Preparation method of triphenyl bismuth diacid compound and application of triphenyl bismuth diacid compound in polyurethane
A technology of bismuth triphenyl diacid and triphenyl bismuth, which is applied in the direction of bismuth organic compounds, can solve the problems of poor reproducible results, poor catalyst solubility, and reduced catalytic activity, so as to enhance the mechanical properties of products and shorten the curing time Time, the effect of improving corrosion resistance
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[0045] The preparation method of oxo-triphenylbismuth is as follows: dichlorophenylbismuth is used as raw material, dilithium salt of biphenyl or phenyl ether is used as ligand, ether is used as solvent, preferably tetrahydrofuran and diethyl ether, and the reaction temperature is -30°C ~30°C, the reaction condition is argon, and the reaction time is 1h~40h, so as to obtain the oxygen-bridged triphenylbismuth;
[0046] The synthetic route of oxygen-bridged triphenylbismuth is as follows:
[0047]
[0048] The preparation method of bismuth triphenyl diacid compound is: take the prepared oxotriphenyl bismuth as raw material, add carboxylic acid, use halogenated hydrocarbon as solvent, preferably dichloromethane, peroxyacid as oxidant, preferably meta Chloroperoxybenzoic acid, the reaction temperature is -30°C~30°C, the reaction condition is argon, and the reaction time is 10min~10h, so as to obtain bismuth triphenyl diacid compound.
[0049] The synthetic route of bismuth tr...
Embodiment 1
[0071]
[0072] Dissolve 1,1'-dibromobiphenyl (1.25g, 4mmol) in 10mL of dry tetrahydrofuran in a Shrek bottle under argon gas, and slowly add n-butyllithium solution (3.5mL, 2.5M ), slowly rose to room temperature and stirred for 2h to obtain a dilithium salt solution.
[0073] Dissolve triphenylbismuth (0.59g, 1.3mmol) and bismuth trichloride (0.84g, 2.6mmol) in 10mL of dry ether in a Shrek bottle under argon atmosphere, and stir at room temperature for 2h. Add 10 mL of dry tetrahydrofuran, cool down to 0°C, slowly add the above dilithium salt into the solution dropwise, and stir overnight. Quenched with water, extracted with ethyl acetate (5mL×3), removed the solvent in vacuo, and recrystallized 3 times with pure petroleum ether to obtain 0.73g of white solid (73% yield)
[0074] Add phenylbiphenylbismuth (0.5g, 0.5mmol), octanoic acid (160mg, 1.1mmol) and 10mL of dichloromethane in a round bottom flask, add m-chloroperoxybenzoic acid (189mg, 0.55mmol, 50 %), stirred fo...
Embodiment 2
[0078]
[0079] Dissolve diphenyl ether (4.08g, 24mmol) in 50mL dry tetrahydrofuran in a Shrek bottle under argon atmosphere, slowly add n-butyllithium solution (21.2mL, 2.5M) dropwise at 0°C, and slowly rise to room temperature Stir for 2h to obtain a dilithium salt solution.
[0080] Dissolve triphenylbismuth (3.52g, 8mmol) and bismuth trichloride (5.04g, 16mmol) in 50mL of dry ether in a Shrek bottle under argon atmosphere, and stir at room temperature for 2h. Add 50 mL of dry tetrahydrofuran, cool down to 0°C, slowly add the above dilithium salt into the solution dropwise, and stir overnight. Quenched with water, extracted with ethyl acetate (15mL×3), removed the solvent in vacuo, recrystallized 3 times with pure petroleum ether to obtain 8.23g of white solid (75.5% yield)
[0081] In a round-bottomed flask, add bismuth phenyldiphenyl ether (1.13 g, 2.5 mmol), octanoic acid (800 mg, 5.5 mmol) and 20 mL of dichloromethane, add m-chloroperoxybenzoic acid (946 mg, 2.75 mm...
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