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Carbon-based asymmetric double-crown supermolecule hybrid material and preparation method and application thereof

A hybrid material and asymmetric technology, applied in chemical instruments and methods, radioactive purification, other chemical processes, etc., can solve diluents and phase modifiers that are easy to hydrolyze and radiolyze, poor stability of silicon-based supramolecular recognition materials, Problems such as radiation resistance and poor chemical stability, to achieve excellent cesium ion selectivity, stable complexes, large capacity and distribution coefficient

Inactive Publication Date: 2019-08-30
EAST CHINA UNIV OF TECH
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Problems solved by technology

Among them, the solvent extraction process has high extraction capacity and strong selectivity for Cs(I), but there are also obvious shortcomings: the extractant, diluent and phase modifier are easy to hydrolyze and radiolyze, resulting in a large amount of secondary waste liquid; the operation process requires Perform multi-step extraction, washing and stripping; the scale of equipment used is large and the amount of organic reagents used is large
However, there are still obvious deficiencies in the extraction chromatography based on silicon-based supramolecular recognition materials: (1) Calixaryl crown ether and the matrix are physically loaded, the load is small, and the combination is weak; (2) Radiation resistance and chemical stability 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: (4 The calixaryl crown ether adopted in ) has a calixaryl single-crown structure or a symmetrical calix[4]-double crown-6 structure, and the calixaryl single-crown structure is compared with the calixaryl double-crown structure, and the cesium ion selectivity is poor; while the symmetrical calix[4] ]-bicrown-6 structure has poor selectivity in separating Cs(I) compared with asymmetric calix[4]arene-bicrown-6, and the silicon-based supramolecular recognition material formed with the matrix has poor stability

Method used

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  • Carbon-based asymmetric double-crown supermolecule hybrid material and preparation method and application thereof
  • Carbon-based asymmetric double-crown supermolecule hybrid material and preparation method and application thereof
  • Carbon-based asymmetric double-crown supermolecule hybrid material and preparation method and application thereof

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preparation example Construction

[0096] A method for preparing a carbon-based asymmetric double-corona supramolecular hybrid material according to an embodiment of the present invention is characterized in that it specifically includes the following steps:

[0097] (1) Synthesis of tert-butylcalix[4]arenes by tert-butylphenol, aqueous formaldehyde and sodium hydroxide:

[0098] First, under the condition of 15-25°C, put 40-60g of tert-butylphenol, 30-40mL of 13-15mol / L formaldehyde aqueous solution and 1-2g of sodium hydroxide into a three-necked flask, pass in argon, and Dissolve tert-butylphenol under heating at ~45°C, then heat up to 95~100°C and heat to reflux for 0.5 to 1.5 hours, then continue to heat up to 100 to 120°C and heat to reflux for 2 to 3 hours;

[0099] Then, after the reaction was completed, the water in the reaction system was distilled off with nitrogen gas, and then 700-900 mL of ethyl acetate was added and stirred for 0.2-0.8 h, and finally tert-butyl-calix[4]arene was obtained after st...

Embodiment 1

[0129] Embodiment 1 of the present invention is a method for preparing a carbon-based asymmetric double-corona supramolecular hybrid material, which is characterized in that it specifically includes the following steps:

[0130] (1) Synthesis of tert-butylcalix[4]arenes by tert-butylphenol, aqueous formaldehyde and sodium hydroxide:

[0131] First, under the condition of 15°C, put 40g of tert-butylphenol, 30mL of 13mol / L aqueous formaldehyde and 1g of sodium hydroxide into a three-necked flask, pass in argon gas, and make the tert-butylphenol Dissolve, then heat up to 95°C and heat to reflux for 0.5h, continue to heat up to 100°C and heat to reflux for 2h;

[0132] Next, after the reaction was completed, the water in the reaction system was distilled off with nitrogen, and then 700 mL of ethyl acetate was added and stirred for 0.2 h, and finally tert-butyl-calix[4]arene was obtained after standing, filtering and washing.

[0133] (2) prepare calix [4] arene by reaction of anh...

Embodiment 2

[0162] Embodiment 2 of the present invention is a method for preparing a carbon-based asymmetric double-corona supramolecular hybrid material, which is characterized in that it specifically includes the following steps:

[0163] (1) Synthesis of tert-butylcalix[4]arenes by tert-butylphenol, aqueous formaldehyde and sodium hydroxide:

[0164] First, at 25°C, put 60g of tert-butylphenol, 40mL of 15mol / L aqueous formaldehyde and 2g of sodium hydroxide into a three-necked flask, pass in argon, and make tert-butylphenol Dissolve, then heat up to 100°C and heat to reflux for 1.5h, then continue to heat up to 120°C and heat to reflux for 3h;

[0165] Next, after the reaction was completed, the water in the reaction system was distilled off with nitrogen, and then 900 mL of ethyl acetate was added and stirred for 0.8 h, and finally tert-butyl-calix[4]arene was obtained after standing, filtering and washing.

[0166] (2) prepare calix [4] arene by reaction of anhydrous toluene, phenol...

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Abstract

The invention discloses a carbon-based asymmetric double-crown supermolecule hybrid material, which is prepared by directionally polymerizing calix [4]arene-crown-6-(benzyl methacrylate)crown-6 onto the inner and outer hole walls of a millimeter-sized macroporous-mesoporous carbon sphere, wherein the structural formula of the calix [4]arene-crown-6-(benzyl methacrylate)crown-6 is shown in the specification. The invention also discloses a preparation method of the carbon-based asymmetric double-crown supermolecule hybrid material, the preparation method is simple, and the obtained carbon-basedasymmetric double-crown supermolecule hybrid material can be used for adsorbing and separating radionuclide Cs and has excellent adsorption and separation effects.

Description

technical field [0001] The invention relates to the technical field of nuclear fuel reprocessing technology, and more specifically relates to a carbon-based asymmetric double-corona supramolecular hybrid material and its preparation and application. Background technique [0002] The reprocessing of high-level liquid waste (HLLW) is 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 storage life, but also simplify the geological disposal process and save costs. Therefore, how ...

Claims

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Application Information

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IPC IPC(8): B01J20/22C02F1/28G21F9/12B01J20/30
CPCB01J20/22C02F1/285G21F9/125C02F2101/006
Inventor 张志宾刘云海戴荧柳玉辉曹小红王有群
Owner EAST CHINA UNIV OF TECH
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