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Amphiphilic porous cyclodextrin polymer

A porous polymer, cyclodextrin technology, applied in the field of environmental protection materials, can solve the problems of low density, limited application, poor wettability, etc., and achieve the effects of high adsorption rate, enhanced hydrophilicity, and good thermal stability

Pending Publication Date: 2021-04-13
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, ultra-highly cross-linked polymers are often very hydrophobic and have low density, and are generally used for gas adsorption, and their poor wettability also limits their application in water treatment.

Method used

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  • Amphiphilic porous cyclodextrin polymer
  • Amphiphilic porous cyclodextrin polymer
  • Amphiphilic porous cyclodextrin polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Preparation of Porous Cyclodextrin Polymer:

[0052] Dissolve the cyclodextrin and cool it in an ice-water bath; add sodium hydride and stir evenly; slowly drop in the benzylation reagent and react overnight to obtain the benzylated cyclodextrin. The molar ratio of benzylation reagent to cyclodextrin is shown in the summary table of the examples below. Then the benzylated cyclodextrin and the alkylating agent are catalyzed by Lewis acid, under the protection of nitrogen, in an oil bath equipped with magnetic stirring, react at a certain speed and temperature for a certain period of time. The molar ratio of alkylating agent to benzylated cyclodextrin is 5–8:1. The temperature is usually 55-100°C, preferably 75-90°C. The reaction time is preferably 15-30h, preferably 19-25h, most preferably 19h. If it is not within the above-mentioned preferred range, incomplete reaction and low yield will occur. The obtained product is washed several times with distilled water and me...

Embodiment 2

[0091] Preparation of high specific surface cyclodextrin polymer PBCD-B-D-H by sulfuric acid route:

[0092] a. Preparation of partially benzylated cyclodextrin PBCD

[0093] 1) In a round bottom flask, dissolve 2g of β-cyclodextrin in 40mL of anhydrous dimethylformamide, cool to 0°C in a low-temperature constant temperature reaction bath, add 0.59g of 60% sodium hydride, and stir for 15min;

[0094] 2) Slowly drop 0.8 mL of benzyl bromide into the solution with a constant pressure funnel, heat to room temperature, and stir overnight;

[0095] 3) After reacting overnight, add 5 mL of methanol to quench the reaction;

[0096] 4) Add 100 mL of distilled water, and extract three times with dichloromethane, 50 mL each time. The obtained solution was dried and filtered with anhydrous sodium sulfate, and concentrated at 35° C. with a rotary evaporator to obtain partially benzylated cyclodextrin PBCD.

[0097] b. Preparation of PBCD-B-D-H

[0098] 1) Take 1.06g of PBCD, 0.82g of ...

Embodiment 3

[0107] In order to fully illustrate the material properties of the amphiphilic high specific surface cyclodextrin polymer PBCD-B-D prepared in Example 1, activated carbon GAC and non-porous cyclodextrin polymer EPI-CDP were used as comparison materials, and different water-soluble Four kinds of model pollutants (3-phenylphenol, 2-naphthol, p-nitrophenol, p-chlorophenol) are carried out adsorption experiment, concrete method is as follows:

[0108] The adsorbents used were all ground into powder (60-80 mesh) before use. The sample taken was filtered with an Agilent 0.22 μm PTFE-Q filter membrane (almost no adsorption to the above pollutants). The concentrations of different pollutants in the water samples were then determined by high performance liquid chromatography (HPLC). The chromatographic column adopts Agilent XDB-C18 analytical column (5 μm, 4.6×250 mm), and the detector is an ultraviolet detector.

[0109] The specific method for the determination of the adsorption is...

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Abstract

The invention provides an amphiphilic porous cyclodextrin polymer. Cyclodextrin is grafted with aromatic molecules, and then is subjected to a Friedel-Crafts alkylation reaction with 4, 4'-bis(chloromethyl)-1,1'-biphenyl and p-xylylene dichloride to obtain the porous polymer with an ultrahigh specific surface area. The material has very high adsorption capacity, is simple to regenerate and can be repeatedly used. Hydroxyl of cyclodextrin is partially reserved, so that the hydrophilicity of the surface of the material is improved, the adsorption rate of the material is high, and the material has multiple adsorption mechanisms and can adsorb hydrophobic and hydrophilic pollutants at the same time.

Description

technical field [0001] The invention relates to the technical field of environmental protection materials, in particular to a method for preparing an amphiphilic cyclodextrin polymer with a high specific surface area and its application. Background technique [0002] The types of organic micro-pollutants are complex and have different properties, including hydrophobic and hydrophilic pollutants. Traditional biological treatment is often limited in their removal. Adsorption is a more commonly used method, and many adsorbents are effective for hydrophilic pollution. Matter removal did not show good results. Activated carbon is currently the most widely used adsorbent in industry, but it has the disadvantages of high regeneration energy consumption and low recycling rate. In addition, the adsorption rate of activated carbon is very slow, it takes a long time to reach equilibrium, and its adsorption effect is often affected by the water solubility of pollutants, which limit its...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/16C08J3/24B01J20/24C02F1/28C02F1/26C02F101/30C08L5/16
CPCC08B37/0012C08J3/24B01J20/24C02F1/285C02F1/26C08J2305/16C02F2101/30C08F251/00
Inventor 谢显传屠一舟
Owner NANJING UNIV
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