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The Synthesis Of Aromatic Amine And N-Alkyl Amine Catalyzed By Supported Amorphous Alloy

Posted on:2008-01-01Degree:MasterType:Thesis
Country:ChinaCandidate:Q L XinFull Text:PDF
GTID:2121360218453263Subject:Industrial Catalysis
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In this dissertation, supported Ni-based amorphous alloy catalysts were preparedby chemical-reduction method. A series of technologies were used to characterize theircomposition, surface area, structure, thermal stability and morphology. Hydrogenationof synthesis of 3-benzylamino-4-methoxy-acetanilide (BAMA) was selected as theprobe reaction to investigate their catalytic performance. Effect of preparation methodsand conditions on the structure, physical properties and catalytic activity of theseamorphous alloys were studied. Also, anilin was prepared by the reaction ofhydrogenation of nitrobenzene over the catalysis of Ni-B/SiO2 amorphous catalyst andthe catalysis of Ni-B/CNF amorphous catalyst.Influence of temperature, solvent, concentration of Ni2+, molar ratio of BH4-/Ni2+,feeding order and feeding rate on the physical properties and catalytic activities of NiBamorphous alloys were investigated. Experimental results showed as follows:Ⅰ.Thermal stability and catalytic activities of catalysts prepared by Ni(Ac)2 were best.Ⅱ.Concentration of Ni(Ac)2 was lower, catalytic activities of NiB catalysts prepared werehigher.Ⅲ. Molar ratio of BH4-/Ni2+ was higher, numbers of Ni2+ were more, and thebest Molar ratio of BH4-/Ni2+ was 2.Ⅳ. The best feeding rate of solution of KBH4added to solution of Ni2+ 2 ml/min.Ⅴ.γ-Al2O3,SiO2, C were used to preparesupported NiB amorphous alloy catalysts. Their physical properties and catalyticactivities were compared. The factors which affected the activity of these supportedcatalysts were also discussed.Ⅵ. At best conditions, a NiB amorphous catalyst, whichwas more active in synthesis of 3-benzylamino-4-methoxy-acetanilide (BAMA) thanRaney Ni catalyst, was prepared.Synthesis of 3-benzylamino-4-methoxy-acetanilide (BAMA) was prepared by thereaction of 3-amino-4-methoxy-acetanilide (AMA) with benzaldehyde (BAD) by thecatalysis of Ni-B/SiO2 amorphous catalyst. The factors of the reaction condition in thesynthesis of 3-benzylamino-4-methoxy-acetanilide (BAMA) were studied. Experiment results indicate that the optimization process conditions are that, n(AMA): n(BAD)=1:1.1, m(cat):m(AMA)=2.5%, reaction temperature is 55~60℃and reaction pressure is1.2Mpa. Under these conditions, product yield of BAMA can reach 92.6%respectively.Carbon nanofibers(CNFs) supported amorphous alloy were tested as the catalystsfor preparation of aromatic amine. The catalysts were characterized by SEM, TEM,XRD. Experimental results showed that, At 130℃and 3.0MPa, nitrobenzeneselectivity could mount to 99.5% and aniline conversion was 100%.
Keywords/Search Tags:amorphous alloys, catalyst hydrogenation, N-reductive alkylation, 3-amino-4-methoxy-acetanilide, carbon nanofibres, nitrobenzene
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