Acetylacetonyl-based magnetic polymer microsphere and preparation method thereof

An acetylacetone and polymer technology, applied in the field of magnetic polymer microspheres and their preparation, can solve the problems of wide particle size range, uneven particle size, irregular shape of magnetic microspheres, etc., and achieves good monodispersity and stability. Good performance and uniform particle size

Active Publication Date: 2020-04-07
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The magnetic microspheres obtained by this method are characterized by magnetic response because of the magnetic particles inside, and the preparation process is simple, but the shape is irregular, the particle size range is wide, and the surface does not contain functional groups, which limits its further application.
Followed by a two-step method, the typical representative is the swelling method (in-situ method). The first step is to prepare cross-linked monodisperse microspheres by traditional methods such as dispersion polymerization and emulsion polymerization. Ferric ions form coordination bonds or ionic bonds such as: -NH 2 , -COOH, -SO 3 H, -NO 2 etc., the second step is to make the polymer microspheres swell in the solution of iron ions, and the iron ions are absorbed and embedded by infiltration. After raising the temperature, they can be oxidized and reduced in situ under a suitable catalyst to obtain a magnetic polymer. Microspheres; however, the available magnetic components are limited, and the use of functional monomers will interfere with the nucleation period of the polymer, resulting in irregular shapes and uneven particle sizes of magnetic microspheres, and it is impossible to obtain monodisperse functional microspheres, and After the microspheres are swelled and reduced in the solvent, the particle size and particle size distribution of the microspheres will also change greatly, which cannot meet the actual needs

Method used

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  • Acetylacetonyl-based magnetic polymer microsphere and preparation method thereof
  • Acetylacetonyl-based magnetic polymer microsphere and preparation method thereof
  • Acetylacetonyl-based magnetic polymer microsphere and preparation method thereof

Examples

Experimental program
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Effect test

experiment example 1

[0040] Preparation of Experimental Example 1 Crosslinked P (AAEM+MMA) Copolymer Microspheres

[0041] A weight ratio of ethanol / water mixture 40 / 60 (7.2g+10.8g) was introduced into a 25mL round bottom flask as a solvent, and then 1.0g of methyl methacrylate (MMA) monomer (5wt% relative to the system) was added , 1.0 g of acetoacetate methacrylate (AAEM) monomer (5 wt % relative to the system), 0.30 g of stabilizing dispersant polyacrylic acid tricarbonate (PAA-TTC) (15 wt % relative to the monomer) , 0.005g of S-1-dodecyl-S'-(α,α'-dimethyl-α"-acetic acid) trithiocarbonate (DDMAT) (0.25wt% relative to the monomer), 0.06 g of Darocur 1173 (3 wt % relative to monomer) and 0.06 g of dipropylene glycol diacrylic acid (3 wt % relative to monomer), magnetically stirred to dissolve.

[0042] The reaction mixture was deoxygenated with nitrogen for 30 minutes, sealed with a glass stopper with a quartz glass sheet, and then illuminated with a 365nm wavelength LED lamp (light intensity 2...

experiment example 2

[0043] Preparation of Experimental Example 2 Crosslinked P (AAEM+MMA) Copolymer Microspheres

[0044] The stable dispersant used in this example is (poly N,N-dimethylacrylamide-trithiocarbonate) PDMA-TTC instead of PAA-TTC in Example 1, the types and amounts of the remaining reagents and the implementation process and implementation Example 1 is the same. The scanning electron micrograph (SEM) of the resulting product is shown in figure 2 , the monodispersity of the obtained microspheres is good, and the particle size is about 700nm.

experiment example 3

[0045] Preparation of experimental example 3 cross-linked P (AAEM+MMA) copolymerized microspheres

[0046] The stable dispersant used in this example is polyvinylpyrrolidone (PVP) instead of PAA-TTC in Example 1, and the types and amounts of the remaining reagents and the implementation process are the same as in Example 1. The scanning electron micrograph (SEM) of the resulting product is shown in image 3 , the monodispersity of the obtained microspheres is good, and the particle size is about 1.0 μm.

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PUM

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Abstract

The invention discloses an acetylacetonyl-based magnetic polymer microsphere and a preparation method thereof. The method includes: firstly copolymerizing acetoacetic acid ethylene glycol methacrylateand an acrylate monomer, adding a cross-linking agent, a photoinitiator, a micromolecular RAFT reagent and a cross-linking agent, taking a macromolecular reversible addition-fragmentation chain transfer agent as a stable dispersing agent, and conducting RAFT photodispersion polymerization to prepare a cross-linked polymer microsphere containing diacetylacetonyl internally; and then swelling the cross-linked polymer microsphere in an organic solvent, adsorbing metal ions by diacetylacetonyl in the microsphere, and carrying out in-situ oxidation reduction under the conditions of heating and catalyst action to obtain the polymer microsphere loaded with magnetism inside. The magnetic polymer microsphere provided by the invention has the characteristics of regular shape, uniform particle size,good monodispersity and stability, and after swelling and reduction in a solvent, can maintain unchanged particle size and particle size distribution, thus having has great application prospects.

Description

technical field [0001] The invention relates to the technical field of polymer materials, more specifically, to an acetylacetone-based magnetic polymer microsphere and a preparation method thereof. Background technique [0002] Magnetic polymer microspheres are usually composed of inorganic magnetic materials and organic polymer materials, and are a new type of inorganic / organic composite materials. Inorganic magnetic nanoparticles bring superparamagnetism to the microspheres, enabling them to be quickly separated under the action of a magnetic field; while organic polymers make the nanoparticles more stable and provide the possibility for subsequent functional applications. In addition to the characteristics of ordinary polymer microspheres, such as uniform particle size, large specific surface area, and good stability, magnetic polymer microspheres also have magnetic responsiveness and diversity of surface functional groups, and can be efficiently removed by various physic...

Claims

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Application Information

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IPC IPC(8): C08F220/28C08F220/14C08F2/48C08K3/08B01J13/18
CPCB01J13/18C08F2/48C08F220/14C08F220/28C08F2438/03C08K3/08C08K2003/0856C08K2201/01
Inventor 曾兆华黄永平王梦真杨建文袁佳宇
Owner SUN YAT SEN UNIV
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