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A kind of preparation method of high-purity ammonium rhenate

A technology of ammonium rhenate and perrhenic acid, applied in chemical instruments and methods, rhenium compounds, inorganic chemistry, etc., can solve problems such as difficult to achieve purification effect, unable to meet the requirements of ultra-high-purity rhenium products, and achieve strong adaptability Effect

Active Publication Date: 2020-12-25
NORTHWEST INSTITUTE FOR NON-FERROUS METAL RESEARCH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, for the ammonium rhenate produced in copper smelters, due to the mineralogical characteristics of Re and Tl, the two are associated in copper ore. During the copper smelting process, Re and Tl are oxidized into volatile Re respectively. 2 o 7 and Tl 2 O enters the flue gas, and the flue gas absorbs the waste acid solution containing rhenium. Most of the ammonium rhenate products recovered from this waste acid solution have a higher Tl content. It is difficult to achieve the purification effect and cannot meet the requirements of ultra-high purity rhenium products for aviation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] This embodiment includes the following steps:

[0025] Step 1. Dissolve 14.4g of ammonium rhenate in 1000mL of pure water to obtain an ammonium rhenate solution, then adjust the pH of the ammonium rhenate solution to 7, and add 10mL of hydrogen peroxide for oxidation reaction for 20min, then add 0.17g of polyferric sulfate for precipitation reaction 10min, obtain the ammonium rhenate solution not containing Tl after centrifugation; The mass content of Tl is 0.1% in the described ammonium rhenate;

[0026] Step 2. Concentrate and crystallize the Tl-free ammonium rhenate solution obtained in step 1 to obtain ammonium rhenate crystals, then place the ammonium rhenate crystals in a closed tube furnace, heat to 400° C. and feed in oxygen for Oxidize and volatilize, and then absorb the volatilized gas with pure water to obtain a perrhenic acid solution;

[0027] Step 3, using C160 type cation exchange resin to exchange and remove impurities from the perrhenic acid solution o...

Embodiment 2

[0033] This embodiment includes the following steps:

[0034] Step 1. Dissolve 43.2g of ammonium rhenate in 1000mL of pure water to obtain an ammonium rhenate solution, then adjust the pH of the ammonium rhenate solution to 8, and add 3g of sodium chlorate for oxidation reaction for 10min, then add 0.54g of ferric sulfate for precipitation Reaction for 20min, after centrifugation, Tl-free ammonium rhenate solution was obtained; the mass content of Tl in the ammonium rhenate was 0.09%;

[0035] Step 2. Concentrate and crystallize the Tl-free ammonium rhenate solution obtained in step 1 to obtain ammonium rhenate crystals, then place the ammonium rhenate crystals in a closed tube furnace, heat to 500° C. and feed oxygen to carry out Oxidize and volatilize, and then absorb the volatilized gas with pure water to obtain a perrhenic acid solution;

[0036] Step 3, using C160 type cation exchange resin to exchange and remove impurities from the perrhenic acid solution obtained in step...

Embodiment 3

[0042] This embodiment includes the following steps:

[0043] Step 1. Dissolve 72.1g of ammonium rhenate in 1000mL of pure water to obtain an ammonium rhenate solution, then adjust the pH of the ammonium rhenate solution to 10, add 6g of sodium chlorate for oxidation reaction for 40min, and then add 0.92g of polymerized chloride Aluminum precipitation reaction 30min, obtain the ammonium rhenate solution not containing Tl after centrifugation; The mass content of Tl in the ammonium rhenate is 0.08%;

[0044] Step 2. Concentrate and crystallize the Tl-free ammonium rhenate solution obtained in step 1 to obtain ammonium rhenate crystals, then place the ammonium rhenate crystals in a closed tube furnace, heat to 600° C. and feed oxygen to carry out Oxidize and volatilize, and then absorb the volatilized gas with pure water to obtain a perrhenic acid solution;

[0045] Step 3, using 001×7 type cation exchange resin to exchange and remove impurities from the perrhenic acid solution...

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Abstract

The invention discloses a preparation method of high purity ammonium rhenate, the method comprises the following steps of S1, dissolving ammonium rhenate in pure water to obtain an ammonium rhenate solution and adjusting pH value to 7 to 10, then performing oxidation and precipitation in sequence, and centrifuging to obtain an ammonium rhenate solution without containing TI; S2, after performing concentration and crystallization on the ammonium rhenate solution without containing TI, performing oxidation volatilization to obtain a perrhenic acid solution; S3, exchanging the perrhenic acid solution by adopting a cation exchange resin for removing impurities; S4, adding ammonia water into the perrhenic acid solution subjected to adsorption and impurities removal and performing concentrationand crystallization to obtain the high purity ammonium rhenate. According to the preparation method of the high purity ammonium rhenate disclosed by the invention, TI<+> in the ammonium rhenate solution is oxidized into TI<3+>, a harmful impurity TI is removed through a synergistic effect of hydrolytic precipitation of TI<3+> and adsorption packaging of a flocculating agent, then trace TI and other impurity elements are removed through oxidation volatilization, ion exchange and concentration crystallization to obtain the high purity ammonium rhenate with low TI content, the high purity ammonium rhenate meets the requirements of rhenium with low TI content in aeronautical material.

Description

technical field [0001] The invention belongs to the technical field of ammonium rhenate purification, and in particular relates to a preparation method of high-purity ammonium rhenate. Background technique [0002] Rhenium is a kind of scattered metal, which has the characteristics of high melting point, high hardness, and strong plasticity, and its compounds have excellent catalytic properties, and are widely used in petroleum, chemical, aerospace, aviation and other fields. The world reserve of rhenium is about 2500t, while the reserves of rhenium in our country are only 237t. With the development of aerospace industry, the importance of rhenium has become more and more prominent. With the increasing maturity of my country's aero-engine technology, the demand for rhenium in aero-engine manufacturing will increase significantly. In the future, the consumption of rhenium in my country will be 10t / year to 20t / year. Due to the low level of comprehensive utilization of rhenium...

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 陈昆昆操齐高张卜升郑晶孟晗琪
Owner NORTHWEST INSTITUTE FOR NON-FERROUS METAL RESEARCH
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