Fundamental Study On Manufacture Of Cyclopendaienyl Manganese Tricarbonyl

Based on the traditional synthesis procedure of cyclopentadienyl manganese tricarbonyl (CMT), we change the process and conditions of manufacture and successfully optimize the operation conditions.Firstly, we compare the two-step and three-step synthesis procedures, it indicated that the reaction time of two-step12-hour less than three-step one, and the yield of two-step procedure is 3 percent higher than three-step one. Optimizing operation conditions are given as following: the cracking time of DCp is 1.5h, and temperature is 180℃; the reaction time of NaCp is 1.5h, and the temperature is 20-30℃; time of carbonylation reaction is 2h, pressure is 6.0 MPa, temperature is 180-200℃.Amount of water in THF is lower than 90ppm.Further, we measure the solubility of CO in THF and THF-MnCl2, and get the relationship of solubility of CO in reaction system with temperature and pressure, which is important data to industrialization design.