Preparation method of anion exchange chromatography stationary phase

A technology of exchange chromatography and anion, applied in the field of preparation of anion exchange chromatography stationary phase, can solve the problems of acid and alkali resistance, difficult chemical modification, poor chemical stability, etc., and achieves low cost, wide pH tolerance range, and reactivity strong effect

Inactive Publication Date: 2016-05-25
杭州飞山浩科技有限公司
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Problems solved by technology

[0005] The present invention aims at the disadvantages that the chromatographic filler matrix inorganic silica gel is not resistant to acid and alkali, has poor chemical stability, and the existing highly cross-linked styrene-divinylbenzene copolymer microspheres are not easy to be chemically modified, and prepare

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  • Preparation method of anion exchange chromatography stationary phase
  • Preparation method of anion exchange chromatography stationary phase
  • Preparation method of anion exchange chromatography stationary phase

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preparation example Construction

[0022] The invention provides a method for preparing an anion-exchange chromatography stationary phase, including the preparation of monodisperse seed microspheres, the preparation of highly cross-linked glycidyl methacrylate-divinylbenzene copolymer microspheres and the preparation of anion-exchange chromatography stationary phase . The specific technical scheme is as follows:

[0023] The invention adopts a dispersion polymerization method to prepare monodisperse linear polystyrene seed microspheres; adopts a two-step seed swelling method to prepare highly cross-linked glycidyl methacrylate-divinylbenzene copolymer microspheres; Amine, trimethylamine, diethylamine, triethylamine and 1,4-butanediol diglycidyl ether were used as raw materials to modify highly cross-linked glycidyl methacrylate-divinylbenzene copolymer microspheres. Introduce quaternary ammonium functional groups on the surface of glycidyl acrylate-divinylbenzene copolymer microspheres; use the homogenate meth...

Embodiment 1

[0034]Embodiment 1: The preparation steps of highly cross-linked glycidyl methacrylate-divinylbenzene copolymerized microspheres weakly acidic cationic stationary phase are:

[0035] 1. First prepare monodisperse linear polystyrene seed microspheres with a particle size of about 1.8 μm by dispersion polymerization. The reaction medium is a mixed solution of ethanol and water, and the amount of ethanol is 75% (v / v); the amount of monomer styrene is the reaction 5% (m / m) of the medium consumption, the stabilizer polyvinylpyrrolidone consumption is 0.5% (m / m) of the reaction medium consumption, and the initiator azobisisobutyronitrile consumption is 1% (m / m) of the monomer consumption ), the reaction temperature is 40°C, the stirring speed is 100r / min, and the reaction time is 12h;

[0036] 2. Monodisperse highly cross-linked glycidyl methacrylate-divinylbenzene copolymer microspheres with a cross-linking degree of 75% were prepared by two-step seed swelling method. Seed microsp...

Embodiment 2

[0040] Embodiment 2: with reference to the method and steps of embodiment 1

[0041] 1. Synthesize 1.8 μm monodisperse polystyrene seed microspheres with a particle size of 1.8 μm earlier by dispersion polymerization, the reaction medium is a mixed solution of ethanol and water, and the amount of ethanol is 100% (v / v); the concentration of monomer styrene is the total amount 30% (m / m), the stabilizing agent polyvinylpyrrolidone consumption is 4% (m / v) of reaction medium, and initiator azobisisobutyronitrile consumption is 5% (m / m) of monomer consumption, reaction temperature 85°C, the stirring speed is 400r / min, and the reaction time is 16 hours;

[0042] 2. Monodisperse highly cross-linked glycidyl methacrylate-divinylbenzene copolymer microspheres with a cross-linking degree of 40% were prepared by two-step seed swelling method. Seed microsphere 0.6g, the consumption of monomer glycidyl methacrylate is 10% (m / m) of total organic phase consumption, and crosslinking agent div...

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Abstract

The invention discloses a preparation method of an anion exchange chromatography stationary phase using highly-crosslinked glycidyl methacrylate-divinyl benzene microspheres as a matrix. The preparation method includes: adopting a dispersion polymerization method to prepare monodispersed linear polystyrene seed microspheres; adopting a two-step seed swelling method to prepare highly-crosslinked glycidyl methacrylate-divinyl benzene copolymer microspheres; using methylamine, dimethylamine, trimethylamine, diethylamine, triethylamine and 1, 4-butane dioldiglycidyl ether as reaction raw materials to modify the highly-crosslinked glycidyl methacrylate-divinyl benzene copolymer microspheres to prepare the anion exchange chromatography stationary phase.

Description

technical field [0001] The invention relates to a chemical preparation method, in particular to a preparation method of anion-exchange chromatographic stationary phase. Background technique [0002] As a well-known stationary phase matrix, silica gel has the characteristics of strong mechanical strength and easy chemical modification, and has been widely used in reversed-phase chromatography stationary phase system; however, silica gel matrix can tolerate a limited range of pH values ​​(usually 2- 8), there are restrictions on the acidity and alkalinity of the mobile phase, which hinders its further application. The polymer stationary phase, such as highly cross-linked styrene-divinylbenzene organic polymer, can tolerate a wide range of pH values ​​and has relatively good mechanical strength, and has been widely used in ion chromatography stationary phase systems; at the same time, single Dispersed micron-sized polymer microspheres are used as chromatographic fillers, which...

Claims

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Application Information

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IPC IPC(8): B01J20/286B01J20/30
CPCB01J20/286B01J2220/52
Inventor 刘军伟钟乃飞朱岩
Owner 杭州飞山浩科技有限公司
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