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Polymer microsphere and preparation method thereof

A polymer and microsphere technology, applied in the preparation of microspheres, microcapsule preparations, etc., can solve the problems of low epoxy group content, poor mechanical properties, reduced mechanical properties, etc., and achieve strong impact resistance, high mechanical strength, The effect of good stability

Inactive Publication Date: 2011-09-14
SUZHOU UNIV +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the research on polymer microspheres is mostly cross-linked polymerization of glycidyl methacrylate and other monomers to form polymer microspheres directly containing epoxy groups on the surface. For example, in the Chinese invention patent (CN101288844A), GMA polymer The polymer microsphere is a cross-linked homopolymer of polyglycidyl methacrylate or a cross-linked copolymer microsphere of glycidyl methacrylate and olefin to obtain a polymer microsphere directly containing epoxy groups on the surface, such The epoxy group content on the surface of the microsphere is relatively small, and the content is not easy to control. Since the epoxy group is also contained inside the microsphere, the surface modification will also affect the internal structure and reduce the mechanical properties to a certain extent.
In the prior art, there are also polychloromethylstyrene microspheres (Journal of Chromatography B, 877, 2009, 1479-1486) that directly contain ATRP initiator molecules on the surface of GMA modification, and the mechanical properties of this class of microspheres themselves are relatively low. Poor, its initiator molecules not only exist on the surface, but also contain initiator molecules inside, so it is possible to initiate GMA polymerization, and this internal polymerization will further reduce the mechanical properties of the microspheres

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  • Polymer microsphere and preparation method thereof
  • Polymer microsphere and preparation method thereof
  • Polymer microsphere and preparation method thereof

Examples

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Embodiment 1

[0025] This embodiment provides a method for preparing polymer microspheres, comprising the following steps:

[0026] 1. Microsphere surface bonds and initiator molecules

[0027] Monodisperse polystyrene-divinylphenyl spheres with a cross-linking degree of 80% and a particle size of 10 microns and α-haloacyl halide, catalyst (the molar ratio of catalyst to α-haloacyl halide is 1:1) and an appropriate amount of solvent, and stirred at 40° C. for 24 hours to obtain microspheres of surface bonds and initiator molecules.

[0028]In this example, the α-haloacyl halide can be selected from α-bromobutyryl bromide, α-bromoisobutyryl bromide, α-bromopropionyl bromide, α-chlorobutyryl bromide, α-chloro One of isobutyryl bromide or α-chloropropionyl bromide. Catalyst can choose FeCl 3 , SnCl 4 , BF 3 , ZnCl 2 Or one of AlCl. The solvent can be selected from one of dichloromethane, 1,2-dichloroethane, carbon disulfide or nitrobenzene.

[0029] 2. Grafting polyglycidyl methacrylat...

Embodiment 2

[0042] This embodiment provides a method for preparing polymer microspheres, comprising the following steps:

[0043] 1. Using Friedel-Crafts acylation reaction to prepare microspheres with surface bonds and initiator molecules

[0044] Add 8 g of raw material microspheres in a dry 250ml two-necked flask, the microspheres are polystyrene-divinylbenzene microspheres that are monodisperse, have a crosslinking degree of 60%, and a particle diameter of 20 microns, and then add solvent 1,2 - 46ml of dichloroethane, slowly add 21.76g of anhydrous aluminum trichloride under magnetic stirring, then dropwise add 7.2ml of acylating reagent chloropropionyl chloride, dropwise, and react at a temperature of 30°C for 24 hours. Add 4 ml of concentrated hydrochloric acid and 144 g of crushed ice to the reacted system, stir for 20 minutes, then filter with suction, and wash with water, ethanol, and acetone several times respectively. The obtained microspheres were subjected to surface element...

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Abstract

The invention discloses a polymer microsphere and preparation method thereof. The microsphere comprises a core and surface graft; wherein the core is monodispersed polystyrene-divinyl benzene microsphere with crosslinking degree of 60-90% and grain diameter of 2-20 microns, and the surface graft is polyglycidyl methacrylate or derivate thereof. Friedel-Crafts acylation is utilized, alpha-halogenacyllhalide is taken as acylation agent, initiator molecule is bonded on the surface of the microsphere; conventional atom transfer radical polymerization method is utilized to initiate monomers glycidyl methacrylate to condense; then different nucleopilic reagent is utilized for opening ring, and amino, hydroxyl, hydrazine, carboxyl and sulfydryl groups are introduced onto the surface of the microsphere. The polymer microsphere can be used as separation material for different chromatographs for high efficiency ion exchange, chelation and high efficiency affiliation, also can be used as carrierfor fixing enzyme and catalyst and is an excellent functional microsphere.

Description

technical field [0001] The invention relates to a polymer microsphere and a preparation method thereof, in particular to a polystyrene-divinylbenzene microsphere modified by polyglycidyl methacrylate and its derivatives and a preparation method thereof. Background technique [0002] Polymer microspheres have the specific properties of good spherical shape, small size, large specific surface area, strong adsorption performance, enrichment of functional groups on the surface, and strong surface reaction ability. As a functional material, the application of monodisperse polymer microspheres penetrates into every corner of our lives, from bulk products such as coatings, paper surface coatings, cosmetics, etc., to chromatographic media for slow and controlled drug release and protein separation. Polymer microspheres are used in high value-added products. At present, improving the mechanical properties of polymer microspheres, such as compression resistance, and preparing monodis...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F257/02C08F220/32C08F8/32C08F8/36C08F8/34B01J13/14
Inventor 范丽娟王丽莎姚敏德李凤彩江必旺
Owner SUZHOU UNIV
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