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Preparation method of cyclodextrin constructed adsorbing material based on micropore structure

A technology of adsorption materials and microporous structures, applied in chemical instruments and methods, alkali metal oxides/hydroxides, inorganic chemistry, etc., to achieve the effects of easy mastery, simple methods, and simple operations

Active Publication Date: 2019-01-08
TIANJIN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to solve the problem of certain difficulty in selective chemical modification, separation and purification due to the special structure and properties of cyclodextrin, and to provide a cyclodextrin-based adsorption Material preparation method

Method used

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  • Preparation method of cyclodextrin constructed adsorbing material based on micropore structure
  • Preparation method of cyclodextrin constructed adsorbing material based on micropore structure

Examples

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Embodiment 1

[0023] A method for preparing an adsorption material based on microporous cyclodextrin, comprising the steps of:

[0024] (1) Preparation of Vilsmeier-Haack reagent.

[0025] Under anaerobic and anhydrous conditions, 14g triphenylphosphine was dissolved in N,N-dimethylformamide (DMF), then 8.6g bromine was added dropwise, and after 0.5h reaction, the Vilsmeier-Haack reagent ([ (CH3)2NCHBr]Br);

[0026] (2) Preparation of perbromo-β-cyclodextrin.

[0027] The DMF solution of β-cyclodextrin (3.4g) was added to the Vilsmeier-Haack reagent prepared in step (1), and the reaction temperature was controlled below 60°C for 16 hours. After the reaction was completed, the pH of the solution was adjusted to 8 with sodium methoxide, and then Add methanol to precipitate, and filter with suction to obtain perbromo-β-cyclodextrin;

[0028] (3) Preparation of all-[6-oxo-6-(4-formylbenzene)]-β-cyclodextrin adsorption material.

[0029] Dissolve 1.22g of p-hydroxybenzaldehyde in DMF, add 1....

Embodiment 2

[0033] A method for preparing an adsorption material based on microporous cyclodextrin, comprising the steps of:

[0034] (1) Preparation of Vilsmeier-Haack reagent.

[0035] Under anaerobic and anhydrous conditions, 14g triphenylphosphine was dissolved in N,N-dimethylformamide (DMF), then 8.6g bromine was added dropwise, and after 0.5h reaction, the Vilsmeier-Haack reagent ([ (CH3)2NCHBr]Br);

[0036] (2) Preparation of perbromo-α-cyclodextrin.

[0037] The DMF solution of α-cyclodextrin (2.9g) was added to the Vilsmeier-Haack reagent prepared in step (1), and the reaction temperature was controlled below 60°C for 8 hours. After the reaction was completed, the pH of the solution was adjusted to 8 with sodium methoxide, and then Add methanol to precipitate, and filter with suction to obtain perbromo-α-cyclodextrin;

[0038] (3) Preparation of all-[6-oxo-6-(4-formylbenzene)]-α-cyclodextrin adsorption material.

[0039] Dissolve 1.22g of p-hydroxybenzaldehyde in DMF, add 1.3...

Embodiment 3

[0043] A method for preparing an adsorption material based on microporous cyclodextrin, comprising the steps of:

[0044] (1) Preparation of Vilsmeier-Haack reagent.

[0045] Under anaerobic and anhydrous conditions, 14g triphenylphosphine was dissolved in N,N-dimethylformamide (DMF), then 8.6g bromine was added dropwise, and after 0.5h reaction, the Vilsmeier-Haack reagent ([ (CH3)2NCHBr]Br);

[0046] (2) Preparation of perbromo-γ-cyclodextrin.

[0047] The DMF solution of γ-cyclodextrin (3.9g) was added to the Vilsmeier-Haack reagent prepared in step (1), and the reaction temperature was controlled below 60°C for 16 hours. After the reaction was completed, the pH of the solution was adjusted to 7 with sodium methoxide, and then Add methanol to precipitate, and filter with suction to obtain perbromo-γ-cyclodextrin;

[0048] (3) Preparation of all-[6-oxo-6-(4-formylbenzene)]-γ-cyclodextrin adsorption material.

[0049] Dissolve 1.22g of p-hydroxybenzaldehyde in DMF, add 1....

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Abstract

The invention discloses a preparation method of a cyclodextrin constructed adsorbing material based on a micropore structure. According to the method, by substituting 6-hydroxy of cyclodextrin by p-hydroxy benzaldehyde, the cavity of the cyclodextrin is widened, and the adsorbing material with a larger pore structure is further obtained. The preparation method comprises the following reaction steps: dissolving triphenylphosphine into N,N-dimethylformamide under oxygen-free and anhydrous conditions, dropwise adding bromine to prepare a Vilsmeier-Haack reagent; dropping a DMF (Dimethyl Formamide) solution of the cyclodextrin into the solution, regulating the pH value of the solution to be 7-8 with sodium methoxide after reaction completion, and performing suction filtration to obtain a crudeproduct; dissolving the crude product into the DMF, dropping into distilled water, and performing suction filtration to obtain hexabromocyclodextrin; substituting bromine in the cyclodextrin by nucleophilicity of phenolic hydroxyl groups in the p-hydroxy benzaldehyde so as to obtain 6-p-methylsulfonylphenyl cyclodextrin, dropping the reaction solution into water to separate, and performing suction filtration, thereby obtaining the crude product. The per-[6-oxo-6-(4-benzoylphenyl)]-cyclodextrin with the micropore structure is prepared by utilizing a solution diffusion method.

Description

technical field [0001] The invention relates to a preparation method of an adsorption material constructed by cyclodextrin based on a microporous structure, and belongs to the technical field of functionalization of supramolecular materials. Background technique [0002] Supramolecular chemistry research has mainly focused on complex, ordered and specific molecular assemblies held together by weak non-covalent interactions. Different from valence bond chemistry studied in molecular chemistry, supramolecules focus on the weak interactions between molecules, usually including hydrogen bonds, π-π stacking, coordination interactions, electrostatic interactions, hydrophobic interactions and other non-covalent interactions effect. In the 1990s, Harada discovered that cyclodextrins can self-assemble with linear polymer molecules to form chain inclusion complexes (polyrotaxanes), thereby self-assembling cyclodextrins from small molecular structures into polymers. This formed polyr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30
CPCB01J20/22B01J20/28011
Inventor 樊志周勇颖王廷廷郭方方郭敏杰李盛华赵金
Owner TIANJIN UNIV OF SCI & TECH
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