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
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[0054] Example 1
[0055] ①, Dissolve 444.4 mg (2.0 mmol) of α-thiopheneformyl acetone trifluoride (commercially available) in 20 mL of tetrahydrofuran, add 48.0 mg (2.0 mmol) of sodium hydride (commercially available), and heat the mixed solution at 65°C for 1.5 h after stirring. Then, 371 μL (2 mmol) of 3-chloropropyltriethoxysilane (commercially available) was added dropwise, and the mixture was heated and stirred at 65° C. for 18 h under the protection of inert gas to obtain a yellow solution.
[0056] ②, suspend the yellow solution to remove the solvent to obtain a yellow oil, dissolve it in ether, filter to remove the filter residue, then suspend the filtrate to remove the ether, and dry at 70°C to obtain a yellow oil, which is TTASi.
[0057] ③, 402.5 mg (0.505 mmol) of 1,3,5,7,9,11,14-heptaisobutyltricyclo[7.3.3.15,11]heptasiloxane-endo-3,7,14-tris The 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 tet...
Example Embodiment
[0068] Example 2
[0069] ①, Dissolve 4.0 g (25.6 mmol) of 2,2'-bipyridine (commercially available) in 30 mL of glacial acetic acid, add 5.5 mL of 30% hydrogen peroxide, heat and stir in an oil bath at 75°C for 3 hours, then add 4 mL of 30% hydrogen peroxide, continue stirring 10h. After the reaction was stopped, the mixture was cooled to room temperature, 100 mL of acetone was added, and white crystals were precipitated, which was 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, and then add 6.5mL of fuming nitric acid, Heated at 95°C under reflux for 20h. After the reaction was completed, the mixture was cooled to room temperature, poured into 50 mL of ice, and stirred continuously, a brown-red gas escaped, and the solution turned light green, and continued stirring until no brown-red gas was produced, and ...
Example Embodiment
[0084] Example 3
[0085] ①, 300.0mg (1.12mmol) 4'-chloro-2,2':6',2"-terpyridine (commercially available), 2.16mL 1,3-propanediamine (commercially available) were added to the reaction flask at the same time, After heating under reflux at 120 °C for 12 h, it was cooled to room temperature, and 25 mL of double-distilled water was added to produce a white precipitate, which was centrifuged and dried at 70 °C to obtain a white powder, denoted as TpyNH 2 .
[0086] ②, 120.0mg (0.39mmol) TpyNH 2 It was dissolved in 6 mL of ethanol, 160 μL (0.60 mmol) of Y-isocyanatopropyl triethoxysilane (ICPTES) was added, and the mixture was stirred and heated in an oil bath at 60 °C for 40 h to obtain a yellow solution. The solvent was removed by suspension, washed with n-hexane, centrifuged, and dried at 70°C to obtain a yellow oil, which was designated as TpySi.
[0087] ③, 402.5 mg (0.505 mmol) of 1,3,5,7,9,11,14-heptaisobutyltricyclo[7.3.3.15,11]heptasiloxane-endo-3,7,14-tris Alcohol (T) (...
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