Dehalogenation and degradation method for halogenated aromatic compound
A technology for aromatic compounds and dehalogenation, which is applied in the preparation of organic compounds, preparation of amino compounds, chemical instruments and methods, etc. It can solve the problems of large equipment investment, long process flow, poor selectivity and safety, and achieve safety High performance, high reactivity, improved selectivity and toxicity resistance
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Embodiment 1
[0025] (1) Catalyst 1% (wt) Pd / La-Al 2 o 3 preparation of
[0026] 1.59gLa(NO 3 ) 3 ·6H 2 O (purity 98%) is impregnated to 50g Al in equal volume 2 o 3 above, soaked overnight, dried at 100°C for 5h, and fired at 300°C for 5h to obtain La-Al 2 o 3 . 0.85gPdCl 2 (Purity is 98%) After dissolving with appropriate amount of water, impregnated into La-Al 2 o 3 After soaking for 2 hours, adjust the pH value of the solution to 9 with NaOH, continue stirring and soaking overnight, and then wash the solution with distilled water to neutrality. Then dry at 110°C for 5h, and bake at 300°C for 5h to get Pd / La-Al 2 o 3 catalyst.
[0027] (2) Pd / La-Al 2 o 3 Catalytic dechlorination of 2,4,6-trichloroaniline
[0028] Add 1% (wt) Pd / La-Al obtained in step (1) into a 300ml reactor 2 o 3 Catalyst 1g, using H 2 After replacing the air in the kettle for 3 times, the temperature was raised to 180 ° C, and the 2 The atmosphere was maintained for 2h. After the catalyst is degas...
Embodiment 2
[0030] (1) Preparation of catalyst Pd / Ba-MgO
[0031] 2.86gBa(NO 3 ) 2 Equal volume was impregnated on 50g MgO, dried at 120°C for 3h after impregnated overnight, and baked at 500°C for 8h to obtain Ba-MgO. Then 7.50gPdCl 2 After dissolving, impregnate it on Ba-MgO, adjust the pH value of the solution to 9 with NaOH after impregnating for 3 hours, continue stirring and impregnating overnight, and then wash the solution with distilled water until neutral. Then dried at 120°C for 3h, and calcined at 500°C for 8h to obtain a Pd / La-MgO catalyst.
[0032] (2) Pd / Ba-MgO catalyzed debromination of 1,3,5-tribromobenzene
[0033] Add 1 g of the prepared Pd / Ba-MgO catalyst in a 300ml reactor, raise the temperature to 100°C, and 2 The atmosphere was maintained for 1h. After the catalyst was reduced and degassed, 70g (2.18mol) of methanol, 80g of water and 1g (0.003mol) of 1,3,5-tribromobenzene were added to the kettle. After the reaction temperature rises to 50°C, adjust the press...
Embodiment 3
[0035] Using the same operating method as in Example 1 (1) and (2), the difference is that the reaction temperature in Example 1 (2) is 190°C, the reaction time is 22h, and the reaction pressure is 1MPa. After analysis: 2,4, The conversion rate of 6-trichloroaniline is 100%, the selectivity of 2,4-dichloroaniline is 76.5%, and the selectivity of o-chloroaniline is 13.2%.
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