Poly-fluorene single-component white radiation macromolecule material containing phosphoric acid ester group, preparation method and application thereof
A technology of polymer materials and phosphate ester groups, applied in the field of optoelectronic materials, can solve the problems of increasing the complexity and cost of device preparation
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Embodiment 1
[0038] Embodiment 1: 2,7-dibromo-9, the synthesis of 9-two (4'-bromobutyl) fluorene
[0039] at 5×10 5 Under Pa argon protection, 8.0g of 2,7-dibromofluorene, 24.0g of 4-(4'-bromobutoxy)toluene, 100mL of toluene, 0.2g of tetrabutylammonium bromide were successively added to the reactor And 50mL of 50% aqueous sodium hydroxide solution, heated to 70°C and stirred for 12 hours. The reaction mixture was diluted with 100 mL of dichloromethane, washed successively with 100 mL of 1 mol / L hydrochloric acid, 100 mL of water, and 100 mL of brine twice, and the organic phase was washed with anhydrous Na 2 SO 4 After drying, the solvent was removed to obtain a crude product, which was separated by column chromatography with petroleum ether as an eluent to obtain 11.2 g of a white solid with a yield of 70%.
[0040] Add the above product to a mixed solution of 4mL 48% hydrobromic acid and 20mL glacial acetic acid, reflux at 110°C for 48 hours, pour into water, extract with 100mL dichlo...
Embodiment 2
[0041] Example 2: Synthesis of 2,7-dibromo-9,9-bis(6'-bromohexyl)fluorene
[0042] at 5×10 5 Under Pa argon protection, 8.0 g of 2,7-dibromofluorene, 16 mL of 1,6-dibromohexane, 100 mL of toluene, 0.2 g of tetrabutylammonium bromide and 50 mL of 50% Sodium hydroxide aqueous solution was heated to 70°C and stirred for 12 hours. The reaction mixture was diluted with 200 mL of dichloromethane, washed successively with 100 mL of 1 mol / L hydrochloric acid, 100 mL of water, and 100 mL of brine twice, and the organic phase was washed with anhydrous Na 2 SO 4 After drying and removing the solvent, excess 1,6-dibromohexane was distilled off under reduced pressure at 3 mmHg, and the residue was separated by column chromatography (eluent: petroleum ether / dichloromethane=8 / 1) to obtain 2, 13.6 g of 7-dibromo-9,9-bis(6'-bromohexyl)fluorene, white solid, yield 85%.
Embodiment 3
[0043] Embodiment 3: the synthesis of 2,7-dibromo-9,9-bis(8'-bromooctyl)fluorene
[0044] at 5×10 5 Under Pa argon protection, 8.0 g of 2,7-dibromofluorene, 22 mL of 1,8-dibromooctane, 100 mL of toluene, 0.2 g of tetrabutylammonium bromide and 50 mL of 50% Sodium hydroxide aqueous solution, the reaction conditions and treatment method were the same as in Example 2 to obtain 14.3 g of 2,7-dibromo-9,9-bis(8'-bromooctyl)fluorene as a white solid with a yield of 82%.
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