Method for preparing fluorescent polymer rare earth complex nano-microsphere

A technology of fluorescent polymers and complexes, which is applied in the preparation of microspheres, microcapsule preparations, chemical instruments and methods, etc., can solve problems such as irregularities, product failures, collapses, etc., and achieve mild conditions, configuration at any time, and low cost low effect

Active Publication Date: 2016-06-08
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the preparation of nano-rare earth complexes by existing methods usually requires complex chemical modification or simple embedding methods. The former leads to cumbersome preparation process, time-consuming and labor-intensive, and is not suitable for industrialization, while the latter means of doping. Irregular shape and size lead to poor storage stability
In addition, it should be noted that the stability of rare earth polymer nanoparticles prepared by traditional methods in organic solvents is extremely poor, especially if the polymer is in a good solvent with extremely similar solubility parameters, it will also collapse, which directly leads to product failure

Method used

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  • Method for preparing fluorescent polymer rare earth complex nano-microsphere

Examples

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Effect test

Embodiment 1

[0020] Add 0.15g sodium lauryl sulfate and 0.6g n-hexadecane to 75mL deionized water, stir at 40°C for 30min, then cool to 10°C, add 3g diacetone acrylamide and 12g styrene dropwise, after the dropwise addition, Disperse in a high-intensity homogenizer at 0°C for 4 minutes, transfer to an oil bath at 60°C, dissolve 0.04 g of potassium persulfate in 10 mL of deionized water, add to the system and react for 6 hours to obtain a seed microsphere emulsion. Dissolve 3g diacetone acrylamide, 4g styrene, 2g acrylic acid, 0.2g sodium lauryl sulfate in 15mL water and stir for 30min to obtain a pre-emulsion, dissolve 0.03g potassium persulfate initiator in 10mL water, and make the seed microsphere emulsion Raise the temperature to 70°C, drop the pre-emulsion and the initiator solution into the system at the same time, react for 3 hours, then raise the temperature to 60°C and react for 30 minutes to obtain a core-shell nano-emulsion. Centrifuge the core-shell nanoscale emulsion to obtain ...

Embodiment 2

[0022] Add 0.2g sodium dodecyl sulfate and 0.6g n-hexadecane to 75mL deionized water, stir at 60°C for 30min, then cool to 8°C, add 2g divinylbenzene and 10g acrylonitrile dropwise, after the dropwise addition, Disperse in a high-strength homogenizer for 2 minutes, transfer to a 60°C oil bath, dissolve 0.04g of potassium persulfate in 10mL of deionized water, add to the system and react for 6 hours to obtain a seed microsphere emulsion. Dissolve 1g of divinylbenzene, 4g of acrylonitrile, 3g of 3-vinylbenzoic acid, and 0.3g of sodium dodecylbenzenesulfonate in 15mL of water and stir for 30min to obtain a pre-emulsion. Dissolve 0.03g of potassium persulfate as an initiator in 10mL of water , the temperature of the core layer emulsion was raised to 70°C, and the pre-emulsion and the initiator solution were added dropwise to the system at the same time. After 3 hours of reaction, the temperature was raised to 75°C for 30 minutes to obtain a core-shell nano-emulsion. Centrifuge the...

Embodiment 3

[0024] Add 0.2g sodium lauryl sulfate and 0.8g n-hexadecane into 75mL deionized water, stir at 60°C for 30min and cool to 8°C, add dropwise 5g of ethylene glycol dimethacrylate, 12g of methyl methacrylate After the ester is added dropwise, disperse in a high-intensity homogenizer at 0°C for 3 minutes, move it into an oil bath at 60°C, dissolve 0.04g of potassium persulfate in 10mL of deionized water, add it to the system and react for 6 hours to obtain a seed microsphere emulsion. Dissolve 1 ethylene glycol dimethacrylate, 4g methyl methacrylate, 2g methacrylic acid, 0.3g sodium lauryl sulfate in 15mL water and stir for 30min to obtain a pre-emulsion, dissolve 0.03g potassium persulfate initiator In 10mL of water, the temperature of the core layer emulsion was raised to 70°C, and the pre-emulsion and the initiator solution were added dropwise to the system at the same time. After reacting for 3 hours, the temperature was raised to 75°C for 30 minutes to obtain a core-shell nano...

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Abstract

The invention provides a method for preparing a fluorescent polymer rare earth complex nano-microsphere. The method comprises the steps: allowing a monomer I to be subjected to miniemulsion polymerization to obtain a polymer seed microsphere emulsion I; adding a monomer II to the polymer seed microsphere emulsion I to be subjected to seed emulsion polymerization to obtain a core-shell nano-microsphere emulsion II; extracting core-shell nano-microspheres by high-speed centrifugation or freeze-drying of the core-shell nano-microsphere emulsion II to be dispersed in an organic solvent, and then adding a rare earth compound and a small molecule ligand to be subjected to a coordination reaction to obtain the solvent-resistant fluorescent polymer rare earth complex nano-microsphere. The prepared nano-microsphere has a uniform size, the preparation method is simple and practicable, high-intensity fluorescent lights of different colors can be obtained by adding different rare earth compounds, the environmental stability is particularly excellent, and the nano-microsphere still can be used after being stored for a year, can be stably dispersed in various organic solvents, and has good development prospects.

Description

technical field [0001] The invention relates to a polymer nanometer microsphere, the field of rare earth, and the field of fluorescence light emission, and more particularly relates to a preparation method of a solvent-resistant nanoscale fluorescent polymer rare earth complex microsphere. Background technique [0002] As a cutting-edge technology, the preparation technology of polymer nanospheres has always attracted the attention of the academic circle. Its specific excellent performance is reflected in its small size, surface and quantum size effects. In addition, it can also be used as a matrix material to compound inorganic elements to prepare composite microspheres. This composite material can not only effectively retain the excellent properties of polymers, but also bring new functionality through the introduction of inorganic materials. In this regard, rare earth elements and polymer composite microspheres are particularly promising research areas. However, the prep...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F257/02C08F212/08C08F220/06C08F222/38C08F265/08C08F265/06C08F222/14C08F220/14C08F212/36C08F220/18B01J13/14C09K11/06
CPCB01J13/14C08F257/02C08F265/06C08F265/08C09K11/06C09K2211/182C08F212/08C08F220/44C08F220/14
Inventor 王忠刚骆新然王泽锋叶维维
Owner DALIAN UNIV OF TECH
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