Water dispersible magnetic high polymer microsphere and preparation thereof

A technology of polymer microspheres and magnetism, applied in the direction of magnetism of organic materials/organic magnetic materials, etc., can solve the problems of large difference in the magnetic strength of microspheres, incomplete magnetic centers embedded in polymers, and uneven magnetic content. , to achieve the effect of convenient storage, transportation and preservation, good monodispersity, and uniform particle size distribution

Inactive Publication Date: 2008-12-24
GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation methods of magnetic polymer microspheres mainly include embedding method and monomer polymerization method: (1) embedding method is to disperse magnetic particles in polymer solution, and obtain magnetic particles by atomization, flocculation, deposition, evaporation and other methods. Polymer microspheres; however, the magnetic polymer microspheres prepared by this method have a wide particle size distribution, irregular shape, difficult to control the size, uneven magnetic content, and a large difference in the magnetic strength of the microspheres. The center is incomplete, the magnetic core is easy to contact with the outside world, and the magnetism is easy to leak
(2) The monomer polymerization method is a core-shell magnetic polymer microsphere formed by adding initiators, stabilizers, etc. in the presence of magnetic particles and monomers; the polymerization methods mainly include: suspension polymerization, dispersion polymerization, and emulsion polymerization etc.; however, the magnetic content of microspheres prepared by this method is low, and phase separation is prone to occur during the polymerization process, resulting in inhomogeneous distribution of magnetic content of the synthesized microspheres, and their chemical and mechanical stability is also poor

Method used

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  • Water dispersible magnetic high polymer microsphere and preparation thereof
  • Water dispersible magnetic high polymer microsphere and preparation thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0031] (1) Preparation of microsphere cores by soap-free emulsion polymerization and formation of active polymerization initiation centers

[0032] Dissolve 0.023g of potassium persulfate (KPS, 0.5% of the total mass of the monomer) into 95.5ml of water, add it to a four-necked flask, pass N2 gas for 10min, put it into an oil bath whose temperature has been adjusted to 83°C, and wait for After the system temperature was stabilized at 80°C, a mixture of styrene (1.73g), tert-butyl acrylate (1.73g), 2-chloropropionic acid ethylene glycol diester (0.52g) and crosslinking agent EGDMA 0.023g was added dropwise After 40 minutes of reaction, 2-chloropropionic acid ethylene glycol diester (0.52 g was added dropwise, the temperature was maintained, and the reaction was continued for 8 hours with stirring, the heating was stopped, and naturally cooled to room temperature under stirring. Centrifuged for 15 minutes, the rotating speed was 3000r / min, separated Afterwards, the emulsion was ...

Embodiment 2

[0038] (1) Preparation of microsphere cores by soap-free emulsion polymerization and formation of active polymerization initiation centers

[0039] Dissolve 0.045g potassium persulfate (KPS, 1% of the total mass of the monomer) into 95.5ml water, join in the four-necked flask, pass N 2 After airing for 10 minutes, put it into an oil bath whose temperature has been adjusted to 83°C. After the system temperature is stable at 80°C, add 1.73g of styrene, 1.73g of tert-butyl acrylate, and 2-chloropropionic acid ethylene glycol diester 0.52g and cross-linking agent EGDMA 0.068g (1.5% of the total monomer mass) of the mixed monomer 5min, after 40min of reaction, dropwise add 0.52g of 2-chloropropionic acid ethylene glycol diester, maintain the temperature, continue to stir the reaction 8h, stop heating, and naturally cool to room temperature under stirring. Centrifuge for 15min at a speed of 3000r / min, and take the emulsion after separation. Its solid content was measured to be 4.2...

Embodiment 3

[0045] (1) Preparation of microsphere cores by soap-free emulsion polymerization and formation of active polymerization initiation centers

[0046] Dissolve 0.09g (2% of the total monomer mass) of potassium persulfate into 90.7ml of water, add it to a four-necked flask, and pass N2 gas for 10 minutes, then put it into an oil bath whose temperature has been adjusted to 83°C. After stabilizing at 80°C, add dropwise a mixture of styrene 3.46g, tert-butyl acrylate 3.46g, 2-chloropropionic acid ethylene glycol diester 1.04g and crosslinking agent EGDMA 0.312g (3.5% of the total monomer mass) After 5 minutes of monomer reaction and 40 minutes of reaction, 1.04 g of 2-chloropropionic acid ethylene glycol diester was added dropwise, and the temperature was maintained. Stirring was continued for 8 hours. Heating was stopped, and the mixture was naturally cooled to room temperature while stirring. Centrifuge for 15min at a speed of 3000r / min, and take the emulsion after separation. Its...

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Abstract

The invention discloses a water dispersion magnetic polymer microsphere and a preparation method thereof. Firstly, a core is prepared by soap-free emulsion polymerization, then atom transfer radical polymerization (ATRP) is utilized to actively polymerize and prepare a hydrophilic shell, and the obtained water dispersion magnetic polymer microsphere is a composite consisting of a superparamagnetic center and a high molecular polymer; an outer layer is a hydrophilic or water-soluble polymer and is prepared through an active polymerization ATRP reaction; an inner layer is a polymer which can produce an even cavity, can load a magnetic center and has good cross-linking fixation, and is generated through the soap-free emulsion polymerization; the superparamagnetic center is formed by the even cavity of the inner layer loaded with an inorganic superparamagnetic material; and the diameter range of the microsphere is between 100 and 2000nm, the magnetic content is between 3 and 50 percent, and the saturated magnetization strength is between 3.0 and 70.0emu/g. The preparation method is simple, and the produced water dispersion magnetic polymer microsphere has a controllable structure, even distribution, regular shape, adjustable magnetic content, and good biocompatibility.

Description

technical field [0001] The invention relates to the field of functional polymer materials, in particular to a water-dispersed magnetic polymer microsphere and a preparation method thereof. Background technique [0002] Magnetic polymer microspheres have both the characteristics of polymers and the magnetic responsiveness of magnetic substances, and are widely used in magnetic plastics, magnetic rubber, solid phase carriers for organic synthesis, affinity chromatography, biomedicine, cell biology and bioengineering, etc. field. There are generally three structures of magnetic polymer microspheres: (1) the core is composed of magnetic metal oxides (such as iron, cobalt, nickel and other oxides), and the shell is composed of polymer materials; (2) the polymer material is used as the core, and the magnetic The material is used as the shell layer; (3) a sandwich structure, the inner and outer layers are made of polymer materials, and the middle layer is made of magnetic material...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J3/20C08L33/04C08K3/22C08F220/18C08F220/22C08F2/22C08F8/12H01F1/42
Inventor 胡继文刘志雷孙建平胡美龙赵发宝
Owner GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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