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Announcing the merger of Zeolites and Microporous Materials 宣布沸石和微孔材料合并
Pub Date : 1997-11-01 DOI: 10.1016/S0144-2449(97)00123-1
Lovat V.C. Rees (Professor), Robert W. Thompson (Professor)
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引用次数: 0
Degree of crystallinity of dealuminated offretites determined by X-ray diffraction and by a new method based on nitrogen adsorption 用x射线衍射和氮吸附新方法测定脱铝铝石的结晶度
Pub Date : 1997-11-01 DOI: 10.1016/S0144-2449(97)00101-2
A.P. Carvalho, M. Brotas de Carvalho, J. Pires

Samples obtained from thermal dealumination (in the presence and absence of water vapour) of three offretite zeolites with, respectively, 4.4, 3.4, and 2.9 aluminium atoms per unit cell, were investigated by i.r. spectroscopy. X-ray diffraction, and nitrogen adsorption. The percentage of crystallinity was then evaluated by two different methods: the standard XRD technique and a new method based on nitrogen adsorption data analysed through the αs-method. In this case the volume of the ultramicropores (width less than 0.7 nm) was considered. Differences between the two estimates, as well as the loss of crystallinity during dealumination, which is expressed by the representation of both crystallinity evaluations, CXRD or CADS, versus ν1 (the frequency of the stretching asymmetric T-O band), were analysed for self-steamed and steamed samples. The results obtained agree within 20%, and often better. For self-steamed samples the crystallinity evaluated from XRD patterns is always smaller than that estimated from adsorption data, whereas for steamed samples the opposite situation is generally observed.

通过热脱铝(存在和不存在水蒸气)获得的三种offrete沸石样品,分别为4.4,3.4和2.9铝原子每单元电池,通过红外光谱进行了研究。x射线衍射和氮吸附。然后用两种不同的方法来评估结晶率:标准的XRD技术和基于αs法分析氮吸附数据的新方法。在这种情况下,考虑了超微孔(宽度小于0.7 nm)的体积。两种估计之间的差异,以及脱铝过程中结晶度的损失,这是由结晶度评估的表示,CXRD或CADS,相对于ν1(拉伸不对称T-O波段的频率),对自蒸和蒸样品进行了分析。所获得的结果在20%以内一致,而且往往更好。对于自蒸样品,通过XRD谱图评价的结晶度总是小于通过吸附数据估计的结晶度,而对于蒸样品,通常观察到相反的情况。
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引用次数: 13
Crystal structure of the zeolite mutinaite, the natural analog of ZSM-5 该沸石的晶体结构为异沸石,是ZSM-5的天然类似物
Pub Date : 1997-11-01 DOI: 10.1016/S0144-2449(97)00124-3
Giovanna Vezzalini, Simona Quartieri, Ermanno Galli, Alberto Alberti, Giuseppe Cruciani, Ake Kvick

We describe the crystal structure of the high-silica zeolite mutinaite, recently found at Mt. Adamson (Northern Victoria Land, Antarctica). Mutinaite is the natural counterpart of the synthetic zeolite ZSM-5. The new mineral, (Na2.76K0.11Mg0.21Ca3.78) (Al11.20Si84.91) · 6O H2O H2O, is orthorhombic, space group Pnma, with a = 20.201(2), b = 19.991(2), and c = 13.469(2) Å. A single-crystal X-ray diffraction experiment was performed at the synchrotron radiation source ESRF (Grenoble). No Si-Al order in the framework has been detected. Large distances between ions in the channels and framework oxygens suggest weak interactions between the framework and extraframework species.

