Ziegler-Natta催化剂内给电子体9,9-双(甲氧甲基)芴的合成新工艺  

STUDY ON SYNTHESIZING 9,9-BIS(METHOXYMETHYL) FLUORENE POLYPROPYLENE USED AS A NEW TYE OF ELECTRON DONOR FOR ZGLER-NATTA POLYPROPYLENE CATALYSTS

作　　者：李小明 余官能 杨锦飞 涂媛鸿 许招会 

机构地区：[1]江西西林科股份有限公司,江西南昌 [2]国家单糖化学合成工程技术中心,江西南昌330027

出　　处：《精细石油化工》2012年第5期18-21,共4页Speciality Petrochemicals

基　　金：国家自然科学基金项目(20566004);国家科技攻关计划项目资助项目(2001BA323C)

摘　　要：实验以芴、金属钠与氯甲基甲醚为原料两步合成了9,9-双(甲氧甲基)芴,包括制备芴二基钠及芴二基钠的烷基化反应。最佳合成工艺条件为:(1)制备芴二基钠:以二乙二醇二甲醚为溶剂,n(芴)∶n(钠)=1.0∶2.2,反应温度为65℃,反应时间为8.0h;(2)芴二基钠的烷基化反应:n(芴)∶n(氯甲基甲醚)=1.0∶2.4,反应温度为20℃,反应时间6.0h,在上述条件下,9,9-双(甲氧甲基)芴收率可达66.9%。9,9-Bis（methoxymethyl） fluorene（BMMF）,a new type of electron donor for Ziegler-Natta polypropylene catalysts,was synthesized from fluorene,metal sodium and chloromethyl methyl ether,which included synthesis of fluorene disodium by reaction of fluorene with metallic sodium and successive methylation of fluorene disodium with chloromethyl methyl ether.The optimal reaction conditions were found as follows：（1） for synthesis of fluorene disodium,diethylene glycol dimethylether was used as solvent,n（fluorene）∶n（metallic sodium）=1∶2.2,the reaction temperature was 65 ℃,the reaction time was 8.0 h;（2） for methylation reaction,n（fluorene）∶n（chloromethyl methyl ether）=1∶2.4,the reaction temperature was 20 ℃,the reaction time was 6.0 h.Under above optimal conditions,the yield of BMMF could be up to 66.9%.

关 键 词：9 9-双(甲氧甲基)芴 芴 氯甲基甲醚 烷基化 

分 类 号：TQ426.94[化学工程]