Cyclohexene catalytic oxidation cyclohexanone preparation reaction catalyst, and preparation method and application thereof
A technology for preparing cyclohexanone by catalytic oxidation of cyclohexene, which is used in the preparation of carbonyl compounds by oxidation, catalysts for physical/chemical processes, molecular sieve catalysts, etc. The effect of separation, high catalytic activity, excellent activity
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[0034] A method for preparing a catalyst for the catalytic oxidation of cyclohexene to cyclohexanone and a process for applying it to the reaction of catalytic oxidation of cyclohexene to cyclohexanone. The experimental steps are as follows:
[0035] (1) Firstly, the synthesized mesoporous molecular sieve SBA-15 (synthesized according to the method reported in the literature) and aminopropyltriethoxysilane silicon coupling agent (the mass ratio of the two is 1:1~2) in the organic solvent toluene or bismuth Reflux reaction in toluene to prepare aminated SBA-15 material.
[0036] (2) Reflux the aminated SBA-15 material and 4,5-diazafluoren-9-one (DAFO) ligand (the mass ratio of the two is 1:1~2) in toluene or xylene for 12~ After 24 hours, the product was washed several times with absolute ethanol to obtain the modified SBA-15 carrier.
[0037] (3) After refluxing the modified SBA-15 carrier and PdCl2 (the mass ratio of the two is 30-100:1) in acetone for 36 hours, cooling and ...
Embodiment 1
[0046] Preparation and modification of SBA-15 mesoporous material:
[0047] (1) Preparation of SBA-15 molecular sieve material: 4g P123 (polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer) and 120g 2mol / L dilute in a 500ml three-necked flask Add hydrochloric acid and 30g of deionized water, and stir in a water bath at 38°C for 2 hours. After mixing evenly, add 8.4g of tetraethyl orthosilicate, continue stirring for 20h, and then move the solution to a Teflon-lined In an autoclave, put it in an oven at 100°C for 24 hours, cool it to room temperature, filter it, and wash it with deionized water and absolute ethanol several times, and dry the product in an oven for 6 hours to obtain a SBA-15 mesoporous material;
[0048] (2) Amination of SBA-15 mesoporous molecular sieves: under nitrogen protection, in a 250ml three-necked flask equipped with a condenser tube, add 2g of the prepared SBA-15 and 150ml of anhydrous xylene respectively, and stir at room temp...
Embodiment 2
[0050] Synthesis of 4,5-diazafluoren-9-one (DAFO) ligand
[0051] (1) Mix 3g of o-phenanthroline, 50ml of 1,4-dioxane solution, 2g of potassium hydroxide and 100ml of distilled water into a 500ml four-necked round bottom flask, and stir at a temperature of 100°C Reflux for 30 minutes to mix the solution evenly;
[0052] (2) 8g of KMnO 4 After mixing and dissolving with 60ml of water, add it dropwise into a four-neck flask through a constant pressure dropping funnel, complete the dropwise addition within half an hour, and then continue to reflux at 100°C for 1 hour;
[0053] (3) After the reflux was completed, it was filtered while it was hot to obtain a red solution, which was left standing in the refrigerator for 24 hours and filtered to obtain yellow needle-shaped crystals, and then recrystallized with ethanol to obtain the DAFO ligand.
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