Preparation method of surface-grafting anion chromatography stationary phase

An anion chromatography and surface grafting technology, which is applied in the field of preparation of surface grafted anion chromatography stationary phase, can solve the problems of low rigidity of organic matrix fillers, non-specific irreversible adsorption, easy expansion and contraction, etc., and achieve low cost , Narrow particle size distribution, uniform filler particle size

Inactive Publication Date: 2013-02-27
ZHEJIANG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The present invention aims at the shortcomings of inorganic matrix fillers that are not resistant to acid and alkali, poor chemical stability, easy to produce non-specific and irreversible adsorption, and organic matrix fillers have low rigidity, complex pore structure, and easy expansion and contraction. Improvement, providing a new method for preparing surface-grafted anion chromatography stationary phase

Method used

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  • Preparation method of surface-grafting anion chromatography stationary phase
  • Preparation method of surface-grafting anion chromatography stationary phase
  • Preparation method of surface-grafting anion chromatography stationary phase

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Embodiment 1

[0029] Embodiment 1: the making process of surface grafted polystyrene-divinylbenzene-glycidyl methacrylate filler is as follows, and its steps are:

[0030] 1. Synthesize monodisperse linear polystyrene seeds with a particle size of 1~3μm by dispersion polymerization first, the reaction medium is ethanol aqueous solution, the concentration is 75~100% (v / v), and the concentration of monomeric styrene is 5% of the total ~30% (m / m), the dosage of stabilizer polyvinylpyrrolidone is 0.5~4% (m / v) of the reaction medium, and the dosage of initiator azobisisobutyronitrile is 1~5% of the monomer dosage (m / m), the reaction temperature is 40~85°C, the stirring speed is 100~400 rpm, and the reaction time is 8~24 hours;

[0031] 2. Then prepare monodisperse polystyrene-divinylbenzene-glycidyl methacrylate microspheres with a crosslinking degree of 10-75% by seed swelling method. The monomer styrene concentration is 10~20% (m / m) of the total organic phase, and the monomer glycidyl methac...

Embodiment 2

[0035] Embodiment 2: with reference to the method and steps of embodiment 1

[0036] 1. Synthesize monodisperse polystyrene seeds with a particle size of 1.8 μm by dispersion polymerization first, the concentration of monomeric styrene is 25% (m / m) of the total amount, and the amount of stabilizer polyvinylpyrrolidone is 1.6% of the reaction medium ( m / v), the amount of initiator azobisisobutyronitrile is 2.2% (m / m) of the monomer amount, the reaction medium is 90% ethanol aqueous solution, the reaction temperature is 80°C, the stirring speed is 300 rpm, and the reaction time 24 hours;

[0037] 2. Then monodisperse polystyrene-divinylbenzene-glycidyl methacrylate microspheres with a crosslinking degree of 50% were prepared by the seed swelling method. The monomer styrene concentration is 14% (m / m), the monomer glycidyl methacrylate concentration is 3% (m / m) of the total organic phase, and the amount of emulsifier sodium lauryl sulfate is 2.5% (m / m), the amount of stabilizer...

Embodiment 3

[0042] 1. Synthesize monodisperse polystyrene seeds with a particle size of 1.8 μm by dispersion polymerization first, the concentration of monomeric styrene is 25% (m / m) of the total amount, and the amount of stabilizer polyvinylpyrrolidone is 1.6% of the reaction medium ( m / v), the amount of initiator azobisisobutyronitrile is 2.2% (m / m) of the monomer amount, the reaction medium is 90% ethanol aqueous solution, the reaction temperature is 80°C, the stirring speed is 300 rpm, and the reaction time 24 hours;

[0043] 2. Then, monodisperse polystyrene-divinylbenzene-glycidyl methacrylate microspheres with a crosslinking degree of 50% were prepared by the seed swelling method, and the monomer styrene concentration was 14% (m / m). The concentration of monomeric glycidyl methacrylate is 2% (m / m) of the total organic phase, the amount of emulsifier sodium lauryl sulfate is 2.5% (m / m), and the amount of stabilizer polyvinyl alcohol is 1.5% ( m / m), the amount of initiator benzoyl pe...

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Abstract

The invention relates to an anion chromatographic column a preparation method thereof, particularly relates to a preparation method of a surface-grafting anion chromatography stationary phase. The method disclosed herein is characterized by: preparing monodispersed linear polystyrene microspheres seeds by dispersion polymerization, activating the seeds, then synthesizing polystyrene-divinyl benzene-glycidyl methacrylate microballoons by one-step seed swelling method, and extracting to remove the pore forming agent; adopting multi-step grafting synthetic method, taking methylamine and 1,4-butanediol diglycidyl ether as raw materials, and introducing a large amount of positively charged quaternary ammonium groups as the anion exchange functional group to the surface of the prepared polystyrene-divinyl benzene-glycidyl methacrylate microballoons; and packing by homogenate method. According to the invention, the method disclosed herein has the advantages of low cost and simple process, the prepared filling material has uniform granularity and has no need to be screened, and the particle size distribution is narrow.

Description

technical field [0001] The invention relates to an anion chromatographic column and a preparation method thereof, in particular to a preparation method of a surface-grafted anion chromatographic stationary phase. Background technique [0002] Ion chromatography (abbreviated as IC) is a kind of high performance liquid chromatography. With the popularization of chromatography technology, it is gradually applied to various fields. Now it has been widely used in environmental monitoring, electric power and energy industry, food and beverage industry, electronics industry, and life science field. , chemical industry and pharmaceutical industry are widely used. In 1975, H.Small and his collaborators published the first paper on ion chromatography, and in the same year, commercial instruments came out. Ion chromatography separation methods can be divided into high-efficiency ion-exchange chromatography, ion-exclusion chromatography, and ion-pair chromatography. Ion chromatography...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/30B01J20/26B01J20/281
Inventor 黄忠平朱岩
Owner ZHEJIANG UNIV
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