Method for preparing cyclodextrin-based polymer adsorbing material by utilizing coupling of chemical reaction and reduced pressure distillation

An adsorption material and chemical reaction technology, applied in chemical instruments and methods, other chemical processes, adsorption water/sewage treatment, etc., can solve problems such as unstable adsorption performance, achieve stable adsorption performance, easy control of conditions, and a preparation method simple effect

Active Publication Date: 2015-05-20
ANHUI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention aims at the practical problem that the adsorption performance of the cyclodextrin-based polymer adsorption material is not stable when cyclodextrin is cross-linked with an acid anhydride or acid chloride to prepare a cyclodextrin-based polymer adsorption material. Method for preparing cyclodextrin-based polymer adsorption material by "distillation"

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] 2.0g styrene-maleic anhydride alternating copolymer was dissolved in 50mL N,N-dimethylformamide, and 11.0 g β - Cyclodextrin, heat up to 70°C and stir for 2 hours. Change the reaction device to vacuum distillation, maintain the reaction system at 80°C, and control the vacuum to distill 38mL of N,N-dimethylformamide within 60min. Cool to room temperature, add warm water at 30-50°C to wash the residue, filter with suction, and dry in vacuum to obtain cyclodextrin-based polymer adsorption material A.

[0018] Put 0.025g of adsorption material A in 100mL of a certain concentration of organic dyes (basic fuchsin, methylene blue), seal, and shake at a constant temperature of 25°C for 8h. The adsorbent was removed by filtration, and the concentration of each dye solution before and after adsorption was measured with a UV-Vis spectrophotometer. The results show that the saturated adsorption capacity of adsorption material A for basic fuchsin and methylene blue calculated by t...

Embodiment 2

[0020] 2.0g maleic ethylenediamine diacid in 10mL SOCl 2 After 7 h of reaction at medium reflux, remove SOCl under reduced pressure 2 . Dissolve the residual acid chloride with 10mL N,N-dimethylformamide, add it to a 2.0g β -CD, 15mL N,N-dimethylformamide and 2.5mL triethylamine in a reaction flask, stirred at 65°C for 2h. Then, the reaction system was maintained at 70°C, and the vacuum degree of the system was controlled to evaporate 20 mL of N,N-dimethylformamide in 2.5 h. Cool with saturated NaHCO 3 The residue was washed with the solution and water, filtered with suction, and dried to obtain 2.1 g of cyclodextrin-based polymer adsorption material B.

[0021] Put 0.05g of B in 50mL of a certain concentration of organic dyes (basic fuchsin, methylene blue, rhodamine B and methyl orange), seal it, and shake at a constant temperature of 25°C for 5h. The adsorbent was removed by filtration, and the concentration of the dye solution before and after adsorption was measured ...

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Abstract

The invention discloses a method for preparing a cyclodextrin-based polymer adsorbing material by utilizing coupling of a chemical reaction and reduced pressure distillation. The method comprises the following steps: in an organic solvent, adding cyclodextrin and an acid anhydride or acid chloride component according to a certain ratio; after reacting for a certain time at a temperature of 50 to 80 DEG C under stirring, in a range of 60 to 85 DEG C of a reaction system, controlling the degree of vacuum of the system, distilling off a certain proportion of organic solvent under reduced pressure, cooling to room temperature, washing residues, performing suction filtration, and drying in a vacuum to obtain the cyclodextrin-based polymer adsorbing material.

Description

technical field [0001] The invention relates to the field of polymer preparation, in particular to a method for preparing a cyclodextrin-based polymer adsorption material by coupling chemical reaction and vacuum distillation. Background technique [0002] The cyclodextrin-based polymer adsorption material prepared by the cross-linking polymerization of cyclodextrin and cross-linking agent anhydride or polyacyl chloride has a good application prospect in the treatment of organic pollutants in water. The preparation methods of such cyclodextrin-based polymers reported in the literature mainly include solution polymerization and inverse emulsion polymerization. Since the hydrophobic cavity of cyclodextrin and the secondary cavity formed by the polymer network are the main sites for this type of adsorption material to adsorb organic pollutants, in the reaction of preparing cyclodextrin-based polymer adsorption material, Controlling the degree of crosslinking and crosslinking un...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/16B01J20/26C02F1/28C02F101/30
Inventor 张晓梅窦李曹曼丽吴超南
Owner ANHUI UNIV OF SCI & TECH
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