Synthesis of coordination type zirconium pyrogallol and application thereof in preparation of cyclohexanol
A technology of zirconium pyrogallol and pyrogallol is applied in the synthesis field of coordination zirconium pyrogallol to achieve the effects of reducing energy consumption, mild reaction conditions and good catalytic effect
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Embodiment 1
[0039] [Example 1] preparation of zirconium pyrogallol catalyst
[0040] 0.127g pyrogallol (PA) and 0.466g zirconium tetrachloride (ZrCl 4 ) were respectively dissolved in 20mL DMF solution, and ultrasonically treated with an ultrasonic cleaner for 10min. First, the sonicated ZrCl 4 The solution was poured into a 100mL PTFE reactor, and then the pyrogallol solution was added dropwise. After the above solution was mixed evenly, 3mL of glacial acetic acid with a concentration of 0.1mmol / L was added dropwise thereto. Then the reactor was moved to a constant temperature drying oven at 140° C., and the reaction was continued for 16 h. After the reaction, the reactor was naturally cooled to room temperature, washed three times with DMF and absolute ethanol, dried at 100° C. under vacuum for 12 hours, and ground to obtain the Zr-PA catalyst.
Embodiment 2
[0041] [Example 2] preparation of zirconium pyrogallol catalyst
[0042] 0.127g pyrogallol (PA) and 0.233g zirconium tetrachloride (ZrCl 4 ) were respectively dissolved in 20mL DMF solution, and ultrasonically treated with an ultrasonic cleaner for 10min. First, the sonicated ZrCl 4 The solution was poured into a 100mL PTFE reactor, and then the pyrogallol solution was added dropwise. After the above solution was mixed evenly, 3mL of glacial acetic acid with a concentration of 0.1mmol / L was added dropwise thereto. Then the reactor was moved to a constant temperature drying oven at 140° C., and the reaction was continued for 16 h. After the reaction, the reactor was naturally cooled to room temperature, washed three times with DMF and absolute ethanol, dried at 100° C. under vacuum for 12 hours, and ground to obtain the Zr-PA catalyst.
Embodiment 3
[0043] [Example 3] preparation of zirconium pyrogallol catalyst
[0044] 0.127g pyrogallol (PA) and 0.466g zirconium tetrachloride (ZrCl 4 ) were respectively dissolved in 20mL DMF solution, and ultrasonically treated with an ultrasonic cleaner for 10min. First, the sonicated ZrCl 4The solution was poured into a 100mL PTFE reactor, and then the pyrogallol solution was added dropwise. After the above solution was mixed evenly, 3mL of glacial acetic acid with a concentration of 0.1mmol / L was added dropwise thereto. Then the reactor was moved to a constant temperature drying oven at 160° C., and the reaction was continued for 16 h. After the reaction, the reactor was naturally cooled to room temperature, washed three times with DMF and absolute ethanol, dried at 100° C. under vacuum for 12 hours, and ground to obtain the Zr-PA catalyst.
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