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Method for preparing quantum dot fluorescent microspheres through ultrasonic initiation

A technology of fluorescent microspheres and quantum dots, which is applied in the direction of luminescent materials, chemical instruments and methods, etc., and can solve problems affecting fluorescence intensity, surface defects of quantum dots, etc.

Pending Publication Date: 2022-03-15
朱小波 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Commonly used initiators, such as persulfate, azo compounds, etc., will generate strong oxidizing free radicals when decomposed, which will easily cause defects on the surface of quantum dots and affect their fluorescence intensity

Method used

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  • Method for preparing quantum dot fluorescent microspheres through ultrasonic initiation
  • Method for preparing quantum dot fluorescent microspheres through ultrasonic initiation
  • Method for preparing quantum dot fluorescent microspheres through ultrasonic initiation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] Weigh 0.6g of quantum dot powder, dissolve in 1g of styrene and 0.2g of divinylbenzene to form a quantum dot-monomer / crosslinking agent solution;

[0059] Pour the above solution into 100mL of 0.1g / L sodium dodecylsulfonate solution;

[0060] Start the ultrasonic reactor, set the temperature to 0°C, the power parameter to 50W, corresponding to a power density of 0.5kW / L, and ultrasonic emulsification for 15 minutes;

[0061] Set the temperature at 0°C, the power parameter is 400W, the corresponding power density is 4kW / L, and the reaction time is 4h;

[0062] Add 0.5mL glycidyl methacrylate dropwise and continue the reaction for 4h;

[0063] The temperature was returned to room temperature, glycine-sodium hydroxide solution (pH=12) was added dropwise, and the reaction was continued for 4h;

[0064] Stop ultrasonication, add dilute hydrochloric acid dropwise, adjust pH to 6, centrifuge at 6000rpm for 10min, disperse with ultrapure water ultrasonically, repeat 3 times t...

Embodiment 2

[0066] Weigh 0.6g quantum dot powder, dissolve in 0.25g styrene and 0.5g divinylbenzene to form quantum dot-monomer / crosslinking agent solution;

[0067] Pour the above solution into 100mL of 0.1g / L sodium dodecylsulfonate solution;

[0068] Start the ultrasonic reactor, set the temperature to 0°C, the power parameter to 300W, corresponding to a power density of 3kW / L, and ultrasonic emulsification for 15 minutes;

[0069] Set the temperature at 0°C, the power parameter is 400W, the corresponding power density is 4kW / L, and the reaction time is 4h;

[0070] Add 0.5mL glycidyl methacrylate dropwise and continue the reaction for 4h;

[0071] The temperature was returned to room temperature, glycine-sodium hydroxide solution (pH=12) was added dropwise, and the reaction was continued for 4h;

[0072] Stop ultrasonication, add dilute hydrochloric acid dropwise, adjust pH to 6, centrifuge at 6000rpm for 10min, disperse with ultrapure water ultrasonically, repeat 3 times to obtain ...

Embodiment 3

[0074] Weigh 0.6g quantum dot powder, dissolve in 0.25g styrene and 0.5g ethylene glycol diacrylate to form quantum dot-monomer / crosslinker solution;

[0075] Pour the above solution into 100mL of 0.1g / L sodium dodecylsulfonate solution;

[0076] Start the ultrasonic reactor, set the temperature to 0°C, the power parameter to 300W, corresponding to a power density of 3kW / L, and ultrasonic emulsification for 15 minutes;

[0077] Set the temperature to 0°C, the power parameter is 800W, the corresponding power density is 8kW / L, and the reaction time is 4h;

[0078] Add 0.5mL glycidyl methacrylate dropwise and continue the reaction for 4h;

[0079] The temperature was returned to room temperature, and aspartic acid-sodium hydroxide solution (pH=12) was added dropwise, and the reaction was continued for 4h;

[0080] Stop ultrasonication, add dilute hydrochloric acid dropwise, adjust pH to 6, centrifuge at 6000rpm for 10min, disperse with ultrapure water ultrasonically, repeat 3 t...

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Abstract

The invention provides a method for preparing quantum dot fluorescent microspheres through ultrasonic initiation, which comprises the following steps: A) mixing quantum dots, monomers and a cross-linking agent to obtain a quantum dot mixed solution; the cross-linking agent is one or more of divinyl benzene, an acrylic acid alcohol ester cross-linking agent and a methacrylic acid alcohol ester cross-linking agent; b) mixing the quantum dot mixed solution with an emulsifier solution, and emulsifying to obtain an emulsion; c) initiating polymerization of the emulsion under an ultrasonic condition to obtain a polymerization system; and D) adding a functional monomer and amino acid into the polymerization system, and reacting to obtain the quantum dot fluorescent microspheres. According to the method, water generates free radicals through ultrasonic waves with proper power, and vinyl monomers in the seeds are initiated to be subjected to polymerization reaction. By controlling the concentration of the quantum dot-oil soluble monomer, an active center can be formed only at the seed, so that the phenomenon of self-nucleation of the monomer is avoided, and polymer empty spheres are not generated.

Description

technical field [0001] The invention belongs to the technical field of fluorescent microsphere synthesis, and in particular relates to a method for preparing quantum dot fluorescent microspheres induced by ultrasound. Background technique [0002] As a new type of fluorescent labeling material, quantum dots have the excellent properties of wider excitation wavelength range, narrower emission peak and photobleaching resistance compared with traditional fluorescent dyes, and are a more ideal fluorescent coding material. However, the shortcomings of quantum dots, such as small particle size, high surface energy, and oxygen resistance, limit their applications. Encapsulating quantum dots in polymer microspheres can significantly improve the optical stability, colloidal stability and biocompatibility of quantum dots. [0003] At present, the preparation of quantum dot nanospheres usually first prepares quantum dot seed micelles, then adds initiators and monomers to polymerize th...

Claims

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Application Information

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IPC IPC(8): C08F212/08C08F212/36C08F220/32C08F222/14C08K3/30C09K11/02
CPCC08F212/08C08F212/36C08F220/325C08F222/102C08K3/30C09K11/025C08K2003/3009C08K2003/3027C08K2003/3036
Inventor 朱小波
Owner 朱小波
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