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Method for preparing monodisperse active function polymer microspheres by means of active free radical dispersion polymerization

A technology of dispersion polymerization and functional polymer, which is applied in the field of preparation of monodisperse active functional polymer microspheres, can solve the problems of difficult control of reaction conditions, complicated process steps, etc., and achieves a wide range of applicable monomers and controllable polymerization process. , smooth surface effect

Inactive Publication Date: 2016-01-20
XIAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But this method still has many deficiencies, especially the process of introducing iniferter groups on the surface of the carrier is cumbersome, and the reaction conditions are not easy to control, etc.

Method used

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  • Method for preparing monodisperse active function polymer microspheres by means of active free radical dispersion polymerization
  • Method for preparing monodisperse active function polymer microspheres by means of active free radical dispersion polymerization
  • Method for preparing monodisperse active function polymer microspheres by means of active free radical dispersion polymerization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] In a 250mL three-necked quartz flask with a stirring device, add 10g of p-chloromethylstyrene, 0.1g of N,N-diethyldithiocarbamate (4-vinyl)benzyl (Iniferter), 0.1g of polyvinylpyrrolidone Mixed solutions of 1g and 100g of ethanol and water (the mass-number ratio of ethanol and water is 90:10). After stirring evenly, pass nitrogen gas for 30 minutes, keep nitrogen atmosphere, stir at a speed of 200 r / min, and polymerize for 15 hours at 25 °C at a distance of 15 cm from an ultraviolet light source (300 W). After the reaction, centrifuge at high speed to obtain polymer particles, then wash the polymer microspheres with ethanol and deionized water three times in sequence, and dry them in a vacuum oven to constant weight to obtain monodisperse active functional polymer microspheres.

[0023] see figure 1 , The particle size of the polymer microspheres obtained in Example 1 is 0.90 micron, the particle size distribution is 1.012, and the yield is 47%.

Embodiment 2

[0025] In a 250mL three-necked quartz flask with a stirring device, add 30g of p-chloromethylstyrene, 0.3g of N,N-diethyldithiocarbamate (4-vinyl)benzyl (Iniferter), 0.3g of polyvinylpyrrolidone Mixed solutions of 1.5g and 100g of ethanol and water (the mass-number ratio of ethanol and water is 90:10). After stirring evenly, pass nitrogen gas for 30 minutes, keep the nitrogen atmosphere, stir at 200r / min, and polymerize at 25°C at a distance of 15cm from the ultraviolet light source (300W) for 24 hours. After the reaction, centrifuge at high speed to obtain polymer particles, then wash the polymer microspheres with ethanol and deionized water three times in sequence, and dry them in a vacuum oven to constant weight to obtain monodisperse active functional polymer microspheres.

[0026] see figure 2 , The particle size of the polymer microspheres obtained in Example 2 is 2.14 microns, the particle size distribution is 1.009, and the yield is 61%.

Embodiment 3

[0028] In a 250mL three-necked quartz flask with a stirring device, add 10g of p-chloromethylstyrene, 0.1g of N,N-diethyldithiocarbamate (4-vinyl)benzyl ester (Iniferter), polyethylene A mixed solution of 1.5 g of pyrrolidone and 100 g of ethanol and water (the mass-number ratio of ethanol to water is 85:15). After stirring evenly, pass nitrogen gas for 30 minutes, keep nitrogen atmosphere, stir at a speed of 200 r / min, and polymerize for 15 hours at 25 °C at a distance of 15 cm from an ultraviolet light source (300 W). After the reaction, centrifuge at high speed to obtain polymer particles, then wash the polymer microspheres with ethanol and deionized water three times in sequence, and dry them in a vacuum oven to constant weight to obtain monodisperse active functional polymer microspheres.

[0029] see image 3 , The particle size of the polymer microspheres obtained in Example 3 was 1.06 microns, the particle size distribution was 1.076, and the yield was 53%.

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Abstract

The invention discloses a method for preparing monodisperse active function polymer microspheres by means of active free radical dispersion polymerization. The method comprises the steps that N,N-dialkyl aminodithioformic acid(4-vinyl)benzyl ester serves as iniferter, in a traditional disperse system, a reaction system is irradiated by means of 300 w high-pressure mercury lamp, and monodisperse active function polymer microspheres are prepared through dispersion polymerization inducted by the iniferter. According to the active polymer microspheres prepared through the method, the surface is smooth, the monodispersity is good, the particle sizes are uniform, the surface has Iniferter active radical initiating groups, and surface modification can be further conducted. According to the method for preparing the monodisperse active function polymer microspheres by means of the active free radical dispersion polymerization, surface active functional groups are controllable, the preparation method is easy, and the prepared monodisperse active function polymer microspheres can be used for relative fields such as biological medicine, chromatographic column filling and carrier materials synthetized through organic solid.

Description

technical field [0001] The invention relates to a method for preparing monodisperse active functional polymer microspheres, in particular to a method for preparing polymer microspheres by active radical dispersion polymerization using an initiator-transfer-termination agent, in particular to a method for preparing active radical dispersion polymerization Method for Monodispersing Active Functional Polymer Microspheres. Background technique [0002] Dispersion polymerization means that the system is homogeneous before the polymerization reaction starts, monomers, initiators and dispersants are all dissolved in the medium, and the generated polymers are insoluble in the reaction medium, and the formation of polymers is carried out by means of steric hindrance and charge interaction in the system. A polymerization method in which polymer particles formed after the reaction are stably dispersed in the medium by micro-crosslinking or micro-crosslinking. Monodisperse polymer micr...

Claims

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Application Information

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IPC IPC(8): C08F112/14C08F2/48C08F2/38C08F2/16B01J13/14
Inventor 杨慧
Owner XIAN UNIV OF SCI & TECH
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