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Method for preparing monodispersed polymer microsphere resin by atom transfer radical precipitation polymerization

An atom transfer and monodisperse technology, which is applied in the field of monodisperse nano/micro polymer microspheres and their preparation, can solve problems such as uncontrollable and controllable limitations of the surface grafting process

Active Publication Date: 2012-12-26
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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  • Method for preparing monodispersed polymer microsphere resin by atom transfer radical precipitation polymerization
  • Method for preparing monodispersed polymer microsphere resin by atom transfer radical precipitation polymerization
  • Method for preparing monodispersed polymer microsphere resin by atom transfer radical precipitation polymerization

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0030] Example 1: Add functional monomer 4-vinylpyridine (4-VP, 0.031 mL), crosslinker EGDMA (0.22 mL) and anhydrous acetonitrile (30 mL) into a round bottom flask (50 mL). The reaction solution was passed through argon to remove oxygen for 15 minutes, then CuCl (1.3 mg) and the catalyst ligand PMDETA (0.0055 mL) were added, and the initiator 2-chloropropionate ethyl ester (0.0016 mL) was added after continuing to pass argon for 15 minutes, and the reaction bottle was After sealing, it was placed in an oil bath at 60° C. for 24 hours of reaction. After the reaction, the product was washed with methanol several times, and then vacuum-dried at 40° C. to constant weight (yield 46%).

[0031] The scanning electron micrographs of the obtained polymer microspheres are shown in figure 2 (number average diameter D n =2.83 μm, particle size polydispersity index U=1.004).

example 2

[0032] Example 2: Add functional monomer 4-VP (0.054 mL), crosslinker EGDMA (0.38 mL) and anhydrous acetonitrile (30 mL) into a round bottom flask (50 mL). The reaction solution was passed through argon to remove oxygen for 15 minutes, then CuCl (2.24 mg) and the catalyst ligand PMDETA (0.0094 mL) were added, and the initiator 2-chloropropionate ethyl ester (0.0029 mL) was added after continuing to flow argon for 15 minutes, and the reaction bottle was After sealing, it was placed in an oil bath at 60° C. for 7 hours of reaction. After the reaction, the product was washed with methanol several times, and then vacuum-dried at 40° C. to constant weight (yield 26%).

[0033] The scanning electron micrographs of the obtained polymer microspheres are shown in image 3 (D n = 1.86 μm, U = 1.007).

example 3

[0034] Example 3: Add functional monomer 4-VP (0.062 mL), crosslinker EGDMA (0.22 mL) and anhydrous acetonitrile (30 mL) into a round bottom flask (50 mL). The reaction solution was passed through argon gas for deoxygenation for 15 min, then CuCl (1.44 mg) and catalyst ligand PMDETA (0.0061 mL) were added, and the initiator 2-chloropropionate ethyl ester (0.00175 mL) was added after continuing to pass argon gas for 15 min, and the reaction bottle was After sealing, it was placed in an oil bath at 60° C. for 24 hours of reaction. After the reaction, the product was washed with methanol several times, and then vacuum-dried at 40° C. to constant weight (yield 35%).

[0035] The scanning electron micrographs of the obtained polymer microspheres are shown in Figure 4 (D n =2.96 μm, U=1.012).

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Abstract

The invention relates to a method for preparing a monodispersed polymer microsphere resin by atom transfer radical precipitation polymerization, characterized in that: the polymer microsphere is a copolymer microsphere of a polyene monomer with the crosslinking degree of 50-95% and other functional monoene monomers, the particle size is 200nm to 5 mum, and the particle size polydispersity is no larger than 1.03%. The polymer microsphere is prepared by atom transfer radical precipitation polymerization, the microsphere surface has atom transfer radical polymerization active initiating groups, and can further be subject to surface modification. The method disclosed herein has the characteristics of simple conditions, easy operation, cheap raw materials, and controllable surface active group content. The obtained monodispersed active nano / micron polymer microsphere can be used as a filling material of chromatographic column, and a carrier of catalysts and bioactive molecules and can be used for drug delivery.

Description

technical field [0001] The invention relates to the preparation of nano / micro polymer microspheres, in particular to a monodisperse nano / micro polymer microspheres with atom transfer radical polymerization active initiator groups on the surface and a preparation method thereof. Background technique [0002] In recent years, precipitation polymerization has become a facile and feasible method to prepare monodisperse nano / micro polymer microspheres. The obtained monodisperse nano / micro polymer microspheres have important application value in many fields such as chromatographic stationary phase, drug sustained release, catalyst and bioactive molecule loading. Compared with the methods of synthesizing polymer microspheres such as emulsion polymerization, suspension polymerization and dispersion polymerization, the precipitation polymerization method does not need to add any surfactant and stabilizer in the polymerization system, and can easily control the size of the polymer mic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F222/14C08F226/06C08F220/28C08F220/56C08F267/06C08F271/02C08F220/54C08F2/06
Inventor 张会旗姜经帅张莹
Owner NANKAI UNIV
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