超重力预混+动态水热法制备ZSM-5分子筛——水热过程影响机制  

Synthesis of ZSM-5 zeolite by dynamic hydrothermal method with premixing in the rotating packed bed:an process mechanism analysis

作　　者：齐婷婷 滕加伟 史静 初广文[1,2] 邹海魁[1,2] 罗勇[1] 张亮亮 孙宝昌[1] QI Tingting;TENG Jiawei;SHI Jing;CHU Guangwen;ZOU Haikui;LUO Yong;ZHANG Liangliang;SUN Baochang(Research Center of the Ministry of Education for High Gravity Engineering and Technology,Beijing University of Chemical Technology,Beijing 100029,China;State Key Laboratory of Organic-Inorganic Composites,Beijing University of Chemical Technology,Beijing 100029,China;State Key Laboratory of Green Chemical Engineering and Industrial Catalysis,SINOPEC Shanghai Research Institute of Petrochemical Technology,Shanghai 201208,China)

机构地区：[1]北京化工大学超重力工程技术研究中心,北京100029 [2]北京化工大学有机-无机复合材料国家重点实验室,北京100029 [3]中国石化上海石油化工研究院绿色化工与工业催化国家重点实验室,上海201208

出　　处：《化工进展》2021年第11期6228-6234,共7页Chemical Industry and Engineering Progress

基　　金：国家重点研发计划(2019YFA0210302)。

摘　　要：ZSM-5分子筛作为一种重要的催化剂,被广泛应用于石油化工行业,其制备工艺一直是分子筛研究的热点。传统静态水热法制备ZSM-5分子筛存在产物粒度分布不均、晶化时间长等问题,本文提出开展超重力预混+动态水热法制备ZSM-5分子筛,考察了晶化过程中晶化方式、搅拌釜转速、晶化时间和晶化凝胶体积对ZSM-5分子筛粒径的影响规律,获得了较优的操作条件;并针对较优条件下制备的产品进行了系统表征。结果表明,相比于超重力预混+静态水热,动态水热更有利于合成粒径小且分布均匀、酸量大、比表面积大的多级孔ZSM-5分子筛,搅拌釜转速越大、晶化凝胶体积越小所制备的产品平均粒径越小,粒径分布越均匀。本文研究结果表明,水热过程参数对分子筛的粒径、结构和酸性具有重要影响。ZSM-5 zeolites with excellent catalytic performance have been widely applied in petrochemical industry as shape-selective catalysts,and therefore it has been a research focus to efficiently prepare zeolites.There are many problems such as poor particle size distributions and long crystallization time in traditional static hydrothermal route.In order to address these problems,ZSM-5 zeolites were prepared by dynamic hydrothermal method in a stirring tank reactor(STR)with premixing in a rotating packed bed(RPB).The effects of crystallization parameters,including crystallization way,rotation speed in the STR,crystallization time,and crystallization gel volume,on the particle size of ZSM-5 zeolites were studied.The ZSM-5 zeolites prepared under the optimal conditions were characterized systematically.The results show that the RPB premixing-STR dynamic hydrothermal synthesis route is conducive to prepare hierarchical ZSM-5 with smaller particle size,more uniform particle size distribution,more acid amount and larger surface areas compared with static hydrothermal route.Faster rotation speed in the STR and smaller crystalline gel volume can facilitate the formation of ZSM-5 zeolites with smaller particle size and more uniform particle size distribution.These results indicated that the hydrothermal process parameters had a significant impact on the particle size,structure and acidity of the zeolites.

关 键 词：水热 分子筛 传递 旋转填料床 

分 类 号：TQ031[化学工程]