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Method for preparing magnetic temperature-sensitive composite microsphere with nuclear shell structure by adopting in-situ grafting technique

A core-shell structure and composite microsphere technology, applied in the fields of polymer materials and biomedical engineering, can solve the problems of poor particle core-shell binding force, low magnetic content, and difficult control of the molecular weight of the shell polymer, and achieve a synthesis method. Simple, easy-to-use effects

Inactive Publication Date: 2009-10-21
TONGJI UNIV
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Problems solved by technology

However, the above-mentioned several preparation methods usually adopt the conventional free radical polymerization method, the molecular weight of the shell layer polymer is not easy to control, and the molecular chain and the core layer inorganic particles are mostly combined by long-distance force (van der Waals force, hydrogen bond), and the interaction force Weaker, the core-shell binding force of the prepared particles is poor, the particle size is large, the distribution is wide, and the magnetic content is low

Method used

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  • Method for preparing magnetic temperature-sensitive composite microsphere with nuclear shell structure by adopting in-situ grafting technique
  • Method for preparing magnetic temperature-sensitive composite microsphere with nuclear shell structure by adopting in-situ grafting technique

Examples

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Effect test

Embodiment 1

[0021] In 100ml of 5% silane coupling agent KH-570 ethanol solution, add 0.5g ferroferric oxide nano-magnetic particles for ultrasonic dispersion, raise the temperature to 60°C for 6 hours, wash the product with ethanol five times after magnetic separation, put Dry in a vacuum oven. Disperse the prepared dry magnetic particles in 50ml N,N-dimethylformamide, weigh 1.13g monomer N-isopropylacrylamide (NIPAAm), 1.00g N,N-dimethylacrylamide, 0.33 g azobisisobutyronitrile, 0.96g isocyanopropyl dithiobenzoate, carry out solution polymerization, the polymerization temperature is 80 ℃, and the polymerization time is 3 hours, after magnetic separation and vacuum drying of the obtained product to obtain magnetic temperature-sensitive composite microspheres, the particle diameter of the composite microspheres is monodisperse and within the range of 30nm-500nm. figure 1 is the molecular structure formula of the magnetic composite microsphere, from figure 2 It can be seen that the compo...

Embodiment 2

[0023] In 500ml of 6% silane coupling agent KH-570 ethanol solution, add 10g ferroferric oxide nano-magnetic particles for ultrasonic dispersion, raise the temperature to 50°C for 16 hours, wash the product with acetone five times after magnetic separation, put Vacuum oven dry. Disperse the prepared dry magnetic particles in 250ml 1,4-dioxane, weigh 22.6g monomer N-isopropylacrylamide (NIPAAm), 40.0g N,N-diethylacrylamide, 0.6568 g benzoyl peroxide, 3.24g cumyl dithiobenzoate, carry out solution polymerization, the polymerization temperature is 75 ℃, and the polymerization time is 6 hours. After magnetic separation and vacuum drying of the obtained product, a magnetic Thermosensitive composite microspheres. The particle size of the composite microsphere is monodisperse and within the range of 30nm-500nm. Fig. 1 is the molecular structural formula of the magnetic composite microsphere, from figure 2 It can be seen that the composite microspheres have good temperature-sensit...

Embodiment 3

[0025] In 1000ml of 4% silane coupling agent KH-570 ethanol solution, add 15g of iron ferric oxide nano-magnetic particles for ultrasonic dispersion, raise the temperature to 70°C for 10 hours, and wash the product with tetrahydrofuran five times after magnetic separation. Vacuum oven dry. Disperse the prepared dry magnetic particles in 150ml N,N-diethylformamide, weigh 11.3g monomer N-isopropylacrylamide (NIPAAm), 10.0g N,N-dimethylacrylamide, 10.0 gN, N-diethylacrylamide, 0.3284g dilauroyl peroxide, 1.21g α-dithionaphthoic acid isobutyronitrile, carry out solution polymerization, the polymerization temperature is 70 ℃, and the polymerization time is 8 hours, will obtain Magnetic temperature-sensitive composite microspheres were obtained after magnetic separation and vacuum drying of the product. The particle size of the composite microsphere is monodisperse and within the range of 30nm-500nm. figure 1 is the molecular structure formula of the magnetic composite microsphere...

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Abstract

The invention belongs to the technical field of medical engineering of polymer material and dust, in particular to a method for preparing magnetic temperature-sensitive composite microsphere with nuclear shell structure by adopting in-situ grafting technique. The preparation method comprises the following steps: carrying out surface modification to ferroferric oxide nano magnetic particles, leading the surface thereof to be carried with polymerisable double bonds, utilizing reversible addition-fragmentation chain transfer (RAFT) polymerization technique, carrying out in-situ grafting polymerization to N-isopropylacrylamide and hydrophilic allyl monomer on the surface of the magnetic particles to form a temperature-sensitive polymer, and obtaining the nuclear shell structure composite material with temperature-sensitive hydrophilic shell and controllable magnetothermal effect magnetic nuclear. The nuclear shell structure composite material has magnetothermal effect of ferroferric oxide, magnetic positioning capability and temperature responsiveness of the temperature-sensitive polymer simultaneously, and has wide application in fields of control release, immunoassay, memory element switches and sensors and the like. The synthesis method is simple and easy to operate, and the materials can be produced industrially, thus having good promotion and application values.

Description

technical field [0001] The invention belongs to the technical field of macromolecular materials and biomedical engineering, and specifically relates to a method for preparing magnetic temperature-sensitive composite microspheres with a core-shell structure by an in-situ grafting process. Background technique [0002] Polymer-modified magnetic particles are widely used in biochemical fields such as immobilized enzymes, cell optimization, protein separation, and targeted drugs because they have both the surface functionality of polymers and the magnetic responsiveness of magnetic cores. The relatively mature preparation method of magnetic polymer particles is monomer polymerization method, including suspension polymerization method, emulsion polymerization method, dispersion polymerization method and so on. However, the above-mentioned several preparation methods usually adopt the conventional free radical polymerization method, the molecular weight of the shell layer polymer ...

Claims

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Application Information

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IPC IPC(8): B01J13/02H01F1/11C12N11/08C07K1/14
CPCC08F4/32
Inventor 任杰曹阳李建波陈大凯
Owner TONGJI UNIV
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