Preparation method of fluorescent polyhedral oligomeric silsesquioxane/polymethyl methacrylate

A technology of polymethyl methacrylate and polysilsesquioxane, which is applied in the field of plastic modification, can solve problems such as poor thermal stability and poor fluorescence performance, and achieve low cost, small environmental impact, good thermal The effect of stability

Inactive Publication Date: 2017-04-26
SHANGHAI AEROSPACE EQUIP MFG GENERAL FACTORY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The problem solved by the present invention is that the fluorescent performance of polymethyl methacrylate (PMMA) is poor, and thermal stability is bad; The preparation method of methyl acrylate

Method used

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  • Preparation method of fluorescent polyhedral oligomeric silsesquioxane/polymethyl methacrylate
  • Preparation method of fluorescent polyhedral oligomeric silsesquioxane/polymethyl methacrylate
  • Preparation method of fluorescent polyhedral oligomeric silsesquioxane/polymethyl methacrylate

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preparation example Construction

[0019] The preparation method of the fluorescent POSS modified PMMA resin provided by the invention not only endows the PMMA with fluorescent properties, but also improves the dispersibility and thermal stability of the material. The preparation method of the fluorescent POSS modified PMMA resin of the present invention comprises two steps of preparing the fluorescent POSS and the fluorescent POSS modified PMMA composite material.

[0020] In the present invention, the EMOF fluorescent agent is selected to modify the fluorescent POSS through the hydrosilylation reaction, and the hydrosilylation reaction is prepared in a nitrogen atmosphere using Schlenk technology in a double-row tube. Put POSS and EMOF into the Schlenk tube with a molar ratio of 1: (7 to 8) and a total mass of 0.3 to 0.5% of the catalyst Pt, use a double-row tube to pump nitrogen, and inject the solvent 1,4-dioxane And react at 75-83°C for 20-30h, stop heating and cool to room temperature to stop the reaction...

Embodiment 1

[0026] Put POSS and EMOF at a molar ratio of 1:7 and catalyst Pt with a total mass of 0.3% into a Schlenk tube, pump nitrogen three times with a double-row tube, inject the solvent 1,4-dioxane and cool at 75 °C Under the reaction 20h, stop heating and cool to room temperature to stop the reaction. The reaction solution was subjected to precipitation-dissolution treatment with n-hexane and THF three times in order to remove the catalyst and excess monomer in the reaction. Finally, the product was dried in a vacuum oven to constant weight and stored in a dry place.

[0027] EMOF-POSS and PMMA with a mass fraction of 0.5% were formulated into THF solutions, blended and stirred for 1 h, and vacuum-dried after the solvent was evaporated to obtain EMOF-POSS / PMMA nanocomposites with uniform dispersion of POSS and high fluorescence emission intensity. The starting temperature of material degradation is 290°C.

Embodiment 2

[0029] Put POSS and EMOF at a molar ratio of 1:8 and catalyst Pt with a total mass of 0.5% into a Schlenk tube, pump nitrogen for 3 times with a double-row tube, inject the solvent 1,4-dioxane and cool at 83 °C Under the reaction 30h, stop heating and cool to room temperature to stop the reaction. The reaction solution was subjected to precipitation-dissolution treatment with n-hexane and THF three times in order to remove the catalyst and excess monomer in the reaction. Finally, the product was dried in a vacuum oven to constant weight and stored in a dry place.

[0030] EMOF-POSS and PMMA with a mass fraction of 4.0% were formulated into THF solutions, blended and stirred for 1.5h, and then vacuum-dried after the solvent was evaporated to obtain an EMOF-POSS / PMMA nanocomposite material with uniform dispersion of POSS and high fluorescence emission intensity. The initial degradation temperature of the composite material is 295℃.

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Abstract

The invention relates to a preparation method of novel fluorescent polyhedral oligomeric silsesquioxane/polymethyl methacrylate (POSS/PMMA). The method comprises the following steps: introducing a long-conjugate fluorine derivative EMOF with high fluorescence quantum yield to POSS by using an addition reaction of a Si-H bond and end alkyne through molecular design to prepare a dendritic organic/inorganic hybrid luminescent material EMOF-POSS with the POSS as a core and a fluorescence chromophore as an arm; and preparing an inorganic/organic composite nanomaterial from the EMOF-POSS and the PMMA through a solution blending technology. Combination of the POSS and the EMOF effectively reduces aggregation of the fluorescence chromophore in the PMMA matrix, so the luminescence properties of the material are obviously improved, and the composite material has good heat stability.

Description

technical field [0001] The invention relates to a novel preparation method of fluorescent multifaceted oligomeric silsesquioxane / polymethyl methacrylate (POSS / PMMA), which belongs to the technical field of plastic modification. Background technique [0002] In recent years, organic light-emitting materials have been widely used in the fields of electroluminescence and display devices, and the main goal is to improve the efficiency of light-emitting devices. Most luminescent materials have a high fluorescence quantum yield in solution, but the phenomenon of fluorescence weakening or even quenching occurs in the aggregated state. In addition, the thermal stability of the luminescent material is poor, and the quenching effect is also prone to occur when the temperature is high. In practical life applications, people often need to make luminescent materials into solids with a certain shape and structure. Therefore, how to effectively eliminate the aggregation quenching effect o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/38C08L33/12C08L83/04C09K11/06
CPCC08G77/045C08L33/12C08L2201/08C09K11/06C09K2211/1491C08L83/04
Inventor 张崇印王蔚张珩堵同亮连爱珍徐世俊龚菊贤郝冬冬韩亚刚玉钰奉
Owner SHANGHAI AEROSPACE EQUIP MFG GENERAL FACTORY
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