The Synthesis Of Ferrocene Carboxylic Acid Methyl Ester, And Bis (cyclopentadienyl) Titanium And Titanocene Sbs Hydrogenation Catalytic Performance

In this thesis, titanocene and ferrocenoyl derivates were synthesized and characterized. Firstly, ferrocene was reacted with acetyl chloride in presence of AlCl₃, and got 1,1'-diacetylferrocene with the yield of 83.3%. Then 1,1'-diacetylferrocene was oxided by bromine, and 1,1'-ferrocene-dicarboxylic acid was obtained with the yield 74.5%. Finally, 1,1'-dimethyl ferrocene carboxylate was formed from the esterification of ferrocene dicarboxylic acid and the yield is 72.0%. The IR spectrum and ¹H-NMR were taken to characterize the compounds. In addition, the methods of CV (Cyclic Voltammetry) and DPV (Differential Pulse Voltammetry) were carried out to investigate the electrochemical properties of the compounds. The experimental results shown that the redox of 1,1'-dimethyl ferrocene carboxylate is a reversible process.The synthesis of titanocene dichloride from the direct reaction of cyclopentadiene with titanic tetrachloride on the presence of diethyl amine was reported in this thesis too. The conditions of the reaction which include the degradation of dicyclopentadiene, redistillation of cyclopentadiene, reaction temperature and reaction time and etc.. The optimistic conditions of the synthesis were obtained. Dicyclopentadiene was degraded at 160-180℃, and collected the distillate of 42-45℃, and got 98% purity of cyclopentadiene with the yield of 74.5%. For the synthesis of TDC, THF was used as solvent, in the presence of ethylamine, cyclopentadiene was reacted with titanium chloride at 65-68℃(reflux) for 4 hours. The total yield of TDC was 72.1%. The IR results and 1H-NMR spectra correspond to that of titanocene dichloride. Biscyclopentadieneyl titanium dichloride was used as hydrogenation catalyst for SBS to make SEBS. SEBS is a kind of general-service thermoplastic elastomer material. The effects of reaction conditions on the hydrogenation degree of SBS were investigated. The experimental results shown that the hydrogenation degree of ofdienein SBS are more than 94.2 % which the hydrogenation at 60-70℃for 2 hours with 2.0 MPa, and the catalyst concentration was 0.4mmol/100g polymer. Furthermore, the relationships of hydrogenation degree and properties of SEBS were investigated.