Bimetal MOF catalyst for synthesizing cyclic lactone by tandem catalysis of cyclic alcohol as well as preparation method and application of bimetal MOF catalyst
A technology for catalyzing cyclic alcohols and bimetals, applied in organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, catalytic reactions, etc., can solve problems such as explosion and expensive, and achieve simple equipment and low cost. , highly selective effect
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Embodiment 1
[0063] Catalyst described in this embodiment is MgMn-MOF catalyst, and its preparation method comprises the following steps:
[0064] (1) Dissolve magnesium nitrate hexahydrate (0.1mmol), manganese nitrate (0.4mmol) and 2-hydroxyterephthalic acid (0.25mmol) in N,N-dimethylformamide (10mL), ethanol (4mL) In a mixed solution composed of water (1mL), stir to prepare the precursor solution;
[0065] (2) Move the precursor solution in step (1) into the reaction kettle, and react at 80°C for 18h;
[0066] (3) Centrifuge the prepared bimetallic MgMn-MOF, wash it several times with DMF and methanol, and dry it in vacuum at 80° C. for 6 hours to obtain the MgMn-MOF catalyst;
[0067] The method of catalyzing cyclic alcohols in series to synthesize cyclic lactones:
[0068] (a) Weigh the MgMn-MOF catalyst (40mg) into a three-necked flask with a condenser, add toluene (10mL), 1mmol cyclobutanol, feed oxygen at a flow rate of 40mL / min, and stir the reaction at 40°C 3h, during the react...
Embodiment 2
[0071] Catalyst described in this embodiment is MgFe-MOF catalyst, and its preparation method comprises the following steps:
[0072] (1) Dissolve magnesium sulfate (0.2mmol), ferrous nitrate (0.3mmol) and 2,5-dihydroxyterephthalic acid (0.24mmol) in N,N-dimethylformamide (10mL), ethanol ( 3mL) and water (2mL) in the mixed solution that forms, stir preparation precursor solution;
[0073] (2) Move the precursor solution in step (1) into the reaction kettle, and react at 90°C for 24h;
[0074] (3) The prepared bimetallic MgFe-MOF was separated by centrifugation, washed several times with DMF and methanol, and dried in vacuum at 90° C. for 7 hours to obtain the MgFe-MOF catalyst.
[0075] The method of catalyzing cyclic alcohols in series to synthesize cyclic lactones:
[0076] (a) Weigh the MgFe-MOF catalyst (30mg) into a three-necked flask with a condenser, add ethanol (10mL), 1mmol cyclopentanol, feed oxygen at a flow rate of 30mL / min, and stir the reaction at 50°C 4h, 2mm...
Embodiment 3
[0079] The catalyst described in this embodiment is a MgCo-MOF catalyst, and its preparation method comprises the following steps:
[0080] (1) Dissolve magnesium acetate (0.3mmol), cobalt nitrate hexahydrate (0.2mmol) and 3-hydroxy-4,4-biphenyldicarboxylic acid (0.23mmol) in N,N-dimethylformamide (10mL) , ethanol (2mL) and water (3mL) in the mixed solution that forms, stir preparation precursor solution;
[0081] (2) Move the precursor solution in step (1) into the reaction kettle, and react at 100°C for 30h;
[0082] (3) The prepared bimetallic MgCo-MOF was separated by centrifugation, washed several times with DMF and methanol, and dried in vacuum at 100 °C for 8 h to obtain the MgCo-MOF catalyst.
[0083] The method of catalyzing cyclic alcohols in series to synthesize cyclic lactones:
[0084](a) Weigh the MgCo-MOF catalyst (20mg) into a three-necked flask with a condenser, add ethyl acetate (10mL), 1mmol cyclohexanol, and feed oxygen at a flow rate of 20mL / min, at 60°C...
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