Zn/HZSM-5分子筛气固相循环法合成苯基二氯化膦  

Synthesis of Dichlorophenylphosphine Over the Catalyst Zn/HZSM-5 in the Gas Phase

作　　者：周志恒[1,2] 范天博[1] 刘云义[1] 高红[3] 

机构地区：[1]沈阳化工大学化学工程学院,辽宁沈阳110142 [2]江苏省格林艾普化工股份有限公司,江苏镇江212000 [3]泛华建设集团有限公司沈阳设计分公司,辽宁沈阳110142

出　　处：《石油学报（石油加工）》2012年第S1期116-121,共6页Acta Petrolei Sinica(Petroleum Processing Section)

基　　金：辽宁省教育厅项目基金(2008B144);沈阳化工大学博士启动基金(200808)项目资助

摘　　要：采用经HZSM-5分子筛改性的Zn/HZSM-5为催化剂,在固定床内由苯和三氯化磷为原料进行气固相催化反应制备苯基二氯化膦(DCPP)。考察了Zn负载量、原料配比、反应温度、反应时间等因素对反应的影响。采用X射线衍射、扫描电镜、傅里叶变换红外、低温氮吸附等手段对催化剂进行了表征。结果表明,Zn负载量为2.5%(质量分数)的Zn/HZSM-5分子筛25g,n(C6H6)∶n(PCl3)=3∶1,反应温度为320℃,反应5h时,苯基二氯化膦收率能达到17.6%。负载Zn后HZSM-5分子筛晶型并未被破坏,Zn组分的引入导致分子筛表面酸性有所变化,反应过程较HZSM-5分子筛易积炭。Dichlorophenylphosphine was synthesized from benzene and phosphorous trichloride with Zn/HZSM-5 as catalyst in the vapor phase through a fixed-bed reactor.Factors,like zinc content,molar ratio of raw materials,reaction temperature and time were investigated.The results showed when using the catalyst of Zn/HZSM-5 with zinc mass fraction of 2.5%,molar ratio of raw materials(benzene/phosphorous trichloride) of 3/1,reaction temperature of 320℃ and reaction time of 5 h,the yield of dichlorophenylphosphine reached 17.6%.The properties of catalysts were characterized by XRD,SEM,FT-IR and BET methods.The results showed that the structure of HZSM-5 was well preserved.The surface acidity of zeolite changed with the increase of zinc content.Carbon coke formation status on Zn/HZSM-5 was inferior to HZSM-5.

关 键 词：Zn/HZSM-5分子筛 苯基二氯化膦(DCPP) 催化 合成 表征 

分 类 号：TQ265.1[化学工程—有机化工]