The Studieds On Preparation And Application Of Metal Sulfonate In Oxidizing Reaction Of N-Butanol

In this paper,three kinds of metal sulfonate was synthesized as catalysts of n-butanol oxidation with p-toluenesulfonic acid and metal hydroxid（M（OH）n）as raw material（Co（OTs）₂·6H₂O,Ni（OTs）₂·6H₂O,Fe（OTs）₃·6H₂O）.The DSC,TGA,IR and EDS of three kinds of catalysts were researched.The synthesis technique optimization of nickel and cobalt salt catalyst was studied and the optimal process condition is:the molar ratio of p-toluenesulfonic acid to M（OH）₂（M = Ni,Co）is 1.1:1,the reaction temperature is 80℃,reaction time is 3 h,the yield of Co（OTs）₂·6H₂O and Ni（OTs）₂·6H₂O were over 91%.The catalytic effects of three kinds of catalyst was studied with hydrogen peroxide as oxidant and acetonitrile as solvent.The effects of process conditions and process optimization of n-butanol oxidation was studied with Fe（OTs）₃·6H₂O as catalyst.The optimal process condition for the reaction is:temperature is 70℃,the mass of catalyst is 0.473 g per 3.7 g n-butanol,n（H₂O₂）:n（n-butanol）is 3 and amount of acetonitrile is 25 g per 3.7 g n-butanol,the yield of total acid was 113.6%.The solubility of Fe（OTs）₃·6H₂O in（ethanol + water）mixtures with a mole fraction of 0-0.327 ethanol was measured from 291.15 to 333.15 K by using a synthetic method.The solubility data were correlated by the modified Apelblat equation,the Redlich-Kister（CNIBS/R-K）model,and the hybrid model,and the results showed that the three models agree well with experimental data.The thermodynamic properties of the dissolution process,including enthalpy,entropy,and Gibbs energy were estimated from the experimental data by the modified van’t Hoff equation,indicating that the process of the dissolution of Fe（OTs）₃·6H₂O is endothermic and spontaneous.