A fluorescent polymer microsphere loaded with quantum dots and its preparation method

A technology of fluorescent polymers and quantum dots, which is applied in the preparation of microspheres, microcapsule preparations, chemical instruments and methods, etc., can solve the problems of difference in fluorescence brightness, decline in fluorescence performance, poor stability, etc., and achieve stable and durable fluorescence performance. Change the fluorescence intensity, good effect of monodispersity

Active Publication Date: 2021-07-13
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The swelling method is simple to operate, but there is a problem of large differences in fluorescence brightness between individual fluorescent microspheres; the method of preparing quantum dot fluorescent microspheres by layer-by-layer self-assembly method is relatively simple, but it faces poor controllability, poor stability, and decreased fluorescence performance. and other problems; the fluorescent microspheres prepared by the copolymerization method have uniform brightness, and the quantum dots and microspheres are firmly combined, but the quantum dots are easily oxidized and aggregated during the polymerization process, which leads to a decrease in the fluorescence intensity of the quantum dots or even quenching

Method used

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  • A fluorescent polymer microsphere loaded with quantum dots and its preparation method
  • A fluorescent polymer microsphere loaded with quantum dots and its preparation method
  • A fluorescent polymer microsphere loaded with quantum dots and its preparation method

Examples

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Embodiment 1

[0032] The synthesis of embodiment 1 macromolecule RAFT reagent PAA-TTC

[0033]Acrylic acid (AA) (14.41g, 200mmol), S-1-dodecyl-S'-(α,α'-dimethyl-α"-acetic acid) trithiocarbonate (DDMAT) (0.1826g , 0.5mmol) and azobisisobutyronitrile (AIBN) (8.23mg, 0.05mmol) were added in a 150mL flask, dissolved with 1,4-dioxane (48.6g), and the solution was ventilated with nitrogen for 30 minutes Degassed, then immersed in a preheated oil bath at 70 °C for 2 hours, after cooling, the product was precipitated into diethyl ether and purified by a precipitation / filtration cycle. After drying at room temperature under vacuum, a yellow large Molecular RAFT agent PAA-TTC polymer powder, molecular weight about 20000.

[0034]

Embodiment 2

[0035] Example 2 Synthesis of cross-linked PMGA microspheres based on PAA-TTC

[0036] The weight ratio of ethanol / water mixture 40 / 60 (7.2g+10.8g) was introduced in a 25mL round bottom flask as a solvent, and then 2.0g of glycidyl methacrylate GMA monomer (10wt% relative to the system) was added, The stabilizing dispersant PAA-TTC of 0.30g (15wt% with respect to monomer), the DDMAT of 0.005g (0.25wt% with respect to monomer), the Darocur1173 of 0.06g (3wt% with respect to monomer) and 0.06g dipropylene glycol diol Acrylic acid (3 wt% relative to monomer), dissolved with magnetic stirring. The reaction mixture was deoxygenated with nitrogen for 30 minutes, sealed with a glass stopper with a quartz glass sheet, and then illuminated with a 365nm wavelength LED lamp (light intensity 2.5mW / cm2) under constant stirring. 2 ) was irradiated from the top of the round bottom flask for 3 hours. The product is separated by centrifugation, washed with ethanol / water (40 / 60, w / w), and cen...

Embodiment 3

[0038] The weight ratio of ethanol / water mixture 40 / 60 (7.6g+11.4g) was introduced in a 25mL round bottom flask as a solvent, and then 1.0g of glycidyl methacrylate GMA monomer (5wt% relative to the system) was added, The stabilizing dispersant PAA-TTC of 0.10g (10wt% with respect to monomer), the DDMAT of 0.005g (0.25% with respect to monomer), the Darocur 1173 of 0.01g (1wt% with respect to monomer) and 0.03g dipropylene glycol diol Acrylic acid (3 wt% relative to monomer), dissolved with magnetic stirring. The reaction mixture was deoxygenated with nitrogen for 30 minutes, sealed with a glass stopper with a quartz glass sheet, and then illuminated with a 365nm wavelength LED lamp (light intensity 2.5mW / cm2) under constant stirring. 2 ) was irradiated from the top of the round bottom flask for 3 hours. The product was separated by centrifugation, washed with ethanol / water (40 / 60, w / w), and repeatedly centrifuged and washed 2 to 3 times to obtain cross-linked PGMA polymer mi...

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Abstract

The invention discloses a fluorescent polymer microsphere with quantum dots inside and a preparation method thereof. First, acrylic acid and S‑1‑dodecyl‑S′‑(α,α′‑dimethyl‑α″‑acetic acid) trithiocarbonate are copolymerized to obtain a macromolecular RAFT agent PAA‑TTC; Glycidyl acrylate is a functional monomer, the macromolecular RAFT reagent PAA-TTC is a stable dispersant, and a cross-linking agent is added to synthesize cross-linked PGMA microspheres through the RAFT light dispersion polymerization method; then the obtained microspheres are placed in an organic solvent After swelling in medium, cadmium selenide quantum dots stabilized by mercaptopropionic acid ligands are added, and a catalyst is added under heating conditions to make the carboxyl groups on the mercaptopropionic acid ligands react with the epoxy groups inside the microspheres, thereby preparing the Polymer microspheres loaded with fluorescent quantum dots inside. By introducing epoxy groups inside the microspheres, they can react with water-soluble quantum dots stabilized by mercaptopropionic acid ligands, providing a basis for the preparation of quantum dot fluorescent polymer microspheres A new path has been developed, and the obtained fluorescent polymer microspheres have uniform particle size, good monodispersity, and very stable and long-lasting fluorescent properties.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a fluorescent polymer microsphere with quantum dots inside and a preparation method thereof. Background technique [0002] Polymer microspheres with sizes ranging from nanometers to micrometers, with fluorescent substances on the surface or inside, are widely used in biomedical detection, in vivo labeling, immunoassays, immobilized enzymes, etc. due to their stable morphology and high luminous efficiency. field has great application potential. At present, the preparation methods of fluorescent polymer microspheres mainly include physical and chemical methods. The physical method to prepare polymer fluorescent microspheres is the most direct and simplest method, often through the physical adsorption force on the surface of the microspheres, or hydrogen bond force, or embedding, encapsulation, etc., to combine fluorescent substances with polymer microspheres. The bigges...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F293/00C08F2/48C09K11/02C09K11/88B01J13/14B01J13/20
CPCB01J13/14B01J13/20C08F2/48C08F293/005C08F2438/03C09K11/025C09K11/883
Inventor 曾兆华黄永平王梦真杨建文袁佳宇
Owner SUN YAT SEN UNIV
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