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第 36 卷第 6 期                             精   细   化   工                                  Vol.36, No.6
             201 9 年 6 月                             FINE CHEMICALS                                 June    2019


              功能材料
                  蒸汽晶化法制备 EMT 分子筛及其烯烃净化性能



                                                                1*
                                        周永贤       1,2 ,陈   伟 ,王鹏飞            1,2*
                 (1.  上海绿强新材料有限公司,上海    201806;2.  聚烯烃催化技术与高性能材料国家重点实验室  上海化
                 工研究院有限公司,上海    200062)

                 摘要:以 18-冠醚-6 为模板剂,运用蒸汽晶化法制备了六方晶型八面沸石类似物(EMT)分子筛(记为 SEMC-2)。
                 在 n(Na 2 O)∶n(Al 2 O 3 )=2.4∶1.0 时,重点考察了蒸汽晶化时间、蒸汽晶化温度对 EMT 分子筛晶型的影响。结果
                 表明,在晶化温度 110 ℃,晶化时间 6 d 时,制备得到了直径为 3~4 m,厚度为 300~400 nm 的六方晶型 SEMC-2
                 分子筛。与传统的水热晶化制备得到的 EMT 分子筛(记为 HEMC-2)类似,该 SEMC-2 分子筛能将氮气和乙烯
                 气体中初始摩尔分数为 0.02%和 0.10%的甲醇、丙醛两种极性含氧杂质深度脱除至摩尔分数 0.0001%以下,且穿
                 透时间及吸附容量均没有表现出明显差异。此外,该 SEMC-2 分子筛具备良好的结构稳定性及较长的使用寿命。
                                                                                       +
                 原位红外谱图表明,SEMC-2 分子筛主要是通过杂质自身氧中的孤电子对与分子筛中的 Na 间相互作用的物理吸
                 附过程来脱除甲醇、丙醛两种杂质。
                 关键词:EMT 分子筛;蒸汽晶化;烯烃深度净化;极性含氧化合物;功能材料
                 中图分类号:TQ170.1      文献标识码:A      文章编号:1003-5214 (2019) 06-1041-08



                      Preparation of EMT Zeolite and Its Purification Performance on
                                         Olefins by Steam Crystallization


                                                    1,2
                                                                 1*
                                    ZHOU Yong-xian , CHEN Wei , WANG Peng-fei     1,2*
                 (1.  Shanghai  Luqiang New Materials Co., Ltd., Shanghai  201806,  China;  2. State Key Laboratory of Polyolefin
                 Catalytic Technology  and High Performance  Materials, Shanghai  Research Institute of  Chemical Industry Co., Ltd.,
                 Shanghai 200062, China)

                 Abstract: Hexagonal EMT zeolite (denoted as SEMC-2) was successfully synthesized using 18-crown-6
                 ether as template by steam crystallization (SAC) method. The effects of both SAC time and temperature on
                 the crystal form were studied when the n(Na 2O)∶n(Al 2O 3)   =2.4∶1.0. The regular hexagonal platelets of
                 3~4  μm  in  diameter  and  300~400  nm  in  thickness  were  synthesized  under  crystallization  temperature
                 110 ℃,  crystallization  time  6  days.  Similar  to  EMT  zeolite  prepared  by  traditional  hydrothermal
                 crystallization method (denoted as HEMC-2), SEMC-2 zeolite could also deeply purify the trace amounts of
                 polar methanol and propanal to below mole percent 0.0001% from gaseous olefins at an initial mole percent
                 0.02%  or  0.10%.  Moreover,  there  was  no  significant  difference  in  breakthrough  time  and  cumulative
                 adsorption amount for HEMC-2 and SEMC-2 zeolite. The regeneration experiment indicated that SEMC-2
                 zeolite had more stable structure and longer service life. In-situ FTIR spectra demonstrated the adsorption
                 processes of SEMC-2 zeolite for methanol and propanal were a physical adsorption mainly via interaction
                                                                       +
                 among the lone pair electrons in the impurity's own oxygen and Na  in SEMC-2 zeolite.
                 Key words: EMT zeolite; steam crystallization; olefins deeply purification; polar-oxygenated compounds;
                 functional materials
                 Foundation item: Shanghai Science and Technology Talent Project (15XD1522300)



                 收稿日期:2018-10-12;  定用日期:2019-01-18; DOI: 10.13550/j.jxhg.20180751
                 基金项目:上海市科技人才计划项目(15XD1522300)
                 作者简介:周永贤(1977—),女,高级工程师,博士生。联系人:陈   伟(1989—),男,工程师,E-mail:charrycechen@sina.cn,
                 电话:021-69577696。王鹏飞(1969—),男,教授级高工,E-mail:wpf@sh-lq.com,电话:021-69577696。
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