我们描述了最近在Adamson山(南极洲北维多利亚地)发现的高硅沸石mutinaite的晶体结构。Mutinaite是合成沸石ZSM-5的天然对应物。新矿物(Na2.76K0.11Mg0.21Ca3.78) (Al11.20Si84.91)·60 H2O H2O为正交晶系,空间群为Pnma, a = 20.201(2), b = 19.991(2), c = 13.469(2) Å。在同步辐射源ESRF(格勒诺布尔)上进行了单晶x射线衍射实验。在框架中没有检测到Si-Al的顺序。通道中的离子与框架氧之间的距离较大,表明框架和框架外物种之间的相互作用较弱。
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引用次数: 55
The transformation of kaolin to low-silica X zeolite 高岭土向低硅X型沸石的转化
Pub Date : 1997-11-01 DOI: 10.1016/S0144-2449(97)00132-2
Deepak Akolekar, Alan Chaffee, Russell F. Howe

The thermal transformation of kaolin extrudates to metakaolin and the subsequent crystallization of low-silica X extrudates has been investigated by X-ray diffraction, scanning electron microscopy, FTIR spectroscopy, N2-adsorption, 27Al and 29Si MAS NMR, and surface analysis. Kaolin transforms to metakaolin at 973 K. The macroporous metakaolin extrudates are converted to zeolite X plus a small amount of zeolite A in alkaline solution at 324 K. The 27Al NMR signals of octahedral and pentacoordinated aluminium in metakaolin are removed after 30 min at 324 K, whereas the first XRD features of zeolites X and A are not detected until 48 h. Likewise, 29Si NMR and FTIR spectra show that zeolite is first present at 48 h synthesis time. The amount of zeolite A decreases with increasing synthesis time, but there is an overall increase in product crystallinity and surface area up to 240 h. SEM analyses show that zeolite crystals first form in the interior of extrudates at the edges of macropores; with time the metakaolin matrix is consumed to produce well-crystalline zeolite extrudates consisting of ca. 95% low-silica X and 5% zeolite A.

采用X射线衍射、扫描电镜、红外光谱、n2吸附、27Al和29Si核磁共振以及表面分析等方法研究了高岭土挤压物向偏高岭土的热转变以及低硅X挤压物的结晶过程。高岭土在973 K时转变为偏高岭土。将大孔偏高岭土挤出物在324 K的碱性溶液中转化为沸石X和少量沸石a。偏高岭土中八面体铝和五配位铝的27Al核磁共振信号在324 K下加热30 min后被去除,而沸石X和A的第一个XRD特征直到48 h才被检测到。同样,29Si核磁共振和FTIR光谱显示沸石在合成时间48 h时首次出现。随着合成时间的增加,A型沸石的含量逐渐减少,但到240 h,产品的结晶度和比表面积总体呈增加趋势。SEM分析表明,沸石晶体首先在挤出物内部的大孔边缘形成;随着时间的推移,偏高岭土基体被消耗,生成由约95%的低硅X和5%的沸石A组成的结晶良好的沸石挤出物。
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引用次数: 153
Pub Date : 1997-11-01 DOI: 10.1016/S0144-2449(97)00137-1
V. Termath
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引用次数: 0
Enterex: Anti-diarrheic drug based on purified natural clinoptilolite Enterex:以纯天然斜沸石为基础的止泻药物
Pub Date : 1997-11-01 DOI: 10.1016/S0144-2449(97)00087-0
G. Rodríguez-Fuentes, M.A. Barrios, A. Iraizoz, I. Perdomo, B. Cedré

A new anti-diarrheic drug for humans has been developed based on the physical and chemical properties of the purified natural clinoptilolite NZ. A series of physical, chemical, technological, pharmacological, microbiological, and clinical studies were successfully conducted to meet the requirements of the Cuban Drug Quality Agency. The most important results concerning the properties and biological mechanism of NZ are decribed in this paper.

根据纯化天然斜沸石NZ的理化性质,研制了一种新的人类抗腹泻药物。为了满足古巴药品质量局的要求,成功地进行了一系列物理、化学、技术、药理学、微生物学和临床研究。本文综述了有关NZ的性质和生物学机制的最新研究成果。
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引用次数: 139
Spectroscopic and catalytic evidence for the incorporation of gallium in the AEL framework 光谱和催化证据的结合镓在AEL框架
Pub Date : 1997-11-01 DOI: 10.1016/S0144-2449(97)00113-9
Francisco J. Machado, Carmen M. López, José Goldwasser, Bernardo Méndez, Yván Campos, Douglas Escalante, Miguel Tovar, María M. Ramírez-Agudelo

