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Method for preparing monodisperse microspheres through ultrasonic induction of RAFT precipitation polymerization

A monodisperse microsphere, precipitation polymerization technology, applied in the preparation of microspheres, microcapsule preparations, etc., can solve the problems of low mechanical properties, lack of functional groups, large internal stress of monodisperse microspheres, etc., to achieve wide application prospects, polymerization rate quick effect

Active Publication Date: 2019-10-15
HUAIYIN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the uneven internal structure of the monodisperse microspheres prepared by the precipitation polymerization of the conventional ordinary free radical polymerization mechanism leads to large internal stress and low mechanical properties; more importantly, the surface of this type of microspheres lacks further functions. oxidized functional groups, limiting its application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment approach 1

[0022] Add 0.4 g of methyl methacrylate, 0.4 g of ethylene glycol dimethacrylate, and 20 mg of CPADB into a transparent reaction vessel, and add a mixture of 7 g of ethanol and 3 g of water as a solvent, and bubble with high-purity argon After deoxygenation, it was placed under a 50w ultrasonic triggering device with a frequency of 450kHz. The ultrasonic mode was ultrasonic 2s, intermittent 2s, and polymerized for 50 minutes. After the polymerization, the reaction vessel was unsealed and centrifuged to obtain a white powder. *20 ml of ethanol was washed and centrifuged, and the resulting solid was o C dried overnight in a vacuum oven to obtain monodisperse polymer microspheres.

Embodiment approach 2

[0024] Add 0.5 g of hydroxyethyl methacrylate, 0.5 g of trimethylolpropane trimethacrylate, and 25 mg of RAFT reagent DDMAT into a transparent reaction vessel, and add a mixture of 6.5 g of ethanol and 3.5 g of water to make Solvent, after bubbling high-purity argon to remove oxygen, place it under a 50w, frequency of 450kHz ultrasonic induction device, the ultrasonic mode is ultrasonic 2s intermittent 2s, polymerization 60 minutes; powder, the white powder was washed with 3*20 ml ethanol and centrifuged, and the resulting solid was o C dried overnight in a vacuum oven to obtain monodisperse polymer microspheres.

Embodiment approach 3

[0026] Add 0.4 g of styrene, 0.6 g of p-divinylbenzene, and 25 mg of CPDN into a transparent reaction vessel, and add a mixture of 7.5 g of ethanol and 5.5 g of water as a solvent. It was placed under a 50w ultrasonic triggering device with a frequency of 450kHz, the ultrasonic mode was ultrasonic 2s, intermittent 2s, and polymerized for 80 minutes; after the polymerization was completed, the reaction vessel was unsealed and centrifuged to obtain a white powder. Wash and centrifuge the resulting solid at 35 o C dried overnight in a vacuum oven to obtain monodisperse polymer microspheres.

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PUM

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Abstract

The invention relates to the field of chemical industry, and discloses a method for preparing monodisperse microspheres through ultrasonic induction of RAFT precipitation polymerization. The method comprises the following steps: adding a monofunctional vinyl monomer, a polyfunctional vinyl monomer and an RAFT reagent into a reaction container, adding a proper amount of ethanol-water mixed solutionthereto as a solvent, bubbling and deoxidizing with high-purity argon, and then placing in ultrasonic wave to trigger polymerization; after completion of the polymerization, unsealing the reaction container, centrifuging and washing white powder for multiple times with ethanol to obtain a monodisperse microsphere sample. The ultrasonic is creatively introduced into preparation of the monodisperseactive microspheres through the RAFT precipitation polymerization, the polymerization rate is high, the conglomeration rate is high and the microsphere monodispersity is strong; the prepared microspheres have dithioester functional groups on the surfaces, so that further functionalization is facilitated; and the monodisperse microspheres have a wide application prospect in the fields of adsorption separation, biomedicine and the like.

Description

technical field [0001] The invention relates to the technical field of controllable radical polymerization, in particular to a method for preparing monodisperse microspheres by ultrasonic-induced RAFT precipitation polymerization. Background technique [0002] At present, highly cross-linked monodisperse microspheres are widely used in many fields such as standard metrology, intelligence information, catalyst carrier, biomedicine and chromatographic separation due to their advantages of large specific surface area, strong adsorption and uniform size. However, the uneven internal structure of the monodisperse microspheres prepared by the precipitation polymerization of the conventional ordinary free radical polymerization mechanism leads to large internal stress and low mechanical properties; more importantly, the surface of this type of microspheres lacks further functions. functionalized groups, limiting its application. Contents of the invention [0003] Purpose of the ...

Claims

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Application Information

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IPC IPC(8): C08F220/14C08F222/14C08F212/36C08F220/20B01J13/18
CPCC08F220/14C08F222/1006C08F212/36C08F220/20B01J13/185C08F2438/03C08F222/103C08F222/102C08F212/08
Inventor 姜孝武夏鑫杨路史建倪伶俐
Owner HUAIYIN INSTITUTE OF TECHNOLOGY
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