Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method and application method of naphthidine molecularly-imprinted polymer

A technology for imprinting polymers and binaphthylamine molecules is applied in separation methods, chemical instruments and methods, solid adsorbent liquid separation, etc. simple method effect

Inactive Publication Date: 2012-01-11
HARBIN ENG UNIV
View PDF0 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the existing literature, there are few reports on the use of molecularly imprinted polymers as chromatographic immobilizers for chiral separation of racemic DABN, and so far there has been no report of a separation factor of 2.4

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method and application method of naphthidine molecularly-imprinted polymer
  • Preparation method and application method of naphthidine molecularly-imprinted polymer
  • Preparation method and application method of naphthidine molecularly-imprinted polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1. Preparation of Molecularly Imprinted Polymers

[0024] In a 100mL two-necked flask, add S-DABN (0.5mmol, 0.1422g) and MAA (2mmol, 0.17mL), then add acetonitrile: chloroform (1: 2, v / v) mixed solvent 6mL, make S-DABN and The MAA was completely dissolved, and nitrogen gas was passed for 5 minutes under ultrasonic conditions to remove oxygen and sealed. Pre-polymerize at 18°C ​​for 10 hours under normal pressure to allow S-DABN and MAA to fully react to form a complex, add EDMA (10mmol, 1.89mL) and AIBN (20mg), and then pass nitrogen gas under ultrasonic conditions for 5 minutes to remove residual oxygen ,seal. Then place it in a constant temperature water bath at 60°C for 12 hours to initiate thermal polymerization to obtain a block molecularly imprinted polymer. Take out the block polymer, grind it, grind it, pass through a 60 μm-20 μm sieve, and settle it with acetone three times to remove very fine particles. , dried under vacuum at 60°C to obtain the S-DABN molec...

Embodiment 2

[0029] 1. Preparation of Molecularly Imprinted Polymers

[0030] In a 100mL two-necked flask, add S-DABN (0.5mmol, 0.1422g) and MAA (2mmol, 0.17mL), then add acetonitrile: chloroform (1: 1, v / v) mixed solvent 6mL, make S-DABN and The MAA was completely dissolved, and nitrogen gas was passed for 5 minutes under ultrasonic conditions to remove oxygen and sealed. Pre-polymerize at 18°C ​​for 10 hours under normal pressure to allow S-DABN and MAA to fully react to form a complex, add EDMA (10mmol, 1.89mL) and AIBN (20mg), and then pass nitrogen gas under ultrasonic conditions for 5 minutes to remove residual oxygen ,seal. Then place it in a constant temperature water bath at 60°C for 12 hours to initiate thermal polymerization to obtain a block molecularly imprinted polymer. Take out the block polymer, grind it, grind it, pass through a 60 μm-20 μm sieve, and settle it with acetone three times to remove very fine particles. , dried under vacuum at 60°C to obtain the S-DABN molec...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
separation factoraaaaaaaaaa
Login to View More

Abstract

The invention provides a preparation method and application method of a naphthidine molecularly-imprinted polymer. The preparation method provided by the invention comprises the following steps: dissolving S-1,1-binaphthyl-2-amine and methacrylic acid into a pore-forming agent, then feeding nitrogen for 5 minutes under an ultrasonic condition, and then carrying out pre-polymerization for 10 hours at the temperature of 18 DEG C and at normal pressure, so that the S-1,1-binaphthyl-2-amines and the methacrylic acid fully act so as to form a compound; adding ethylene glycol dimethacrylate and azo-bis-iso-butyrynitrile, and then feeding nitrogen for 5 minutes under the ultrasonic condition; placing the obtained product in a water bath kettle at the constant temperature of 60 DEG C to polymerize for 12 hours so as to obtain a bulk molecularly-imprinted polymer; crushing and grinding the obtained bulk molecularly-imprinted polymer; sieving with a sieve of 60mu m-20mu m meshes, and then carrying out repeated settlement with acetone to remove ultra-fine particles; and drying so as to obtain the naphthidine molecularly-imprinted polymer. As a HPLC (high performance liquid chromatography) stationary phase, the imprinted polymer can achieve the chiral separation of racemic DABN (1,1-binaphthyl-2-amine), and the separation factor of the imprinted polymer on the racemic DABN can reach 2.4. The preparation method provided by the invention is high in separation performance, low in cost, simple in operation, and good in stability.

Description

technical field [0001] The invention relates to a preparation method of an imprinted polymer. The invention also relates to the application of an imprinted polymer as the stationary phase of liquid chromatography in the chiral resolution of racemic DABN. Background technique [0002] 1,1-Binaphth-2-amine (DABN) is an important precursor of chiral reagents and chiral catalysts with C2 symmetry factors, and its optically active isomers and their derivatives have been widely used in asymmetric synthesis , the alkylation reaction of aldehydes of some important compounds, the asymmetric allylation reaction of aldehydes, the asymmetric allylic substitution reaction, and the synthesis of chiral lactones all require the participation of single enantiomer DABN or its derivatives . Therefore, there is an increasing demand for single enantiomer DABN. At present, the resolution of racemic DABN is often obtained by chromatographic resolution methods, mainly capillary electrophoresis (...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C08F265/02C08F2/44C08J9/26B01J20/285B01J20/30B01D15/10
Inventor 董红星王艳辉李俊青佟飞王振兴沈贤德
Owner HARBIN ENG UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com