Method for preparing high molecular fluorescent microballoons

A fluorescent microsphere and polymer technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of changing the properties of fluorescent substances, changing fluorescent substances, difficult chemical reactions, etc., and achieves high repeatability, low price, and high efficiency. Effect

Inactive Publication Date: 2008-12-31
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the fluorescent microspheres prepared by the above two methods have stable fluorescence content and low toxicity, but these two methods have specific requirements for the monomer, which makes the price of the reagent very high. In addition, most of the fluoresceins contain benzene rings and hetero The rigid planar structure of the conjugated double bond of the ring makes it difficult for the chemical reaction to proceed. In addition, the chemical reaction changes the structure of the fluorescent substance, thereby changing the properties of the fluorescent substance, such as red shift

Method used

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  • Method for preparing high molecular fluorescent microballoons
  • Method for preparing high molecular fluorescent microballoons
  • Method for preparing high molecular fluorescent microballoons

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Embodiment 1: Preparation of polymer fluorescent (coumarin 6) microspheres

[0035] (1) Prepare a stabilizer solution; in an argon atmosphere, add the dispersion stabilizer polyvinylpyrrolidone to the polar medium ethanol, and the mass ratio of the dispersion stabilizer to the polar medium is 1 / 65;

[0036] (2) Prepare the monomer solution; in argon gas, add the initiator azodiethylbutyrocyanide and fluorescein coumarin 6 into the monomer styrene at a temperature of -5°C, and achieve a homogeneous phase by ultrasonic oscillation to obtain In the monomer solution, the mass ratio of the fluorescein to the initiator is 1 / 75, and the mass ratio of the sum of the initiator and the fluorescein to the monomer is 1 / 30;

[0037] (3) Stirring reaction; in an argon atmosphere, the monomer solution is added to the stabilizer solution, the stirring speed is 50 rpm, at a temperature of 70°C, the reaction is for 12 hours, the mass ratio of the monomer solution and the stabilizer solut...

Embodiment 2

[0040]Embodiment 2: Preparation of polymer fluorescent (rhodamine 6G) microspheres

[0041] (1) Prepare a stabilizer solution; in a nitrogen atmosphere, add the dispersion stabilizer polyoxyethylene to the polar medium methanol, and the mass ratio of the dispersion stabilizer to the polar medium is 1 / 130;

[0042] (2) Prepare the monomer solution; in nitrogen gas, add the initiator benzoyl peroxide and fluorescein rhodamine 6G into the monomer methyl methacrylate at a temperature of 10°C, and achieve a homogeneous phase by ultrasonic oscillation to obtain a single Body solution, the mass ratio of fluorescein and initiator is 7 / 50, and the mass ratio of the sum of initiator and fluorescein to the monomer is 1 / 90;

[0043] (3) stirring reaction; in nitrogen atmosphere, monomer solution is joined in the stabilizer solution, stirring speed is 500 rev / mins, at 40 ℃ of temperature, reaction 24 hours, the mass ratio of monomer solution and stabilizer solution is 1 / 9;

[0044] (4) c...

Embodiment 3

[0046] Example 3: Preparation of polymer fluorescent (coumarin 6 / rhodamine 6G=1 / 2) microspheres

[0047] (1) Prepare a stabilizer solution; in a mixed atmosphere of argon and nitrogen, the dispersion stabilizer polyethylene glycol is added to the mixed solution of polar medium ethanol and water, the mass ratio of ethanol to water is 25 / 1, and the dispersion is stable The mass ratio of agent and polar medium is 1 / 85;

[0048] (2) Prepare the monomer solution; in the mixed gas of argon and nitrogen, add the mixture of initiator azodiethylbutyronitrile and fluorescein coumarin 6 and rhodamine 6G in the monomer methacrylic acid, coumarin The mass ratio of 6 and rhodamine 6G is 1 / 2, the temperature is 5°C, and the homogeneous phase is obtained by ultrasonic oscillation, and the monomer solution is obtained. The mass ratio of fluorescein and initiator is 1 / 50, and the two kinds of initiator and fluorescein The mass ratio of the sum of substances to the monomer is 1 / 30;

[0049] (3...

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Abstract

Disclosed is a method for preparing fluorescent polymer beads, belonging to methods for preparing nano-material and micron material and aiming at providing a preparation method which requires no strict conditions and is easy and convenient to operate, and the raw materials are safe, easy to get, low in cost and high in reproducibility and efficiency. The method includes the following steps:(1)preparing stabilizing agent solution; (2) preparing monomer solution; (3)blending for reaction; (4)cleaning repeatedly for 3-5times; the deposit finally got is fluorescent beads. The invention is capable of preparing a plurality of fluorescent beads with even granularity distribution through dispersion-polymerization in one step; requirements to fluorescent dye are low, and the fluorescent dye is low in cost and is of no need to change the intrinsical structure of the fluorescein, thus avoiding changing the fluorescence and solving the problem that the fluorescent dye is easy to lose in direct adsorption method. The monodisperse particles of the fluorescent polymer beads prepared through the method are 1-5 microns and the fluorescent polymer beads are of high reproducibility and high efficiency and of no special compatibility to biological tissue cells.

Description

technical field [0001] The invention belongs to a method for preparing nano and micro materials, in particular to a method for preparing polymer fluorescent microspheres by a dispersion polymerization method. Background technique [0002] Fluorescent microspheres refer to solid particles with a diameter ranging from nanometer to micrometer, loaded with fluorescent substances, and can be stimulated by external energy to emit fluorescence. The shape can be any shape, and the typical shape is spherical. The carriers of fluorescent microspheres are mostly organic or inorganic polymer materials, which have relatively stable morphological structure and luminescent behavior, and are less affected by external conditions such as solvents, heat, electricity, and magnetism than pure fluorescent compounds. As a new type of carrier material, it has been widely used in the field of biomedicine, such as directional delivery of drugs in biochemistry and biomedicine, medical latex reagents, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F212/08C08F220/14C08F220/06C08F2/44C09K11/00
Inventor 杜桂焕韩文敏刘祖黎夏星孙绪燕方敏
Owner HUAZHONG UNIV OF SCI & TECH
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