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Copolymerization-immobilized beta-cyclodextrin porous separation material as well as preparation method and application thereof

A separation material, cyclodextrin technology, applied in chemical instruments and methods, other chemical processes, adsorption water/sewage treatment, etc., can solve the problem of particle surface reduction

Active Publication Date: 2013-11-20
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the adsorbent particles after adsorbing phenol will stick together, resulting in a rapid decrease in the surface of the particles. After a period of use, the adsorbent particles must be replaced to ensure the separation efficiency

Method used

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  • Copolymerization-immobilized beta-cyclodextrin porous separation material as well as preparation method and application thereof
  • Copolymerization-immobilized beta-cyclodextrin porous separation material as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Firstly, 2.27g β-CD was added into 50mL / 50mL anhydrous DMF / anhydrous DMSO mixed solution to fully dissolve β-CD, then 8.96g NaOH was added and stirred vigorously for 1h to mix well. Slowly add 14.4 mL of LC in an ice-water bath at 5°C while stirring 3 h 5 Br, reacted under vigorous stirring for 48 hours, filtered to remove the solid precipitate after the reaction stopped, added 8 to 10 times of water to the filtrate to precipitate the product, extracted with ethyl acetate and then rotary evaporated to obtain vinyl β-CD.

[0023] At room temperature, mix 1g of vinyl β-CD and 2g of styrene evenly, add 0.75g of p-vinylbenzene and 1.01g of Span 80 to form a continuous phase; mix 0.188g of K 2 SO 4 and 0.075gK 2 S 2 o 8 Dissolve in 45g of deionized water to form a dispersed phase. Slowly drop the dispersed phase into the continuous phase under high-speed stirring, and stir evenly after the dropwise addition to form a reverse-phase thick emulsion. Then, the concentrate...

Embodiment 2

[0025] Firstly, add 2.27g β-CD into 40mL / 60mL anhydrous DMF / anhydrous DMSO mixed solution to fully dissolve β-CD, then add 5.04g NaOH and stir vigorously for 1h to mix well. Slowly add 11.4 mL of LC in a water bath at 20°C while stirring 3 h 5 Br, reacted under vigorous stirring for 72 hours, filtered to remove the solid precipitate after the reaction stopped, added 8 to 10 times of water to the filtrate to precipitate the product, extracted with ethyl acetate and rotary evaporated to obtain vinyl β-CD.

[0026] At room temperature, stir and mix 0.6g vinyl β-CD and 2.4g styrene evenly, add 0.375g p-vinylbenzene and 0.505g Span 80 to configure the continuous phase; mix 0.188g K 2 SO 4 and 0.075gK 2 S 2 o 8 Dissolve in 47g of deionized water to form a dispersed phase. Slowly drop the dispersed phase into the continuous phase under high-speed stirring, and stir evenly after the dropwise addition to form a reverse-phase thick emulsion. Then, the concentrated emulsion was pl...

Embodiment 3

[0028] First, add 2.27g β-CD into 40mL / 60mL anhydrous DMF / anhydrous DMSO mixed solution to fully dissolve β-CD, then add 4.04g NaOH and stir vigorously for 1h to mix well. Slowly add 11.4 mL of LC in a water bath at 20°C while stirring 3 h 5 Br, reacted under vigorous stirring for 72 hours, filtered to remove the solid precipitate after the reaction stopped, added 8 to 10 times of water to the filtrate to precipitate the product, extracted with ethyl acetate and rotary evaporated to obtain vinyl β-CD.

[0029] At room temperature, stir and mix 1g vinyl β-CD and 2g styrene evenly, add 0.375g p-vinylbenzene, 1.405g Span 20 to configure the continuous phase; mix 0.188g K 2 SO 4 and 0.075gK 2 S 2 o 8 Dissolve in 45g of deionized water to form a dispersed phase. Slowly drop the dispersed phase into the continuous phase under high-speed stirring, and stir evenly after the dropwise addition to form a reverse-phase thick emulsion. Then, the concentrated emulsion was placed in a...

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Abstract

The invention discloses a copolymerization-immobilized beta-cyclodextrin porous separation material as well as a preparation method and an application thereof belongs to a porous separation material technology. The preparation method comprises the following steps of: preparing vinyl beta-cyclodextrin; uniformly mixing vinyl beta-cyclodextrin with styrene, p-vinyltoluene and an emulsifier, and then adding an initiator and aqueous solution containing an electrolyte to prepare a stable concentrated emulsion; polymerizing for 6-48 hours at 50-80 DEG C to obtain the copolymerization-immobilized beta-cyclodextrin porous separation material, wherein the mixture of vinyl beta-CD, styrene, p-vinyltoluene and the emulsifier is continuous-phase, the aqueous solution containing the electrolyte is disperse-phase, and the volume fraction of the disperse phase occupying the concentrated emulsion is 74-95%; the dosages of the initiator and the electrolyte are 3-10% of the mass of the mixture of vinyl beta-CD, styrene and p-vinyltoluene. The porous separation material can be used for phenolic wastewater treatment, and can achieve certain separation efficiency.

Description

technical field [0001] The invention belongs to the technology of porous separation materials, and in particular relates to the preparation of a copolymerized immobilized β-cyclodextrin porous separation material by a reverse-phase concentrated emulsion method, a preparation method and an application. Background technique [0002] Cyclodextrin is a cyclic oligosaccharide formed by α-D-glucopyranose linked by α-1,4 glycosidic bonds, among which β-cyclodextrin is most widely used in polymer polymerization, it contains 7 glucose units, It is a conical structure with the top truncated, the primary hydroxyl group is located on the smaller diameter surface, and the secondary hydroxyl group is located on the larger diameter surface. The hydroxyl groups of β-cyclodextrin are all located on its outer surface, so the inside of the ring is a hydrophobic cavity and the outside is hydrophilic. Because of its special molecular structure, unique enveloping properties, environmental friend...

Claims

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Application Information

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IPC IPC(8): C08F290/10C08F212/08C08F2/32C08B37/16B01J20/26B01J20/30C02F1/28
Inventor 杜中杰谢恺君张晨邹威励杭泉
Owner BEIJING UNIV OF CHEM TECH
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