高岭土微球原位晶化合成高岭土-NaY-MCM-41复合物

在高岭土微球上原位晶化合成了高岭土-NaY-MCM-41复合物．利用XRD、SEM、TEM和BET等测试手段对合成的样品进行了表征．研究了高岭土表面原位生长NaY-MCM-41复合分子筛的合成化学．考察了合成体系的pH值、模板剂、H2O用量和SiO2／Al2O3比的影响．高岭土-NaY-MCM-41复合物具有大、介、微梯度分布的孔结构和合理的酸性分布．克服了单独的微孔分子筛孔径和介孔分子筛的局限性．实现了介孔、微孔分子筛的优势互补．     

高岭土原位无溶剂法合成小粒径ZSM-5分子筛

结合原位水热法和无溶剂法的优点,在不添加有机模板剂和溶剂的基础上,以高岭土为原料通过晶种诱导绿色高效地合成出ZSM-5分子筛。运用X射线衍射、N2吸附-脱附、扫描电镜、透射电镜和NH3程序升温脱附(TPD-NH3)等技术对ZSM-5分子筛进行表征。表征结果与原位水热法合成的ZSM-5分子筛相比,原位无溶剂法合成ZSM-5分子筛的结晶度较高、晶体粒径较小、酸强度略高、孔结构相似。     

晶种导向下干胶法合成ZSM-5分子筛

以廉价水玻璃为硅源,在晶种替代有机模板剂的条件下采用干胶法合成了ZSM-5分子筛。利用XRD、SEM、TEM、FTIR、N_2吸附-脱附和NH_3-TPD等分析方法对合成样品进行了表征和测试,考察了合成条件对ZSM-5分子筛晶化过程的影响。结果表明,在硅铝比(n/n)为30~70,钠硅比(n/n)为0.12~0.20时都可以得到结晶度良好的ZSM-5分子筛。研究发现,干胶法合成ZSM-5,在不引入外加水的情况下也可以得到ZSM-5样品,外加水的引入能够有效地提高晶化速率;与水热法合成ZSM-5分子筛相比,干胶法可以显著地缩短晶化时间,同时,合成样品的晶体尺寸也有所减小。     

晶种导向下干胶法合成ZSM-5分子筛

以廉价水玻璃为硅源,在晶种替代有机模板剂的条件下采用干胶法合成了ZSM-5分子筛。利用XRD、SEM、TEM、FTIR、N₂吸附-脱附和NH₃-TPD等分析方法对合成样品进行了表征和测试,考察了合成条件对ZSM-5分子筛晶化过程的影响。结果表明,在硅铝比（n/n）为30~70,钠硅比（n/n）为0.12~0.20时都可以得到结晶度良好的ZSM-5分子筛。研究发现,干胶法合成ZSM-5,在不引入外加水的情况下也可以得到ZSM-5样品,外加水的引入能够有效地提高晶化速率;与水热法合成ZSM-5分子筛相比,干胶法可以显著地缩短晶化时间,同时,合成样品的晶体尺寸也有所减小。     

一种在堇青石蜂窝陶瓷上合成ZSM-5分子筛的新途径

Cordierite honeycombs are widely used as mono lith reactors in high gas flux circumstances due to their high thermal stability and low-pressure drop,such as catalytic converters in automotive emission control. In recent years, some attempts have been made to support zeolites onto cordierite honey combs[1-4]. In view of the relative complex config uration of the cordierite honeycombs, there have been some difficulties to obtain a zeolite layer with an even and enough thickness on every channel wall by the traditional hydrothermal technique. In the present paper, we for the first time apply vapor phase transport (VPT) technique to the synthesis of ZSM-5 onto cordierite honeycombs. And, to verify the feasibility of this technique, we prepared the Cu/ZSM-5 monolith catalyst by ion exchange, and tested its catalytic performance for NO reduction with C3H8.     

堇青石蜂窝陶瓷载体上ZSM-5及Anacime沸石的原位合成

 采用水热合成法,在堇青石蜂窝陶瓷载体上原位合成了ZSM-5沸石和Anacime沸石,并用XRD和SEM等技术进行了表征. 结果表明,当改变合成条件时,在堇青石表面可分别生长出厚度为30~40 μm的ZSM-5沸石和厚度为30~180 μm的Anacime沸石. 随着凝胶中SiO2/Al2O3比的增大和含水量的减少,在堇青石蜂窝陶瓷上生长的分子筛的量也增加.     

ZSM-5催化绿色合成烯胺酮化合物

以环境友好的ZSM-5分子筛为催化剂,催化β-二羰基化合物与胺反应,绿色合成β-烯胺酮类化合物.该方法环境友好、处理方法简单、收率高、催化剂可回收使用.     

