Preparation method of surface-grafted type anion chromatographic filling material

An anion chromatography and surface grafting technology, applied in anion exchange, chromatographic anion exchanger, ion exchange, etc., can solve the problems of small capacity of anion chromatography column, uneven filler ball diameter, complicated preparation process, etc., and achieve low cost , Narrow particle size distribution, good chemical stability

Inactive Publication Date: 2012-06-20
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The most widely used chromatographic packing is the latex agglomerated chromatographic packing. The surface agglomerated anion chromatographic packing has the advantages of high separation efficiency and fast analysis speed. The column capacity of the column is small, and it is not resistant to acid and alkali.

Method used

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  • Preparation method of surface-grafted type anion chromatographic filling material
  • Preparation method of surface-grafted type anion chromatographic filling material
  • Preparation method of surface-grafted type anion chromatographic filling material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1: the making process of surface grafted polystyrene-divinylbenzene filler is as follows, and its steps are:

[0026] 1. Synthesize monodisperse polystyrene seeds with a particle size of 1 to 3 μm by emulsion dispersion polymerization, the concentration of monomeric styrene is 5 to 30% (m / m) of the total amount, and the amount of stabilizer polyvinylpyrrolidone is the reaction medium 0.5-4% (m / v), the amount of initiator azobisisobutyronitrile is 1-5% (m / m) of the amount of monomer, the reaction medium is aqueous ethanol, and the concentration is 75-100% (v / v), the reaction temperature is 40-85°C, the stirring speed is 100-400 rpm, and the reaction time is 8-24 hours;

[0027]2. Then prepare monodisperse polystyrene-divinylbenzene microspheres with a crosslinking degree of 10-75% by a seed swelling method. The concentration of monomer styrene is 10-20% (m / m) of the total organic phase, and the range of cross-linking degree of the composite microspheres is 1...

Embodiment 2

[0031] Embodiment 2: with reference to the method and steps of embodiment 1

[0032] 1. Synthesize monodisperse polystyrene seeds with a particle size of 1.6 μm by emulsion dispersion polymerization, 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), initiator azobisisobutyronitrile consumption is 2.2% (m / m) of monomer consumption, reaction medium is 90% ethanol aqueous solution, 80 ℃ of reaction temperature, stirring speed, at 300 rev / mins, reaction Time 24 hours;

[0033] 2. Then prepare monodisperse polystyrene-divinylbenzene microspheres with a crosslinking degree of 50% by seed swelling method. Monomer styrene concentration is 14% (m / m), emulsifier sodium lauryl sulfate consumption is 2.5% (m / m), stabilizer polyvinyl alcohol consumption is 1.5% (m / m), initiator over The amount of benzoyl oxide is 0.8% (m / m), the amount of porogen toluene is 50% (m / m), the swelli...

Embodiment 3

[0038] 1. Synthesize monodisperse polystyrene seeds with a particle size of 1.6 μm by emulsion dispersion polymerization, 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), initiator azobisisobutyronitrile consumption is 2.2% (m / m) of monomer consumption, reaction medium is 90% ethanol aqueous solution, 80 ℃ of reaction temperature, stirring speed, at 300 rev / mins, reaction Time 24 hours;

[0039] 2. Then prepare monodisperse polystyrene-divinylbenzene microspheres with a degree of crosslinking of 50% by the seed swelling method, the monomer styrene concentration is 14% (m / m), and the emulsifier lauryl sulfate Sodium consumption is 2.5% (m / m), stabilizer polyvinyl alcohol consumption is 1.5% (m / m), initiator benzoyl peroxide consumption is 0.8% (m / m), porogen toluene consumption is 50% % (m / m), the swelling ratio is 55 times, the emulsification temperature is 20°C, th...

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Abstract

The invention relates to an anion chromatographic column and a preparation method thereof, and particularly relates to a preparation method of a surface-grafted type anion chromatographic filling material. The preparation method of a novel surface-grafted type anion chromatographic filling material comprises the steps of: preparing monodispersed linear polystyrene microsphere seeds with polystyrene-divinylbenzene as a medium by adopting a dispersion polymerization method, activating the seeds, synthesizing polystyrene-divinylbenzene microspheres by adopting a single-step seed swelling method,and extracting to remove the pore-forming agent. According to the invention, the preparation method of the polystyrene-divinylbenzene microspheres is low in cost and simple in process; and the prepared filling material is uniform in particle size, narrow in particle size distribution and good in chemical stability, and needs no screening.

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 filler. Background technique [0002] As one of the branches of high performance liquid chromatography, ion chromatography is mainly used for the separation of anions and cations, and is one of the fastest-growing analytical methods in the field of chromatography. Because of its high sensitivity to the analysis of common anions and cations, especially the ability to analyze different valence ions of the same metal, it has been widely used in food, electric power, environment, semiconductor, pharmaceutical and chemical industries and other fields. Ion chromatography packings consist of an insoluble matrix and fixed charged ionic moieties, the selectivity of which depends mainly on the nature of the chromatographic stationary phase. At present, the stationary phases widely used in the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J41/20B01J41/12B01J41/14
Inventor 黄忠平朱岩
Owner ZHEJIANG UNIV
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