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One-pot dispersion polymerization for the preparation of non-spherical, raspberry-like or hollow polymer microspheres

A technology of dispersion polymerization and polymer, applied in the field of dispersion polymerization, to achieve the effect of obvious advantages and simple methods

Inactive Publication Date: 2016-08-17
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method still requires the preparation of seed microspheres first, and then the hollow microspheres can be obtained by seed polymerization

Method used

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  • One-pot dispersion polymerization for the preparation of non-spherical, raspberry-like or hollow polymer microspheres
  • One-pot dispersion polymerization for the preparation of non-spherical, raspberry-like or hollow polymer microspheres
  • One-pot dispersion polymerization for the preparation of non-spherical, raspberry-like or hollow polymer microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] Place a 100ml four-necked round-bottom reaction flask equipped with mechanical stirring and reflux condenser in a constant temperature water bath, add 12.5ml of ethylene glycol and 12.5ml of deionized water (ethylene glycol / water=5 / 5, vol.) Add monomer styrene St 2.5ml (concentration 8wt.% in the reaction solution), sodium styrene sulfonate NaSS 0.0453g (2wt.%, relative to St weight), initiator azobisisobutyronitrile AIBN 0.0453g ( 2wt.%, relative to the weight of St); start stirring, the speed is 200r / min; 2 Deoxygenated for 30min and kept at N 2 Under the atmosphere, the constant temperature water bath was heated to 80°C at the same time to start the reaction. After 180min, add ATRP reagent CuBr to the reaction system 2 0.0138g (0.6wt.%, relative to the initial St weight) and MA 5 DETA0.0512g (2.3wt.%, relative to the initial St weight) and water 1ml (40vol.%, relative to the initial St volume), add cross-linking agent DBPMA 0.0906g (4wt.%, relative to the initial...

Embodiment 2

[0062] Others are as embodiment 1, just after dispersion polymerization reaction 180min, add cross-linking agent DBPMA 0.0906g (4wt.%, relative initial St weight) and DVB 1.6ml (65.4wt.%, relative initial St weight) to reaction system ), the microspheres observed by SEM are snowman-like polymer microspheres with smooth head and body surfaces (similar to the figure 1 ), the diameter of the head is 186nm, and the diameter of the body is 228nm.

Embodiment 3

[0064] Others are as embodiment 1, just after dispersion polymerization reaction 180min, add MAEDCA 0.0138g (0.6wt.%, relative initial St weight) and water 1ml to reaction system, add cross-linking agent DBPMA0.0906g (4wt.%, relative Initial St weight) and DVB 1.6ml (65.4wt.%, relative to the initial St weight), continue to react for 5h. The microspheres observed by SEM and TEM are that the head surface is smooth and the body surface is very rough-the body is a raspberry-like snowman-like polymer microsphere (see the appendix figure 2 ), the head diameter is 130nm, and the body diameter is 233nm.

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Abstract

The invention provides a method for preparing nonspherical, raspberry-shaped or hollow polymer microspheres through one-pot dispersion polymerization, and belongs to the technical field of dispersion polymerization. The method comprises the steps of stirring monomers styrene St and sodium styrenesulfonate NaSS and an initiator azodiisobutyronitrile AIBN, and dissolving the mixture in the mixed solution of an organic solvent and water to form a reaction solution; increasing the temperature of the reaction solution to the range from 75 to 80 DEG C and reacting for a certain of time; next, dropwise adding a cross-linking agent or the cross-linking and other reaction reagents to the reaction system, and further reacting for a while to obtain nonspherical, raspberry-shaped or hollow polymer microspheres. According to the invention, a method for directly preparing different types (nonspherical, raspberry-shaped or hollow) of polymer microspheres based on conventional dispersion polymerization and by controlling the cross-linking reaction process and adjusting reaction parameters is established.

Description

technical field [0001] The invention relates to a method for directly preparing non-spherical, raspberry-shaped and hollow polymer microspheres by one-pot dispersion polymerization, in particular to adding a cross-linking agent after the nucleation period by one-pot dispersion polymerization to cross-link and / or grow particles Phase separation to prepare non-spherical, raspberry-like and hollow polymer microspheres belongs to the technical field of dispersion polymerization. Background technique [0002] Compared with homogeneous spherical particles, non-spherical particles have the characteristics of asymmetric or uneven distribution of shape, structure, surface and / or bulk composition, and performance. They have many excellent physical and chemical properties and have great application potential in many aspects: such as non-spherical Particles can be used as basic building blocks, assembled to form photonic crystals, display structural colors related to particle size, impr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F212/08C08F212/14C08F218/08C08F220/06C08F2/16
Inventor 刘莲英杨青杨万泰马育红刘亚男刘旺
Owner BEIJING UNIV OF CHEM TECH
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