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Monodisperse surface functionalized polymer microsphere resin and preparation method thereof

A surface functionalization, monodisperse technology, applied in the preparation of microspheres, microcapsule preparations, etc., can solve the problems of uncontrollability and controllability of the surface grafting process.

Active Publication Date: 2011-11-09
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the uncontrollable characteristics of ordinary free radical polymerization methods, the controllability of the surface grafting process is limited.

Method used

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  • Monodisperse surface functionalized polymer microsphere resin and preparation method thereof
  • Monodisperse surface functionalized polymer microsphere resin and preparation method thereof
  • Monodisperse surface functionalized polymer microsphere resin and preparation method thereof

Examples

Experimental program
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Effect test

example 1

[0024] Example 1: Add 0.47mL EGDMA, 27.3mg N,N-benzyl diethyldithiocarbamate (BDC) and 30mL acetonitrile in sequence into a 100mL round bottom flask, and stir it with a magnet to dissolve it completely. After deoxygenating with argon gas for 30 minutes, the reaction system was sealed, and reacted for 10 hours under the irradiation of a high-pressure mercury lamp (the distance between the reaction bottle and the lamp was 10 cm, and the reaction temperature was 26° C.). After the reaction, the reaction system was subjected to ultracentrifugation (10000 r / min), and the obtained polymer microspheres were washed 4 times with methanol, and then vacuum-dried at 40° C. to constant weight (yield 31%).

[0025] The scanning electron micrographs of the obtained polymer microspheres are shown in figure 2 (number average diameter D n =1.35μm, weight average diameter D w =1.37 μm, particle size polydispersity index U=1.015).

example 2

[0026] Example 2: Add 0.47mL of EGDMA, 27.3mg of BDC and 15mL of acetonitrile into a 100mL round bottom flask in sequence, and stir it with a magnet to dissolve it completely. After deoxygenating with argon gas for 30 minutes, the reaction system was sealed, and reacted for 10 hours under the irradiation of a high-pressure mercury lamp (the distance between the reaction bottle and the lamp was 10 cm, and the reaction temperature was 26° C.). After the reaction, the reaction system was subjected to ultracentrifugation (10000 r / min), and the obtained polymer microspheres were washed 4 times with methanol, and then vacuum-dried at 40° C. to constant weight (yield 46%).

[0027] The scanning electron micrographs of the obtained polymer microspheres are shown in image 3 (D n = 1.98 μm, D w = 2.03 μm, U = 1.025).

example 3

[0028] Example 3: Add 0.47mL of EGDMA, 27.3mg of BDC and 45mL of acetonitrile into a 100mL round bottom flask in sequence, and stir it with a magnet to dissolve it completely. After deoxygenating with argon gas for 30 minutes, the reaction system was sealed, and reacted for 10 hours under the irradiation of a high-pressure mercury lamp (the distance between the reaction bottle and the lamp was 10 cm, and the reaction temperature was 26° C.). After the reaction, the reaction system was subjected to ultracentrifugation (10000 r / min), and the obtained polymer microspheres were washed 4 times with methanol, and then vacuum-dried at 40° C. to constant weight (yield 16%).

[0029] The scanning electron micrographs of the obtained polymer microspheres are shown in Figure 4 (D n = 1.16 μm, D w = 1.19 μm, U = 1.026).

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Abstract

The invention relates to a monodisperse surface functionalized polymer microsphere resin and a preparation method thereof. The polymer microsphere resin is a gel polyene monomer homopolymer having a cross linking degree more than 30%, or a copolymer microsphere formed through a polyene monomer and a compound selected from other functional monoene monomers, and has a particle size of 300 nm to 5 [mu]m, a dispersity of 1.010-1.082. The polymer microsphere resin is prepared through a precipitation polymerization initiated through an iniferter; the microsphere surface has iniferter active groups (a content range from 0.05-0.3 mmol / g ) so as to be further subjected to surface modifications. The method provided by the present invention has characteristics of simple conditions, easy operation, cheap raw materials and controllable surface functional group content. The prepared monodisperse surface functionalized nanometer / micrometer polymer microsphere can be applicable for a filling material of a chromatographic column, drug controlled release and carriers for catalysts and bioactive molecules.

Description

technical field [0001] The invention relates to the preparation of nano / micro polymer microspheres, in particular to monodisperse nano / micro polymer microspheres with active polymerization initiation groups on the surface and a preparation method thereof. Background technique [0002] Monodisperse nano / micro polymer microspheres have become an important part of international academic and industrial research because of their important application value in many fields such as chromatographic stationary phase, drug sustained release, catalyst and bioactive molecule loading. At present, the main methods of synthesizing monodisperse polymer microspheres include emulsion polymerization, suspension polymerization, dispersion polymerization and precipitation polymerization. Compared with other polymerization methods, the precipitation polymerization method has the advantages of not needing to add any surfactant and stabilizer in the polymerization system, and the size of the polymer...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F122/14C08F222/14C08F226/06C08F2/48C08F2/38B01J13/14
Inventor 张会旗李俊义张莹祖佰祎
Owner NANKAI UNIV
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