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.
出处
《石油化工》
CAS
CSCD
北大核心
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)
关键词
IM-5沸石
动态水热法
绿色合成
沸石催化剂
IM-5 zeolite
dynamic hydrothermal method
green synthesis
zeolite catalyst