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Method for preparing functionalized crosslinked monodisperse polymer microspheres by one-step dispersion polymerization

A technology of dispersion polymerization and functionalization, which is applied in the field of preparation of functionalized cross-linked monodisperse polymer microspheres, can solve the problems of limited application range, low degree of cross-linking and functionalization of microspheres, and achieve efficient and efficient preparation process. Ease of large-scale preparation and popularization, and the effect of energy-saving preparation methods

Active Publication Date: 2017-12-15
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method solves the preparation of cross-linked functionalized microspheres to a certain extent, but the addition of its cross-linking monomer and functional monomer is still very little (no more than 5%), so the degree of cross-linking of the microspheres prepared and The degree of functionalization is not high, which limits its application range

Method used

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  • Method for preparing functionalized crosslinked monodisperse polymer microspheres by one-step dispersion polymerization
  • Method for preparing functionalized crosslinked monodisperse polymer microspheres by one-step dispersion polymerization

Examples

Experimental program
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Effect test

example 1

[0028] Example 1: Preparation of alkyne-functionalized, cross-linked, monodisperse polymer microspheres

[0029] 50g of ethanol, 1g of distilled water and 1g of PVP were dispersed uniformly by ultrasonic at room temperature to make a uniform continuous phase; Propyl ester is mixed evenly to make a uniform transparent oil phase. Add the prepared dispersed phase into a three-neck flask equipped with stirring, start the stirring and control the rotation speed at 100 rpm, add the prepared oil phase into the three-necked flask, and react at room temperature for 4 hours to obtain microspheres. The obtained microspheres were washed three times with distilled water, filtered, and dried in air for 24 hours to obtain dry, highly cross-linked, alkyne-functionalized polymer microspheres.

example 2

[0030] Example 2: Preparation of alkyne-functionalized, cross-linked, monodisperse polymer microspheres

[0031] 50g ethanol, 50g distilled water and 1g PVP were dispersed uniformly by ultrasonic at room temperature to make a uniform continuous phase; Propyl ester is mixed evenly to make a uniform transparent oil phase. Add the prepared dispersed phase into a three-necked flask equipped with stirring, start stirring and control the rotation speed at 400 rpm, add the prepared oil phase into the three-necked flask, and react at room temperature for 8 hours to obtain microspheres. The obtained microspheres were washed three times with distilled water, filtered, and dried in air for 24 hours to obtain dry, highly cross-linked, alkyne-functionalized polymer microspheres.

example 3

[0032] Example 3: Preparation of fluorescently labeled, crosslinked, monodisperse polymer microspheres

[0033] 50g ethanol, 1g distilled water and 1g PVP were uniformly dispersed at room temperature by ultrasonic to make a uniform continuous phase; Ester fluorescein is mixed evenly to make a uniform transparent oil phase. Add the prepared dispersed phase into a three-necked flask equipped with stirring, start stirring and control the rotation speed at 400 rpm, add the prepared oil phase into the three-necked flask, and react at room temperature for 8 hours to obtain microspheres. The obtained microspheres were washed three times with distilled water, filtered, and dried in air for 24 hours to obtain dry, highly cross-linked, and fluorescently labeled polymer microspheres.

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Abstract

The invention relates to a method for preparing functionalized crosslinked monodisperse polymer microspheres through one-step dispersion polymerization. The method takes polyfunctional thiol, isocyanate and functional monomers as disperse phases and takes an alcohol-water solution of polyvinyl pyrrolidone as a continuous phase and carries out one-step dispersion polymerization at room temperature under the condition of no additional catalyst / initiator so as to obtain the functionalized crosslinked monodisperse microspheres. Different from the traditional free radical chain polymerization mechanism, the thiol-isocyanate reaction follows the anionic step polymerization mechanism, the reaction can be efficiently carried out in the presence of few nucleophilic reagents, and no side reaction is generated in the presence of water, alcohol and amine. A very high monomer conversion rate can be obtained within a very short period of time in polymerization. The method is very suitable for preparing polymer microspheres in heterogeneous system polymerization. Therefore, compared with the traditional dispersion polymerization, the method provided by the invention has the advantages of being efficient and energy-saving in preparation process, simple in technological operation and easy to realize large-scale preparation and popularization.

Description

technical field [0001] The invention belongs to a preparation method of functionalized crosslinked monodisperse polymer microspheres, and relates to a method for preparing functionalized crosslinked monodisperse polymer microspheres by one-step dispersion polymerization. With polyfunctional thiol, isocyanate and functional monomer as the dispersed phase, polyvinylpyrrolidone alcohol aqueous solution as the continuous phase, the next step of dispersion polymerization at room temperature and without external catalyst / initiator to obtain functionalized cross-linked monodisperse microparticles ball. Background technique [0002] Micron-sized monodisperse microspheres are widely used in the fields of standard metering, biomedicine, dyes, colloid science and chromatographic separation, but the main preparation methods are suspension polymerization, dispersion polymerization and seed swelling method, and the polymerization reaction system is styrene, acrylic acid Free radical chai...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/32C08G18/67C08G18/75B01J13/14
CPCB01J13/14C08G18/3876C08G18/672C08G18/755
Inventor 张秋禹谭蕉君李春梅淡少敏张宝亮
Owner NORTHWESTERN POLYTECHNICAL UNIV
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