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Carbon-based asymmetric naphthalene-containing double-crown supramolecular hybrid material, and preparation method and application thereof

A hybrid material, asymmetric technology, applied in chemical instruments and methods, radioactive purification, other chemical processes, etc., can solve the problems of poor radiation resistance and chemical stability, decreased saturation capacity, large equipment scale, etc., to achieve radiation resistance. The effect of strong chemical stability, large capacity and distribution coefficient, and high distribution coefficient

Inactive Publication Date: 2019-08-30
EAST CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The solvent extraction process has significant advantages such as high extraction capacity and strong selectivity for Cs(I), but it also has the following disadvantages: the extractant, diluent and phase modifier are easily hydrolyzed and radiolyzed, resulting in a large amount of secondary waste liquid; The process requires multi-step extraction, washing and stripping; the equipment used is large-scale and the amount of organic reagents used is large
However, the extraction chromatography based on silicon-based supramolecular recognition materials has the following disadvantages: (1) calixaryncrown and matrix are physically loaded, the load is small, and the combination is not firm; (2) radiation resistance and chemical stability are relatively low. Poor, such as at 3.0mol·L -1 In nitric acid system, Calix[4]arene-R14 / SiO 2 -P is irradiated by 150Gy, and the saturation capacity of cesium adsorption decreases by 45%; (3) Due to the small particle size of the matrix, the column pressure is relatively high when the high-level waste liquid flows through the chromatographic column, and an additional pressure of 0.25-0.35MPa needs to be applied

Method used

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  • Carbon-based asymmetric naphthalene-containing double-crown supramolecular hybrid material, and preparation method and application thereof
  • Carbon-based asymmetric naphthalene-containing double-crown supramolecular hybrid material, and preparation method and application thereof
  • Carbon-based asymmetric naphthalene-containing double-crown supramolecular hybrid material, and preparation method and application thereof

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preparation example Construction

[0096] The embodiment of the present invention discloses a preparation method of a carbon-based asymmetric naphthobicrown-containing supramolecular hybrid material, which specifically includes the following steps:

[0097] (1) Synthesize tert-butyl calix[4]arene first, and then synthesize calix[4]arene from tert-butyl calix[4]arene

[0098] (a) Synthesis of tert-butylcalix[4]arene

[0099] Put 40-60g of tert-butylphenol, 35-45mL of 10-15mol / L formaldehyde aqueous solution and 1.0-1.5g of sodium hydroxide into a three-necked flask under the condition of 15-25°C, and add diphenyl ether solvent, Introduce argon, and dissolve the tert-butylphenol under the heating condition of 30-50°C, then raise the temperature to 90-100°C and heat to reflux for 0.5-2h, and continue to heat up to 105-115°C and heat to reflux for 2-3h;

[0100] Next, after the reaction was completed, the water in the reaction system was distilled off with nitrogen gas, then 600-1000 mL of ethyl acetate was added ...

Embodiment 1

[0128] Embodiment 1 of the present invention discloses a preparation method of a carbon-based asymmetric naphthobicrown-containing supramolecular hybrid material, which specifically includes the following steps:

[0129] (1) Synthesize tert-butyl calix[4]arene first, and then synthesize calix[4]arene from tert-butyl calix[4]arene

[0130] (a) Synthesis of tert-butylcalix[4]arene

[0131] Put 40g of tert-butylphenol, 35mL of 10mol / L aqueous formaldehyde solution and 1.0g of sodium hydroxide into a three-necked flask at 15°C, add diphenyl ether solvent, pass in argon, and heat at 30°C Dissolve tert-butylphenol under certain conditions, then heat up to 90°C and heat to reflux for 0.5h, then continue to heat up to 105°C and heat to reflux for 2h;

[0132] Then, after the reaction was completed, the water in the reaction system was distilled off with nitrogen, and then 600 mL of ethyl acetate was added and stirred for 0.5 h, and finally tert-butyl-calix[4]arene was obtained after ...

Embodiment 2

[0160] Embodiment 2 of the present invention discloses a preparation method of a carbon-based asymmetric naphthobicrown-containing supramolecular hybrid material, which specifically includes the following steps:

[0161] (1) Synthesize tert-butyl calix[4]arene first, and then synthesize calix[4]arene from tert-butyl calix[4]arene

[0162] (a) Synthesis of tert-butylcalix[4]arene

[0163] At 25°C, put 60g of tert-butylphenol, 45mL of 15mol / L aqueous formaldehyde and 1.5g of sodium hydroxide into a three-necked flask, add diphenyl ether solvent, pass in argon, and heat at 50°C Dissolve tert-butylphenol under certain conditions, then heat up to 100°C and heat to reflux for 2 hours, then continue to heat up to 115°C and heat to reflux for 3 hours;

[0164] Then, after the reaction was completed, the water in the reaction system was distilled off with nitrogen, and then 1000 mL of ethyl acetate was added and stirred for 1.0 h, and finally tert-butyl-calix[4]arene was obtained afte...

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Abstract

The invention discloses a carbon-based asymmetric naphthalene-containing double-crown supramolecular hybrid material. The material is prepared by directionally polymerizing calix[4]arene-(naphtho)crown-6-(benzyl methacrylate)crown-6 to inner and outer pore walls of millimeter-scale macroporous-mesoporous carbon spheres, and the structural formula of the calix[4]arene-(naphtho)crown-6-(benzyl methacrylate)crown-6 is as the follows. The invention discloses a preparation method of the carbon-based asymmetric naphthalene-containing double-crown supramolecular hybrid material. The preparation method is simple, and the obtained carbon-based asymmetric naphthalene-containing double-crown supramolecular hybrid material can be used for adsorbing and separating radionuclide Cs in high level liquid waste and has an excellent adsorption separation effect.

Description

technical field [0001] The present invention relates to the technical field of nuclear fuel reprocessing technology, and more specifically relates to a carbon-based asymmetric naphthobicrown-containing supramolecular hybrid material and its preparation method and application. Background technique [0002] The reprocessing of high-level liquid waste (HLLW) is one of the key links in the nuclear fuel cycle, and it is also a worldwide problem, which is of great significance to the sustainable development of nuclear power. HLLW contains a large number of radionuclides, of which 135 Cs has a long half-life, is easy to migrate, and has great potential harm to the environment; 137 Although Cs has a short half-life, it will release a lot of heat during the decay process, which is one of the most dangerous elements that affect the safe disposal of solidified bodies. If it can be separated, it can not only reduce the volume of the solidified body, shorten the cooling time and storag...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26C02F1/28G21F9/12B01J20/30
CPCB01J20/26C02F1/285C02F2101/006G21F9/12
Inventor 张志宾刘云海柳玉辉曹小红戴荧王有群
Owner EAST CHINA UNIV OF TECH
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