A kind of preparation method of s-triazine derivative monomer and polyarylether fluorescent material
A technology of fluorescent materials and polyarylene ethers, which is used in luminescent materials, chemical instruments and methods, organic chemistry, etc., can solve the problems of long reaction time, few research reports and high reaction temperature, and achieves short reaction time and good thermal stability. , the effect of high purity
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Embodiment 1
[0043] Dissolve p-fluorobenzonitrile (12.11g, 0.1mol) in 20mL of nitromethane at room temperature, cool in an ice-water bath to 10°C, add sulfur trioxide-pyridine complex (23.87g, 0.15mol), and stir at room temperature 1h, add anhydrous ether, filter with suction, wash with ether and ethanol several times, and dry in vacuum to obtain 4,6-bis(4-fluorophenyl)-2-oxo-1,2,3,5-oxathio Substituted diazine, the yield is 75%. Melting point: 132.2-133.9°C. FTIR (KBr): 1680cm -1 (C=N stretching vibration peak), 1586cm -1 , 1530cm -1 , 1477cm -1 (stretching vibration generated by the benzene ring skeleton), 1215cm -1 (S=O stretching vibration), 851cm -1 (C-H bending vibration peak).
[0044] 4,6-bis(4-fluorophenyl)-2-oxo1,2,3,5-oxathiodiazine (3.22g, 0.01mol) and p-fluorobenzamidine hydrochloride (1.75 g, 0.01mol) was dissolved in 50mL of acetone, potassium n-butoxide (3.37, 0.03mol) was added, stirred at room temperature for 1h, heated to 50°C and reacted for 1h. Cool to room te...
Embodiment 2
[0046] 2,4,6-tris(4-fluorophenyl)-1,3,5-triazine (1.82 g, 0.005mol) and 6-(4-hydroxyphenyl)pyridazin-3(2H)-one (1.41g, 0.0075mol) were dissolved in 20mL of N,N-dimethylacetamide, 50mL of toluene was added, and potassium carbonate was added (1.38g, 0.01mol), heated up to 150°C to remove water for 2h, removed toluene and water, heated up to 170°C until stirring was impossible, and kept warm for 1h. The product was poured into an aqueous solution containing hydrochloric acid and methanol, filtered with suction, washed with methanol and water, and dried. Grinding in a ball mill, Soxhlet extraction to remove solvent and unreacted raw materials, and vacuum drying to obtain 3.04 g of polyarylether-s-triazine product. The yield was 94%. FTIR: 3446cm -1 (O-H, N-H stretching vibration peak), 1679cm -1 (C=O, C=N stretching vibration peak), 1596cm -1 , 1540cm -1 , 1499cm -1 (stretching vibration generated by the benzene ring skeleton), 1239cm -1 (C-O-C stretching vibration peak), ...
Embodiment 3
[0050] 2,4,6-tris(4-fluorophenyl)-1,3,5-triazine (1.82 g, 0.005mol) and biphenol (1.49g, 0.008mol) were dissolved in 25mL of N,N-dimethylacetamide, 60mL of toluene was added, potassium carbonate (1.38g, 0.01mol) was added, and the temperature was raised to 150°C to remove water 2h, toluene and water were removed, the temperature was raised to 170°C until the reaction could not be stirred, and the temperature was kept for 1h. The product was poured into an aqueous solution containing hydrochloric acid and methanol, filtered with suction, washed with methanol and water, and dried. Grinding with a ball mill, Soxhlet extraction to remove solvent and unreacted raw materials, and vacuum drying to obtain 2.93 g of polyarylether-s-triazine product. The yield was 91%. FTIR: 3390cm -1 (O-H, N-H stretching vibration peak), 1600cm -1 , 1550cm -1 , 1490cm -1 (stretching vibration generated by the benzene ring skeleton), 1239cm -1 (C-O-C stretching vibration peak), 874cm -1 , 819cm ...
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