Process for preparing 3-hydroxypropionate
A technology of hydroxypropionate and acrylonitrile, applied in chemical instruments and methods, carbon monoxide or formate reaction preparation, physical/chemical process catalysts, etc., can solve the problem of difficult separation of catalysts, and achieve mild catalytic reaction conditions and high activity High, the effect of solving separation difficulties
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Embodiment 1
[0038] 1. Synthetic catalyst
[0039] 1.0 mmol Co 2 (CO) 8 Dissolve in 740 mmol of methanol, add polyacrylonitrile powder with a degree of polymerization of 1000, make the molar ratio of nitrogen to cobalt carbonyl 2:1, and stir at room temperature for 2 hours to obtain a catalyst mixture.
[0040] 2. Preparation of methyl 3-hydroxypropionate
[0041] The obtained catalyst mixture was transferred to a 100 mL reactor; the reactor was purged three times with nitrogen, and carbon monoxide and 50 mmol ethylene oxide were added to make the system pressure 5 MPa; reacted at 60° C. for 6 hours. After the reaction was completed, the reactor body was cooled to 0° C., the pressure was slowly released to normal pressure, and the reactor was purged three times with nitrogen. Sampling analysis showed that the conversion rate of ethylene oxide was 39%, and the selectivity of methyl 3-hydroxypropionate was 77%.
[0042] For the convenience of comparison, the results of the synthesis reac...
Embodiment 2
[0044] 1. Synthetic catalyst
[0045] 1.0 mmol Co 2 (CO) 8 Be dissolved in the methyl alcohol of 740mmol, add the poly(acrylonitrile-co-vinylidene chloride) powder that the number of acrylonitrile monomer unit is 1000 (acrylonitrile monomer unit and vinylidene chloride monomer unit in the copolymer The molar ratio of nitrogen and carbonyl cobalt is 1:1), and the molar ratio of nitrogen and cobalt carbonyl is 2:1, and stirred at room temperature for 2 hours to obtain a catalyst mixture.
[0046] 2. Preparation of methyl 3-hydroxypropionate
[0047] The obtained catalyst mixture was transferred to a 100 mL reactor; the reactor was purged three times with nitrogen, and carbon monoxide and 50 mmol ethylene oxide were added to make the system pressure 5 MPa; reacted at 60° C. for 6 hours. After the reaction was completed, the reactor body was cooled to 0° C., the pressure was slowly released to normal pressure, and the reactor was purged three times with nitrogen. Sampling anal...
Embodiment 3
[0050] 1. Synthetic catalyst
[0051] 1.0 mmol Co2 (CO) 8 Be dissolved in the methyl alcohol of 740mmol, add the poly(acrylonitrile-co-butadiene) powder that the number of acrylonitrile monomer unit is 1000 (the mole of acrylonitrile monomer unit and butadiene monomer unit in the described copolymer The ratio is 1:1), the molar ratio of nitrogen and cobalt carbonyl is 2:1, and stirred at room temperature for 2 hours to obtain a catalyst mixture.
[0052] 2. Preparation of methyl 3-hydroxypropionate
[0053] The obtained catalyst mixture was transferred to a 100 mL reactor; the reactor was purged three times with nitrogen, and carbon monoxide and 50 mmol ethylene oxide were added to make the system pressure 5 MPa; reacted at 60° C. for 6 hours. After the reaction was completed, the reactor body was cooled to 0° C., the pressure was slowly released to normal pressure, and the reactor was purged three times with nitrogen. Sampling analysis showed that the conversion rate of et...
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