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Novel cage type low polysilsesquioxane and rare earth light-emitting material thereof

A technology of polysilsesquioxane and luminescent materials, which is applied in the fields of luminescent materials, silicon organic compounds, chemical instruments and methods, etc. It can solve the problems of rare research reports and achieve good luminescent performance

Inactive Publication Date: 2015-03-11
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Given that POSS is a nanoparticle with a new structure and a matrix for the preparation of new inorganic-organic hybrid materials, combining POSS with rare earth ions is undoubtedly a topic worthy of research, and there are no research reports in this area yet. more common

Method used

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  • Novel cage type low polysilsesquioxane and rare earth light-emitting material thereof
  • Novel cage type low polysilsesquioxane and rare earth light-emitting material thereof
  • Novel cage type low polysilsesquioxane and rare earth light-emitting material thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] ①. Dissolve 444.4mg (2.0mmol) of α-thienoyltrifluoroacetone (commercially available) in 20mL of tetrahydrofuran, add 48.0mg (2mmol) of sodium hydride (commercially available), and heat and stir the mixed solution at 65°C for 1.5h Then 371 μL (2 mmol) of 3-chloropropyltriethoxysilane (commercially available) was added dropwise, and heated and stirred at 65° C. for 18 h under the protection of an inert gas to obtain a yellow solution.

[0056] ②, the yellow solution was suspended and evaporated to remove the solvent to obtain a yellow oil, which was dissolved in ether, filtered to remove the filter residue, then the filtrate was suspended to remove the ether, and dried at 70°C to obtain a yellow oil, which was TTASi.

[0057] ③, 402.5mg (0.505mmol) 1,3,5,7,9,11,14-heptaisobutyltricyclo[7.3.3.15,11]heptasiloxane-endo-3,7,14-three Alcohol (T) was dissolved in 30 mL of chloroform (99.5%), 229.0 mg (0.527 mmol) of TTASi was dissolved in 2 mL of tetrahydrofuran (99.5%), protec...

Embodiment 2

[0069] ① Dissolve 4.0g (25.6mmol) of 2,2'-bipyridine (commercially available) in 30mL of glacial acetic acid, add 5.5mL of 30% hydrogen peroxide, heat and stir in an oil bath at 75°C for 3 hours, then add 4mL of 30% hydrogen peroxide, and continue stirring 10h. After stopping the reaction, the mixture was cooled to room temperature, and 100 mL of acetone was added to precipitate white crystals, which were filtered to obtain 2,2-bipyridine-N,N'-dioxide.

[0070] ②, add 3.7g (18.0mol) of 2,2'-bipyridine-N,N'-dioxide, add 18mL of 98% concentrated sulfuric acid in an ice-water bath, heat at 95°C until completely dissolved, then add 6.5mL of fuming nitric acid, Heat to reflux at 95°C for 20h. After the reaction was over, the mixture was cooled to room temperature, poured into 50mL of ice, and stirred constantly, and brown-red gas escaped, and the solution turned light green. Continue stirring until no brown-red gas was produced, and the solution turned light yellow. There was a l...

Embodiment 3

[0085] ①, Add 300.0mg (1.12mmol) 4'-chloro-2,2':6',2"-terpyridine (commercially available) and 2.16mL 1,3-propanediamine (commercially available) into the reaction flask at the same time, Heat and reflux at 120°C for 12h, then cool it down to room temperature, add 25mL double distilled water to produce a white precipitate, centrifuge, and dry at 70°C to obtain a white powder, which is designated as TpyNH 2 .

[0086] ②, 120.0mg (0.39mmol) TpyNH 2 Dissolve in 6mL ethanol, then add 160μL (0.60mmol) Y-isocyanatopropyltriethoxysilane (ICPTES), stir and heat in an oil bath at 60°C for 40h to obtain a yellow solution. The solvent was removed by suspension evaporation, washed with n-hexane, centrifuged, and dried at 70°C to obtain a yellow oil, which was designated as TpySi.

[0087] ③, 402.5mg (0.505mmol) 1,3,5,7,9,11,14-heptaisobutyltricyclo[7.3.3.15,11]heptasiloxane-endo-3,7,14-three Alcohol (T) (commercially available) was dissolved in 30 mL of chloroform (99.5%), 244.9 mg (0....

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Abstract

The invention discloses a cage type low polysilsesquioxane and a rare earth ion light-emitting material. 1,3,5,7,9,11,14-heptaisobutyltricyclo[7.3.3.15,11]heptasiloxane-endo-3,7,14-triol is used as a matrix, and an alpha-thenoyltrifluoroacetone silanization derivative, a dipyridyl silanization derivative and a terpyridyl silanization derivative are used as angle complementing bodies, and the complementing bodies react with the matrix in an angle complementing manner to form the complete novel cage type low polysilsesquioxane; and the novel cage type low polysilsesquioxane is combined with a rare earth element to form a cage type low polysilsesquioxane (POSS) / rare earth ion light-emitting material. The rare earth compound / low polysilsesquioxane material is rich in light-emitting colors, is high in color purity, long in fluorescence lifetime (0.5-1.5ms), high in quantum efficiency (20), and strong in heat stability (350 DEG C) and light stability, is a valuable optical material, and can be applied to the fields of display and development, new light sources, X ray intensifying screens and the like.

Description

Technical field: [0001] The invention belongs to the field of rare earth functional materials, in particular to a preparation method of a cage-type oligomeric silsesquioxane and a rare earth ion luminescent material. Background technique [0002] Rare earth ions have excellent luminescent properties (such as high color purity, long fluorescence lifetime, rich emission lines, etc.) due to their unique 4f-layer electron configuration. , Luminescent materials and other fields have potential application value. [0003] The general molecular formula of polysilsesquioxane is (RSiO3 / 2)n (the atomic ratio of O and Si in the molecule is 3:2), and R in the formula can be H, alkyl, alkylene, aryl, Aryl groups or substituents of these groups. Polysilsesquioxanes have random, cage, trapezoidal, and bridge structures, among which polysilsesquioxanes with cage structures are called polyhedral oligomeric silsesquioxanes (POSS for short). The molecular structure of POSS is a hybrid struct...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/21C09K11/06
Inventor 李焕荣陈晓凡张盼宁
Owner HEBEI UNIV OF TECH
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