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A photoresponsive surface molecularly imprinted material and its preparation method and application

A technology of surface molecular imprinting and light response, applied in the fields of chemistry and material and molecular separation, can solve the problems of expensive separation and purification of chromatographic columns, low industrial output, etc., and achieve difficult elution of template molecules, remarkable separation effect, and good identification. performance effect

Active Publication Date: 2019-01-08
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation process of the present invention is simple, and the prepared surface molecular imprinted material has good chemical stability, large adsorption capacity, and high reuse rate, and can separate and purify branched cyclodextrins in complex environments, and overcomes the high cost of separation and purification of chromatographic columns and the low industrial yield. High disadvantage

Method used

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  • A photoresponsive surface molecularly imprinted material and its preparation method and application
  • A photoresponsive surface molecularly imprinted material and its preparation method and application
  • A photoresponsive surface molecularly imprinted material and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (1) Preparation of azobenzene derivatives: 4-hydroxyazobenzene (0.3964g) was dissolved in 50.0ml of anhydrous, N,N'-dimethylformamide (DMF), and 0.20g of NaH was added thereto. The mixture was stirred at room temperature until no bubbles evolved. The excess NaH was then filtered off, and the filtrate was transferred to a three-necked flask. After 1.0ml of γ-glycidyltrimethoxysilane (GOTMS) was slowly added dropwise to the filtrate, the reaction mixture was reacted at 50°C for 8h under the protection of nitrogen. Through this reaction, 4-hydroxyazobenzene is covalently bonded to the epoxy group of GOTMS.

[0037] (2) Preparation of silica gel particles: add 0.5mL tetraethoxysilane to 11.35mL ethanol solution, then quickly add 2mL ammonia solution (mass fraction: 12%), stir at room temperature for 48h, centrifuge, filter, and wash with water for several times Dry under vacuum.

[0038] (3) Activation of silica gel: take 2.0 g of silica gel particles, add 20.0 mL of hyd...

Embodiment 2

[0043] (1) Preparation of azobenzene derivatives: 4-hydroxyazobenzene (0.9911g) was dissolved in 100.0ml of anhydrous, N,N'-dimethylformamide (DMF), and 0.50g of NaH was added thereto. The mixture was stirred at room temperature until no bubbles evolved. The excess NaH was then filtered off, and the filtrate was transferred to a three-necked flask. After 2.0 ml of γ-glycidyltrimethoxysilane (GOTMS) was slowly added dropwise to the filtrate, the reaction mixture was reacted at 80° C. for 5 h under the protection of nitrogen. Through this reaction, 4-hydroxyazobenzene is covalently bonded to the epoxy group of GOTMS.

[0044] (2) Preparation of silica gel particles: add 3mL tetraethoxysilane to 11.35mL ethanol solution, then quickly add 15mL ammonia solution (mass fraction: 16.7%), stir at room temperature for 24 hours, centrifuge, filter, wash with water several times, and then pour Vacuum dry.

[0045] (3) Activation of silica gel: Take 10.0 g of silica gel particles, add 1...

Embodiment 3

[0050] (1) Preparation of azobenzene derivatives: 4-hydroxyazobenzene (1.9822g) was dissolved in 250.0ml of anhydrous, N,N'-dimethylformamide (DMF), and 1.0g of NaH was added thereto. The mixture was stirred at room temperature until no bubbles evolved. The excess NaH was then filtered off, and the filtrate was transferred to a three-necked flask. After 5.0ml of γ-glycidyltrimethoxysilane (GOTMS) was slowly added dropwise to the filtrate, the reaction mixture was reacted at 100° C. for 2 h under the protection of nitrogen. Through this reaction, 4-hydroxyazobenzene is covalently bonded to the epoxy group of GOTMS.

[0051] (2) Preparation of silica gel particles: Add 6 mL of tetraethoxysilane to 11.35 mL of ethanol solution, then quickly add 30 mL of ammonia solution (20% by mass), stir at room temperature for 12 hours, centrifuge, filter, wash with water several times, and then pour Vacuum dry.

[0052] (3) Activation of silica gel: Take 20.0 g of silica gel particles, add...

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Abstract

The invention provides a preparation method of a photoresponsive surface molecular imprinting material for realizing high-efficiency selective separation and purification of branched cyclodextrin. The method comprises a step of preparing an azobenzene derivative recognizing branched cyclodextrin and a step of synthesizing a photoresponsive surface molecular imprinting polymer. The surface molecular imprinting polymer capable of specifically recognizing branched cyclodextrin is prepared by taking the azobenzene derivative as a functional monomer and the branched cyclodextrin as a template molecule under the action of a crosslinking agent, an initiator and a catalyst. According to the invention, the preparation process is simple; and the prepared molecular imprinting material has favorable chemical stability, high adsorption capacity and high reutilization rate, and can separate and purify branched cyclodextrin in a complex environment.

Description

technical field [0001] The invention relates to the technical field of chemistry, materials and molecular separation, in particular to a new method for preparing a light-responsive surface molecular imprinted material for efficient and selective separation and purification of branched cyclodextrins. 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 . However, cyclodextrin has poor water solubility, hemolysis and nephrotoxicity. Chemical or biological enzymatic methods are usually used...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F292/00C08F222/14C08J9/26B01J20/26B01J20/30B01D15/08
CPCB01D15/08B01J20/103B01J20/264C08F292/00C08J9/26C08J2201/0422C08J2351/10C08J2405/16C08F222/102
Inventor 金征宇王金鹏范浩然周星田耀旗焦爱权柏玉香王留留谢正军赵建伟徐学明
Owner JIANGNAN UNIV
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