Preparation method of metal organic framework material and application of metal organic framework material in cyclohexyl hydroperoxide decomposition reaction
A technology of cyclohexyl hydroperoxide and metal-organic framework, which is applied in the field of fine chemicals, can solve the problems that the catalyst cannot be recycled many times, the loss of chromium, and the irreversible deactivation of molecular sieves, etc., and achieves good catalytic effect, short synthesis cycle and excellent preparation process. simple effect
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Embodiment 1
[0033] 2.0gCr (NO 3 ) 3 9H 2 O and 0.82g terephthalic acid dissolved in 25mL0.05mol L -1 sodium acetate solution, stirred at room temperature for 30 min. The obtained solution was transferred to a 50 mL self-generating autoclave with polytetrafluoroethylene, and the reaction autoclave was placed in a blast drying oven heated to 200° C. for 12 hours. After the reaction, the reaction kettle was left to stand, slowly cooled to room temperature, and the obtained liquid was centrifuged, and the separated solid was first washed with N,N-dimethylimide at 70°C for 1 hour, then washed with ethanol for 1 hour, and finally Wash with water for 1h. The obtained solid was vacuum-dried at 150° C. for 12 h to obtain a Cr metal-organic framework material, which was denoted as MIL-101 (Cr).
[0034] The following examples illustrate the catalytic decomposition method of cyclohexyl hydroperoxide in the cyclohexane oxidation solution provided by the present invention.
[0035] The cyclohexa...
Embodiment 2
[0038] Take 0.05g of the catalyst prepared in Example 1 and 10mL (about 8.22g) of cyclohexane oxidation solution, and add them into a 50mL three-necked flask. Heat to 70°C while stirring, and react at constant temperature for 100 minutes. After cooling to room temperature, the reaction solution was taken out for analysis. The conversion rate of cyclohexyl hydroperoxide is 97.9%, the selectivity of cyclohexanone and cyclohexanol is 100%, and cyclohexanone:cyclohexanol=6.5:1 (molar ratio).
Embodiment 3
[0040] According to the operation process of embodiment 2, the difference with embodiment 2 is: the catalyst quality of catalyzing the decomposition of cyclohexyl hydroperoxide is 0.1g. The conversion rate of cyclohexyl hydroperoxide is 98.2%, the selectivity of cyclohexanone and cyclohexanol is 100%, and cyclohexanone:cyclohexanol=6.7:1 (molar ratio).
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