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Catalysis Today 227 (2014) 9–14

Contents lists available at ScienceDirect

Catalysis Today

j our na l ho me page: www.elsev ier .com/ locate /ca t tod

omprehensive system integrating 3D and 2D zeolite structures withecent new types of layered geometries

ieslaw J. Rotha,b,∗, Barbara Gila, Bartosz Marszaleka

Faculty of Chemistry, Jagiellonian University, Ingardena 3, 30-060 Krakow, PolandJ. Heyrovsky Institute of Physical Chemistry, Academy of Sciences of Czech Republic, v.v.i., Dolejskova 3, 182 23 Prague 8, Czech Republic

r t i c l e i n f o

rticle history:eceived 1 July 2013eceived in revised form7 September 2013ccepted 23 September 2013vailable online 23 October 2013

a b s t r a c t

Zeolites have been recognized as 3D framework materials but are now known to also exist in various 2Dlayered forms with sheets of one unit cell or smaller thickness. We propose a classification system andan expanded concept of zeolite structures integrating various 2D and the traditional 3D forms. Zeolitetopology is defined as the primary structure. Various kinds of zeolite mono-layer assemblies are secondarystructures. Based on the literature 15 distinct layered forms are recognized. A detailed table is generated

eywords:D zeolitesayered zeolite formWW familyFI family

eolite framework

showing layered forms that have been reported for various topologies. It provides a classification tool forrecognition and verification of known materials. It may be used to identify unknown ones of particularinterest to pursue.

© 2013 Elsevier B.V. All rights reserved.

. Introduction

Zeolites have been studied and developed for practical appli-ations as valuable catalysts and sorbents [1–3]. They are widelysed in chemical and petroleum industries [4–7]. Zeolites areistinguished by having a framework structure with microporesf molecular dimensions that can accommodate internal activeenters for catalysis and ion exchange [8]. Discovery of novelrameworks and expanding knowledge about zeolite structures ineneral is the primary focus of interest and driver of innovation inhis area [9]. This is understandable because framework structureetermines usefulness through the size, shape and connectivity of

ts internal pores. Other important properties, especially composi-ion like Si/Al ratio and stability, are also to large extent dependentn the framework. New frameworks, especially with larger poresnd multi-dimensional channels, are desired to expand zeolitepplications by enabling processing of large molecules.

In formal terms zeolites are defined as 4-connected tetrahedralrameworks [10,11]. It means they are constructed from TO4

etrahedra, T = Si or suitable heteroatom like Al, Ti, etc., whichhare corners but each one with a different neighbor (making it4-connected’). Frameworks without microporosity are formally

∗ Corresponding author at: Faculty of Chemistry, Jagiellonian University, Ingar-ena 3, 30-060 Krakow, Poland. Tel.: +48 6632016/+420 26605 3795.

E-mail address: wies.roth@gmail.com (W.J. Roth).

920-5861/$ – see front matter © 2013 Elsevier B.V. All rights reserved.ttp://dx.doi.org/10.1016/j.cattod.2013.09.032

excluded by applying cutoff limit based on the number of tetrahe-dra per unit volume (19–20/10003 A) [11]. While the theoreticalnumber of frameworks seems to be infinite, 213 have been formallyrecognized so far. The IZA Structure Commission has the task ofmaintaining the database of known zeolite structures, recognizingand approving new ones, and assigning 3 letter Framework TypeCode [6,11]. There is no comprehensive system of classificationcovering all zeolite frameworks.

Zeolites have been historically viewed as 3D materials. Theirstructures/frameworks were considered to be extended in all 3directions, covalently bonded and 4-connected throughout, exceptfor possible defects. This was the state in which they have beenused in practice and formed during synthesis. Some zeolite frame-works, starting with MWW in 1990s [12,13], were found to formvia precursors made up of thin layers with thickness of the orderof one unit cell. It was also possible to expand these precursorsand obtain other structures in terms of layer spatial packing andinterlayer bonding [14]. The number and diversity of these lay-ered zeolite structures have been constantly increasing [15]. Weshall refer to them as layered or 2D zeolite forms [16,17]. They aresimilar to classical 2D solids, but with zeolite layers. This is signif-icant because layered solids such as clays have been extensivelystudied and used as catalysts and sorbents [18]. In contrast to zeo-

lites they are lacking strong acid sites and layer stability. On theother hand, 2D solids in general could produce various structuralmodifications, especially expanded and more open, by intercala-tion, exfoliation, pillaring, etc. [19]. The discovery of layered zeolite

10 W.J. Roth et al. / Catalysis Today 227 (2014) 9–14

F tandari

fsomtMc

(lifiFlbbbad

oovsiwisptsswpocdpw2f

ig. 1. Modified layered zeolite materials produced from layered precursors. The ss not shown.