71Ga MAS n.m.r. analysis and the catalytic behavior during the transformation of 1-butene and n-butane strongly suggest the incorporation of Ga into the AlPO4-11 (AEL) framework during the synthesis of GaAPSO-11. A unique clear signal at around +120 ppm is proposed to be associated with the presence of tetrahedral Ga in the AEL framework of the unmodified GaAPSO-11. Migration of structural Ga atoms to the silicon domain of the AEL framework seems to occur as a result of a mild hydrothermal treatment, giving rise to an additional signal at +156 ppm, previously associated with tetrahedral gallium in gallosilicates with the MFI topology. The fact that GaAPO-11 and GaAPSO-11 behaved in a way similar to their counterparts AlPO4-11 and SAPO-11 during the skeletal isomerization of n-butenes reinforces the idea of an isomorphous substitution of Al(III) by Ga(III) in the AEL framework. The transformation of n-butane was shown to be a valuable test for detecting the presence of small amounts of hydro-dehydrogenating extraframework gallium species (EFGS) in Ga-supported SAPO-11 (Ga/SAPO-11). The fact that the sample of GaAPSO-11 was completely inactive for this transformation leads us to believe that the incorporation of gallium into the tetrahedral positions of the AEL framework was almost complete.

在GaAPSO-11的合成过程中,Ga在AlPO4-11 (AEL)框架中被掺入。在+120 ppm左右,一个独特的清晰信号被提出与未修饰的GaAPSO-11的AEL框架中四面体Ga的存在有关。结构Ga原子迁移到AEL框架的硅畴似乎是温和水热处理的结果,在+156 ppm时产生额外的信号,以前与具有MFI拓扑结构的低硅硅酸盐中的四面体镓有关。在正丁烯的骨架异构化过程中,GaAPO-11和GaAPSO-11的行为方式与它们的对应物AlPO4-11和SAPO-11相似,这一事实加强了在AEL框架中Al(III)被Ga(III)同构取代的观点。正丁烷的转化被证明是检测Ga负载的SAPO-11 (Ga/SAPO-11)中存在少量氢化脱氢的框架外镓(EFGS)的有价值的测试。GaAPSO-11样品对这种转变完全不活跃,这一事实使我们相信镓在AEL框架四面体位置的结合几乎完成了。
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引用次数: 11
On the synthesis of nitrate enclathrated sodalite in organic solvents 有机溶剂中硝酸包合钠石料的合成
Pub Date : 1997-11-01 DOI: 10.1016/S0144-2449(97)00098-5
M. Fechtelkord, B. Posnatzki, J.-Chr. Buhl

Hydrothermal synthesis of sodalite has been investigated in the system NaOCH3-2SiO3-Al2O3-NaNO3-(CH3OH, C5H11OH) at temperatures of 423 K and 473 K. For the first time the organic solvents methanol or pentanol together with sodium methylate as base were used besides common inorganic educts as Si/Al source and sodium nitrate salt. The sodalites have been characterized by X-ray powder diffraction, as well as by 29Si, 23Na MAS NMR, and 23Na DOR NMR measurements. IR-FT spectroscopy shows the successful enclathration of nitrate anions in the β-cages of sodalite. Reaction products of the solvent/base have been identified by 1H 13C CPMAS NMR and 1H MAS NMR. Scanning-electron micrographs show crystals larger than 15 μm grown at 473 K in pentanol.

以NaOCH3-2SiO3-Al2O3-NaNO3-(CH3OH, C5H11OH)为体系,在423 K和473 K条件下进行了水热合成钠盐的研究。除常用无机溶剂硅铝源和硝酸钠外,首次采用有机溶剂甲醇或戊醇和甲基化钠作为碱。通过x射线粉末衍射以及29Si, 23Na MAS NMR和23Na DOR NMR测量对钠盐进行了表征。红外-傅立叶变换光谱显示硝酸根阴离子在钠盐的β笼中成功笼化。溶剂/碱的反应产物经1H - 13C CPMAS NMR和1H - MAS NMR鉴定。扫描电镜显示,在473 K的正戊醇中生长的晶体大于15 μm。
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引用次数: 10
Hydrothermal synthesis of alkali cation heulandite aluminosilicate molecular sieves 水热合成碱阳离子水镁铝硅酸盐分子筛
Pub Date : 1997-11-01 DOI: 10.1016/S0144-2449(97)00134-6
Dongyuan Zhao, Larry Kevan, Rosemarie Szostak

