solution, which belongs to the field of separation and purification of scattered metals. The method for deeply purifying and removing lead from ammonium perrhenate solution of the present invention includes preparation of ammonium perrhenate solution, selective deep adsorption and removal of Pb in ammonium perrhenate solution, and high-purity ammonium perrhenate liquid evaporation crystallization after adsorption and purification . In the present invention, a special crown ether resin is synthesized for lead ions, and the lead ion in the ammonium perrhenate solution is adsorbed and removed as a lead ion adsorbent, and the specific process and parameters of the lead removal are optimized and designed, so that the selection can be efficiently selected. It ensures that the solution after lead removal can evaporate and crystallize to produce 99.99% or higher ammonium perrhenate, reduces the loss of valuable element rhenium, and meets the requirements of various industries for low impurities in ammonium perrhenate , the technological process is short, the product qualification rate is high, and the production cost is low.

Description

technical field [0001] The invention belongs to the field of separation and purification of scattered metals, and more particularly relates to synthesizing a new type of molecular recognition cation resin, which deeply purifies divalent 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 applications in manufacturing, nuclear reactor alloys, missile high-temperature components, special crucibles, and over-temperature materials. At the same time, because rhenium has an unsaturated 4d electron layer and is easy to give 5 electrons, rhenium and its compounds have...

Claims

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Application Information

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Patent Type & Authority Patents(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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