orms enabled similar procedures for zeolites in contrast to theirtandard 3D forms, which could not be structurally modified with-ut some kind of degradation. Some of the new layered zeoliteaterials showed promising catalytic performance in comparison

o parent zeolites as exemplified by pillared MCM-36 [20] andCM-56 [21]. Delaminated zeolites were reported as selective acid

atalysts with enhanced accessibility for bulky molecules [22].This new area has been expanding in 2 general directions:

i) new layered zeolite forms were being discovered and (ii)ayered precursors and other 2D structures were identified forncreasing number of frameworks [23]. Particularly notable wasnding layered derivatives of well established frameworks likeER [24], SOD [25] and recently MFI [26]. This suggested thatayered precursors may be common among zeolite frameworksut have not been found yet, i.e. other known frameworks cane obtained as layered structures. Lamellar MFI was obtainedy using a specially prepared template, which could make thepproach quite general and applicable to other frameworks byesign [26–28].

Before the emergence of 2D zeolite forms the general problemf zeolite structure was relatively simple to handle – there was onlyne category of materials – 3D frameworks. They included the con-entional fully connected ones with Q4 T-atoms only, along withome interrupted frameworks designated with a hyphen preced-ng the three letter code and by intergrown frameworks designated

ith an asterisk preceding the three letter code. To address thencreasing number and variety of layered zeolite materials in aystematic way an expanded concept of zeolite structures wasroposed [23]. Zeolite topologies were considered as primary struc-ures while various layered forms were denoted as secondarytructures. This led to the classification in the form of a table, a ‘2Dystem’. The initial illustration presented only the MWW familyith seven layered forms known (as-synthesized and uncalcinedairs) [23]. It was obvious that a similar list could be made withther frameworks and this is one of the goals of this article espe-ially since new 2D zeolites have been described. The number ofifferent layered zeolite forms has doubled compared to the first

ublication and they are slowly spreading among various frame-orks. The objective of this publication is to present all known

D zeolite materials in the previously proposed 2D format for allrameworks.

d zeolite framework is included at top left; the presence of templates in the pores

2. Discussion

So far no uniform approach has been adopted in the literature torecognize, name and keep track of various layered zeolite materials.As the first step we will try to identify and make the list of varioustypes based on their unique structure and properties. It will includedefining new forms based on materials reported in the literature.Some cases may be found questionable but they are subject to revi-sion as more examples are found in the future. The list will be madeby considering the methods of generating layered zeolite forms.There are basically 2 ways: direct synthesis or modification of lay-ered precursors. The precursors are typically obtained by directsynthesis but there is one special case of making the precursor,IPC-1P, by 3D to 2D transformation from another framework, UTL[29]. It has resulted in modifications similar to other precursors [30]but was also the source of remarkable and novel chemistry [31].We will begin with known modifications of the layered precursor,which are shown in Fig. 1.

2.1. Layered forms obtained by precursor modification

In simple terms the species shown in Fig. 1 represent differentways in which the layers, as building blocks, can be assembled inmore or less regular fashion. It includes only those already knownand more possibilities are expected to be identified in the future.MWW framework was the first source of most of the examplesbut any framework with layered precursor should allow thesemodifications. There are 3 main transformations for the precursorin addition to the calcination that produces 3D zeolite frame-work: detemplation by chemical extraction [32,33], stabilizationproducing Interlamellar Expanded Zeolites (IEZ) [34,35] and inter-calation/swelling with organic molecules [13,14,36,37]. The latterenables further modification producing pillared [14,36], delami-nated [22,38] and colloidal zeolites [39]. Some of these treatmentshave been applied to other layered materials before zeolites [40].Typically, when adopted for layered zeolite precursors, these pro-cedures required more effort and increased severity. It remains to

be seen whether this is a problem inherent to layered zeolites orjust some typical difficulties one encounters at the beginning ofthe investigation. Detailed description and discussion of individualcases is presented in Section 2.3.

W.J. Roth et al. / Catalysis To

Fig. 2. Direct synthesis routes to 2D zeolites.

