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An amidoxime-based porous framework material, its preparation method and its application in adsorption and separation of uranium ions

A skeleton material and porous skeleton technology, applied in chemical instruments and methods, adsorption water/sewage treatment, other chemical processes, etc., can solve problems such as unsatisfactory adsorption effect of uranium ions

Active Publication Date: 2022-04-15
NORTHEAST NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, people study the adsorption of uranium through porous materials, but the adsorption effect of porous materials in the prior art on uranium ions is not ideal

Method used

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  • An amidoxime-based porous framework material, its preparation method and its application in adsorption and separation of uranium ions
  • An amidoxime-based porous framework material, its preparation method and its application in adsorption and separation of uranium ions
  • An amidoxime-based porous framework material, its preparation method and its application in adsorption and separation of uranium ions

Examples

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preparation example Construction

[0025] The invention provides a method for preparing an amidoxime-based porous framework material, comprising the following steps:

[0026] (1) Carrying out Sholl reaction of aromatic cyano compound and aromatic compound under the action of catalyst to obtain cyano porous skeleton material; the catalyst is activated aluminum chloride;

[0027] (2) Carrying out amidoximation reaction of the cyano-based porous framework material obtained in the step (1), hydroxylamine hydrochloride and triethylamine to obtain the amidoxime-based porous framework material.

[0028] In the invention, the aromatic cyano compound and the aromatic compound are subjected to Shorer reaction under the action of a catalyst to obtain a cyano porous framework material.

[0029] In the present invention, the aromatic cyano compound preferably includes one or more of benzonitrile, 4-cyanobiphenyl, terephthalonitrile and 4,4'-biphenyldinitrile; the aromatic Compounds preferably include benzene, biphenyl, o-t...

Embodiment 1

[0041] Add 500 mg of aluminum trichloride to the round bottom flask, vacuumize the flask, fill with nitrogen, then inject chloroform, and heat to 60° C. for 3 hours. Then add the chloroform solution of benzonitrile and biphenyl (ratio: 1:4) into the round-bottomed flask, and keep it at 60°C for 21 hours. After the reaction is completed and cooled, it is filtered, and the crude product obtained by filtration is washed with 1mol / L HCl solution treatment, followed by Soxhlet extraction with methanol, tetrahydrofuran and chloroform, respectively. Next, the obtained product was heated to 80° C. for 24 hours in a vacuum environment to obtain a cyano-based porous framework material. 200 mg of the cyano porous framework material was taken out and uniformly dispersed in ethanol, 0.5 g of hydroxylamine hydrochloride and 0.75 g of triethylamine were added, and then heated to 70° C. for 48 hours. After the reaction is cooled and filtered, the obtained product is first treated with 1mol / L...

Embodiment 2

[0044] Add 500 mg of aluminum trichloride to the round bottom flask, vacuumize the flask, fill with nitrogen, then inject chloroform, and heat to 60° C. for 3 hours. Then add the chloroform solution of benzonitrile and biphenyl (ratio: 1:2) into the round-bottomed flask, and keep it at 60°C for 21 hours. After the reaction is completed and cooled, filter, and the crude product obtained by filtration is washed with 1mol / L HCl solution treatment, followed by Soxhlet extraction with methanol, tetrahydrofuran and chloroform, respectively. Next, the obtained product was heated to 80° C. for 24 hours in a vacuum environment to obtain a cyano-based porous framework material. 200 mg of the cyano porous framework material was taken out and uniformly dispersed in ethanol, 0.5 g of hydroxylamine hydrochloride and 0.75 g of triethylamine were added, and then heated to 70° C. for 48 hours. After the reaction is cooled and filtered, the obtained product is first treated with 1mol / L NaOH so...

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Abstract

The invention provides an amidoxime-based porous framework material, its preparation method and its application in adsorption and separation of uranium ions. The preparation method of the amidoxime-based porous framework material provided by the present invention comprises the following steps: performing Sholl reaction on an aromatic cyano compound and an aromatic compound under the action of a catalyst to obtain a cyano-based porous framework material; the catalyst is activated chlorination Aluminum; subjecting the cyano-based porous framework material, hydroxylamine hydrochloride and triethylamine to an amidoximylation reaction to obtain the amidoxime-based porous framework material. The amidoxime-based porous framework material provided by the invention has good structural stability and chemical stability, and has a high adsorption capacity for uranium ions. The results of the examples show that the amidoxime-based porous framework material provided by the present invention can adsorb up to 703 mg·g of uranium ions ‑1 .

Description

technical field [0001] The invention relates to the field of functional materials, in particular to an amidoxime-based porous framework material, a preparation method thereof and an application in adsorption and separation of uranium ions. Background technique [0002] As a clean, safe and efficient energy source, nuclear energy plays an irreplaceable role in ensuring global energy security and addressing climate change. The International Atomic Energy (IAEA) and other agencies predict that in the next few decades, the energy generated by uranium nuclear fission will become the main energy source in the world. Uranium is the main raw material for nuclear power generation. With the rapid development of the nuclear power industry, uranium resources that are easier to mine on land will be exhausted in the next few decades. The content of dissolved uranium in seawater is as high as 4.5 billion tons. Efficient and large-scale enrichment of uranium from seawater will greatly redu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/22B01J20/30C02F1/28C02F103/08
CPCB01J20/22B01J20/3085C02F1/285C02F2103/08
Inventor 朱广山元野李樟楠
Owner NORTHEAST NORMAL UNIVERSITY
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