Preparation method for monodisperse functionalized polymer microsphere with surface chain transfer activity

A technology of chain transfer and functionalization, which is applied in the field of preparation of monodisperse surface chain transfer active functionalized polymer microspheres, can solve problems such as poor spheroid formation, achieve stable surface functional groups, high chain transfer activity, and synthetic conditions easy to control effects

Inactive Publication Date: 2014-01-01
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The surface of the microspheres prepared by the precipitation polymerization method is clean and the post-treatment is simple, but the spheroidization is poorer than the first three methods

Method used

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  • Preparation method for monodisperse functionalized polymer microsphere with surface chain transfer activity
  • Preparation method for monodisperse functionalized polymer microsphere with surface chain transfer activity
  • Preparation method for monodisperse functionalized polymer microsphere with surface chain transfer activity

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1: 2mL of DVB, 0.0430g of AIBN, 0.1557g of cumyl dithiobenzoate (CDB) and 100mL of acetonitrile were added to a 250mL single-necked flask in sequence, and 0.5g of zeolite was added until the mixture was fully dissolved. Access to N 2 Remove oxygen for 30 minutes, then install a Soxhlet extractor with a volume of 60mL and a condenser tube (the volume of the distilled solvent and the remaining solution = 3:2), seal the system and feed condensed water. Put the reaction device in a 1000mL electric heating mantle and start heating, the power is set to 150W, the reaction temperature is 82°C, and the reaction is carried out for 6h. After the reaction, the pink suspension was passed through a 60mL G6 sand core funnel, filtered under reduced pressure (vacuum degree 0.08), and the obtained polymer was washed with methanol 5 times (rinsing with 20mL methanol each time), and then in Dry to constant weight in a vacuum oven at 50°C, and the obtained microspheres are named M-...

Embodiment 2

[0032] Example 2: Add 4mL of DVB, 1mL of MAA, 0.1002g of AIBN, 0.3514g of cumyl dithiobenzoate (CDB) and 240mL of acetonitrile into a 500mL single-necked flask in sequence, add 0.5g of zeolite, and wait The mixture was fully dissolved. Access to N 2Remove oxygen for 30 minutes, then install a Soxhlet extractor with a volume of 60mL and a condenser tube (the volume of the distilled solvent and the remaining solution = 1:4), seal the system and pass in condensed water. Put the reaction device in a 1000mL electric heating mantle and start heating, the power is set to 150W, the reaction temperature is 82°C, and the reaction is carried out for 6h. After the reaction, the pink suspension was passed through a 60mL G6 sand core funnel, filtered under reduced pressure (vacuum degree 0.08), and the obtained polymer was washed with methanol 5 times (rinsing with 20mL methanol each time), and then in Dry in a vacuum oven at 50°C until constant weight, and the obtained microspheres are n...

Embodiment 3

[0034] Example 3: 2mL of DVB, 0.0442g of AIBN, 0.1549g of cumyl dithiobenzoate (CDB) and 100mL of acetonitrile were added to a 250mL single-necked flask in sequence, and 0.5g of zeolite was added until the mixture was fully dissolved. Access to N 2 Remove oxygen for 15 minutes, then install a Soxhlet extractor with a volume of 60mL and a condenser tube, and inject condensed water after the system is sealed. Put the reaction device in a 1000mL electric heating mantle and start heating, the power is set to 300W, the reaction temperature is 82°C, and the reaction is carried out for 6h. After the reaction, the pink suspension was passed through a 60mL G6 sand core funnel, filtered under reduced pressure (vacuum degree 0.08), and the obtained polymer was washed with methanol 5 times (rinsing with 20mL methanol each time), and then in Dry to constant weight in a vacuum oven at 50°C, and the obtained microspheres are named M-3.

[0035] The scanning electron microscope picture of t...

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Abstract

The invention relates to a preparation method for a monodisperse functionalized polymer microsphere with the surface chain transfer activity. An RAFT (Reversible Addition-Fragmentation Chain-Transfer) distillation-precipitation polymerization method is adopted, and polyene monomers or polyene and monoene mixed monomers are used, as a result, the monodisperse polymer microsphere of which the crosslinking degree is greater than 30 percent, particle diameter is within a range of 50 nanometers-8 micrometers, particle dispersion index is 1.038-1.164, surface chain transfer functional group content is 0.75-1.88 mmol/g, and surface can be further modified, is prepared. The preparation method has the characteristics that a particle diameter and surface functional group content are controllable; surface functional groups are stable; chain transfer activity is high; metal impurities difficult to treat are not introduced; synthesis conditions are easy to be controlled; the price of the raw material is low, and the like. The prepared monodisperse surface functionalized polymer microsphere can be applied to a chromatogram stationary phase, medicine slow release, catalysts, active bio-molecule carries and the like.

Description

technical field [0001] The invention relates to a method for preparing monodisperse surface chain transfer active functionalized polymer microspheres, in particular to a method based on reversible addition-fragmentation chain transfer (RAFT) active free radical distillation precipitation polymerization method to prepare monodisperse surface with reversible Method for Functionalizing Polymer Microspheres by Addition-Fragmentation Chain Transfer of Reactive Groups. Background technique [0002] In recent years, polymer core-shell microspheres have been widely used in solid phase chromatography packing, separation analysis, drug release control, immunoassay and other fields, and the method of preparing core-shell microspheres has also attracted international academic circles. and great attention from the industry. At present, the "grafting from..." method is the most direct and effective method for preparing shell-core polymer microspheres. Due to the introduction of RAFT rea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F112/36C08F212/36C08F220/06C08F226/06C08F212/08C08F2/38
Inventor 胡小玲管萍李季张向荣宋任远
Owner NORTHWESTERN POLYTECHNICAL UNIV
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