Method for preparing 3-acetoxypropanol from vinyl acetate
A technology of acetoxy propanol and vinyl acetate, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, and can solve the problem of limited loading of phosphorus ligands, loss of catalytically active components, and limited Catalyst industrial application and other issues, to achieve excellent low-temperature activity and selectivity of alcohol products, reduce separation costs, high economic value and industrial application prospects
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Embodiment 1
[0023] 1) Preparation of Heterogeneous Catalysts for Hydroformylation
[0024] Under the protective atmosphere of 298K and inert gas, dissolve 10.0 g of tris(4-vinylphenyl) phosphine ligand in 100 ml of tetrahydrofuran solvent, add 0.25 g of free radical initiator azobisisobutyronitrile to the above solution, and stir 0.5 hours. The stirred solution was transferred to a hydrothermal autoclave, and solvothermally polymerized at 373K under the protective atmosphere of inert gas for 24h. After the above-mentioned polymerization, it was cooled to room temperature, and the solvent was removed by vacuum pumping to obtain a specific surface area of 1121m. 2 / g, pore volume 1.87cm 3 / g of porous organic polymer containing phosphine ligands. Under the protective atmosphere of 298K and inert gas, 0.1253 g of acetylacetonate dicarbonyl rhodium was weighed and dissolved in 200 ml of tetrahydrofuran solvent, and 10.0 g of the above-prepared porous organic polymer containing phosphine ...
Embodiment 2
[0032] 1) Preparation of Heterogeneous Catalysts for Hydroformylation
[0033] The preparation of the heterogeneous catalyst for hydroformylation is the same as that in Example 1.
[0034] 2) Vinyl acetate hydroformylation reaction process
[0035] The hydroformylation heterogeneous catalyst prepared above was charged into a fixed bed reactor, and both ends were charged with quartz sand. Introduce syngas (H 2 :CO=1:1) and raw material vinyl acetate, vinyl acetate is transported into the reaction system by a high-pressure pump, and the synthesis gas is directly fed in the form of gas. At 373K, 3MPa, the space velocity of vinyl acetate liquid is 2.13h -1 , syngas gas space velocity 1125h -1 The hydroformylation reaction was carried out under the conditions. The reaction product was collected at 2.5°C via a collection tank equipped with recirculating cooling. The obtained liquid-phase product was analyzed by HP-7890N gas chromatography, and the internal standard method was ...
Embodiment 3
[0041] 1) Preparation of Heterogeneous Catalysts for Hydroformylation
[0042] The preparation of the heterogeneous catalyst for hydroformylation is the same as that in Example 1.
[0043] 2) Vinyl acetate hydroformylation reaction process
[0044] The hydroformylation heterogeneous catalyst prepared above was charged into a fixed bed reactor, and both ends were charged with quartz sand. Introduce syngas (H 2 :CO=1:1) and raw material vinyl acetate, vinyl acetate is transported into the reaction system by a high-pressure pump, and the synthesis gas is directly fed in the form of gas. At 413K, 5MPa, the space velocity of vinyl acetate liquid is 0.2h -1 , syngas gas space velocity 1125h -1 The hydroformylation reaction was carried out under the conditions. The reaction product was collected at 2.5°C via a collection tank equipped with recirculating cooling. The obtained liquid-phase product was analyzed by HP-7890N gas chromatography, and the internal standard method was a...
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