Heulandite molecular sieves with a Si/Al ratio of 3.2 ~ 3.8 have been synthesized hydrothermally in the presence of the alkali cations Li+; Li+, K+; and Na+, K+ at 190 °C at autogenous pressure. They have been characterized by X-ray powder diffraction and scanning electron micrographs. Heulandites can be formed in the Li+ and Na+, K+ cation systems only with ~10 wt% seed crystals. But heulandite can be synthesized in the presence of Li+, K+ cations without seed crystals. The formation of heulandite-type zeolites occurs over a narrow crystallization field and depends on the Si/Al ratio, the OH/Si ratio, and on the presence of seed crystals. Scanning electron micrographs show a thin-plate topology for the crystals. Heulandite is thermally unstable for calcination beyond 350 ~ 450 °C.

在碱离子Li+的存在下,水热合成了硅铝比为3.2 ~ 3.8的沸石分子筛;李+,K +;和Na+, K+在190℃自压下。用x射线粉末衍射和扫描电子显微图对其进行了表征。在Li+和Na+、K+阳离子体系中,只有~10 wt%的种子晶体才能形成heullandite。而在Li+、K+离子存在的情况下,可以合成不含种子晶体的菱铁矿。沸石型沸石的形成发生在一个狭窄的结晶场,取决于Si/Al比、OH - /Si比和种子晶体的存在。扫描电子显微图显示了晶体的薄板拓扑结构。沸石在350 ~ 450°C以上的煅烧时热不稳定。
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引用次数: 13
Zeolite-catalyzed chlorination of toluene by sulfuryl chloride: The role of sulfuryl chloride decomposition in chlorination 沸石催化硫酰氯对甲苯的氯化反应:硫酰氯分解在氯化反应中的作用
Pub Date : 1997-11-01 DOI: 10.1016/S0144-2449(97)00119-X
Brian W. Satterley, Michael C. Hausladen , Carl R.F. Lund

The catalytic decomposition of sulfuryl chloride was studied over dried sodium forms of zeolites ZSM-5, L, and Y. NaZSM-5 did not catalyze the decomposition, whereas NaKL and NaY did. During the chlorination of aromatic hydrocarbons using NaKL or NaY, the chlorinating agent sulfuryl chloride must compete with molecular chlorine produced by its own decomposition. The rate of reaction with molecular chlorine alone is much faster than that with sulfuryl chloride. In the presence of sulfuryl chloride, however, the rate of chlorination by molecular chlorine is greatly reduced. Both chlorinating agents use Lewis acid sites, suggesting that these sites are predominantly covered by sulfuryl chloride. Sulfuryl chloride is slightly more selective for para-chlorotoluene than is molecular chlorine. NaZSM-5 catalyzes chlorination using either molecular chlorine or sulfuryl chloride alone, but the latter reactant is not simultaneously decomposed by NaZSM-5. The decomposition may require a basic site adjacent to the Lewis acid site, and NaZSM-5 may not possess basic sites of sufficient strength.

研究了ZSM-5、L和y分子筛对硫酰氯的催化分解作用。NaZSM-5分子筛没有催化作用,而NaKL分子筛和NaY分子筛有催化作用。在使用NaKL或NaY对芳烃进行氯化时,氯化剂硫酰氯必须与其自身分解产生的氯分子相竞争。单独与氯分子的反应速度比与硫酰氯的反应速度快得多。然而,在硫酰氯存在的情况下,分子氯的氯化反应速率大大降低。两种氯化剂都使用路易斯酸位点,这表明这些位点主要被硫酰氯覆盖。硫酰氯对对氯甲苯的选择性略高于氯分子。NaZSM-5可以单独使用分子氯或硫酰氯催化氯化反应,但后者的反应物不能同时被NaZSM-5分解。分解可能需要一个与Lewis酸位点相邻的碱基位点,而NaZSM-5可能没有足够强度的碱基位点。
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引用次数: 5
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Zeolites
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