Preparation method of grafted high-capacity dendrimer ion chromatography stationary phase packing

A dendrimer and ion chromatography technology, which is applied to the application field of the preparation of grafted high-capacity ion chromatography packing, can solve the problems of difficult separation, insurmountable, low separation degree of monosaccharides and disaccharides, etc., and achieves the synthesis cycle. Short, high capacity, high separation effect

Inactive Publication Date: 2017-11-21
ZHEJIANG UNIV
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  • Description
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Problems solved by technology

At present, there are many methods for the determination of sugars, but all of them have various deficiencies. The use of ion chromatography to measure sugars still has insurmountable problems.
Common monosaccharides or disaccharides such as fructose, glucose or sucrose are weakly acidic substances (pKa is about 12), and separation of monosaccharides and disaccharides by anion exchange chromatography will cause low separation and difficulty in separation. For this, we need Further Enhancement of Ion Chromatography Column Capacity and Selectivity

Method used

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  • Preparation method of grafted high-capacity dendrimer ion chromatography stationary phase packing
  • Preparation method of grafted high-capacity dendrimer ion chromatography stationary phase packing
  • Preparation method of grafted high-capacity dendrimer ion chromatography stationary phase packing

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preparation example Construction

[0027] The invention discloses a preparation method of a high-capacity dendrimer graft type ion chromatography stationary phase, comprising: preparation of dendrimers, polystyrene-divinylbenzene-glycidyl methacrylate (PS- The preparation of DVB-GMA) microspheres, the grafting of dendrimers on the surface of microspheres, the quaternization modification of dendrimers and the preparation of quaternized dendrimer grafted chromatographic stationary phase fillers, the present invention The specific technical scheme is as follows:

[0028] Using styrene-divinylbenzene-glycidyl methacrylate (PS-DVB-GMA) as the matrix, monodisperse linear polystyrene microsphere seeds were prepared by dispersion polymerization, and the activated The seeds synthesized polystyrene-divinylbenzene-glycidyl methacrylate (PS-DVB-GMA) microspheres with a large number of epoxy groups on the surface, and extracted to remove the porogen. Then the synthesized polyamide-amine dendrimers were grafted onto the sur...

Embodiment 1

[0036] Embodiment 1: The preparation process of grafted high-capacity dendrimer ion chromatography stationary phase packing is as follows, and its steps are:

[0037] 1. Preparation of PAMAM: Dissolve 2mL of ethylenediamine in 25mL of methanol, slowly add 25g of methyl acrylate under stirring in an ice-water bath, slowly raise the temperature to 28°C after the dropwise addition, and stir React for 24 hours to obtain 0.5G of PAMAM; dissolve 5g of 0.5GPAMAM in 25mL of methanol, and slowly add 15g of ethylenediamine dropwise under stirring in an ice-water bath. Macromolecules (1.0 GPAMAM).

[0038] 2, the preparation of polystyrene seed, synthetic particle diameter 1~3 μm monodisperse polystyrene seed by emulsion dispersion polymerization method, the concentration of monomeric styrene is 15% (m / m) of total amount, stabilizer polyvinylpyrrolidone Consumption is 2% (m / v) of reaction medium, and initiator azobisisobutyronitrile consumption is 1% (m / m) of monomer consumption, and re...

Embodiment 2

[0043] Embodiment 2: with reference to the method and steps of embodiment 1

[0044] 1. Preparation of PAMAM: Dissolve 2mL of ethylenediamine in 25mL of methanol, slowly add 25g of methyl acrylate under stirring in an ice-water bath, slowly raise the temperature to 28°C after the dropwise addition, and stir React for 24 hours to obtain 0.5G of PAMAM; dissolve 5g of 0.5GPAMAM in 25mL of methanol, and slowly add 15g of ethylenediamine dropwise under stirring in an ice-water bath. Macromolecules (1.0 GPAMAM).

[0045] 2, the preparation of polystyrene seed, synthetic particle diameter 1~3 μm monodisperse polystyrene seed by emulsion dispersion polymerization method, the concentration of monomeric styrene is 15% (m / m) of total amount, stabilizer polyvinylpyrrolidone Consumption is 2% (m / v) of reaction medium, and initiator azobisisobutyronitrile consumption is 1% (m / m) of monomer consumption, and reaction medium is dehydrated alcohol, and 60 ℃ of reaction temperatures, stirring s...

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Abstract

The present invention relates to a preparation method of a novel grafted high-capacity dendritic macromolecular ion chromatographic stationary phase filler, and provides a preparation method for a grafted high-capacity dendritic macromolecular ion chromatographic stationary phase, including an integer generation dendritic macromolecule Preparation, preparation of polystyrene-divinylbenzene-glycidyl methacrylate (PS-DVB-GMA) microspheres, grafting of dendrimers, quaternization of dendrimers and high-capacity dendrimers Preparation of macromolecule grafted anion chromatography packing. This method makes full use of a large number of epoxy groups on the surface of PS-DVB-GMA microspheres and a large number of terminal amine groups of integer-generation dendrimers to modify the surface of the microspheres. The reaction is fast, the cycle is short, the method is simple, and the synthesized The packing exchange capacity is high, the prepared ion chromatographic column has good resolution and high peak shape symmetry, and can be used for the separation of fluoride ions, organic acids and sugars.

Description

technical field [0001] The invention relates to a preparation method of ion chromatography, in particular to the application in the preparation of grafted high-capacity ion chromatography filler modified by dendritic macromolecular materials. Background technique [0002] Since the invention of ion chromatography in 1975, the development speed has always been among the best, and ion chromatography analysis technology is more and more widely used in the establishment of various complex analysis methods and the analysis of multi-component substances. Even so, ion chromatography methods still have great deficiencies in the analysis of certain substances. [0003] Fluoride ion is a nutritional trace element in the human body. Excessive fluoride ion will cause considerable harm to the human body and the environment. Therefore, accurate measurement of fluoride ion content is of great significance for environmental monitoring and human health. But, still there is very big deficien...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/286B01J20/30
Inventor 郭丹丹朱岩
Owner ZHEJIANG UNIV
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