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Method for separating and recovering rhenium

A technology of perrhenic acid and calixarene, applied in chemical instruments and methods, rhenium compounds, inorganic chemistry, etc., can solve the problems of complex process, poor anti-interference ability, low adsorption capacity, etc., and achieve high extraction efficiency and cost saving , the effect of high purity

Inactive Publication Date: 2014-02-05
LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

Precipitation and separation is to extract rhenium from molybdenite, which is mostly used to convert rhenium into potassium perrhenate which is insoluble in water and separate it from molybdenum. After repeated recrystallization and refining, it is reduced under high temperature and hydrogen to make metal rhenium powder. However, the process is complicated and the yield is low; in the solid phase adsorption method, the commonly used solid phase adsorbent is activated carbon, and the stability, oxygen resistance, osmotic pressure resistance, friction resistance and service life of activated carbon are all better than ion exchange resin, activated carbon Strong adsorption, certain separation selectivity, and low price, but its disadvantages are low adsorption capacity and poor anti-interference ability

Method used

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  • Method for separating and recovering rhenium

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preparation example Construction

[0024] (1) Preparation of sample solution containing rhenium: Re(VII) standard solution: Accurately weigh 1.0000g of rhenium powder dried at 105℃~110℃ for 2h in a beaker, add 10mL of hydrogen peroxide after wetting with water, heat to dissolve After complete cooling, add 30mL of hydrochloric acid, shake well, slightly boil for 20min to remove excess hydrogen peroxide, then pour into a 100mL volumetric flask and dilute to the mark to obtain a standard solution of 10mg / mL Re(VII).

[0025] Standard solution of rhenium: 0.01mg·mL -1 , Weigh 0.1000g of rhenium powder, add 10-20mL of nitric acid to a 100ml beaker, place in a heating mantle and heat slowly until completely dissolved. Then add 20ml of hydrochloric acid, heat to drive out NO 3 - Until no brown-yellow gas is emitted. Remove and cool to room temperature. Transfer to a 100ml volumetric flask, add water to dilute to the mark, and shake well. Then take 1ml of the above solution in a 100mL volumetric flask, add water t...

Embodiment 1

[0028] Dissolve 0.4mmol of calix[4]arenediethylamine mannich base in 10mL of 1mol / L hydrochloric acid solution, add dropwise to 25mL of Re(VII) standard solution under stirring, a white solid is formed, stir for 30min and then filter, spectrophotometrically Determination of rhenium content in the filtrate.

[0029] Add the white solid obtained above to 10mL of 1mol / L NH 3 ·H 2 In O, keep pH = 10, heat and stir, there is still precipitation in the system, stop stirring and heating after about 30 minutes of reaction, carry out solid-liquid separation, take out 1mL of liquid, measure the concentration of rhenium in the solution according to the above method, and calculate the concentration of rhenium content, the recovery rate is about 85.7%. Then the liquid is further concentrated to finally obtain white crystals of ammonium perrhenate; the solid is filtered, washed and dried to finally obtain calix[4]arene diethylamine mannich base again.

Embodiment 2

[0031] Dissolve 0.4 mmol of calix[4]arene dimethylamine mannich base in 10 mL of 1mol / L hydrochloric acid solution, add dropwise to 25 mL of the standard solution of Re(VII) under stirring, a white solid is formed, stir for 30 min, filter, and spectrophotometrically Determination of rhenium content in the filtrate.

[0032] Add the white solid obtained above to 10mL of 1mol / L NH 3 ·H 2 In O, keep pH=10, heat and stir, there is still precipitation in the system, stop stirring and heating after reacting for about 30min, carry out solid-liquid separation, take out 1mL of liquid, measure the content of rhenium in the solution according to the above method, the recovery rate is about was 82.4%. Then the liquid is further concentrated to finally obtain white crystals of ammonium perrhenate; the solid is filtered, washed and dried to finally obtain calix[4]arene dimethylamine mannich base again.

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Abstract

The invention belongs to the field of separation and reclamation of dispersed elements, and particularly relates to a method for separating and recovering a rhenium element. The method comprises the following steps: transforming a sample containing rhenium into a perrhenic acid ReO4<-> solution; enabling mannich alkali of calixarene to react with perrhenic acid ReO4<-> under an acid condition, so as to generate a white precipitate of perrhenic acid calixarenes ammonium salt; enabling the white precipitate of the perrhenic acid calixarenes ammonium salt to react under an alkaline condition; degrading the product into the perrhenic acid ReO4<-> and the mannich alkali of calixarene; concentrating the perrhenic acid ReO4<-> dissolved into the alkali; finally separating out perrhenate; recycling the calixarene mannich alkali after filtering. The method disclosed by the invention is simple, low in cost, free of pollution, and high in yield; no organic solvent is used in an operation process, and the pH value is controlled, so as to achieve the targets of separation and recovery. The reagent calixarene mannich alkali for recovery can be recycled.

Description

technical field [0001] The invention belongs to the technical field of separation, recovery and utilization of rare elements, and in particular relates to a method for separation and recovery of rhenium elements. Background technique [0002] Rhenium (Re) is the latest important element discovered in the rare element (RSE) group, which belongs to a kind of precious rare metal element, and its content is very small in the earth's crust. Rhenium has high hardness, corrosion resistance, wear resistance and good ductility. It is widely used in national defense and aerospace, ultra-high temperature emission, and thermionic materials for special lamps. In the electronic structure of rhenium, the 5 electrons of the unsaturated 4d layer are easy to release, and the 2 electrons of the 6s layer are easy to participate in the interaction to form a covalent bond. In addition, its lattice parameters are large, so rhenium and its compounds It has excellent catalytic activity and is used ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G47/00
Inventor 陈平臧树良吴爽周明东赵群力刘丽梅
Owner LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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