Preparation、characterization And Applications Of Carbon Based Solid Sulfonic Acid

The magnetic carbon solid acid named Fe3O4@AC-SO3H(FAS) was parpared by ultrasonic-dispersion and self-assembly mathods with TaiXi-Coal Active Carbon as carbon sources.The surface morphology、structure and surface chemical characteristics were characterized by TEM、IR、XPS and VSM.Morever,the catalytic character and technological was investigated by FAS as a catalyst for synthesis of n-Butyl acetate on atmospheric-heating conditions and Microwave-assisted conditions.On the other hand,for increasing acid density of carbon solid acid,a core-shell carbon solid acid named AC@PANI-SO3H(APS) that TaiXi-Coal Carbon was cladding by polyaniline parpared by n-situ chemical oxidative polymerization. The surface morphology、structure and surface chemical characteristics were characterized by SEM、TEM、IR and XPS.Morever,the effects of acid density and technological was investigated by APS as a catalyst for synthesis of amidealkyl naphthol on solvnt-free conditions. The main results of this paper are as follows:(1) The FAS catalyst was characterized by IR, TG techniques. The IR results indicated that the-SO3H appeared at 1000 cm-1 comparing with unsulfonated moreover, the TG results showed that FAS catalyst has good thermal stability under 500 ℃.(2) FAS catalyst was applied to synthesize N-butyl acetate. The results showed that the molar ration of alcohol to aldehyde is 3:1, the amount of catalyst is 7% to the alcohol, Microwave power is 400 W, reflowed for 10 min, the highest yield was 34.7%. However, the molar ration of alcohol to aldehyde is 3:1, reaction time is 160 min,reaction temperature is 82 ℃ and the highest yield was 42.1 % when used atmospheric heating.(3) The preparation process of substrate and sulfonated condition impact on acid value was explored. The results showed that the molar ration of carbon core and shell is 5:2, the molar ration of aniline and initiator is 1:1,(4) The surface morphology and structure was characteristiced by IR, TEM, SEM and XPS.Result of IR showed that there was appeared peak of-SO3H on 900 cm-1 to 1500 cm-1 on the surface of catalyst compare before sulfonate.In this way,-SO3H was bonding on the surface of catalyst could be backing combine with S2p peak characteristiced by XPS. Result of SEM and TEM found that the catalyst has relatively obvious core-shell structure, and particle size distribution more uniform, concentrated in about 100 nm.(5) On the research of FAS and APS catalystic synthesis amidealkyl naphthol,the effects of reaction tempreature、amounts of catalyst and solvent conditions were investigated. Results found that the good yield on solvent-free condition and the good yield from 61% to 92% with reaction tempreature was 120 ℃ and amounts of catalyst was 2% for FAS.On the other hand,the good yield from 76%to 95%with reaction tempreature was 100 ℃ and amounts of catalyst was 1% for APS.The structures of products was characterized by point、IR、1H NMR and 13C NMR.