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Magnetic fluorescent polymer microsphere with high load stability and preparation method of magnetic fluorescent polymer microsphere

A fluorescent polymer and polymer technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of large particle size of microspheres, easy quenching of quantum dot fluorescence, and complex structure of preparation instruments.

Inactive Publication Date: 2015-01-07
HUBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Monodisperse fluorescent microspheres with stable and precisely encoded signals have broad application prospects in the field of biomedicine, and monodisperse fluorescent microspheres can be prepared by polymerization, layer-by-layer self-assembly, electrospray, microfluidic and porous microspheres. However, there are still many shortcomings in these methods, such as poor monodispersity of microspheres in the polymerization method, and easy quenching of the fluorescence of quantum dots during the polymerization process; the operation of the layer-by-layer self-assembly method The steps are complicated; the monodispersity and spherical shape of microspheres obtained by electrospray technology are not good; The method realizes the loading of fluorescent, magnetic and other nanoparticles, but there is also the problem that the quantum dots are easy to leak due to the large pore size of the microspheres

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Add 1g of PVP to the dispersion medium of 160mL ethanol and 20mL water, stir for 30min to dissolve; dissolve 0.16g of azobisisobutyronitrile in 18.4g of styrene, 1g of divinylbenzene and 0.6g of acrylic acid, and add Put it into the above dispersion liquid; raise the temperature to 70°C for constant temperature reaction for 12 hours, centrifuge the emulsion and wash with ethanol to obtain polymer microspheres with a particle size of 1.35 μm and a monodispersity coefficient of 0.008.

[0027] (2) Take 1 g of the polymer microspheres described in (1), swell with magnetic stirring in 20 mL of 1,2-dichloroethane for 4 h, place in a water bath at 45 ° C, add 1.7 mL of dimethoxymethane and 3 g Anhydrous ferric chloride, after 5 hours of reaction, the temperature was raised to 80°C, and the reaction was continued for 20 hours. The obtained product was filtered by suction and then extracted for 24 hours with a Soxhlet extractor, and finally freeze-dried to obtain multi-level...

Embodiment 2

[0031] (1) Add 1g of PVP to the dispersion medium of 160mL ethanol and 15mL water, stir for 30min to dissolve; dissolve 0.2g of azobisisobutyronitrile in 21.75g ​​of styrene, 2.5g of divinylbenzene and 0.75g of acrylic acid, and Add it to the above dispersion liquid; raise the temperature to 70°C for constant temperature reaction for 12 hours, centrifuge the emulsion and wash with ethanol to obtain polymer microspheres with a particle size of 3.45 μm and a monodispersity coefficient of 0.005.

[0032] (2) Take 1 g of the polymer microspheres described in (1), swell with magnetic stirring in 20 mL of 1,2-dichloroethane for 4 h, place in a water bath at 45 ° C, add 1.7 mL of p-dimethoxybenzene and 3g of anhydrous ferric chloride, heated up to 80°C after reacting for 5 hours, and continued to react for 20 hours. The obtained product was filtered by suction and extracted for 24 hours with a Soxhlet extractor, and finally freeze-dried to obtain hierarchical porous polymer microspher...

Embodiment 3

[0036] (1) Add 1.6g of PVP to the dispersion medium of 140mL ethanol and 20mL water, stir for 30min to dissolve; dissolve 0.32g of azobisisobutyronitrile in 30.8g of styrene, 8g of divinylbenzene and 1.2g of acrylic acid, and Add it to the above dispersion liquid; raise the temperature to 70°C for constant temperature reaction for 12 hours, centrifuge the emulsion and wash with ethanol to obtain polymer microspheres with a particle size of 6.60 μm and a monodispersity coefficient of 0.012.

[0037] (2) The method for preparing hierarchically porous polymer microspheres by hypercrosslinking is the same as step (2) in Example 2, and the BET specific surface area of ​​the obtained hierarchically porous polymer microspheres is 885.4m 2 · g -1 , The pore size distribution is 0.5nm ~ 8nm.

[0038] (3) The preparation method of the magnetic hierarchical porous polymer microspheres is the same as step (3) in Example 2.

[0039] (4) Take 0.5g of the above-mentioned magnetic hierarch...

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Abstract

The invention discloses a magnetic fluorescent polymer microsphere with high load stability and a preparation method of the magnetic fluorescent polymer microsphere, belonging to the technical field of functional polymer materials. The preparation method comprises the following steps: on the basis of polystyrene-divinylbenzene copolymer microsphere the surface of which is carboxylated, obtaining multi-stage pore polymer microspheres with pore size ranging from 0.4nm to 15nm adopting a micropore knitting method firstly; and then successively loading magnetic particles and fluorescent matters by using an in-situ coprecipitation method and a swelling method to obtain the magnetic fluorescent polymer microspheres with the particle size being 1-10 microns. With the adoption of the preparation method, the multi-stage pore polymer microspheres can be controlled within a scale range equivalent to the loaded magnetic fluorescent material, and then with fixed functions combined with a functional group, the loading function and the stability of the magnetic fluorescent material are remarkably improved, flexible loading of the functional microspheres with different magnetic strengths, different fluorescent strengths and different fluorescent wave lengths can be further realized, and thus the preparation method has an important application value in the biological medicine field.

Description

[0001] technical field [0002] The invention belongs to the technical field of functional polymer materials, and in particular relates to a magnetic fluorescent polymer microsphere with high load stability and a preparation method thereof. Background technique [0003] Monodisperse fluorescent microspheres with stable and precisely encoded signals have broad application prospects in the field of biomedicine, and monodisperse fluorescent microspheres can be prepared by polymerization, layer-by-layer self-assembly, electrospray, microfluidic and porous microspheres. However, there are still many shortcomings in these methods, such as poor monodispersity of microspheres in the polymerization method, and easy quenching of the fluorescence of quantum dots during the polymerization process; the operation of the layer-by-layer self-assembly method The steps are complicated; the monodispersity and spherical shape of microspheres obtained by electrospray technology are not good; Th...

Claims

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Application Information

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IPC IPC(8): C08L25/08C08K13/02C08K3/16C08K3/30C08K3/10C08K5/01C08F212/08C08F212/36C08F220/06C08J9/28C08J3/24C09K11/60
Inventor 张高文陈苗
Owner HUBEI UNIV OF TECH
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