Tri (4-acetylene phenyl) amine conjugated microporous polymer as well as preparation method and application thereof
A technology of acetylene phenyl and conjugated micropores, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, chemical/physical processes, etc., can solve the problem of limited building units and limited CMPs photocatalysts Research progress and other issues
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Embodiment 1
[0035] The synthetic method of the present embodiment polymer FS1 is as follows:
[0036] Under argon, M0 (158.9 mg, 0.5 mmol), M1 (147.3 mg, 0.5 mmol), tetrakis(triphenylphosphine) palladium (40.8 mg, 0.03 mmol), cuprous iodide (20.5 mg, 0.10 mmol), anhydrous DMF (5 mL) and anhydrous triethylamine (5 mL), sealed, and the reaction was stirred at 100 °C for 72 h. Naturally cooled to room temperature to obtain a mixture containing light reddish-black solids. Filtration, the obtained solid was washed with chloroform, water, methanol, and acetone in turn, then chloroform and methanol were used as solvents, extracted with a Soxhlet extractor, and vacuum-dried at 60 °C for 24 h to obtain 220.0 mg of light black-red solid powder FS1, yield: 98 %.FT-IR(KBr,cm -1 ):2194,1588,1496,1310,1116,828.Anal.calcd forC 30 H 14 N 3 S: C, 80.34; H, 3.15; 9.37. Found: C, 75.32; H, 3.77; N, 7.91%. The deviation between the theoretical value and the measured value of elemental analysis may be ca...
Embodiment 2
[0046] The synthetic method of the present embodiment polymer FS2 is as follows:
[0047] FS2 uses the same synthetic method as FS1.
[0048] M0 (158.6 mg, 0.5 mmol), M2 (145.3 mg, 0.5 mmol), tetrakis(triphenylphosphine)palladium (40.3 mg, 0.03 mmol), cuprous iodide (21.0 mg, 0.1 mmol) to give 210.0 mg of black Yellow solid powder FS2, yield: 94%. FT-IR (KBr, cm -1) :2189,1595,1496,1314,1182,833.Anal.calcd for C 30 H 14 N 3 S: C, 80.34; H, 3.15; 9.37. Found: C, 72.96; H, 3.96; N, 8.55%.
[0049] The synthetic method of 4,5-dibromo-2,1,3-benzothiadiazole (M2) is as follows:
[0050] In the solution containing stannous chloride dihydrate (120 g, 0.53 mol) and hydrochloric acid (220 mL), 4-bromo-6-nitroaniline was added in batches, and the addition was completed for about 2 h. After the addition, the reaction solution was kept at 55°C. The reaction was carried out for 10 h, the reaction solution was poured into ice water, neutralized with sodium hydroxide to a pH value of 1...
Embodiment 3
[0055] The synthetic method of the present embodiment polymer FS3 is as follows:
[0056] FS3 uses the same synthetic method as FS1.
[0057] M0 (157.8mg, 0.5mmol), M3 (145.8mg, 0.5mmol), tetrakis(triphenylphosphine)palladium (40.5mg, 0.03mmol), cuprous iodide (21.5mg, 0.1mmol) to give 210.0mg light brown Solid powder FS3, yield: 94%. FT-IR (KBr, cm -1 ): 3026, 2199, 1582, 1500, 1315, 1093, 825. Anal.calcd for C 30 H 14 N 3 S: C, 80.34; H, 3.15; 9.37. Found: C, 71.48; H, 3.92; N, 7.80%.
[0058] The synthetic method of 4,6-dibromo-2,1,3-benzothiadiazole (M3) is as follows:
[0059] In a 250 mL reaction flask, o-nitroaniline (20 g, 0.145 mol) and acetic acid (100 mL) were added, and the reaction mixture was heated to 55° C. to completely dissolve the o-nitroaniline. NBS (77.391 g, 0.435 mol) was added to the reaction mixture in batches within 40 min, the temperature of the reaction solution was lowered to 40-50° C. and the reaction was carried out within this temperature ...
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