2

mae[iiitmpoidmutftfoloovtp

zeolite materials were reported and indicating possible ones to syn-

.2. Layered forms obtained by direct synthesis

Layered zeolite materials obtained by direct synthesis comple-ent those that can be generated by precursor modification. They

re shown in Fig. 2 which also shows the unique case of the lay-red precursor, IPC-1P. The latter is formally a detemplated species30]. It does not contribute another new layered zeolite form but isncluded for completeness to illustrate synthetic pathways to mod-fiable materials. Also included in Fig. 2 are 3D frameworks as anntegral part and to show all zeolite forms together. The presen-ation of MFI and MWW as giving different species is temporary,

ainly because for the time being only the existing materials areresented. A future ‘cross-over’ and discovery of MWW forms anal-gous to the MFI ones, and vice versa is expected. As describedn earlier publications [16,41], framework MWW can produce byirect synthesis 4 different types of layer packing (‘as-synthesizedaterials’), including the standard 3D framework. This remains

nprecedented but as already emphasized on several occasionshere are no fundamental reasons to this exclusiveness. Otherrameworks are expected to behave similarly and it is just a mat-er of finding appropriate synthesis procedures. Of course, severalrameworks already show 2 forms, i.e. 3D framework and therdered layered precursor. The formation of disordered (multi)-ayered precursor is related to nature of the template in the casef MWW [42–44]. For the frameworks already showing formationf layered precursors (ordered) the disordered one should be quite

iable. In fact one can produce such examples if not by direct syn-hesis then by post-synthesis modification, e.g. via de-templatedrecursor. It is also possible that disordered precursors have been

day 227 (2014) 9–14 11

already made, even reported in the literature, but went unnoticedas disordered materials are more difficult to identify. MCM-56 asthe single layer disordered material may be particularly importantas the representative of delaminated zeolites [45]. The fact thatit is obtained by direct synthesis makes it particularly attractivein comparison with delaminated zeolites, which are prepared viaswelling and additional processing steps. The details of MCM-56formation remain obscure but if elucidated may help in synthesisof related materials with other frameworks. A material designatedERS-12 [46] (pointed out during review) and composed of ferrieritelayers may represent yet another new 2D zeolite type worth consid-ering. It shows partial disorder after calcination, which may bequite separate from presently recognized ordered and disorderedprecursors.

MFI provides 3 additional layered forms obtained by directsynthesis: surfactant-templated multi- and mono-layer precursors[26,28] and self-pillared [47]. The 1st two are somewhat similar toMWW materials: layered precursor (ordered or dis-ordered) andmono-layer (MCM-56). On the other hand they appear to showsignificant differences and are therefore considered as separatedistinct forms. In the MFI ‘layered precursors’ the template is par-tially encapsulated in the layers and cannot be removed exceptby degradation (calcination). Furthermore, some of the precur-sor modifications shown in Fig. 1 appear not possible with theseMFI structures by simple treatments, e.g. detemplation and stabi-lization. The uni-layer MFI is an intergrowth and in contrast (asfar as we know) to MCM-56 cannot be expanded, e.g. swollen.The third unique MFI material, i.e. self-pillared, is linked to theMFI ability to produce intergrowths with another framework MEL[47]. While this appears to rule out similar self-pillared types forother frameworks it may be premature to consider them a prioriimpossible.

As discussed, the possibility of obtaining layered precursor fromother frameworks, via top down 3D to 2D transformation, is rep-resented by PCR precursor IPC-1P [29]. It is obtained from zeoliteUTL [48,49] by selective degradation. It is anticipated that IPC-1Pand PCR may be also obtained in the future by the conventionaldirect synthesis. Nonetheless, the decomposition of a 3D frame-work to layered zeolite is a very significant and valuable syntheticapproach. It may enable the discovery of additional new layeredprecursors by design and ahead of discovery by direct synthesis,which is typically a matter of serendipity.

2.3. Integrated scheme of 3D and 2D zeolite structures

The above discussion of known directly synthesized and mod-ified materials results in recognition of 15 distinct layered zeoliteforms (see Fig. 3). Each case corresponds to the uncalcined/calcinedpair. One or the other species in the pair may be of little significance,e.g. calcined forms of swollen precursor or organic pillared MWW,but must be considered as part of complete system. From the struc-ture point of view some materials can be equivalent but method ofobtaining is additional distinguishing factor.

The integrated scheme in Fig. 3 shows frameworks and the lay-ered materials that have been reported for them. The entries arebased on literature reports without attempt to verify independentlythe existence of a particular species. In most cases the structureswere confirmed by the authors based on detailed analysis of XRDpeak positions and sometimes included complete refinement. Noseparate verification was undertaken for this paper. XRD patternsfor MWW layered materials are presented in Fig. 4 as illustration.