无有机胺体系中高硅ZSM-5沸石的一步合成

在无有机胺模板剂和不加晶种体系中,采用较低晶化温度(130℃),在水热体系中一步合成了形貌均一的板块状高硅ZSM-5沸石(n_(SiO_2)/n_(Al_2O_390)。系统地考察了合成体系中原料的物质的量之比对合成ZSM-5沸石的影响。通过X射线衍射(XRD),傅里叶红外光谱(FT-IR),扫描电镜(SEM),低温氮气吸附/脱附和固体核磁共振(~(29)Si MAS NMR)等技术手段对合成的ZSM-5沸石进行了物化表征。结果表明,当原料的物质的量之比n_(C_2H_5OH)/n_(SiO_2)=2.8、n_(Na_2O)/n_(SiO_2)=0.14和n_(SiO_2)/n_(Al_2O_3)=150时,可合成具有高结晶度的ZSM-5纯相沸石。比表面积和微孔孔容分别为409 m~2·g~(-1)和0.14 cm~3·g~(-1),其骨架n_(SiO_2)/n_(Al_2O_3)达到96.4。     

沸石分子筛在高岭土微球上的生长

 通过不同的合成方法,在高岭土微球上生长了沸石分子筛P与沸\r\n石分子筛KSO1的混合物、单一沸石分子筛KSO1和小晶粒沸石分子筛Y,\r\n并用多种物理手段如X射线衍射、电子显微镜和固体核磁共振波谱等对\r\n合成样品进行了表征．     

硅胶原位合成ZSM-5分子筛及其催化性能的研究

以正丁胺为模板剂,采用水热晶化法在固体硅胶小球上原位合成了ZSM-5分子筛。考察了晶化温度、晶化时间、初始凝胶硅铝比及H2O/ SiO2、BuNH2/ SiO2、OH-/SiO2对ZSM-5相对结晶度的影响,得到了ZSM 5的合成化学规律。采用XRD、SEM、FT IR及N2吸附手段对固体硅胶小球上原位合成的复合结构分子筛进行了表征。结果表明,这种材料具有介孔和微孔的复合结构特征,而且很好地保持了硅胶小球的形貌。以大庆VGO为原料,在重油微反装置上对该复合结构分子筛进行催化性能评价。结果表明,使用硅胶原位合成的ZSM-5分子筛可显著提高低碳烯烃选择性和收率。     

In-situ Synthesis of Binderless ZSM-5 Zeolitic Coatings on Aluminum

ZSM-5 zeolitic coatings on aluminum have been prepared successfully by in-situ hydrothermal synthesis method and ZSM-5/Al monolith was formed. The effects of pH value and crystallization time on the in-situ synthesis were discussed.     

In-situ Synthesis of ZSM-5 with Different Si/AlRatios on Honeycombshaped Cordierite and their Behavior on NO Decomposition

Thecleaningtechniquestoreduceairpollutionproducedbytheedriaustgasesfromvehicles'enginearefocusedbyresearchworkersinrecentyearsl-2.Amongthem,thecatalyticconversionofthepoisonoussubstances,suchasCO,HCandNOxintonon-orlesspoisonousonesmaybethemosteffective.Thecatalystthatiscalled"monolithiccatalyst"wascomposedofthreepartsfsubstrate,activecoatingandactivecomponents3.Thesubstrateincommonusewasthehoneycomb-shapedcordierite,whosemaincomponentwasfZMgO.ZAI,O,.SSiO,.Theactivecoatings(Y-Al,O,,zeol…     

In Situ Synthesis of NaY Zeolite with Coal—Based Kaolin

NaY zeolites were in-situ synthesized form coal-based kaolin via the hydrothermal method. The effects of various factors on the structure of the samples were extensively investigated.The samples were characterized by N2 adsorption,XRD,IR and DTG-DTA methods,and the results show that the crystallization temperature and amount of added water play an important role in the formation of the zeolite structure.The 4A and P zeolites are the competitive Phaes present in the resulting product.However,NaY zeolites wiht a higher relative crystallinity,excluding impure crystals and the well hydrothermal stapore size distribution,and this means that optimization of this process might result in a commercial route to synthesize NaY zeolites form coal-based kaolin.     

Synthesis and Characterization of ZSM-5/β Co-Crystalline Zeolite

ZSM-5/β co-crystalline zeolites with different content of ZSM-5 have been synthesized by adding different amount of ZSM-5 to the synthetic system ofβ zeolite with NaAlO2, silica sol as the source of aluminum and silica, respectively, and TEA as the template under controlled condition of the synthesis. The ZSM-5/β co-crystalline zeolite was studied by XRD, SEM, BET and NH3-TPD. The reaction activity of toluene alkylation was investigated with a mixture of toluene-methanol as the feedstock in a pulse micro-reactor over the ZSM-5/β co-crystalline zeolite. It is found that ZSM-5/β co-crystalline zeolite has two kinds of zeolite structure including ZSM-5 and β zeolite, not in the form of a physical mixture. The pore structure of ZSM-5/β co-crystalline zeolites is different from that forβ zeolite, ZSM-5and their physical mixture. In addition, the peaks of both high and low temperature desorption of ammonia over the ZSM-5/β co-crystalline zeolite shift 23 ℃ to lower temperatures and the acid amount of its strong acid is 3% more than the physical mixture. So the ZSM-5/β co-crystalline zeolite produces the highest content of xylene, which is 10.4% higher than the physical mixture. And the ZSM-5/β co-crystalline zeolite has better selectivity for toluene alkylation and weaker de-methylation than β zeolite, ZSM-5 and their physical mixture.     

