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Highly cross-linked monodisperse epoxy-group-containing polymeric microsphere and preparation method thereof

An epoxy group, monodisperse technology, applied in the field of highly cross-linked monodisperse polymer microspheres and their preparation, can solve the problems of microspheres lack of active groups, unsuitable for chromatographic media, difficult to derivatize, etc., and achieve safe reaction conditions Reliable, cheap and easy to obtain raw materials, quick response effect

Inactive Publication Date: 2015-07-22
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent document CN 101306352A also prepared epoxy-containing polymer microspheres (5-10 μm) by seed swelling polymerization, but the resulting microspheres are non-crosslinked microspheres, which are not suitable as chromatographic media
However, the microspheres obtained by this method lack active groups, are not easy to derivatize, and are relatively hydrophobic, which is prone to non-specific adsorption.

Method used

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  • Highly cross-linked monodisperse epoxy-group-containing polymeric microsphere and preparation method thereof
  • Highly cross-linked monodisperse epoxy-group-containing polymeric microsphere and preparation method thereof
  • Highly cross-linked monodisperse epoxy-group-containing polymeric microsphere and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0036] A preparation method of highly cross-linked monodisperse polymer microspheres containing epoxy groups, comprising steps as follows:

[0037] (1) Add 2.18ml of divinylbenzene monomer, 0.51ml of glycidyl methacrylate and 0.20g of azobisisobutyronitrile into 32.31ml of acetonitrile. After mixing, add them to the polytetrafluoroethylene in the stainless steel reactor In the lining, nitrogen gas was introduced for 15 minutes, and after removing oxygen, it was sealed; then placed in an oil bath, the temperature of the oil bath was set at 85°C, and the reaction time was 4 hours;

[0038] (2) Stop heating, wash with 50ml of methanol, and dry at 50°C to constant weight to obtain polymer microspheres. Recording its average particle diameter is 4.41 μ m, polydispersity coefficient is 1.07, and productive rate is 83.1%, and the scanning electron micrograph of product polymer microsphere is as follows figure 1 shown.

Embodiment 2

[0040] A preparation method of highly cross-linked monodisperse polymer microspheres containing epoxy groups, comprising steps as follows:

[0041] (1) 4.19ml of divinylbenzene monomer, 0.44ml of glycidyl methacrylate and 0.35g of azobisisobutyronitrile were added to 30.37ml of acetonitrile, and after being miscible, they were added to the polytetrafluoroethylene of the stainless steel reactor In the lining, nitrogen gas was introduced for 15 minutes, and after removing oxygen, it was sealed; then placed in an oil bath, the temperature of the oil bath was set at 85°C, and the reaction time was 4 hours;

[0042] (2) Stop heating, wash with 50ml of methanol, and dry at 50°C to constant weight to obtain polymer microspheres. Recording its average particle diameter is 5.70 μ m, polydispersity coefficient is 1.04, and productive rate is 90.9%; The scanning electron micrograph of product polymer microsphere is as figure 2 shown.

Embodiment 3

[0044]A preparation method of highly cross-linked monodisperse polymer microspheres containing epoxy groups, comprising steps as follows:

[0045] (1) Add 3.21ml of divinylbenzene monomer, 1.29ml of glycidyl methacrylate and 0.35g of azobisisobutyronitrile into 30.5ml of acetonitrile. After mixing, add them to the polytetrafluoroethylene in the stainless steel reactor In the lining, nitrogen gas was introduced for 15 minutes, and after removing oxygen, it was sealed; then placed in an oil bath, the temperature of the oil bath was set at 85°C, and the reaction time was 4 hours;

[0046] (2) Stop heating, wash with 50ml of methanol, and dry at 50°C to constant weight to obtain polymer microspheres. Recording its average particle diameter is 5.82 μ m, polydispersity coefficient is 1.06, and productive rate is 92.5%; The scanning electron micrograph of product polymer microsphere is as image 3 shown.

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Abstract

The invention relates to a highly cross-linked monodisperse epoxy-group-containing polymer microsphere and a preparation method thereof. The microsphere contains an epoxy group, methacrylic acid glycidyl ester is used as a monomer, divinyl benzene (DVB) is used as a cross-linking agent, and the microsphere is obtained through polymerization; the particle size of the microsphere is 2 to 10 [mu]m, and the polydispersity index is 1.04 to 1.07. The preparation method comprises the following steps: (1), methacrylic acid glycidyl ester, the DVB and an initiating agent are together added into a solvent for uniform mixing, after nitrogen is introduced, sealing is performed, the reaction temperature is controlled to be 82 to 90 DEG C, and the reaction time lasts for 3 to 5 hours; (2), a reaction product obtained in the step (1) is washed and dried, so that the polymer microsphere is obtained. The polymer microsphere prepared by the invention contains the epoxy group, the epoxy group is an active group, derivative reaction is facilitated, and the problems of high hydrophobicity, high probability of non-specific adsorption can be solved.

Description

technical field [0001] The invention relates to a highly cross-linked monodisperse polymer microsphere containing epoxy groups and a preparation method thereof, belonging to the technical field of polymer materials. Background technique [0002] Liquid chromatography is an important purification and separation technique today. Highly cross-linked monodisperse polymer microspheres containing epoxy groups have become an important class of chromatographic media due to their advantages of easy derivatization, good rigidity, and small non-specific adsorption. [0003] At present, the methods for preparing monodisperse polymer microspheres containing epoxy groups for chromatography mainly include microporous membrane emulsification, seed swelling polymerization and precipitation polymerization. The microporous membrane emulsification method is to use a hydrophilic microporous glass membrane to prepare a uniform and stable oil / water emulsion, and then perform suspension polymeriza...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/32C08F212/36C08F2/00B01J13/14
Inventor 陈志勇丁园园张书香
Owner UNIV OF JINAN
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