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两步晶化法合成纳米SAPO-34分子筛及其催化性能
引用本文:杨德兴,王鹏飞,徐华胜,吕爱玲,胡杰,吕待清.两步晶化法合成纳米SAPO-34分子筛及其催化性能[J].高等学校化学学报,2011,32(4):939-945.
作者姓名:杨德兴  王鹏飞  徐华胜  吕爱玲  胡杰  吕待清
作者单位:上海化工研究院;上海绿强新材料有限公司;
基金项目:国家“八六三”计划项目(批准号:2007AA05Z326); 上海市科委纳米专项基金(批准号:0952nm01200)资助
摘    要:分别以拟薄水铝石、硅溶胶和磷酸为铝源、硅源和磷源,四乙基氢氧化铵为模板剂,采用两步水热晶化-双氧水氧化法合成出粒径200~300nm的小粒径SAPO-34分子筛。采用X射线衍射(XRD)、扫描电子显微镜(SEM)、NH3-TPD、BET等方法对合成的SAPO-34分子筛进行了表征。进一步考察了纳米SAPO-34分子筛在固定床甲醇制取烯烃(MTO)反应中的催化性能。结果表明,通过控制水热晶化过程的条件可有效地调控SAPO-34的晶粒大小。特别当第一步和第二步晶化温度为130℃和180℃时,可得到大小在200~300nm、晶型完整的SAPO-34分子筛。对于MTO反应,合成的纳米级SAPO-34的C2~C4选择性可达92%,单程寿命接近10h,显著优于以传统方法合成的大粒径SAPO-34。

关 键 词:纳米SAPO-34  两步晶化  双氧水氧化处理  MTO
收稿时间:2010-06-23

Two-step Crystallization Synthesis and Catalytic Performance of Nano-scaled SAPO-34 Molecular Sieve
YANG De-Xing,WANG Peng-Fei,XU Hua-Sheng,L Ai-Ling,HU Jie,L Dai-Qing.Two-step Crystallization Synthesis and Catalytic Performance of Nano-scaled SAPO-34 Molecular Sieve[J].Chemical Research In Chinese Universities,2011,32(4):939-945.
Authors:YANG De-Xing  WANG Peng-Fei  XU Hua-Sheng  L Ai-Ling  HU Jie  L Dai-Qing
Institution:YANG De-Xing,WANG Peng-Fei,XU Hua-Sheng,L(U) Ai-Ling,HU Jie,L(U) Dai-Qing
Abstract:In this study, nano-scaled SAPO-34 molecualr sieves with size in the range of 200~300 nm were synthesized by the two-step crystallization and H2O2 oxidation process, with pseudoboehmite, colloidal silica and H3PO4 as sources of aluminum, silicon and phosphorous and TEAOH as templates. The prepared SAPO-34 was characterized by XRD, SEM, NH3-TPD, BET and so on. The catalytic performance of the SAPO-34 on the methanol-to-olefins reactions (MTO) was carried out on a fixed bed. The results showed that the particle size of the SAPO-34 could be effectively modulated by the crystallization temperature of the two-step crystallization process. In particular, when the first and second crystallization were conducted at 130℃ and 180℃, cubic SAPO-34 with 200~300 nm size could be successfully synthesized. Compared with the micro-scaled SAPO-34 prepared by the traditional hydrothermal process, the nano-scaled SAPO-34 crystals synthesized here showed better performance in the MTO reaction and the selectivity of C2~C4 and the lifetime for one-turn could attained about 92% and 10 hours, respectively.
Keywords:Nano-scaled SAPO-34 molecular sieve  Two-step crystallization  H2O2 oxidizing treatment  Methanol-to-olefins(MTO) reaction  
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