Silica gel surface molecularly imprinted polymer with specific adsorption of DEHP and preparation method and application thereof

A surface molecular imprinting and species-specific technology, applied in selective adsorption, chemical instruments and methods, ion exchange, etc., can solve problems such as lack of coverage, instability, and chemical stability effects, and achieve high specificity recognition and selective adsorption , enhanced binding force, and high adsorption capacity

Inactive Publication Date: 2015-09-09
JIANGSU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the synthesis of molecularly imprinted polymers on the surface of silica gel reported in the literature, most of them only use aminopropyltriethoxysilane (KH-550), γ-(2,3-epoxypropoxy)propyltrimethoxysilane (KH-560), γ-methacryloxypropyltrimethoxysilane (KH-570) or vinyltriethoxysilane (VTEO) and other silane coupling agents for one-step modification, KH-550 and After modification of KH-560, the end groups are -NH 2 and 2,3-glycidyloxy, so that the resulting imprinted polymer is not firmly covered on the surface of the silica gel due to the lack of con

Method used

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  • Silica gel surface molecularly imprinted polymer with specific adsorption of DEHP and preparation method and application thereof
  • Silica gel surface molecularly imprinted polymer with specific adsorption of DEHP and preparation method and application thereof
  • Silica gel surface molecularly imprinted polymer with specific adsorption of DEHP and preparation method and application thereof

Examples

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Effect test

Embodiment 1

[0040] Take 15g of silica gel and add 200mL of hydrochloric acid solution with a mass fraction of 10%, heat and reflux in an oil bath at 120°C for 24h, wash with acetone and absolute ethanol respectively, then wash with distilled water until neutral, and vacuum dry at 150°C for 12h to obtain the activated Silica gel. Add 5g of activated silica gel into 50mL of toluene solution, ultrasonically disperse and degas for 30min, N 2 Add 15mL KH-550 dropwise under protection, then add 5mL triethylamine, heat and reflux at 90°C for 12h, alternately wash with toluene, acetone, methanol and then wash with distilled water, and vacuum dry at 60°C for 12h to obtain aminated silica gel. Take 4g of aminated silica gel and 80mL of toluene in a three-necked flask, N 2 Add 5 mL of acryloyl chloride dropwise under protection, stir for 10 min, then add 12 mL of triethylamine, stir and react at room temperature for 24 hours, wash the product with toluene, methanol, and deionized water several time...

Embodiment 2

[0047] Take 10g of silica gel and add it to 100mL of hydrochloric acid solution with a mass fraction of 5%, heat and reflux in an oil bath at 110°C for 15h, wash with acetone and absolute ethanol respectively, then wash with distilled water until neutral, and dry in vacuum at 130°C for 12h to obtain activation Silica gel. Add 3g of activated silica gel into 30mL of toluene solution, ultrasonically disperse and degas for 20min, N 2 Add 10mL KH-550 dropwise under protection, then add 5mL triethylamine, heat and reflux at 90°C for 10h, alternately wash with toluene, acetone, methanol, then wash with distilled water, and vacuum dry at 60°C for 12h to obtain aminated silica gel. Take 2g of aminated silica gel and 50mL of toluene in a three-necked flask, N 2 Add 4 mL of acryloyl chloride dropwise under protection, stir for 10 minutes, then add 10 mL of triethylamine, stir and react at room temperature for 20 hours, wash the product with toluene, methanol and deionized water several...

Embodiment 3

[0049]Take 20g of silica gel and add 200mL of hydrochloric acid solution with a mass fraction of 20%, heat and reflux in an oil bath at 130°C for 30h, wash with acetone and absolute ethanol respectively, then wash with distilled water until neutral, and vacuum dry at 160°C for 15h to obtain activated Silica gel. Take 10g of activated silica gel and add it to 80mL toluene solution, ultrasonically disperse and degas for 40min, N 2 Under protection, add 30mL KH-550 dropwise, then add 10mL triethylamine, heat and reflux at 120°C for 20h, alternately wash with toluene, acetone, methanol, then wash with distilled water, and vacuum dry at 80°C for 24h to obtain aminated silica gel. Take 6g of aminated silica gel and 120mL of toluene in a three-necked flask, N 2 Add 10 mL of acryloyl chloride dropwise under protection, stir for 10 min, then add 20 mL of triethylamine, stir and react at room temperature for 36 h, wash the product with toluene, methanol, and deionized water several tim...

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Abstract

The present invention discloses a silica surface molecularly imprinted polymer with specific adsorption of DEHP and a preparation method and application thereof. The imprinted polymer is subjected to by activation treatment silica surface; KH-550 is used for aminated graft on the silica gel surface to obtain aminated silica gel; acrylic acid chloride with aminated silica gel are subjected to an acylation reaction for double bond modification of the silica gel; then AIBN as initiator is used for polymerization of a so that template molecule DEHP with functional monomer and a crosslinking agent on the double bond modified silica surface; and the template molecules are eluted. The present invention uses a two-step reaction for silica surface modification, and overcomes self-polymerization of silane coupling agent in the process, so that the silica surface is uniformly grafted with structure containing C=C; the method is in favor of synthesis of molecularly imprinted polymers on the silica surface, so the molecularly imprinted polymer can be evenly and firmly coat on the silica surface to improve its stability, and can be reused when used as a solid-phase extraction agent.

Description

technical field [0001] The present invention relates to a molecularly imprinted polymer, in particular to a surface molecularly imprinted polymer suitable for selectively adsorbing the plasticizer DEHP (di(2-ethylhexyl) phthalate), and to the molecule The preparation method of imprinted polymer and its application in solid phase extraction belong to the field of preparation technology and application of environmental protection functional materials. Background technique [0002] Phthalates are a type of environmental endocrine disruptors, and are often used as plasticizers in materials such as resins, plastics, rubber, and adhesives to increase the elasticity, ductility, and softness of products. According to data, toys, food packaging materials, medical blood bags and hoses, cooking oil, dairy products, personal care products and other products are all contaminated by phthalate plasticizers. Phthalates are extremely difficult to degrade under natural conditions, and are ea...

Claims

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Application Information

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IPC IPC(8): C08F292/00C08F220/06C08F220/56C08F222/14C08F222/38B01J20/286B01J20/30B01D15/08
Inventor 陈芳艳杨占唐玉斌王新刚陈海丰
Owner JIANGSU UNIV OF SCI & TECH
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