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化学工业与工程 2014, Vol. 31 Issue (5) :37-42    DOI: doi: 10.13353/j.issn.1004.9533.2014.05.007
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低模数水玻璃合成ZSM-5分子筛及工艺条件优化
孙浩,汪宝和
(天津大学石油化工技术开发中心,绿色合成与转化教育部重点实验室,天津 300072)
Synthesis of ZSM-5 from Low Modulus Sodium Metasilicate System and Optimization of  Process Conditions
SUN  Hao, WANG  Bao-He
(R & D Center for Petrochemical Technology, Key Laboratory for Green Chemical Technology of State Education Ministry, Tianjin University, Tianjin 300072, China)

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摘要 以低模数(n=1.03)水玻璃为硅源,通过改良水热合成途径,成功制备出无模板剂ZSM-5分子筛。借助X射线衍射仪(XRD)和扫描电镜(SEM)对ZSM-5分子筛结晶度及晶貌进行表征。在n(硅)/n(铝)为50 的情况下,通过考察晶化温度、时间、pH值、水含量、有无搅拌或晶种对ZSM-5分子筛物性的影响,优化合成工艺。结果表明,静置或晶种法得到的ZSM-5分子筛,晶体粒径大且晶貌不规整,不适合用于低模数水玻璃合成ZSM-5体系。ZSM-5沸石最适宜制备工艺为:n(H2O)/n(SiO2)=40,pH=10的合成混合物经室温老化24 h,搅拌状态下,170 ℃下水热晶化24 h。与商业级ZSM-5相比,低模数水玻璃合成的ZSM-5分子筛在环己烯水合反应中表现出更高的催化活性和选择性。
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孙浩
汪宝和
关键词水玻璃   ZSM-5   无模板剂   工艺优化     
Abstract: Template-Free ZSM-5 from low modulus (n=1.03) sodium metasilicate synthesis mixture were successfully synthesized through an improvement hydrothermal synthesis route. The crystallinities and morphologies of the ZSM-5 zeolites were characterized with X-ray diffraction (XRD) and scanning electron microscopy (SEM). In the case of silica alumina ratio of 50, the synthesis process was optimized by examining the effect of crystallization temperature, time, pH, water content, stir and seed crystal on the properties of ZSM-5 zeolites. ZSM-5 zeolites with big crystal size, irregular morphology were obtained from static or crystal seed method,the results showed that those two methods were not suitable for synthesis of ZSM-5 system. The suitable synthesis conditions of ZSM-5 zeolite are as follows: pH=10, n(H2O)/n(SiO2)=40, aged at room temperature for 24 h, hydrothermal crystallization at 170 ℃ for 24 h. Compared with the commercial ZSM-5, ZSM-5 zeolites obtained from low modulus sodium metasilicate synthesis mixture exhibited a higher catalytic activity and selectivity in the hydration reaction of cyclohexene.
Keywordssodium silicate   ZSM-5   template-free;   process optimization     
Received 2013-01-18;
Corresponding Authors: 汪宝和,电话: (022)27403763,E-mail: wangbh2012@yeah.net。     Email: wangbh2012@yeah.net
About author: 孙浩(1987-),男,硕士,从事环己烯水合催化剂研究。
引用本文:   
孙浩, 汪宝和.低模数水玻璃合成ZSM-5分子筛及工艺条件优化[J].  化学工业与工程, 2014,31(5): 37-42
SUN Hao, WANG Bao-He.Synthesis of ZSM-5 from Low Modulus Sodium Metasilicate System and Optimization of  Process Conditions[J].  Chemcial Industry and Engineering, 2014,31(5): 37-42
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