Method for preparing highly crosslinked polystyrene microsphere by stable dispersion polymerization of charge

A polystyrene microsphere and dispersion polymerization technology, which is applied in the field of polymer microsphere materials, can solve the problems of low crosslinking degree of microspheres, and achieve the effect of simple and easy preparation method, fast reaction speed and increased crosslinking degree

Inactive Publication Date: 2010-10-20
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Kobayashi et al. (Kobayashi K, Senna M.J.Appl.Polym.Sci., 1992,46:27) used seed dispersion polymerization to prepare highly crosslinked polymer particles; Song et al. (Song JS, WinnikMA.Macromolecules, 2005, 38 : 8300) reported a two-step dispersion polymerization method to prepare crosslinked polystyrene microspheres, that is, after the nucleation period, the crosslinking agent was added to the reaction system, and 3wt% divinylbenzene or 6wt% dimethyl Polyethylene glycol acrylate can still prepare monodisperse polystyrene microspheres; the Chinese patent with the publication number CN 101058617A discloses the preparation of polystyrene microspheres in a polyvinylpyrrolidone stable dispersion polymerization system by adding divinylbenzene dropwise afterward. Linked polystyrene microspheres, the degree of cross-linking of the microspheres was increased to 12.94%, but the degree of cross-linking of the prepared microspheres was still far lower than that prepared by emulsion polymerization

Method used

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  • Method for preparing highly crosslinked polystyrene microsphere by stable dispersion polymerization of charge
  • Method for preparing highly crosslinked polystyrene microsphere by stable dispersion polymerization of charge
  • Method for preparing highly crosslinked polystyrene microsphere by stable dispersion polymerization of charge

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Experimental program
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Effect test

Embodiment 1

[0024] Styrene (St) 5.0ml, crosslinking agent divinylbenzene 0.02265g, initiator azobisisobutyronitrile 0.0453g, stabilizer methacryloyloxyethyltrimethylammonium chloride 0.0906g, methanol 40ml , 10ml of deionized water was added into a 250ml three-neck flask, then it was placed in a water bath, a condensate pipe was installed and the mechanical stirring was turned on (rotating speed was 200rpm). Turn on the heating device, keep the reaction temperature at 75°C, and react for 8 hours. After the reaction, the polystyrene microspheres were separated from the emulsion by centrifugation (3500 rpm, 30 min), and then placed in a vacuum oven at 50° C. for drying. Before test characterization, the particles were washed three times with methanol to remove oligomers adsorbed on the surface of the microspheres.

[0025] Gained polystyrene microsphere particle size is 650nm, and particle size distribution coefficient is 5.63%, and productive rate is 75.48%, and gel content is 35.25%, and...

Embodiment 2

[0027] St 7.5ml, crosslinking agent divinylbenzene 0.1812g, initiator azobisisobutyronitrile 0.0906g, stabilizer methacryloyloxyethyltrimethylammonium chloride 0.0453g, methanol 42.5ml, deionized Add 7.5ml of water into a 250ml three-neck flask, then place it in a water bath, install a condensate pipe and turn on mechanical stirring (rotating speed is 200rpm). Turn on the heating device, keep the reaction temperature at 75°C, and react for 8 hours. After the reaction, the polystyrene microspheres were separated from the emulsion by centrifugation (3500 rpm, 30 min), and then placed in a vacuum oven at 50° C. for drying. Before test characterization, the particles were washed three times with methanol to remove oligomers adsorbed on the surface of the microspheres.

[0028] Gained polystyrene microsphere particle size is 700nm, and particle size distribution coefficient is 2.99%, and productive rate is 75.15%, and gel content is 84.16%, and glass transition temperature is 108....

Embodiment 3

[0030] St 5.0ml, crosslinking agent divinylbenzene 0.3624g, initiator azobisisobutyronitrile 0.0906g, stabilizer methacryloyloxyethyltrimethylammonium chloride 0.01133g, methanol 40ml, deionized water 10ml was added into a 250ml three-neck flask, then it was placed in a water bath, a condensate pipe was installed and the mechanical stirring was turned on (rotating speed was 200rpm). Turn on the heating device, keep the reaction temperature at 75°C, and react for 8 hours. After the reaction, the polystyrene microspheres were separated from the emulsion by centrifugation (3500 rpm, 30 min), and then placed in a vacuum oven at 50° C. for drying. Before test characterization, the particles were washed three times with methanol to remove oligomers adsorbed on the surface of the microspheres.

[0031]The particle size of the obtained polystyrene microspheres is 740nm, the particle size distribution coefficient is 2.45%, the yield rate is 70.15%, the gel content is 85.84%, the DSC c...

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Abstract

The invention relates to a preparation method of a single-dispersion highly crosslinked polystyrene microsphere, belonging to the field of polymer microsphere materials. The preparation method is characterized in that a polymerizable charged micromolecule monomer is used as a stabilizing agent, polymer particles are stabilized through the static function of a charge, and then the crosslinked polystyrene microsphere is prepared by adopting a one-step charging method. The preparation method comprises the following steps of: adding the stabilizing agent and an initiator in a container, then adding a methanol/water mixing solvent, monomer styrene and divinylbenzene as a cross-linking agent, heating to 75 DEG C, stirring for dispersion polymerization, reacting for 8h, and then centrifugally separating and drying products, wherein the stabilizing agent is methacrylatoethyl trimethyl ammonium chloride or sodium p-styrene sulfonate. The invention can improve the gel content of the microsphere to 85.84% by adopting the one-step charging method to prepare the polystyrene microsphere capable of basically keeping the shape in tetrahydrofuran, the particle size of the microsphere is 0.5-1.5 micrometers, and the polystyrene microsphere can be used in the fields of chromatographic separation, biomedicine, coatings and the like.

Description

technical field [0001] The invention relates to a preparation method of monodisperse highly cross-linked polystyrene microspheres, belonging to the field of polymer microsphere materials. Background technique [0002] Cross-linked polymer microspheres have high strength and good heat resistance and solvent resistance, so they are widely used in chromatographic column packing, sliding boosters, biochemical separation, polymer catalysis, etc. There are many ways to prepare cross-linked polymer particles, among which emulsion polymerization and seed emulsion polymerization are the most commonly used methods. The particle size of the microspheres prepared by the former is generally less than 1 μm, which cannot meet certain application fields. The operation steps of the latter are lengthy and the process cumbersome; etc. (LiK, HDH.J.Polym.Sci.Part A: Polym.Chem., 1993, 31:3257) prepared highly cross-linked polydivinylbenzene microspheres in acetonitrile solvent by means of pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F212/08C08F2/12
Inventor 杨万泰张芬马育红
Owner BEIJING UNIV OF CHEM TECH
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