Nano-lattice and nano-polymer lattice materials and their preparation and application methods
A nano-polymer and nano-lattice technology, applied in chemical instruments and methods, luminescent materials, semiconductor/solid-state device manufacturing, etc., can solve problems such as structural uncertainty, difficulty in large-scale preparation, and poor material solubility, and achieve simple operation , Easy solution processing, low cost effect
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[0058] The key step of the preparation method of the nano-lattice of the present invention is that the tertiary alcohol undergoes an acid-catalyzed Friedel-Crafts reaction, and the nano-lattice is obtained by self-ring closure. Taking nanolattice I as an example, the specific reaction is as follows:
[0059]
[0060] This type of material is obtained by polymerization of nano-lattice through Suzuki coupling polymerization, Stille coupling polymerization or Yamamoto coupling. Taking nano-polymer lattice material II as an example, the details are as follows:
[0061]
Embodiment 1
[0065] Embodiment 1, 2,7-dibromo-9-(4-octyloxyphenyl)-fluorene-9-alcohol (10g, 18.37mmol) and N-octylcarbazole (51.33g, 183.70mmol) were dissolved in 1000mL anhydrous CH 2 Cl 2 , was added dropwise in 100 mL of anhydrous CH with rapid stirring 2 Cl 2 boron trifluoride ether solution (7.80g). Stir at room temperature for 24 hours. After the reaction is complete, add 100 mL of water to quench the reaction and use CH 2 Cl 2 The organic layer was extracted, combined, dried with anhydrous magnesium sulfate, concentrated by rotary evaporation to remove the solvent, separated and purified by column chromatography to obtain a white solid powder (14.10g, 97%) MALDI-TOF-MS (m / z): 805.2 / 805.2[M+], 1 H-NMR (400MHz, CDCl 3 )δ7.96(d, J=8Hz, 1H), 7.84(s, 1H), 7.61(d, J=8.4Hz, 2H), 7.55(d, J=1.6Hz, 2H), 7.48(m, 2H ),7.43(m,1H),7.37(d,J=8Hz,1H),7.27(m,1H),7.17(m,4H),δ6.80(m,2H),4.24(t,J 1 =7.2Hz,J 2 =7.2Hz,2H),3.93(t,J 1 =6.8Hz,J 2 = 6.4Hz, 2H).
Embodiment 2
[0066] Implementation Example 2, 11.80g (14.64mmol) 3-(2,7-dibromo-9-(4-octyloxyphenyl)-fluorenyl)-9-octylcarbazole and 2.50g (4.88mmol) 2-Boronic acid pinacol ester-9-(4-octyloxyphenyl)-fluorene-9-ol and 340 mg (029 mmol) tetrakistriphenylphosphine palladium were added to the reaction bottle, coated with vaseline, and sealed with a sealing tape. Evacuate the nitrogen three times. Add the bubbling toluene and tetrahydrofuran mixed solution with a syringe, inject 2mol L of bubbling after 15min -1 Potassium carbonate solution 20mL, react at 85°C for 48h, add 100mL water to quench the reaction, use CH 2 Cl 2 The organic layer was extracted, combined, dried over anhydrous magnesium sulfate, concentrated by rotary evaporation to remove the solvent, separated and purified by column chromatography to obtain a yellow solid (5.0 g, 92%). MALDI-TOF-MS (m / z): 1109.1 / 1109.5 [M+], 1 H NMR (400MHz, CDCl 3 )δ7.91-7.97(m,2H),7.77(d,J=8Hz,1H),7.63-7.66(m,4H),7.55-7.58(m,2H),7.47-7.53(m,3H...
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