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Quasi-three-dimensional phosphazene covalent organic framework material and its preparation method and use

A covalent organic framework, three-dimensional phosphazene technology, applied in separation methods, chemical instruments and methods, and other chemical processes, can solve the problems of expensive, limited, and insufficient three-dimensional COFs, and achieve improved adsorption capacity and mass transfer The effect of increasing the rate and improving the permeability of the pores

Active Publication Date: 2021-09-07
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, three-dimensional COFs must use tetrahedral reactive monomers as building blocks, and the structures and types of monomers that can be selected are very limited. The three-dimensional COFs that have been reported so far are less than one-tenth of the total.
Not only that, the limited availability of three-dimensional reactive monomers is difficult and expensive to synthesize
These unfavorable factors, as well as the difficulties in preparation and structure analysis of 3D COFs, severely limit its development and practical application.

Method used

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  • Quasi-three-dimensional phosphazene covalent organic framework material and its preparation method and use
  • Quasi-three-dimensional phosphazene covalent organic framework material and its preparation method and use
  • Quasi-three-dimensional phosphazene covalent organic framework material and its preparation method and use

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preparation example Construction

[0039] A method for preparing a quasi-three-dimensional phosphazene covalent organic framework material, comprising the following steps:

[0040] a. Dissolve p-hydroxybenzaldehyde in tetrahydrofuran, slowly add potassium carbonate to the system, stir at 0-5°C for 20-50 minutes, then slowly add the HCCP solution dissolved in tetrahydrofuran dropwise, ice-bath for 2 hours, and then stir at room temperature for 2- 4 days; the reaction was completed and filtered, the filtrate was removed from the solvent, and the obtained solid was extracted. After the organic phase was washed and dried, it was distilled under reduced pressure to obtain six (4-formylphenoxy)cyclotriphosphazene (CTP-6-CHO) ;

[0041] b. CTP-6-CHO and XH 4 Uniformly dispersed in the mixed solvent of o-dichlorobenzene and n-butanol respectively, then, the above-mentioned CTP-6-CHO dispersion system was added to XH 4 In the dispersion system, mix evenly (or first add acetic acid solution and let stand at room temper...

Embodiment 1 6

[0048] Embodiment 1 Preparation of six (4-formylphenoxy) cyclotriphosphazene (CTP-6-CHO)

[0049]

[0050] Dissolve 14.92g of p-hydroxybenzaldehyde in 300mL of THF (tetrahydrofuran), slowly add 33.4g of potassium carbonate to the system, stir in an ice bath for 30min, then slowly add 50mL of THF-dissolved HCCP (6.96g) solution dropwise, and ice-bath for 2h , Stir the reaction at room temperature for 3d. After the reaction was completed, the filtrate was filtered, and the filtrate was distilled under reduced pressure. The obtained solid was extracted with dichloromethane, and then washed with saturated brine. The organic phase was dried with anhydrous sodium sulfate, and a white solid was obtained by distillation under reduced pressure. The solid powder was recrystallized in ethyl acetate. , 14.98 g of white crystals were obtained with a yield of 87%.

[0051] 1 H NMR (400MHz, DMSO) δ 9.92 (s, 6H), 7.79 (d, J = 8.6Hz, 12H), 7.18 (d, J = 8.5Hz, 12H).

[0052] 13 C NMR (10...

Embodiment 2

[0053] Example 2 Preparation of quasi-three-dimensional phosphazene covalent organic framework material QTD-COF-1

[0054]

[0055] CTP-6-CHO (86mg) and p-phenylenediamine (33mg) were placed in a 15mL pressure-resistant bottle, and then o-dichlorobenzene and n-butanol (9:1v / v, 1.5mL) were added, and the two mixtures were ultrasonicated for 5 Minutes to obtain a uniform dispersion. Then, CTP-6-CHO was added to the p-phenylenediamine dispersion system, and the resulting suspension was briefly shaken for 10 s. Subsequently, acetic acid (6M, 0.3 mL) was slowly added, the bottle was sealed, and the reaction was left to stand at 120° C. for 7 days. The solid was collected by filtration and washed with DMF (N,N-dimethylformamide), acetone and THF respectively. The solid was vacuum-dried overnight at 50° C. to obtain a yellow crystalline solid with a yield of 91%, and the molecular formula was (C 20 h 14 N 3 o 2 P)n (% predicted / experimental: C 66.85 / 67.03, H 3.93 / 2.67, N 11....

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Abstract

The invention belongs to the field of organic porous material adsorbents, and in particular relates to a quasi-three-dimensional phosphazene covalent organic framework material and its preparation method and application. The invention provides a quasi-three-dimensional phosphazene covalent organic framework material, the structure of which is shown in formula I. The quasi-three-dimensional phosphazene covalent organic framework material and its preparation method provided by the present invention can not only greatly reduce the preparation cost and difficulty of COFs materials, but also effectively realize the substantial improvement of the iodine adsorption rate and capacity of two-dimensional COFs, which is the basis for nuclear accidents. The rapid enrichment and separation of radioactive iodine in emergencies such as emergency response provides an effective solution.

Description

technical field [0001] The invention belongs to the field of organic porous material adsorbents, in particular to a quasi-three-dimensional phosphazene covalent organic framework material and its preparation method and application. Background technique [0002] As a main gaseous fission product, radioactive iodine is one of the most important radioactive pollutants in radioactive nuclear waste and nuclear accidents. It is easy to volatilize, has strong fluidity and fast diffusion speed, and it is very difficult to deal with in the actual environment. . In addition, the extremely long radioactive half-life of radioactive iodine ( 129 I-1.57×107 years), high radiation ( 131 I) and biocompatibility also make it a potential threat to ecological environment safety and human health, if not handled properly will seriously restrict the development and application of nuclear energy. On the other hand, radioactive iodine has important application value in the medical field. For ex...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00B01J20/30B01D53/02G21F9/02
CPCB01D53/02B01D2253/202B01D2257/2068B01J20/262C08G83/008G21F9/02
Inventor 马利建郭兴华
Owner SICHUAN UNIV
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