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Cage oligomeric silsesquioxane and its rare earth luminescent material prepared with bipysi as supplementary angle

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: 2017-05-03
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] 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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  • Cage oligomeric silsesquioxane and its rare earth luminescent material prepared with bipysi as supplementary angle
  • Cage oligomeric silsesquioxane and its rare earth luminescent material prepared with bipysi as supplementary angle
  • Cage oligomeric silsesquioxane and its rare earth luminescent material prepared with bipysi as supplementary angle

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] 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.

[0058] 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.

[0059] ③, 402.5 mg (0.505 mmol) of 1,3,5,7,9,11,14-heptaisobutyltricyclo[7.3.3.15,11]heptasiloxane-3,7,14-tri Alcohol (T) was dissolved in 30 mL of chloroform (99.5%), 229.0 mg (0.527 mmol) TTASi was dissolved in 2 mL of tetrahydrofuran (99.5%), protected b...

Embodiment 2

[0071] 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.

[0072] 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 to 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

[0087] 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 .

[0088] ②, 120.0mg (0.39mmol) TpyNH 2 Dissolve in 6 mL of ethanol, then add 160 μL (0.60 mmol) of γ-isocyanatopropyltriethoxysilane (ICPTES), stir and heat in an oil bath at 60°C for 40 hours 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.

[0089] ③, 402.5 mg (0.505 mmol) of 1,3,5,7,9,11,14-heptaisobutyltricyclo[7.3.3.15,11]heptasiloxane-3,7,14-tri Alcohol (T) (commercially available) was dissolved in 30 mL of chloroform (99.5%), ...

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Abstract

The invention relates to a cage type oligomeric silsesquioxane prepared by taking BipySi as supplement bodies and a rare earth luminescent material prepared from cage type oligomeric silsesquioxane. By taking 1,3,5,7,9,11,14-heptaisobutyl tricyclic[7,3.3.15,11] heptatrisiloxane-intra-3,7,14-triol as a matrix, alpha-thenoyl trifluoroacetone silanized derivative, a dipyridine silanized derivative and a terpyridyl silanized derivative as supplement bodies, the supplement bodies react with the matrix in form of supplements to form integrated novel cage type oligomeric silsesquioxane. The cage type oligomeric silsesquioxane is combined with rare earth elements to form a POSS / rare earth ion luminescent material. The obtained rare earth ion luminescent material / POSS is rich in luminescent color, high in color purity, long in fluorescent lifetime (0.5-1.5ms), high in quantum efficiency (20) and strong in thermal stability (350 DEG C) and light stability, is a valuable optical material and can be applied to the field of display and development, light source, X-ray intensifying screen and the like.

Description

[0001] (Original case of divisional case: Novel cage-type oligomeric silsesquioxane and its rare earth luminescent material, application number 2013100103130, application date January 11, 2013) [0002] Technical field: [0003] 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 [0004] 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. [0005] 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, tra...

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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