Catalyst for synthesizing diphenyl carbonate in phenol oxidative carbonylation as well as preparation method and application method of catalyst
A technology of diphenyl carbonate and its application method, which is applied in the field of rod-shaped nano-CeO2 supported Pd catalyst and its preparation, can solve the problems of difficult post-processing, slow reaction rate, large amount of additives, etc., and achieve difficult recycling and low cost , highly active effect
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Embodiment 1
[0030] (1) Weigh 0.064g PdCl 2 (containing Pd0.038g), and dissolved in 5mL of 25% ammonia water;
[0031] (2) Weigh 6.0g Ce(NO 3 ) 3 ·6H 2 O, (theory gives CeO 2 2.379g) was fully mixed with 84.2g NaOH (2.104mol) in the form of solid, and 150mL deionized water was added and stirred to obtain a suspension;
[0032] (3) Add the solution obtained in step (1) to the suspension obtained in step (2), and then transfer to a crystallization kettle lined with polytetrafluoroethylene. Put the crystallization kettle into an oven, and react for 24 hours at 110°C;
[0033] (4) After the reaction, the reaction mixture was taken out from the crystallization kettle, centrifuged, and the obtained solid was washed with deionized water, and then dried at 80°C for 20 hours;
[0034] (5) Calcining the dried solid material at 500°C for 4 hours to obtain rod-shaped nano-CeO 2 supported Pd catalyst.
[0035] The prepared catalyst was characterized by transmission electron microscopy, and the ...
Embodiment 2
[0037] With the rod-shaped nano-CeO that makes in embodiment 1 2 Supported Pd catalyst for oxidative carbonylation of phenol to prepare diphenyl carbonate.
[0038] 2.4g phenol (0.0255mol), 0.5g catalyst (calculated as Pd is 6.94×10 -5 mol) and 0.55g tetrabutylammonium bromide (0.0017mol) were added to the kettle reactor, and then 4g of dehydrating agent 4A molecular sieve and 20mL of solvent methylene chloride were added to the reactor; 0.6MPa oxygen and 6MPa carbon monoxide were charged, React at 100°C for 4 hours. The reaction solution was filtered under reduced pressure to separate the catalyst from the reaction solution, and the reaction solution was analyzed by liquid chromatography. The yield of diphenyl carbonate was 39.1%.
Embodiment 3~5
[0040] The same as the preparation method of Example 1, just change the Ce(NO 3 ) 3 ·6H 2 The amount of O was 9.0g, 4.5g and 3.0g, respectively, and different Pd loadings (Pd / CeO 2 mass ratio) rod-shaped nano-CeO 2 supported Pd catalyst.
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