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Millimeter-scale macroporous-mesoporous carbon sphere/cup [4]-double crown-6 interpenetrating composite material and preparation method and application thereof

A composite material and mesoporous carbon technology, applied in chemical instruments and methods, other chemical processes, water/sewage treatment, etc., can solve the problems of radiation resistance and poor chemical stability, large equipment scale, large column pressure, etc., to achieve Strong radiation resistance and chemical stability, large capacity and distribution coefficient, and simple solid-liquid separation

Inactive Publication Date: 2020-08-28
EAST CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The solvent extraction process has 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 operation process requires multiple 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 deficiencies: (1) Calixaryl crown ether and silicon-based are physically loaded, with a small load and weak combination; (2) radiation resistance and chemical stability Poor; (3) Due to the small particle size of the matrix, the column pressure is relatively high when the high-level radioactive waste liquid flows through the chromatographic column, and an additional pressure of 0.25-0.35 MPa needs to be applied; (3) The calix aromatic crown ether used has a calix aromatic single crown structure , compared with the calixarene double-crown structure, the selectivity of cesium ions is poor, which leads to the poor application effect of the obtained silicon-based supramolecular recognition materials in the process of separation of high-level radioactive waste liquid by extraction chromatography

Method used

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  • Millimeter-scale macroporous-mesoporous carbon sphere/cup [4]-double crown-6 interpenetrating composite material and preparation method and application thereof
  • Millimeter-scale macroporous-mesoporous carbon sphere/cup [4]-double crown-6 interpenetrating composite material and preparation method and application thereof
  • Millimeter-scale macroporous-mesoporous carbon sphere/cup [4]-double crown-6 interpenetrating composite material and preparation method and application thereof

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Effect test

Embodiment 1

[0119] The embodiment of the present invention discloses a preparation method of a millimeter-scale macroporous-mesoporous carbon ball / cup[4]-double crown-6 interpenetrating composite material, which specifically includes the following steps:

[0120] (1) Synthesize tert-tert-butylcalix[4]arene from tert-tert-butylphenol, aqueous formaldehyde solution and sodium hydroxide first; [4] Arene reaction to prepare calix[4]arene:

[0121] (a) Synthesis of tert-butylcalix[4]arene

[0122] First, under the condition of 15°C, 40g of tert-tert-butylphenol, 35mL of 10mol / L aqueous formaldehyde solution and 1.0g of sodium hydroxide were placed in a three-necked flask, and diphenyl ether solvent was added, and argon was introduced, and heated at 30°C Under the conditions, the tert-butylphenol was dissolved, then the temperature was raised to 90 °C and heated to reflux for 0.5 h, and then the temperature was continued to be heated to 105 °C and heated to reflux for 2 h;

[0123] Next, after ...

Embodiment 2

[0162] Embodiment 2 of the present invention discloses a preparation method of a millimeter-scale macroporous-mesoporous carbon sphere / cup[4]-dual-crown-6 interpenetrating composite material, which specifically includes the following steps:

[0163] (1) Synthesize tert-butyl calix[4]arene from tert-tert-butyl phenol, aqueous formaldehyde solution and sodium hydroxide first; [4] Arene reaction to prepare calix[4]arene:

[0164] (a) Synthesis of tert-butylcalix[4]arene

[0165] Under the condition of 25°C, 60g of tert-tert-butylphenol, 45mL of 15mol / L aqueous formaldehyde solution and 1.5g of sodium hydroxide were placed in a three-necked flask, and a diphenyl ether solvent was added, and argon was introduced, and heated at 50°C Under the conditions, the tert-butylphenol was dissolved, then the temperature was raised to 100 °C and heated to reflux for 2 hours, and then the temperature was continued to be heated to 115 °C and heated to reflux for 3 hours;

[0166] Next, after t...

Embodiment 3

[0205] Embodiment 3 of the present invention discloses a method for preparing a millimeter-scale macroporous-mesoporous carbon sphere / cup[4]-dual-crown-6 interpenetrating composite material, which specifically includes the following steps:

[0206] (1) Synthesize tert-tert-butylcalix[4]arene from tert-tert-butylphenol, aqueous formaldehyde solution and sodium hydroxide first; [4] Arene reaction to prepare calix[4]arene:

[0207] (a) Synthesis of tert-butylcalix[4]arene

[0208] Under the condition of 18°C, 48g of tert-tert-butylphenol, 38mL of 12mol / L aqueous formaldehyde solution and 1.3g of sodium hydroxide were placed in a three-necked flask, and a diphenyl ether solvent was added, and argon was introduced, and heated at 40°C Under the conditions, the tert-butylphenol was dissolved, then the temperature was raised to 96°C and heated to reflux for 0.8h, and then the temperature was continued to rise to 109°C and heated to reflux for 2.3h;

[0209] Next, after the reaction ...

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Abstract

The invention discloses a millimeter-scale macroporous-mesoporous carbon sphere / cup [4]-double crown-6 interpenetrating composite material which is obtained by directionally polymerizing cup [4] arene-(benzo) crown-6-(phenylmethyl methacrylate) crown-6 to the inner surface and the outer surface of a millimeter-scale macroporous-mesoporous carbon sphere. The structural formula of the cup [4] arene-(benzo) crown-6-(phenylmethyl methacrylate) crown-6 is shown in the specification. The invention further discloses a preparation method of the millimeter-scale macroporous-mesoporous carbon sphere / cup[4]-double crown-6 interpenetrating composite material, the preparation method is simple, and the obtained millimeter-scale macroporous-mesoporous carbon sphere / cup [4]-double crown-6 interpenetrating composite material can be used for adsorbing and separating radionuclide Cs and is excellent in adsorption and separation effect.

Description

technical field [0001] The invention relates to the technical field of nuclear fuel post-processing technology, and more particularly to a preparation method and application of a millimeter-scale macroporous-mesoporous carbon ball / cup[4]-double crown-6 interpenetrating composite material. Background technique [0002] The reprocessing of high-level radioactive 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, among which 135 Cs has a long half-life and is easy to migrate, and has a 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, and it is one of the most dangerous elements that affects 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 th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22C02F1/28G21F9/12B01J20/30
CPCB01J20/20B01J20/22G21F9/12C02F1/283C02F1/285C02F2101/006
Inventor 张志宾刘云海曹小红柳玉辉花榕戴荧
Owner EAST CHINA UNIV OF TECH
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