A method for olefin hydroformylation using a solid heterogeneous catalyst
A kind of technology of olefin hydroformyl, heterogeneous catalyst
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Embodiment 1
[0055] Under 298K and a nitrogen gas protection atmosphere, 10.0 grams of tris (4-vinylphenyl) phosphine was dissolved in 100.0 ml of tetrahydrofuran solvent, and 1.0 grams of free radical initiator azobisisobutyronitrile was added to the above solution, and stirred for 2 hours . The stirred solution was allowed to stand at 373K under a nitrogen atmosphere for 24h. After the above-mentioned standing solution is cooled to room temperature, the solvent is vacuumed off at room temperature (about 298K), and the tris(4-vinylphenyl)ylphosphine is polymerized by solvothermal method to obtain a compound containing P ligand polymer. The three (4-vinylphenyl) phosphine ligand polymer carrier polymerization technical route in the present embodiment is as follows:
[0056]
[0057] Among them, the degree of polymerization n is 450-550, with a hierarchical pore structure including macropores, mesopores and micropores, and the measured BET specific surface area is 981m 2 / g, the pore ...
Embodiment 2
[0060] Refer to Example 1 for the synthesis of tris(4-vinylphenyl)phosphine ligand polymer carrier. Under 298K and a nitrogen gas protection atmosphere, take 0.5 mg of acetylacetonate dicarbonyl rhodium (I), join in a three-necked flask filled with 100.0 ml of tetrahydrofuran solvent, stir and dissolve, add 1.0 g of the above-mentioned preparation with a hierarchical porous structure The P-ligand-containing polymer, the mixture was stirred at 298K and nitrogen gas protection atmosphere for 24 hours, and then the solvent was vacuumed off at room temperature, and the self-supported P-ligand polymer with a hierarchical porous structure was obtained. Metallic Rh as solid heterogeneous catalysts. Add the solid heterogeneous catalyst of the metal Rh self-supported by the P ligand-containing polymer with a hierarchical porous structure prepared above into the fixed-bed reactor, and feed ethylene gas as the olefin raw material with a molar ratio of 1:2 and CO / H 2 Mixed gas (wherein ...
Embodiment 3
[0062] Refer to Example 1 for the synthesis of tris(4-vinylphenyl)phosphine ligand polymer carrier. Under 298K and a nitrogen gas protection atmosphere, get 12.53 mg of acetylacetonate dicarbonyl rhodium (I) and join in a three-necked flask filled with 100.0 ml of tetrahydrofuran solvent, stir and dissolve, add 1.0 g of the above-mentioned prepared rhodium with hierarchical pore structure P ligand-containing polymer, the mixture was stirred at 298K and a nitrogen gas protection atmosphere for 24 hours, and then the solvent was vacuumed off at room temperature to obtain a self-supported P-ligand polymer with a hierarchical pore structure. Solid heterogeneous catalysts for metallic Rh. Add the solid heterogeneous catalyst prepared above into a fixed-bed reactor, and feed propylene gas and CO / H 2 Mixed gas (wherein H 2 :CO volume ratio=1:1), at 393K, 1.0MPa, the olefin gas volume space velocity is 1000h -1 , CO / H 2 The volume space velocity of the mixed gas is 2000h -1 condi...
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