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Macromolecular fluorescent microspheres and preparation method thereof

A fluorescent microsphere and macromolecule technology, applied in the field of fluorescent sensing material preparation, can solve the problems of poor solubility of conjugated macromolecules, difficult adjustability and controllability of fluorescent properties, etc., and achieves easy characterization and heterogeneous phase. Simple and controllable response

Inactive Publication Date: 2011-09-14
SUZHOU UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It has been reported in the literature that fluorescent microspheres are prepared by adsorbing conjugated polymer electrolytes on the surface of microspheres by electrostatic adsorption, and its application in sensors is discussed (Langmuir2007, 23, 112-115). Although this method is relatively simple, it has There are also some problems, such as conjugated polymers must be well dissolved in a certain solvent before adsorption, however, the poor solubility of conjugated polymers is well known, even if the introduction of solubilizing groups in the side groups may not be able to In addition, the solubility of the conjugated polymer on the surface of the microsphere will bring about whether the conjugated polymer can exist stably on the surface of the microsphere, that is, the stability of the fluorescent performance of the microsphere
There are also documents disclosing that the surface of the microsphere is functionalized, reacted with a conjugated polymer monomer, and cross-coupled on the surface of the microsphere to form a method of microspheres with conjugated polymers on the surface (Langmuir 2007, 23, 4541-4548 ), this method can stably link conjugated polymers to the surface of microspheres through covalent bonds, but the cross-coupling reaction on the surface of microspheres to generate conjugated polymers is a heterogeneous polymerization reaction, which has certain difficulties.
In the Chinese invention patent "copolymerized cross-linked polymer fluorescent microspheres and its preparation method" (CN101177607A), it is disclosed that fluorescent monomers and other multifunctional monomers are used in the action of initiators to free-radical copolymerize the preparation of fluorescent polymers. Microspheres, the fluorescent microspheres prepared by this method have good stability, but it is relatively difficult to adjust and control their fluorescence properties

Method used

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  • Macromolecular fluorescent microspheres and preparation method thereof
  • Macromolecular fluorescent microspheres and preparation method thereof
  • Macromolecular fluorescent microspheres and preparation method thereof

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Embodiment 1

[0023] 1. Use Wessling’s salt polymer precursor method: In a 50ml two-necked flask, protected by nitrogen, add 1.0g of polymerized monomers with dodecyloxy side chains on the benzene ring, and dissolve them in 10ml of tetrahydrofuran solution , magnetic stirring to make it completely dissolved, put it into an ice-water bath, keep the reaction system at 0-5°C under the protection of nitrogen, slowly add 2.4ml of 1.25M NaOH / MeOH solution, react for 1 hour, add HCl to terminate the reaction, and The reaction solution was put into a dialysis bag with a molecular weight of 14000 and dialyzed in water for 24 hours to prepare the precursor of polymer PPV. The synthetic route is as follows:

[0024]

[0025] Wherein, n is the number of repeating units.

[0026] See attached figure 1 , which is the nuclear magnetic spectrum (HNMR) of the above-mentioned polyphenylene (PPV) precursor, with deuterated chloroform as the solvent, at 7.0-6.7ppm, 4.5ppm, 3.9ppm, 2.9ppm, 1.9ppm and 0.9ppm...

Embodiment 2

[0031] 1. In a 50ml two-necked flask, protected by nitrogen, add 0.5g of side-group-free polymerized monomer, dissolve it in 10ml of water, stir it with magnetic force to completely dissolve it, put it in an ice-water bath, and keep the reaction system under the protection of nitrogen Keep 0~5℃, add 1.25M NaOH / H 2 O solution 1ml, after reacting for 1 hour, add HCl to terminate the reaction, put the reaction solution into a dialysis bag with a molecular weight of 14000 and dialyze in water for 24 hours to prepare the precursor of polymer PPV. The synthetic route is as follows:

[0032]

[0033]2. Add 0.5g of the precursor prepared in step 1 into the conical flask, dissolve it with 10ml of water, add 0.5g of monodisperse polystyrene microspheres with a particle size of 25 microns on the surface, and use 1.25M Adjust the pH value to 9 with NaOH, ultrasonically oscillate for 1 hour in an ultrasonic oscillator, keep the water temperature of the ultrasonic oscillator below 30°C, ...

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Abstract

The invention discloses macromolecular fluorescent microspheres and a preparation method thereof. The macromolecular fluorescent microspheres use monodisperse sulfonated polystyrene microspheres as core microspheres, and the surfaces of the macromolecular fluorescent microspheres are coated with a shell layer of a p-phenylene vinylene (PPV) fluorescent conjugated macromolecular polymer. The preparation method of the macromolecular fluorescent microspheres comprises the following steps of: synthesizing a positively charged PPV fluorescent conjugated macromolecular polymer precursor in solutionby using a Wessling sulfosalt polymer precursor method; adding the monodisperse sulfonated polystyrene microspheres into the precursor, and then processing the mixture for 0.5 to 2 hours under a vacuum condition that the temperature is between 90 and 150 DEG C; and washing and drying the mixture to obtain PPV conjugated macromolecular fluorescent microspheres. An inhomogeneous reaction for synthesizing the conjugated polymer in the method is simple and controllable, and the stability of the fluorescence of the microspheres is effectively improved.

Description

technical field [0001] The invention relates to a polymer fluorescent microsphere and a preparation method thereof, in particular to polystyrene fluorescent microspheres loaded with polystyrene (PPV) conjugated polymers on the surface and a preparation method thereof, belonging to the field of fluorescence sensing material preparation . Background technique [0002] Fluorescent microspheres refer to solid particles with diameters ranging from nanometers to micrometers, loaded with fluorescent substances, and excited by external energy to fluoresce. In recent years, the application of fluorescent microspheres in the field of biomedicine has attracted more and more attention. This is due to their stable shape, large specific surface area, strong adsorption, strong agglutination, strong surface reaction ability, and stable and efficient luminous efficiency. In addition, various properties such as biospecific binding, hollow porosity, magnetism, etc. can be endowed according to...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L25/06C08L25/18C09K11/06C09K11/02B01J13/02
Inventor 范丽娟王尚丽江必旺程丝王丽莎赵伟
Owner SUZHOU UNIV
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