A kind of olefin hydroformylation reaction method
A technology for the hydroformylation of olefins, which is applied to the preparation of carbon monoxide reaction, chemical instruments and methods, organic compound/hydride/coordination complex catalysts, etc. Inactivation, etc.
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Embodiment 1
[0038] In a glove box under an inert atmosphere, according to the molar ratio of 1-octene to rhodium in the rhodium complex catalyst of 4000:1, measure 12.14 mL of 1-octene and dissolve it in 12.86 mL of toluene, and add it to a glass syringe . Take by weighing 17.50mg three (triphenylphosphine) carbonyl rhodium hydride (the catalyst of formula I structure, wherein L 1 for H, L 2 for CO, L 3 is triphenylphosphine, x=y=1, z=3) and 630mg triphenylphosphine (compound of formula II structure, wherein R 1 , R 2 and R 3 are hydrogen) mixed (the molar ratio of triphenylphosphine to rhodium is 126:1) was dissolved in 10 mL of toluene, added to another glass syringe, and the syringe was sealed and taken out from the glove box.
[0039] The hydroformylation reaction device adopts a 50mL autoclave reaction device. The autoclave was heated to 80°C, and after vacuuming, the synthesis gas (CO:H 2 =1:1) replacement several times, the vent valve is opened, then the toluene solution (th...
Embodiment 2
[0042] Same as Example 1, except that the added amount of triphenylphosphine was changed to 450 mg (the molar ratio of organic phosphine compound to rhodium was 90:1). The test results are shown in Table 1.
[0043] The color of the toluene solution of the catalyst recovered has no obvious change before the reaction, indicating that rhodium has not been oxidized. pass at the same time 31 PNMR analysis of the chemical environment of the P atom in the rhodium-bound ligand shows that the chemical environment has not changed significantly after the reaction, indicating that the phosphine ligand bound to the catalyst has not been separated, and the structure of the catalyst has not been destroyed. The recovered catalyst does not need to be reprocessed, and the recovered catalyst is used to carry out the above reaction again. After the reaction is completed, the reaction solution is collected and subjected to chromatographic analysis. The results are shown in Table 1.
Embodiment 3
[0045] Same as Example 1, except that the amount of triphenylphosphine added was changed to 200 mg (the molar ratio of organophosphine compound to rhodium was 40:1). The test results are shown in Table 1.
[0046] The color of the toluene solution of the catalyst recovered is slightly darker than before the reaction, indicating that a small amount of rhodium is oxidized. pass at the same time 31 PNMR analysis of the chemical environment of the P atom in the rhodium-bound ligand shows that the chemical environment has not changed significantly after the reaction, indicating that the phosphine ligand bound to the catalyst has not been separated, and the structure of the catalyst has not been destroyed. The recovered catalyst does not need to be reprocessed, and the recovered catalyst is used to carry out the above reaction again. After the reaction is completed, the reaction solution is collected and subjected to chromatographic analysis. The results are shown in Table 1.
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