Sulfonyl bridged calix[4]arene iron-based porous complex for extracting uranium from seawater and preparation method of complex

A technology of sulfonyl bridges and complexes, applied in the field of metal porous complex materials, can solve the problems of low specific surface area, limited adsorption capacity and selectivity of materials, and achieve large specific surface area, fast adsorption rate and good water stability Effect

Inactive Publication Date: 2021-08-27
HAINAN UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Calixarene is a kind of cyclic compound obtained by the condensation reaction of phenol units. The phenolic hydroxyl group and bridging atoms at the lower edge of the calixarene structure serve as potential coordination points, which can bind and coordinate with other ligands. Research attempts to apply calixarene derivatives to metal ion extraction, but the specific surface area of ​​the material is low, and the adsorption capacity and selectivity are limited

Method used

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  • Sulfonyl bridged calix[4]arene iron-based porous complex for extracting uranium from seawater and preparation method of complex
  • Sulfonyl bridged calix[4]arene iron-based porous complex for extracting uranium from seawater and preparation method of complex
  • Sulfonyl bridged calix[4]arene iron-based porous complex for extracting uranium from seawater and preparation method of complex

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Embodiment 1

[0022] Embodiment 1: A method for preparing a sulfonyl bridged calix[4]arene iron-based porous complex for extracting uranium from seawater, comprising the following steps:

[0023] (1) Preparation of sulfonyl bridged calix[4]arene

[0024] Weigh (1.38mmol, 5g) p-tert-butylthiacalix [4] arene (H 4 TC4A) was placed in a 500mL round bottom flask and dissolved with 150mL of chloroform. After complete dissolution, sodium perborate (0.13mol, 11g) and glacial acetic acid (250mL) were added, placed in an oil bath at 50°C and heated to reflux for 18h, then cooled to room temperature. Then extract with 400mL distilled water and 450mL chloroform in sequence. The extracted solution was recrystallized to obtain sulfonyl bridged calix[4]arene with a yield of 80%.

[0025] (2) isophthalonitrile tetrazole (H 2 L) preparation

[0026] Take isophthalonitrile (20mmol, 2.564g), sodium azide (120mmol, 7.8g) and triethylamine hydrochloride (120mmol, 16.47g) and place in a 250mL round bottom f...

Embodiment 2

[0029] Embodiment two: The difference between embodiment two and embodiment one is that the single crystal cultivation solvent adopted in step (3) is methanol, ethanol, N,N-dimethylformamide (DMF), N,N-di Methylacetamide (DMA) and mixed solvents in different proportions, the results are shown in Table 1, which shows that only when the ratio of ethanol and N,N-dimethylformamide (DMF) is 1:1, brownish yellow blocky crystals can be obtained .

[0030] The impact on material crystallization performance under the condition of table 1 different reaction solvents

[0031]

Embodiment 3

[0032] Embodiment three: the difference between embodiment three and embodiment one is that the sulfonyl bridging calix[4]arene adopted in step (3), the molar ratio of iron trichloride and isophthalonitrile tetrazole is different. The results are shown in Table 2. When H 4 TC4A-SO 2 : FeCl 3 :H 2 When L=1:4:1, brownish-yellow block crystals can be obtained.

[0033] The impact of the input molar ratio of different raw materials in table 2 on product crystallization

[0034]

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Abstract

The invention discloses a preparation method of a sulfonyl bridged calix[4]arene iron-based porous complex for extracting uranium from seawater, which comprises the following steps: adding sulfonyl bridged calix[4]arene, ferric trichloride and isophthalonitrile tetrazole into a composite solvent containing ethanol and N,N-dimethylformamide, and uniformly conducting mixing; and then rapidly conducting heating in a reaction kettle, conducting reacting under a constant temperature condition, slowly conducting cooling to obtain a brown yellow blocky transparent crystal, and conducting cleaning and drying to obtain a product, wherein the molar ratio of the sulfonyl bridged calix[4]arene to the ferric trichloride to the isophthalonitrile tetrazole is 1:4:1, and the volume ratio of the ethanol to the N,N-dimethylformamide is 1:1. The porous complex material prepared by the method is a monoclinic crystal, has a cuboid structure with a cavity, and has a molecular formula of Fe4(H2O)(TC4A-SO2)]4(H2L)8. The material has a proper pore structure, unsaturated coordination sites in the bridged ligand isophthalonitrile tetrazole and uranyl ions have a complexing effect, the uranium extraction performance of the material is enhanced through mutual synergism of the unsaturated coordination sites and the uranyl ions, and the material has the advantages of being high in adsorption rate, excellent in selectivity and stability and the like.

Description

technical field [0001] The invention relates to a metal porous complex material, in particular to a sulfonyl bridging calix[4]arene iron-based porous complex for uranium extraction from seawater and a preparation method thereof. Background technique [0002] Extracting uranium from seawater is essential to meet the growing demand for uranium resources from the nuclear energy industry. However, due to the complex environment of natural seawater, the concentration of uranium is low (3.3ppb, μg L -1 ) and severe marine microbial fouling have resulted in the failure of the existing uranium extraction adsorbents to be industrialized. Among them, the most widely studied uranium-extracting adsorbent is amidoxime-based material, but the biofouling in natural seawater not only greatly reduces its uranium adsorption capacity, but even destroys the structure of the adsorbent, thereby reducing the reusability of the adsorbent and increasing the uranium concentration. The economic cost...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00C02F1/28B01J20/22B01J20/30C02F103/08
CPCC08G83/008C02F1/285B01J20/223C02F2101/006C02F2103/08
Inventor 刘涛陈梦伟王宁张若倩
Owner HAINAN UNIVERSITY
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