A novel preparation method of grafted dendritic macromolecular microspheres

A technology of dendritic macromolecules and microspheres, which is applied in the field of ion chromatography preparation, can solve the problems of complicated process and limited quantity, and achieve the effects of uniform particle size, stable performance and long service life

Inactive Publication Date: 2018-01-09
ZHEJIANG UNIV
View PDF5 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, in the ion chromatography modification methods we often use, the number of ionic sites modified by surface agglomeration method and direct reaction on the surface of microspheres is limited by the surface area of ​​microspheres, and it is difficult to further improve column efficiency. [1] , if you want to obtain a stationary phase with a higher capacity, you can only obtain more ionic sites by grafting layer by layer, and this method is through repeated reactions, grafting layer by layer, the process is very complicated [2]

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
  • A novel preparation method of grafted dendritic macromolecular microspheres
  • A novel preparation method of grafted dendritic macromolecular microspheres

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0034] The invention discloses a preparation method of a dendrimer graft type ion chromatography stationary phase, comprising: preparation of 1.0G dendrimer, preparation of polystyrene divinylbenzene microspheres, dendrimer and microsphere The grafting of spheres, the quaternization modification of dendrimers and the preparation of quaternized dendrimer grafted anion chromatographic fillers, using polystyrene-divinylbenzene as the matrix, prepared by dispersion polymerization For the dispersed linear polystyrene microsphere seeds, after the seeds are activated, the polystyrene-divinylbenzene microspheres are synthesized by a single-step seed swelling method, and the porogen is removed by extraction. Then by chemical grafting method, polyamide-amine (PAMAM) dendrimers are grafted onto the surface of microspheres and modified by quaternization with 1,4-butanediol glycidyl ether; , the specific preparation steps are:

[0035] a. Preparation of 1.0GPAMAM dendrimers by divergent m...

Embodiment 1

[0045] Embodiment 1: The preparation process of 1.0GPAMAM grafted polystyrene-divinylbenzene anion chromatography stationary phase packing is as follows, and its steps are:

[0046] 1. Preparation of 0.5GPAMAM: Dissolve 2mL of ethylenediamine in 20mL of methanol, slowly add 23g of methyl acrylate under stirring in an ice-water bath, slowly raise the temperature to 25°C after the dropwise addition, and stir for 24 hours to obtain 0.5G of PAMAM .

[0047] 2. Preparation of 1.0 GPAMAM: Dissolve 5 g of 0.5 GPAMAM in 20 mL of methanol, slowly add 15 g of ethylenediamine dropwise under stirring in an ice-water bath, slowly raise the temperature to 25°C after the addition, and stir for 24 hours to obtain 1.0 g of PAMAM.

[0048] 3, the preparation of polystyrene seed, synthetic particle diameter 1~3 μ m monodisperse polystyrene seed by emulsion dispersion polymerization method, the concentration of monomeric styrene is 5% (m / m) of total amount, stabilizing agent polyvinylpyrrolidone ...

Embodiment 2

[0053] Embodiment 2: with reference to the method and steps of embodiment 1

[0054] 1. Preparation of 0.5GPAMAM: Dissolve 2mL of ethylenediamine in 20mL of methanol, slowly add 23g of methyl acrylate under stirring in an ice-water bath, slowly raise the temperature to 25°C after the dropwise addition, and stir for 24 hours to obtain 0.5G of PAMAM .

[0055] 2. Preparation of 1.0 GPAMAM: Dissolve 5 g of 0.5 GPAMAM in 20 mL of methanol, slowly add 15 g of ethylenediamine dropwise under stirring in an ice-water bath, slowly raise the temperature to 25°C after the addition, and stir for 24 hours to obtain 1.0 g of PAMAM.

[0056] 3, the preparation of polystyrene seed, synthetic particle diameter 1~3 μ m monodisperse polystyrene seed by emulsion dispersion polymerization method, the concentration of monomeric styrene is 5% (m / m) of total amount, stabilizing agent polyvinylpyrrolidone Consumption is 0.5% (m / v) of reaction medium, and initiator azobisisobutyronitrile consumption i...

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
particle diameteraaaaaaaaaa
particle diameteraaaaaaaaaa
Login to view more

Abstract

The invention discloses a preparation method of a novel grafted dendrimer microsphere, and provides a preparation method of the first generation (1.0G) dendrimer grafted ion chromatography stationary phase, including: 1.0G dendrimer Preparation of macromolecules, preparation of polystyrene divinylbenzene microspheres, grafting of dendrimers and microspheres, quaternization modification of dendrimers and grafted anion chromatography of quaternized dendrimers Preparation of filler. The method makes full use of the branched structure of the dendritic macromolecule to modify the surface of the microsphere, has the advantages of fast reaction, short period, simple method and excellent performance of the synthesized filler.

Description

technical field [0001] The invention relates to a preparation method of ion chromatography, in particular to a preparation method of novel grafted dendritic macromolecular microspheres, and the application of the first generation of dendritic macromolecular materials in the preparation of surface grafted ion chromatography fillers. Background technique [0002] As one of the core components affecting the separation effect of ion chromatography, ion chromatography packing is mainly composed of two parts: insoluble matrix and ionic part of stationary phase. Among them, the matrix can be divided into two types: organic matrix and inorganic matrix, and the ionic part of the stationary phase is mainly completed by chemical modification of the stationary phase. The main chemical modification methods are: chemical grafting method, surface agglomeration method and direct reaction modification on the surface of microspheres. At present, in the ion chromatography modification methods...

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 Patents(China)
IPC IPC(8): C08G81/02B01J20/26B01J20/30B01J13/02B01J20/281
Inventor 郭丹丹朱岩
Owner ZHEJIANG UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap