A kind of mofs material that adsorbs and separates rhenium or technetium and its preparation method and application

An adsorption separation and reaction technology, applied in chemical instruments and methods, other chemical processes, organic chemistry, etc., can solve the problems of slow adsorption kinetics, poor adsorption selectivity, and low adsorption capacity, and achieve good stability and high adsorption performance. , strong selective effect

Active Publication Date: 2022-03-25
ZHEJIANG UNIV
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Problems solved by technology

[0007] Aiming at the problems of poor adsorption selectivity, slow adsorption kinetics and low adsorption capacity of pertechnetic acid adsorption materials in the prior art, the present invention provides a MOFs material for adsorbing and separating rhenium or technetium, which uses 4-(4-(pyridyl) Ethynyl)tetraphenylethylene is used as a ligand to form a cationic MOFs material af

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  • A kind of mofs material that adsorbs and separates rhenium or technetium and its preparation method and application
  • A kind of mofs material that adsorbs and separates rhenium or technetium and its preparation method and application
  • A kind of mofs material that adsorbs and separates rhenium or technetium and its preparation method and application

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Embodiment 1

[0045] (1) Weigh 1.2g of tetrabromotetraphenylethylene, 8.7mg of cuprous iodide, and 64.7mg of bis(triphenylphosphine)palladium dichloride in 70mL of mixed solvent (THF / Et 3 N, 1 / 1) to start stirring, and feed argon gas at 60°C to start bubbling to remove the oxygen in the reaction system, add 1.7g trimethylethynyl silicon to it after 1h for reaction; after 12h, the reaction is complete, and the The reaction solution was removed by distillation under pressure, followed by dichloromethane extraction, anhydrous Na 2 SO 4 Drying, distilling off the solvent under reduced pressure, and then separating and purifying by column chromatography yielded 1.2 g of intermediate A with a yield of 90.2%; the reaction equation is as follows:

[0046]

[0047] (2) The obtained intermediate A was dissolved with 50 mL of dichloromethane, and 30 mL of methanol solution containing 0.54 g of sodium hydroxide was added thereto, stirred overnight, followed by extraction with dichloromethane, anhyd...

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Abstract

The invention discloses a MOFs material for adsorbing and separating rhenium or technetium and its preparation method and application. The preparation method comprises the following steps: under the action of a catalyst, tetrakis (4-bromophenyl) ethylene and silicon trimethylacetylene are mixed in a solvent Reaction obtains 4-(2-(trimethylsilyl) ethynyl) tetraphenylethylene; reacts with sodium hydroxide again, and the obtained tetra(4-ethynylphenyl) ethylene and 4-iodopyridine act as catalysts , react in a solvent to obtain 4-(4-(pyridyl) ethynyl) tetraphenylethylene ligand, the ligand and nickel nitrate are mixed in an organic solvent, after heating and reacting, the product is filtered, washed, and dried to obtain the obtained The above MOFs materials. Because of its triple interspersed structure, compared with most adsorbed TcO 4 ‑ Due to the existence of large-sized one-dimensional channels, the material has stronger selectivity and better stability, and the structure remains unchanged after the adsorption of pertechnetate.

Description

technical field [0001] The invention relates to the technical field of nuclear fuel reprocessing, in particular to a MOFs material for adsorbing and separating rhenium or technetium, a preparation method and application thereof. Background technique [0002] As a clean and effective energy source, nuclear energy has undergone rapid development in the first half century, providing an indispensable energy supply for the country with the rapid economic growth of our country, but the strong radioactive waste it produces has gradually become a major threat to the ecological environment. threaten. Accidents, nuclear weapons experiments and nuclear accidents will produce a large amount of radioactive waste, which will have a bad impact on the environment. The radioactive product Tc-99 acts as a long-lived fission product (t 1 / 2 =2.13×10 5 Years), because it is easy to form steam and volatilize during the process of vitrification of waste, it is difficult to fix it. Pertechnetat...

Claims

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Application Information

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IPC IPC(8): C08G83/00B01J20/22C07D213/127
CPCC08G83/008B01J20/226C07D213/127
Inventor 肖成梁康康
Owner ZHEJIANG UNIV
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