Studies Of Synthesis And Technics Of 9,9-bis (methomethyl) Fluorene

Diether is a new kind of electron donors for Ziegler-Natta catalyst. Used 9,9-bis(methomethyl)fluorene as electron donor of Ziegler-Natta catalyst, the isotacticity of polymer is good , the productivy is 3-5 times higer than the fourth Ziegler-Natta catalyst.The two steps in synthesis of 9,9-bis(methomethyl)fluorene were studied. It was concluded that low temperature had positive effect on the first reaction and that adding a bit of ethanol to DMSO could reduce the reaction temperature effectively and increase the productivity of 9,9-bis(hydromethyl)fluorene. By the three phase transfer catalyzing method, 9,9-bis(methomethyl)fluorene was synthesized by 9,9-bis(hydromethyl)fluorene. The reaction conditions were optimized so that the productivities of the two reactions reached 73% and 71% respectively, the total productivity of 9,9-bis(methomethyl)fluorine exceeded 50%. The 9,9-bis(methomethyl)fluorene was tested by some plant. It was showed that act as the electron donor in Ziegler-Natta catalyst resulted in good effect, the productivity was 130kg/gCat and the isotacticity of polymer exceeded 97%. The process producing 9,9-bis(methomemyl)fluorene was studied and had been applied for China patent. The process was accepted by industry. According to the process some plant designed the industrial equipments and will put into production in the near future. By using thin layer chromatgram, column chromatgram, high performance liquid chromatgram and nuclear magnetic resonance, some important components of the accessory substances produced from the two reactions were analyzed and the structures were obtained, which provided references to recycling of them. Only 9-hydromethyl-9-methomehylfluorene belonging to mono-etherized substance was produced in the second reaction. It would increase the productivity of 9,9-bis(methomethyl)fluorene by using repeatedly. The new technics of 9,9-bis(methomethyl)fluorene synthesized by 9,9-bis(hydromethyl)fluorene in DMSO solution was investigated, which provided references to the improvement of process of 9,9-bis(methomethyl)fluorene in the future.