Preparation method of high-molecular fluorescent microsphere

A fluorescent microsphere and polymer technology, applied in the field of preparation of polymer fluorescent microspheres, can solve problems such as coating materials that are easily affected by the surrounding environment and lack biocompatibility, and achieve good surface reactivity, good Optical properties, easy functionalization effects

Active Publication Date: 2014-12-17
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, some unstable fluorescein molecules are exposed on the surface of the microspheres and are easily affected by the surrounding environment.
In addition, the surface of polystyrene microspheres lacks a layer of biocompatible coating material

Method used

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  • Preparation method of high-molecular fluorescent microsphere
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  • Preparation method of high-molecular fluorescent microsphere

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] 1. Preparation of Surface Carboxylated Polystyrene Microspheres

[0052] Surface carboxylated polystyrene microspheres were prepared by two-step dispersion polymerization. First, 0.12g of initiator azobisisovaleronitrile (AMBN), 0.135g of stabilizer polyvinylpyrrolidone PVP360 (Mw=360000g / mol), 0.15g of co-stabilizer TX3050, and 3.0g of styrene monomer were dissolved in anhydrous Add 16.15mL of ethanol and 0.85mL of ultrapure water into a reaction kettle equipped with a stirrer, thermometer and reflux condensing device, stir and mix evenly, pass nitrogen to the reaction system for deoxidation treatment, and then place the above reaction kettle in an oil bath , heated to 60°C for 1 h; dissolve 3 g of styrene and 0.06 g of acrylic acid in a mixed solution of 7.6 mL of absolute ethanol and 0.4 mL of ultrapure water, add it to another reaction kettle, and pass nitrogen to the reaction system Deoxidize and heat to 60°C; react for 60min, add hot styrene and acrylic acid solu...

Embodiment 2

[0058] 1. Preparation of Surface Carboxylated Polystyrene Microspheres

[0059] Surface carboxylated polystyrene microspheres were prepared by two-step dispersion polymerization. First, 0.175g of initiator azobisisovaleronitrile (AMBN), 0.7g of stabilizer polyvinylpyrrolidone PVP55 (Mw=55000g / mol), 0.245g of co-stabilizer TX305, and 3.125g of styrene monomer were dissolved in anhydrous Add 13 mL of ethanol to a reaction kettle equipped with a stirrer, a thermometer and a reflux condensing device, stir and mix evenly, pass nitrogen gas through the reaction system for deoxidation treatment, then place the above reaction kettle in an oil bath, and heat to 60°C for 1 hour; Dissolve 3.125g of styrene and 0.125g of acrylic acid in 13mL of absolute ethanol, add to another reaction kettle, pass nitrogen gas to the reaction system for deoxidation treatment, and heat to 60°C; react for 90min, put the hot styrene and alkene The propionic acid solution was added into the reaction kettle,...

example 3

[0065] 1. Preparation of Surface Carboxylated Polystyrene Microspheres

[0066] Surface carboxylated polystyrene microspheres were prepared by two-step dispersion polymerization. First, 0.125g of initiator azobisisovaleronitrile (AMBN), 0.5g of stabilizer polyvinylpyrrolidone PVP55 (Mw=55000g / mol), 0.175g of co-stabilizer TX305, and 3.125g of styrene monomer were dissolved in anhydrous Add 25 mL of ethanol to a reaction kettle equipped with a stirrer, a thermometer and a reflux condensing device, stir and mix evenly, pass nitrogen gas through the reaction system for deoxidation treatment, then place the above reaction kettle in an oil bath, and heat to 60°C for 1 hour; Dissolve 3.125g of styrene and 0.125g of acrylic acid in 25mL of absolute ethanol, add to another reaction kettle, pass nitrogen gas to the reaction system for deoxidation treatment, and heat to 60°C; react for 60min, put the hot styrene and alkene The propionic acid solution was added into the reaction kettle,...

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Abstract

The invention discloses a preparation method of a high-molecular fluorescent microsphere. The method includes following steps: dispersing 1 part by weight of polystyrene microspheres in 0.1-1 ml of ultrapure water; adding dropwisely the polystyrene microsphere aqueous dispersion to 3-10 ml of a polydiallyldimethylamine hydrochloride solution with a concentration being 1.0-4.0 mg/ml with stirring; continuously stirring the solution for 1-4 h; performing centrifugation and removing a supernate; performing a washing process through ultrapure water; performing a centrifugation and collecting precipitate; vibratingly dispersing the precipitate in 1-2 ml of ultrapure water; adding dropwisely the polystyrene microsphere aqueous dispersion to 5-50 ml of a marked or an unmarked polysaccharide-type polyelectrolyte macromolecule solution with a concentration being 1.0-6.0 mg/ml with stirring; continuously stirring the solution for 1-4 h; performing centrifugation and removing a supernate; dispersing a precipitate in pure water; performing a centrifugation and collecting precipitate; and dispersing the precipitate in ultrapure water to obtain polysaccharide-modified fluorescent microsphere. The high-molecular fluorescent microsphere is 1-10 [mu]m in particle size, is 350-800 nm in fluorescent excitation wavelength, and has excellent biocompatibility and stability.

Description

Technical field: [0001] The invention relates to a preparation method of polymer fluorescent microspheres. The invention belongs to the field of biomedical polymer materials. Background technique [0002] Fluorescent microspheres are enriched in organic or inorganic fluorescent substances that can emit fluorescence in a single microsphere, and the luminous intensity and fluorescence sensitivity are relatively high. The field has been widely used (Macromolecules2011, 44, 4801; Macromol. Chem. Phys. 2005, 206, 2440). Among the various characteristics of microspheres, the important factors affecting their application are the size, dispersion and shape of microspheres. In addition, their biocompatibility requirements are also very important (Macromolecules2005, 38, 8300 ). [0003] In recent years, breakthroughs have been made in the synthesis of monodisperse polystyrene fluorescent microspheres with predetermined sizes. The prepared microspheres have the advantages of regula...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/02B01J13/14G01N15/14C08F257/02C08F8/32C09K11/06
Inventor 艾华王丹
Owner SICHUAN UNIV
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