Palladium supported heterogeneous catalyst based on micro-mesoporous phenolic resin and preparation method thereof
A heterogeneous catalyst and phenolic resin technology, which is applied in chemical instruments and methods, preparation of organic compounds, physical/chemical process catalysts, etc., can solve the problem of uneven distribution of coordination groups, easy loss of palladium metal, and heterogeneous catalytic efficiency Low-level problems, to achieve the effect of improving catalytic efficiency, easy recycling, and preventing loss
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Embodiment 1
[0020] Synthesis of triphenylphosphino-based micro-mesoporous phenolic resin (PFN-P-1) with large specific surface area:
[0021] In a 100 ml three-necked flask, add 1.92 gram of trisphenol, 1.41 gram of three (4-formyl phenyl) phosphine and 20 milliliters of mixed solvent of cyclohexane and dioxane (volume of cyclohexane / dioxane The ratio is 0.5 / 9.5). The mixture was warmed to 80°C and stirred for 2 hours to obtain a clear solution. The resulting solution was transferred to a 100 ml autoclave and reacted at 200° C. for 6 days. After cooling and filtering, the obtained solid was extracted with tetrahydrofuran in a Soxhlet extractor for 24 hours, and vacuum-dried at 120° C. to constant weight, with a yield of 90%. The BET specific surface area is 655 square meters per gram, and the pore size is 0.9-28 nanometers.
Embodiment 2
[0023] Synthesis of triphenylphosphino-based micro-mesoporous phenolic resin (PFN-P-2) with large specific surface area:
[0024] Add 1.22 gram of resorcinol, 0.75 gram of tris (4-formyl phenyl) phosphine and 20 milliliters of tetrahydrofuran and dioxane mixed solvent (tetrahydrofuran / dioxane ratio is 1 / 9) in the three-necked flask of 50 milliliters ). The mixture was warmed to 60°C and stirred for 2 hours to obtain a clear solution. The resulting solution was transferred to a 100 ml autoclave and reacted at 190° C. for 5 days. After cooling, it was filtered, and the obtained solid was extracted with tetrahydrofuran in a Soxhlet extractor for 48 hours, and vacuum-dried at 120° C. to constant weight, with a yield of 95%. The BET specific surface area is 645 square meters per gram, and the pore size is 0.6-32 nanometers.
Embodiment 3
[0026] Synthesis of triphenylphosphino-based micro-mesoporous phenolic resin (PFN-P-3) with large specific surface area:
[0027] Add 0.85 g of 2,5-dihydroxy-1,4-benzoquinone, 0.70 g of tris(4-formylphenyl)phosphine and 10 ml of dioxane into a 50 ml three-necked flask. The mixture was warmed to 90°C and stirred for 1 hour to obtain a clear solution. The resulting solution was transferred to a 100 ml autoclave and reacted at 220° C. for 4 days. After cooling, it was filtered, and the obtained solid was extracted with tetrahydrofuran for 24 hours with a Soxhlet extractor, and vacuum-dried at 120° C. to constant weight, with a yield of 95%. The specific surface area of BET is 775 square meters per gram, and the pore size is 0.6nm-23.8nm.
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