The scheme shown in Fig. 3 is very useful in showing what 2D

thesize. The area of 2D zeolites continues to expand and is expectedto do so in both directions – more frameworks showing 2D formsand increasing variety of the latter. It was postulated that many

12 W.J. Roth et al. / Catalysis Today 227 (2014) 9–14

F le exac ence n

mc1bsTolnnbefsc

ig. 3. Summary of reported 2D zeolite forms represented by the 1st and/or notabolor of the box (visible in the on-line version) and underline of the name and refer

ore, maybe all, topologies can form monolayers [15]. So far nolear cut examples are available for zeolites with pores bigger than0-ring. We do not see the reason for this to be the limit. Layers cane clearly distinguished in 12-ring zeolites like FAU and beta, whichhould probably be the most significant to pursue in this regard.he scheme also implies that there should be effort toward fillingf gaps by synthesizing materials expected but not made yet. In theong run this will have to be carried out selectively because of theumber of potential materials and the amount of labor involved. Forow we are still in the stage of discovery and any addition shoulde viewed as valuable. In the future the criterion for selective pref-

rential approach may be the potential practical use or particularundamental significance or insight. Overall, since any such con-iderations are quite nebulous it is hard to suggest any particularourse to follow at this point.

mples with corresponding references (separate from the main references). Yellowumber designate materials obtained by direct synthesis, gray – all others.

Regarding the scheme in Fig. 3 we will now discuss selectedpoints of particular interest. The materials such as swollen, pillaredand stabilized precursors have been extensively covered earlier andwe will not dwell on them [18,40]. Among the materials listed inFig. 3 the top pair: zeolite obtained by 3D and its layered precursor,usually ordered, and are the most prominent so far. Interestingly,5 frameworks have been obtained only via layered precursor while2 frameworks do not have corresponding 2D precursor (excludingsurfactant templated one for MFI). These are certainly the gaps onewould like to see filled. CAS zeolite is interesting in that no pre-cursor is known but was postulated to form in parts of the crystals

upon calcination from NSI precursor EU-19 [50] (it has NSI layersbut no corresponding zeolite is formed upon calcination [51,52]).

Special attention is warranted for several MWW and MFI mate-rials prepared by direct synthesis as they are the only example

W.J. Roth et al. / Catalysis To

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[31] W.J. Roth, P. Nachtigall, R.E. Morris, P.S. Wheatley, V.R. Seymour, S.E. Ashbrook,

ig. 4. Representative XRD patterns for layered MWW materials in either calcinedr uncalcined form.

n their class. Some, like MCM-56 and self-pillared MFI, seem inosition to compete immediately with their standard counterparts,hich are used commercially [53]. The reason is because a rela-

ively uncomplicated template and straightforward synthesis aresed to prepare them. Regarding the whole group of these 5 MWWnd MFI materials it would be highly desirable to obtain additionalxamples with other frameworks.

Some discussion is in order concerning the detemplated species.ayered zeolite precursors are usually obtained as 3D orderedtructures comprising zeolite mono-layers with silanols on theurface and separated by template molecules [54–56]. Their cal-ination typically causes contraction and congruent fusion of theilanols producing continuous zeolite framework similar to the onebtained by direct synthesis. The template can be usually removedy extraction, often with an acid [32]. In some cases it was reporteds pre-requisite to enable swelling [37]. Detemplated precursorsan retain 3D ordered structure like MCM-39 and MCM-69 but inome cases there are indications of lateral disorder (IPC-1P, MCM-2P). Calcination of the detemplated precursors often results indditional disorder indicated by lowering of intensity and broad-ning of reflections in XRD. Sometimes the interlayer distancestacking repeat) becomes shorter than in the corresponding zeo-ite itself [30,37]. We propose to designate them with a prefix ‘Sub’nd in general denote as ‘Sub-zeolite’. We know little about suchtructures but it is possible that they result from positional mis-atch between silanols from opposing layers [57]. If the standard

i O Si vertical bridge is not formed the silanols may collapse ontohe adjacent layers and produce even shorter separation then in theeolite. MCM-22P treated with acid resulting in ‘MCM-56 analogue’

33,58] may be such case but we have no data concerning exactalues of c-unit cell. It is also possible that transformation of EU-1959], having the same layers as NSI zeolite precursor NU-6(1), to

[

day 227 (2014) 9–14 13

EU-20 [51] (structure unknown but apparently not NSI) representsformation of Sub-zeolite material, i.e. Sub-NSI.

3. Conclusions

Zeolite frameworks can grow as layers and produce variousstructures based on their different arrangement in space and inter-layer bonding. Based on the literature 15 different types have beenidentified. A 2D scheme has been proposed to integrate 3D zeoliteframeworks and various 2D zeolite structures. It can be used as adatabase and to identify prospective materials for synthesis and ofparticular interest.

Acknowledgements

This work was financed with the funds from the NarodoweCentrum Nauki provided on the basis of decision number DEC-2011/03/B/ST5/01551; WJR also acknowledges the Czech ScienceFoundation (P106/12/0189) for partial support of this research.

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