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Nitrogen-containing cyclodextrin polymer porous material and preparation method and application thereof

A technology for cyclodextrin polymers and porous materials, which is applied in the direction of separation methods, chemical instruments and methods, educts, etc., can solve problems such as the preparation of nitrogen-containing cyclodextrin polymer porous materials, and achieve low cost and selectivity. High performance and high adsorption capacity

Active Publication Date: 2020-02-04
SHAANXI SCI TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, no porous materials based on nitrogen-containing cyclodextrin polymers have been prepared and used for CO 2 Adsorption research

Method used

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  • Nitrogen-containing cyclodextrin polymer porous material and preparation method and application thereof
  • Nitrogen-containing cyclodextrin polymer porous material and preparation method and application thereof
  • Nitrogen-containing cyclodextrin polymer porous material and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0029] (1) Under a nitrogen atmosphere, in a 500mL round-bottomed flask, take 17g of β-cyclodextrin and put it into 100mL of tetrahydrofuran solution containing 7.46g of potassium carbonate, fully stir and dissolve it and place it in an ice-water bath to obtain solution 1; take 2.77g Add cyanuric chloride to 50mL of tetrahydrofuran, stir to dissolve it to obtain solution 2;

[0030] Under a nitrogen atmosphere, slowly drop solution 2 into the above solution 1 with a dropping funnel for 30 minutes, control the temperature at 0-5°C, and react for 12 hours to obtain reaction solution 1;

[0031] (2) Dissolve 4.5 g of polyethyleneimine with a molecular weight of 600 into 50 mL of tetrahydrofuran to obtain solution 3, add solution 3 dropwise to the above reaction solution 1, raise the temperature to 80° C. and continue the reaction for 24 hours to obtain reaction solution 2;

[0032] (3) Cool the reaction solution 2 to room temperature, filter, wash the solid on the filter paper to...

Embodiment 2

[0035] (1) Under a nitrogen atmosphere, in a 500mL round-bottomed flask, take 17g of β-cyclodextrin and put it into 100mL of dioxane solution containing 5.45g of triethylamine, fully stir and dissolve it and place it in an ice-water bath to obtain a solution 1; Take 2.77g of cyanuric chloride and add it to 50mL of dioxane, stir to dissolve it, and obtain solution 2;

[0036] Under a nitrogen atmosphere, slowly drop solution 2 into the above solution 1 with a dropping funnel for 30 minutes, control the temperature at 0-5°C, and react for 12 hours to obtain reaction solution 1;

[0037] (2) Take 4.5 g of polyethyleneimine with a molecular weight of 600 and dissolve it in 50 mL of dioxane to obtain solution 3; add solution 3 dropwise to the above reaction solution 1, raise the temperature to 100°C and continue the reaction for 18 hours to obtain the reaction Liquid 2;

[0038] (3) Cool the reaction solution 2 to room temperature, filter, wash the solid on the filter paper to neu...

Embodiment 3

[0041] (1) Under nitrogen atmosphere, in a 500mL round-bottomed flask, take 17g of β-cyclodextrin and put it into 100mL of acetonitrile solution containing 4.26g of pyridine, stir and dissolve it and place it in an ice-water bath to obtain solution 1; take 2.77g Add cyanuric chloride to 50mL of acetonitrile, stir to dissolve it, and obtain solution 2;

[0042] Slowly add solution 2 to the above solution 1 with a dropping funnel for 30 minutes, control the temperature at 0-5°C, and react for 12 hours to obtain reaction solution 1;

[0043] (2) 2.3 g of polyethyleneimine with a molecular weight of 1800 was dissolved in 50 mL of acetonitrile to obtain solution 3; solution 3 was added dropwise to the above reaction solution 1, and the temperature was raised to 90° C. to continue the reaction for 24 hours to obtain reaction solution 2;

[0044](3) Cool the reaction solution 2 to room temperature, filter, wash the solid on the filter paper to neutral with deionized water, then wash ...

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Abstract

The invention discloses a nitrogen-containing cyclodextrin polymer porous material and a preparation method and application thereof. The preparation method comprises the steps that under the inert gasatmosphere, 15 mmol of beta-cyclodextrin is added into 100-150 mL of an organic solvent containing 54 mmol of alkali, after sufficient stirring and dissolving, a solution 1 is obtained, the solution1 is placed in a ice-water bath, 50 mL of a solution 2 is added into the solution 1 dropwise, a reaction is conducted at the temperature of 0-5 DEG C for 12 h, and reaction liquid 1 is obtained; 7.5 mmol of polyethyleneimine is dissolved in 50-75 mL of an organic solvent to obtain a solution 3, the solution 3 is added into the reaction liquid 1 dropwise, the temperature is increased to 80-100 DEGC for continuous reaction for 12-24 h, and reaction liquid 2 is obtained; and the reaction liquid 2 is cooled to the room temperature and filtered, and solid powder obtained by filtering is washed anddried to obtain the nitrogen-containing cyclodextrin polymer porous material. The preparation method is simple, the cost is low, and the obtained material can utilize hydroxide radicals of cyclodextrin and nitrogen-containing function groups of organic amine to realize high adsorption amount and high selectivity of CO2, and has the advantages of large adsorption amount, high selectivity, easy regeneration and the like.

Description

technical field [0001] The invention belongs to the technical field of novel material synthesis, and in particular relates to a nitrogen-containing cyclodextrin polymer porous material and its preparation method and application. Background technique [0002] Porous materials have attracted much attention of researchers due to their many properties such as catalysis, photoelectricity, gas storage and separation. In recent years, with the continuous development of society, people's demand for energy has continued to increase, and the massive consumption of fossil energy has led to a large amount of carbon dioxide gas being emitted, resulting in the greenhouse effect. Therefore, the development of efficient CO 2 The adsorbent becomes CO 2 A hot issue in the field of emission reduction. Solid CO 2 Adsorption materials include: metal-organic framework materials, conjugated microporous materials, microporous polymers, and porous aromatic framework materials. However, the abov...

Claims

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Application Information

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IPC IPC(8): C08G81/00C08J9/28B01J20/26B01J20/30B01D53/02C08L87/00
CPCB01D53/02B01D2253/202B01J20/262B01J2220/4812C08G81/00C08J9/28C08J2387/00Y02P20/151Y02C20/40
Inventor 邵先钊任传清季建伟王伟季晓晖
Owner SHAANXI SCI TECH UNIV
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