不同晶粒大小ZSM－5的合成和表征

采用水热合成法，由不同途径合成出晶粒大小不同的几种ＺＳＭ－５分子筛，这几种分子筛具有大致相同的硅铝比．采用ＮＨ３－ＴＧ－ＴＰＤ，Ｐｙｒｉｄｉｎｅ－ＩＲ－ＴＰＤ表征其酸性，用ＸＰＳ表征其外表面的硅铝比（体相的硅铝比用元素原子吸收法测定）．研究结果表明，应用导向剂可以合成出要求的晶粒大小而且粒度均匀；加晶种的合成得不到较大的晶体，粒度亦不均匀．分子筛的晶粒大小对其酸性有一定的影响，一般来讲，小晶粒分子筛的酸量多．本文中大晶粒分子筛的硅铝比基本上是不均匀的．     

不同形貌ZSM-5分子筛的合成及苯-乙醇烷基化反应性能

采用水热法制备了环状、薄片、类球状聚集体和小晶粒4种不同形貌和尺寸的纳米ZSM-5分子筛,用XRD、SEM、BET和NH3-TPD对所合成分子筛进行了表征,并考察分子筛形貌对苯和乙醇烷基化性能的影响。实验结果表明：在相同的硅铝比下,不同形貌的分子筛具有相似的弱酸峰强度,短b轴和中空结构的存在会降低分子筛的强酸峰强度,分子筛的强酸峰强度直接影响烷基化性能;分子筛颗粒形貌对催化烷基化性能有较大影响,四种形貌分子筛催化苯和乙醇烷基化性能优劣顺序为：薄片ZSM-5>环状ZSM-5>类球状团聚体ZSM-5>小晶粒ZSM-5。其中,具有薄片结构的H-ZSM-5分子筛在烷基化反应过程中表现出最佳的催化性能。综合对比结果表明：较低的强酸强度、较大的比表面积和孔容、较多的直形孔道占比下,分子筛的烷基化性能最佳,产物乙苯的选择性越高。     

含铁微孔EU-1/ZSM-5复合分子筛的合成和表征

采用预置晶种法合成了含铁的微孔EU-1/ZSM-5复合分子筛,并采用X射线粉末衍射(XRD)、扫描电子显微镜(SEM)、热重-微分热重(TG-DTG)、N₂吸附-脱附、紫外-可见吸收光谱(UV-vis DRS)、X射线吸收精细结构(XAFS)等手段进行了表征。结果表明,复合分子筛具有EU-1和ZSM-5的特征衍射峰,是两种晶相相互作用的分子分散晶相材料,微孔孔径较Fe-EU-1分子筛有所增大。随原始溶胶中铁的质量分数增加,复合分子筛具有的23.09°和23.94°处的特征衍射峰逐渐向低角度方向偏移;紫外-可见漫反射谱图中在220~245 nm出现了宽的吸收谱带;XAFS表征表明,1s→3d电子跃迁的弱吸收峰逐渐增强,同时在吸收边顶部出现的1s→4p吸收峰逐渐由宽变窄。合成工艺的最佳条件为,原始溶胶中铁的质量分数为0.075%~0.15%,晶种添加比例为15.0%~21.0%,晶种SiO₂/Al₂O₃物质的量比为50~60。     

碱金属盐对ZSM-5分子筛晶化的影响

Effect of different alkali metal salts on the crystal size and the crystallization rate of ZSM-5 zeolite was de-tailedly investigated in this paper. The samples prepared by adding the different alkali metal salts were character-ized by using XRD， TEM， TG-DSC， BET and IR techniques. The XRD results showed that， for the nanosized ZSM-5 zeolite， the characteristic peaks broadened on the XRD patterns in comparison with the microsized ZSM-5 zeolite. The SEM results verified that the crystal size of zeolites prepared by adding different alkali metal salts had different results， and adding NaCl， NaC₂H₃O₂ and KCl showed the better effect of reducing crystal size， which are about of 40～60nm size. The crystallization curve of adding the different alkali metal salts suggested that the crystallization rate was significantly affected by the anions in the alkali metal salt besides the cations. Moreover， the crystal size likewise depended on the anion in the alkali metal salt. In addition， the BET results suggested that the nanosized ZSM-5 zeolite possessed a larger outer surface area in comparison with the microsized ZSM-5 zeolite. The thermostability of the samples was determined by TG-DSC technique， indicating that the nanosized ZSM-5 zeolite had a poor thermostability as compared with the microsized ZSM-5 zeolite. The possible difference of the samples with different crystal sizes on IR spectra was also given.