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Preparation method of fluorescent microspheres based on cross-linked polymer

A technology of cross-linked polymers and fluorescent microspheres, which is applied in the field of preparation of functional polymer microspheres, can solve the problems of poor fluorescence and poor monodispersity of microspheres, and achieve easy operation, improved monodispersity, Effect of improving luminous efficiency

Inactive Publication Date: 2020-05-08
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The fluorescent microspheres prepared by this method will cause polymer aggregation to deteriorate the monodispersity and fluorescence of the microspheres due to the addition of a crosslinking agent at the beginning of the reaction.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A method for preparing fluorescent microspheres based on cross-linked polymers, the steps comprising:

[0026] 1. In a 250ml four-necked round-bottom flask equipped with a mechanical stirrer, a condenser tube and a nitrogen conduit, add 5wt% dispersant polyvinylpyrrolidone and a certain proportion of methanol and aqueous solution at a temperature of 60°C and a mechanical stirring rate of 190r / min It forms a clear and transparent dispersant solution.

[0027] 2. Weigh 0.1g of initiator azobisisobutyronitrile, 20mg of fluorescent dye Rhodamine 6G or Rhodamine B, dissolve them in 5.0g of styrene monomer, and ultrasonically oscillate to mix and disperse evenly to form a fluorescent monomer mixture liquid.

[0028] 3. Add the fluorescent monomer mixture in the above 2 into the dispersant solution, stir and mix evenly, pass nitrogen gas to remove oxygen for 0.5h, and then seal. Placed in a constant temperature water bath, reacted for 12 hours under the conditions of a const...

Embodiment 2

[0030] A method for preparing fluorescent microspheres based on cross-linked polymers, the steps comprising:

[0031] 1. In a 250ml four-necked round-bottom flask equipped with a mechanical stirrer, a condenser tube and a nitrogen conduit, add 5wt% dispersant polyvinylpyrrolidone and a certain proportion of methanol and aqueous solution at a temperature of 60°C and a mechanical stirring rate of 190r / min It forms a clear and transparent dispersant solution.

[0032] 2. Weigh 0.1g of initiator azobisisobutyronitrile, 20mg of fluorescent dye rhodamine 6G or rhodamine B, dissolve them in 5.0g of methyl methacrylate monomer, and ultrasonically vibrate to make them mix and disperse evenly to form Fluorescent monomer mixture.

[0033] 3. Add the fluorescent monomer mixture in the above 2 into the dispersant solution, stir and mix evenly, pass nitrogen gas to remove oxygen for 0.5h, and then seal. Place in a constant temperature water bath, and react for 12 hours under the condition...

Embodiment 3

[0035] A method for preparing fluorescent microspheres based on cross-linked polymers, the steps comprising:

[0036] 1. In a 250ml four-necked round-bottomed flask equipped with a mechanical stirrer, a condenser tube and a nitrogen conduit, add 5wt% dispersant polyvinylpyrrolidone and a certain proportion of isopropanol and aqueous solution at a temperature of 60°C and a mechanical stirring rate of 190r / min to form a clear and transparent dispersant solution.

[0037] 2. Weigh 0.1 g of the initiator azobisisobutyronitrile and 20 mg of the fluorescent dye rhodamine 6G, dissolve them in 5.0 g of styrene monomer, and ultrasonically oscillate to make them evenly mixed and dispersed to form a fluorescent monomer mixture.

[0038] 3. Add the fluorescent monomer mixture in the above 2 into the dispersant solution, stir and mix evenly, pass nitrogen gas to remove oxygen for 0.5h, and then seal. Place in a constant temperature water bath, and react for 12 hours under the conditions ...

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Abstract

The invention discloses a preparation method of fluorescent microspheres based on a cross-linked polymer, wherein a fluorescent substance in the microspheres is an organic fluorescent dye. The preparation method comprises the following steps: 1, dissolving a dispersing agent polyvinylpyrrolidone into an alcohol-water polar medium in a certain proportion, and dispersing to obtain a clear and transparent solution; 2, adding an initiator azodiisobutyronitrile, a rhodamine fluorescent monomer and a polymer monomer into the system; 3, adding a cross-linking agent solution dissolved with an initiator and a monomer, uniformly stirring and dispersing the solution, and carrying out polymerization reaction at a certain temperature under the protection of nitrogen to obtain the monodisperse cross-linked polymer fluorescent microspheres. On the basis of adopting a traditional dispersion polymerization method, the feeding time is changed, so that the monodispersity of the fluorescent microspheres is improved; rhodamine fluorescent dyes are used and can be directly obtained; the fluorescent microsphere prepared by copolymerizing and wrapping the fluorescent dye with the cross-linked polymer hasa stable body structure and fluorescence efficiency, and good solvent resistance and thermal stability.

Description

technical field [0001] The invention relates to a preparation method of functional polymer microspheres, in particular to a preparation method based on cross-linked polymer fluorescent microspheres. Background technique [0002] Fluorescent microspheres refer to solid particles with diameters ranging from nanometers to micrometers, with fluorescent substances loaded on the surface or inside of the microspheres, which can be excited by external energy or visible light to fluoresce. Fluorescent microspheres have a stable morphological structure and high luminous efficiency, and are less affected by external conditions such as heat, magnetism, and solution than single fluorescent substances. As a new type of functional polymer material, they have been widely used in the field of biomedicine , such as directional drug delivery in biomedicine, immune detection, cell labeling, high-throughput drug screening, etc., and can also be used in some experimental tests, such as flow cytom...

Claims

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Application Information

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IPC IPC(8): C08F212/08C08F220/14C08F220/06C08F220/56C08F212/36C08F2/44C08K5/19C09K11/06
CPCC08F212/08C08F220/14C08F220/56C08F2/44C08K5/19C09K11/06C09K2211/14
Inventor 孙姣郭子轩陈文义
Owner HEBEI UNIV OF TECH
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