Non-covalent polymer catalyst suitable for oxidation of 2,3,6-trimethylphenol and preparation method thereof
A technology of trimethylphenol and catalyst, which is applied in the field of non-covalent polymer catalyst for 2,3,6-trimethylphenol oxidation and its preparation, can solve the problem of difficult separation of product and catalyst, environmental pollution, and stability of small molecules It has the advantages of good industrial application prospect, simple preparation method, and product selectivity preservation effect.
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Embodiment 1
[0041] The invention provides a method for preparing a non-covalent polymer catalyst suitable for oxidation of 2,3,6-trimethylphenol, comprising the following steps:
[0042] (1) Synthesis of Salphen: In a 500ml three-necked flask, add 3,3-diaminobenzidine (1g, 4.67mmol) and 150ml of methanol, under nitrogen protection, dissolve salicylaldehyde (2.74g, 22.4mmol) in 100ml of methanol dropwise Added to the reaction solution, stirred at room temperature for 24h, filtered, washed with methanol to obtain the crude product, recrystallized from THF to obtain the desired Salphen compound, wherein the bisalphen structure is as follows:
[0043]
[0044] (2) Synthesis of cobalt (Salphen): In a 250ml three-necked flask, add Salphen (251mg, 0.4mmol) and 100ml THF, ultrasonically dissolve, under nitrogen protection, methanol (30ml) of cobalt acetate tetrahydrate (238mg, 0.95mmol) The solution was added dropwise to the THF solution of bi-Salphen, stirred at room temperature for 24 h, fil...
Embodiment 2
[0049] The invention provides a method for preparing a non-covalent polymer catalyst suitable for oxidation of 2,3,6-trimethylphenol, comprising the following steps:
[0050] (1) Synthesis of Salphen: In a 500ml three-necked flask, add 3,3-diaminobenzidine (1g, 4.67mmol) and 150ml of methanol, under nitrogen protection, dissolve salicylaldehyde (2.74g, 22.4mmol) in 100ml of methanol dropwise Added to the reaction solution, stirred at room temperature for 24h, filtered and washed with methanol to obtain the crude product, THF recrystallized to obtain the desired Salphen compound;
[0051] (2) Synthesis of cobalt (Salphen): In a 250ml three-necked flask, add Salphen (251mg, 0.4mmol) and 100ml THF, ultrasonically dissolve, under nitrogen protection, methanol (30ml) of cobalt acetate tetrahydrate (238mg, 0.95mmol) The solution was added dropwise to the THF solution of Salphen, stirred at room temperature for 24h, filtered, washed with methanol and water to obtain the desired Co(Sa...
Embodiment 3
[0055] The invention provides a method for preparing a non-covalent polymer catalyst suitable for oxidation of 2,3,6-trimethylphenol, comprising the following steps:
[0056] (1) Synthesis of Salphen: In a 500ml three-necked flask, add 3,3-diaminobenzidine (1g, 4.67mmol) and 150ml of methanol, under nitrogen protection, dissolve salicylaldehyde (2.74g, 22.4mmol) in 100ml of methanol dropwise Added to the reaction solution, stirred at room temperature for 24h, filtered and washed with methanol to obtain the crude product, THF recrystallized to obtain the desired Salphen compound;
[0057] (2) Synthesis of cobalt (Salphen): In a 250ml three-necked flask, add Salphen (251mg, 0.4mmol) and 100ml THF, ultrasonically dissolve, under nitrogen protection, methanol (30ml) of cobalt acetate tetrahydrate (238mg, 0.95mmol) The solution was added dropwise to the THF solution of Salphen, stirred at room temperature for 24h, filtered, washed with methanol and water to obtain the desired Co(Sa...
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