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Preparation method for monodisperse high-crosslinking-degree core-shell P(GMA-DVB) (glycidyl methacrylate-divinyl benzene)/Fe3O4 sphere

A high cross-linking, monodisperse technology, applied in the preparation of microspheres, microcapsule preparations, etc., can solve the problem of single particle size of monodisperse ferrite nano-magnetic beads, and achieve the improvement of monodispersity and magnetic responsiveness, Particle size controllable effect

Inactive Publication Date: 2012-06-20
NORTHWESTERN POLYTECHNICAL UNIV
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  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to overcome the deficiency that the monodisperse ferrite nano-magnetic beads prepared by the existing preparation method have a single particle size, the present invention provides a monodisperse high cross-linking degree core-shell P(GMA-DVB) / Fe 3 o 4 Preparation method of microspheres

Method used

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  • Preparation method for monodisperse high-crosslinking-degree core-shell P(GMA-DVB) (glycidyl methacrylate-divinyl benzene)/Fe3O4 sphere
  • Preparation method for monodisperse high-crosslinking-degree core-shell P(GMA-DVB) (glycidyl methacrylate-divinyl benzene)/Fe3O4 sphere
  • Preparation method for monodisperse high-crosslinking-degree core-shell P(GMA-DVB) (glycidyl methacrylate-divinyl benzene)/Fe3O4 sphere

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1: in the 100mL reactor that is equipped with condenser tube, add 60g acetonitrile and 10g methyl alcohol; 0.010g Fe 3 o 4 Add the microspheres into a 100mL reactor; weigh a monomer mixture composed of 0.19g DVB (divinylbenzene) and 0.01g GMA (glycidyl methacrylate) and 0.001g of AIBN (azobisisobutyronitrile ), after oscillating and dissolving, add it to the reactor and mix evenly; gradually raise the temperature to 70°C, and polymerize for 12 hours; perform magnetic separation on the obtained product, pour off the supernatant liquid, add absolute ethanol to disperse by ultrasonic, and then magnetically separate ; So repeated washing several times to remove excess monomer and polymer. Vacuum drying at room temperature yields dark brown P(GMA-DVB) / Fe 3 o 4 Magnetic Composite Microspheres.

[0017] After testing, the obtained magnetic P(GMA-DVB) / Fe 3 o 4 The particle size of the microsphere is 480nm, the magnetic response is 78.5emu / g, and the magnetic co...

Embodiment 2

[0018] Embodiment 2: in the 150mL reactor that is equipped with condenser tube, add 100g acetonitrile; With 0.021g Fe 3 o 4 The microspheres were added into a 150mL reactor; the monomer mixture composed of 0.21g DVB (divinylbenzene) and 0.13g GMA (glycidyl methacrylate) and 0.021g AIBN (azobisisobutyronitrile) were weighed ), after oscillating and dissolving, add it to the reactor and mix evenly; gradually raise the temperature to 75°C, and polymerize for 17 hours; perform magnetic separation on the obtained product, pour off the supernatant liquid, add absolute ethanol to disperse by ultrasonic, and then magnetically separate ; So repeated washing several times to remove excess monomer and polymer. Vacuum drying at room temperature yields dark brown P(GMA-DVB) / Fe 3 o 4 Magnetic Composite Microspheres.

[0019] After testing, the obtained magnetic P(GMA-DVB) / Fe 3 o 4 The particle size of the microsphere is 510nm, the magnetic response is 76.8emu / g, and the magnetic conte...

Embodiment 3

[0020] Embodiment 3: in the 150mL reactor that is equipped with condenser tube, add 100g acetonitrile and 10g ethanol; With 0.029g Fe 3 o 4 The microspheres were added into a 150mL reactor; the monomer mixture composed of 0.27g DVB (divinylbenzene) and 0.21g GMA (glycidyl methacrylate) and 0.007g of BPO (dibenzoyl peroxide) were weighed ), after oscillating and dissolving, add it to the reactor and mix evenly; gradually raise the temperature to 85°C, and polymerize for 10 hours; perform magnetic separation on the obtained product, pour off the supernatant liquid, add absolute ethanol for ultrasonic dispersion, and then magnetically separate ; So repeated washing several times to remove excess monomer and polymer. Vacuum drying at room temperature yields dark brown P(GMA-DVB) / Fe 3 o 4 Magnetic Composite Microspheres.

[0021] After testing, the obtained magnetic P(GMA-DVB) / Fe 3 o 4 The particle diameter of the microsphere is 530nm, the magnetic response is 75.7emu / g, and ...

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Abstract

The invention relates to a preparation method for a monodisperse high-crosslinking-degree core-shell P(GMA-DVB) (glycidyl methacrylate-divinyl benzene) / Fe3O4 sphere, which is used for solving the technical problem that the monodisperse ferrate magnetic nanometer sphere prepared with the traditional preparation method is uniform in participle size. The invention provides a technical scheme as follows: the monodisperse nanoscale high-crosslinking-degree core-shell P(GMA-DVB) / Fe3O4 sphere with controllable particle size, high magnetic responsiveness and high magnetic content is prepared with a precipitation polymerization method in which monodisperse high-magnetic-responsiveness Fe3O4 prepared with a thermal solvent method is used as a kernel and the GMA is used as a functional monomer, and the prepared magnetic P(GMA-DVB) / Fe3O4 sphere has a particle size of 480-650 nanometers. Compared with the preparation method in the prior art, the preparation method disclosed by the invention has the advantages of controllable particle size of the magnetic sphere and greatly improved monodispersity and magnetic responsiveness of the prepared magnetic sphere. Meanwhile, a great deal of freedom and flexibility is brought to users for further functionalizing a polymer because a GMA monomer has a reactive epoxy group.

Description

technical field [0001] The invention relates to a core-shell P(GMA-DVB) / Fe 3 o 4 The preparation method of microsphere, especially relates to a kind of core-shell P(GMA-DVB) / Fe 3 o 4 Preparation method of microspheres. Background technique [0002] Magnetic polymer composite microspheres refer to microspheres formed by combining magnetic inorganic particles and organic polymers by appropriate methods. Because it has both the magnetic responsiveness of magnetic substances and the multifunctionality of polymers (such as -COOH, -OH, -NH 2 , -SH, etc.), so it has broad application prospects in fields such as medicine, molecular biology, and biochemistry. [0003] The preparation methods of magnetic polymer composite microspheres mainly include soap-free emulsion polymerization, miniemulsion polymerization, dispersion polymerization, suspension polymerization, and inverse microemulsion polymerization. However, emulsion polymerization usually obtains monodisperse submicron s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/02
Inventor 张秋禹马明亮张和鹏耿旺昌窦金波张宝亮赵兴波
Owner NORTHWESTERN POLYTECHNICAL UNIV
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