Water soluble ligand rhodium complex catalyst used for preparing aldehyde with dicyclopentadiene hydroformylation
A technology of dicyclopentadiene hydroformyl and water-soluble ligands, applied in organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, carbon-based compound preparation, etc. problem, to achieve the effect of simple and convenient synthesis method, improved activity and easy separation
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Embodiment 1
[0007] Embodiment 1: earlier with 190.0ml damping fluid (pH is about 7.3), 10.0ml dicyclopentadiene, RhCl 3 (Concentration is 1.0×10 -3 M), 0.328g triphenylphosphine trisodium sulfonate (TPPTS) and 0.603g phase transfer agent cetyltrimethylammonium bromide (CTAB) are mixed, then the mixed solution is added in the autoclave, first use N 2 (1.0MPa) replacement three times, remove the air in the kettle, and then use synthesis gas (H 2 / CO=1, 1.0MPa) to wash once, pressurize to the required pressure of 4.8Mpa, start the stirrer and raise the temperature to the set reaction temperature of 110°C for 3.0h. After the reaction is completed, pass water to cool, take out the reaction kettle material, and after standing still for 1.0 h, separate the catalyst water phase and the product oil phase, recycle the catalyst water phase, and analyze the product oil phase with a gas chromatograph. The reaction results are shown in Table 1.
Embodiment 2
[0008] Embodiment 2: earlier with 190.0ml buffer (pH is about 7.3), 10.0ml dicyclopentadiene, RhCl 3 and CoCl 2 (The total concentration of metal ions is 1.0×10 -3 M, wherein the Co / Rh molar ratio is 0.5), 0.328g triphenylphosphine trisodium sulfonate (TPPTS) and 0.603g phase transfer agent cetyltrimethylammonium bromide (CTAB) are mixed, and then The mixed solution was added to the autoclave, and the N 2 (1.0MPa) replacement three times, remove the air in the kettle, and then use synthesis gas (H 2 / CO=1.0, 1.0MPa) to wash once, pressurize to the required pressure of 4.8MPa, start the stirrer and raise the temperature to the set reaction temperature of 110°C for 3.0h. The reaction results are shown in Table 1.
Embodiment 3
[0009] Embodiment 3: earlier with 190.0ml buffer (pH is about 7.3), 10.0ml dicyclopentadiene, RhCl 3 and MnCl 2 (The total concentration of metal ions is 1.0×10 -3 M, wherein the Mn / Rh molar ratio is 0.5), 0.328g triphenylphosphine trisodium sulfonate (TPPTS) and 0.6025g phase transfer agent cetyltrimethylammonium bromide (CTAB) are mixed, and then The mixed solution was added to the autoclave, and the N 2 (1.0MPa) replacement three times, remove the air in the kettle, and then use synthesis gas (H 2 / CO=1.0, 1.0MPa) to wash once, pressurize to the required pressure of 4.8MPa, start the stirrer and raise the temperature to the set reaction temperature of 110°C for 3.0h. The reaction results are shown in Table 1.
[0010]
project
catalyst component
Conversion rates
(%)
Aldehyde selectivity
(%)
Dialdehyde selectivity
(%)
space-time yield
(mol h -1 mol -1
metal)
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