Preparation method of photo-responding molecularly imprinted material for selectively separating and purifying cyclodextrin and derivatives of cyclodextrin

A separation, purification and molecular imprinting technology, applied in the fields of chemistry and material and molecular separation, can solve the problems of restricting the industrial production of cyclodextrin, low industrial yield and high price, and achieve excellent light response characteristics, remarkable separation effect, and use long life effect

Active Publication Date: 2017-02-22
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Most enzymes will transform into α-CD, β-CD, γ-CD and branched cyclodextrin when they act on starch or its hydrolyzate. Salt, concentration and other processes have disadvantages such as complex operation, long time consumption, and low yield; if nanofiltration membrane

Method used

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  • Preparation method of photo-responding molecularly imprinted material for selectively separating and purifying cyclodextrin and derivatives of cyclodextrin
  • Preparation method of photo-responding molecularly imprinted material for selectively separating and purifying cyclodextrin and derivatives of cyclodextrin
  • Preparation method of photo-responding molecularly imprinted material for selectively separating and purifying cyclodextrin and derivatives of cyclodextrin

Examples

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Example Embodiment

[0038] Example 1

[0039] (1) Aniline (15g, 162mmol), 10mL of water and 10mL of concentrated hydrochloric acid with a concentration of 12mol / L are mixed and stirred for 10min, then NaNO dissolved in 20mL of water is added dropwise 2 (12g). After stirring for 20 minutes under ice bath conditions, a phenol solution dissolved in 40 mL of 8% NaOH was added dropwise. After the addition, keep the ice bath and continue to stir for 40 minutes. After the reaction, the filter cake was filtered with suction, and the filter cake was washed with water, and then recrystallized with a mixture of ethanol and water in a volume ratio of 1:1 to obtain 4-hydroxyazobenzene as a dark orange-red product;

[0040] (2) 0.15g N,N-dimethylaminopyridine, 2.0g triethylamine and 2.0g 4-hydroxyazobenzene are dissolved in 100.0mL acetonitrile, the mixture is placed in an ice water bath, and 2.0 is slowly added dropwise. g methacrylic acid chloride and 5.0mL acetonitrile mixture, moved to 35℃ oil bath and reacte...

Example Embodiment

[0042] Example 2

[0043] (1) Aniline (15g, 162mmol), 80mL water and 30mL concentrated hydrochloric acid with a concentration of 11mol / L are mixed and stirred for 20 minutes, then NaNO dissolved in 30mL water is added dropwise 2 (13g). After continuing to stir for 40 minutes under ice bath conditions, a phenol solution dissolved in 90 mL of 10% NaOH was added dropwise. After the addition, keep the ice bath and continue to stir for 300 min. After the reaction, the filter cake was filtered with suction, and the filter cake was washed with water, and then recrystallized with a mixture of ethanol and water in a volume ratio of 1:1 to obtain 4-hydroxyazobenzene as a dark orange-red product;

[0044] (2) 0.75g of N,N-dimethylaminopyridine, 20.0g of triethylamine and 6.0g of 4-hydroxyazobenzene are dissolved in 150.0mL of acetonitrile, the mixture is placed in an ice water bath, and 10.0 is slowly added dropwise. g methacrylic acid chloride and 10.0mL acetonitrile mixture, moved to 50℃ ...

Example Embodiment

[0046] Example 3

[0047] (1) Aniline (15g, 162mmol), 160mL water and 50mL concentrated hydrochloric acid with a concentration of 10mol / L are mixed and stirred for 30min, then NaNO dissolved in 40mL water is added dropwise 2 (14g). After continuing to stir for 60 min under ice bath conditions, a phenol solution dissolved in 150 mL of 12% NaOH was added dropwise. After the addition, keep the ice bath and continue to stir for 600 min. After the reaction is completed, filter with suction, wash the filter cake with water, and recrystallize with a mixture of ethanol and water in a volume ratio of 1:1 to obtain 4-hydroxyazobenzene as a dark orange-red product;

[0048] (2) 1.5g of N,N-dimethylaminopyridine, 40.0g of triethylamine and 10.0g of 4-hydroxyazobenzene were dissolved in 200.0mL of acetonitrile, the mixture was placed in an ice water bath, and 20.0 was slowly added dropwise. g methacrylic acid chloride and 20.0mL acetonitrile mixed solution, moved to 60℃ oil bath and reacted f...

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Abstract

The invention provides a preparation method of a photo-responding molecularly imprinted material for selectively separating and purifying cyclodextrin and derivatives of cyclodextrin. The method includes the steps of preparation of 4-hydroxyazobenzene and preparation of a functional monomer 4-methylacryloyl azoxybenzene and also includes preparation of a photo-responding molecularly imprinted polymer, wherein the 4-methylacryloyl azoxybenzene is used as the functional monomer, and the cyclodextrin and the derivatives of the cyclodextrin are used as template molecules to prepare the molecularly imprinted polymer having the capability of separating and purifying the cyclodextrin and the derivatives of the cyclodextrin under the effects of a crosslinking agent, an initiator and a catalyst. The preparation process is simple, the prepared molecularly imprinted material is good in chemistry stability, large in adsorption capacity and high in repeated utilization rate and can separate and purify the cyclodextrin and the derivatives of the cyclodextrin in a complex environment.

Description

technical field [0001] The invention relates to the technical fields of chemistry, materials and molecular separation, in particular to a new method for preparing a light-responsive molecular imprinted material for selective separation and purification of cyclodextrin and its derivatives. Background technique [0002] Cyclodextrin (CD for short) is a kind of cyclic oligosaccharide produced by glucosyltransferase (CGTase) produced by certain species of Bacillus acting on starch. Depending on the number of glucose units, common cyclodextrins contain 6, 7 and 8 glucose units (α-CD, β-CD, γ-CD). Due to its unique amphiphilic cavity structure, which is hydrophilic on the outside and hydrophobic on the inside, cyclodextrin can be used as a "host" molecule to complex different "guest" compounds to form a host-guest inclusion complex . [0003] Azobenzene and its derivatives are a class of compounds that can undergo photoisomerization. The trans conformation is the stable conform...

Claims

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Application Information

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IPC IPC(8): C08F220/34C08F222/14C08J9/28B01J20/26B01J20/30C08B37/16
CPCB01J20/268C08B37/0012C08F220/34C08F222/102
Inventor 金征宇王金鹏范浩然周星田耀旗柏玉香谢正军赵建伟焦爱权徐学明
Owner JIANGNAN UNIV
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