IM-5沸石的绿色合成与表征  

Green Synthesis and Characterization of IM-5 Zeolite

作　　者：王将[1,2] 马波[2] 杨卫亚[1] 凌凤香[1,2] 沈智奇[1] 侯宇鑫 

机构地区：[1]中国石化抚顺石油化工研究院,辽宁抚顺113001 [2]辽宁石油化工大学石油化工学院,辽宁抚顺113001 [3]中国石油抚顺石化公司大乙烯联合装置生产区,辽宁抚顺113004

出　　处：《石油化工》2014年第8期897-902,共6页Petrochemical Technology

基　　金：中国石油化工股份有限公司项目(512034)

摘　　要：采用动态水热法合成了新型沸石IM-5,考察了反应温度、碱度、凝胶硅铝比和模版剂用量对合成反应的影响,通过XRD、SEM、TEM、NMR、N2吸附-脱附和吡啶吸附-FTIR方法对合成产物进行了表征。实验结果表明,在动态水热体系下,在反应温度170℃、n（NaOH）∶n（SiO2）=0.63-0.73、凝胶硅铝比40-120、n（溴代1,5-二氮-甲基吡咯基戊烷）∶n（SiO2）=0.05-0.10的条件下反应7 d,合成出了高纯度、高结晶度的IM-5沸石,缩短了反应时间,模板剂消耗量降低30%-60%;IM-5沸石的晶粒呈表面褶皱的平板状,长度400-500 nm,宽度100-200 nm;所得IM-5沸石的晶体结构完整,无明显的骨架缺陷;IM-5沸石的比表面积为400 m2/g,具有5种10元环微孔孔道,孔径尺寸分别为0.519,0.522,0.529,0.545,0.549 nm;氢型IM-5沸石拥有较高的总酸量,且中强酸、强酸的含量较多,使其在催化反应中具备优良的活性。A novel zeolite,IM-5,was synthesized by dynamic hydrothermal method and characterized by means of XRD,SEM,TEM,NMR,N2 adsorption-desorption and pyridineFTIR. The effects of reaction temperature,n（NaOH）∶n（SiO2）,n（SiO2）∶n（Al2O3） and n（1,5-bis（Nmethylpyrrolidinium）-pentane bromide（SDA））∶n（SiO2） on the synthesis were studied. The results showed that pure IM-5 zeolite with high crystallinity could be synthesized under the condition of n（NaOH）∶n（SiO2） 0.63-0.73,n（SiO2）∶n（Al2O3） 40-120,n（SDA）∶n（SiO2） 0.05-0.10,reaction temperature 170 ℃ and reaction time 7 d. The reaction time was shortened and the template dosage was reduced by 30%-60%. The IM-5 zeolite crystal was lath-like with wrinkle,and the length of 400-500 nm and the width of 100-200 nm. The NMR and XRD results indicated that the IM-5 zeolite did not have obvious skeletal defects. BET specific surface area of the IM-5 zeolite was 400 m2/g. The IM-5 zeolite had five kinds of micropores with 10-membered rings,and their pore sizes were 0.519,0.522,0.529,0.545 and 0.549 nm,separately. The IM-5 zeolite contains high total acid amount,especially,mid-strong acid and strong acid,which will lead to high catalytic activity.

关 键 词：IM-5沸石 动态水热法 绿色合成 沸石催化剂 

分 类 号：TQ426.6[化学工程]