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Millimeter-scale macroporous-mesoporous carbon sphere/calix[4]-crown-6 hybrid material, and preparation method and application thereof

A hybrid material, mesoporous carbon technology, applied in chemical instruments and methods, radioactive purification, other chemical processes, etc., can solve the problems of easy hydrolysis and radiolysis of diluents and phase modifiers, poor radiation resistance and chemical stability, Problems such as large amount of organic reagents are used to achieve the effect of large capacity and distribution coefficient, high distribution coefficient and large load

Inactive Publication Date: 2019-09-24
EAST CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the solvent extraction process has significant advantages, 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 operation process requires multi-step extraction, washing and stripping; The scale of equipment used is large 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) Calixaryl crown ether and the matrix are physically loaded, the load is small, and the combination is not firm; (2) The 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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  • Millimeter-scale macroporous-mesoporous carbon sphere/calix[4]-crown-6 hybrid material, and preparation method and application thereof
  • Millimeter-scale macroporous-mesoporous carbon sphere/calix[4]-crown-6 hybrid material, and preparation method and application thereof
  • Millimeter-scale macroporous-mesoporous carbon sphere/calix[4]-crown-6 hybrid material, and preparation method and application thereof

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Embodiment 1

[0106] Embodiment 1 of the present invention discloses a preparation method of a millimeter-scale macroporous-mesoporous carbon sphere / cup[4]-crown-6 hybrid material, specifically comprising the following steps:

[0107] (1) Synthesis of tert-butylcalix[4]arenes by tert-butylphenol, aqueous formaldehyde and sodium hydroxide:

[0108] 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;

[0109] Then, after the reaction was completed, the water in the reaction system was distilled off by nitrogen gas, and then 600 mL of ethyl acetate was added and stirred for 0.5 h. Finally, tert-butyl-calix[4]arene was obtained after standing, filtering and washing.

[0110] (2) Preparatio...

Embodiment 2

[0130] The embodiment of the present invention discloses a method for preparing a millimeter-scale macroporous-mesoporous carbon sphere / cup[4]-crown-6 hybrid material, which specifically includes the following steps:

[0131] (1) Synthesis of tert-butylcalix[4]arenes by tert-butylphenol, aqueous formaldehyde and sodium hydroxide:

[0132] 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;

[0133] 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 after standing, filtering and washing.

[0134] (2) Pr...

Embodiment 3

[0154] The embodiment of the present invention discloses a method for preparing a millimeter-scale macroporous-mesoporous carbon sphere / cup[4]-crown-6 hybrid material, which specifically includes the following steps:

[0155] (1) Synthesis of tert-butylcalix[4]arenes by tert-butylphenol, aqueous formaldehyde and sodium hydroxide:

[0156] At 22°C, put 48g of tert-butylphenol, 38mL of 14mol / L formaldehyde solution and 1.4g of sodium hydroxide into a three-necked flask, add diphenyl ether solvent, pass in argon, and heat at 39°C Dissolve tert-butylphenol under certain conditions, then heat up to 98°C and heat to reflux for 0.7h, then continue to heat up to 109°C and heat to reflux for 2.5h;

[0157] Then, after the reaction was completed, the water in the reaction system was distilled off with nitrogen, and then 800 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.

[0158] (2) Preparati...

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Abstract

The invention discloses a millimeter-scale macroporous-mesoporous carbon sphere / calix[4]-crown-6 hybrid material. The millimeter-scale macroporous-mesoporous carbon sphere / calix[4]-crown-6 hybrid material is obtained by directionally polymerizing propenyl calix[4]arene-crown-6 onto the inner and outer pore walls of a millimeter-scale macroporous-mesoporous carbon sphere, wherein the propenyl calix[4]arene-crown-6 has a structural formula which is described in the specification. The invention also discloses a preparation method for the millimeter-scale macroporous-mesoporous carbon sphere / calix[4]-crown-6 hybrid material. The preparation method provided by the invention is simple; and the millimeter-scale macroporous-mesoporous carbon sphere / calix[4]-crown-6 hybrid material prepared by using the preparation method provided by the invention can be used for adsorption and separation of radionuclide Cs in a high-level liquid waste, and has excellent adsorption and separation effects.

Description

technical field [0001] The present invention relates to the technical field of nuclear fuel reprocessing technology, and more specifically relates to a preparation method and application of a millimeter-scale macroporous-mesoporous carbon sphere / cup[4]-crown-6 hybrid material. 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 affecting 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...

Claims

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Application Information

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IPC IPC(8): B01J20/22C02F1/28G21F9/12B01J20/30
CPCB01J20/20B01J20/22C02F1/285C02F2101/006G21F9/12
Inventor 张志宾刘云海董志敏戴荧柳玉辉曹小红
Owner EAST CHINA UNIV OF TECH
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