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Frontiers of Chemical Science and Engineering

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Front. Chem. Sci. Eng.    2020, Vol. 14 Issue (2) : 127-142    https://doi.org/10.1007/s11705-019-1883-3
REVIEW ARTICLE
Layer-like FAU-type zeolites: A comparative view on different preparation routes
Bastian Reiprich, Tobias Weissenberger, Wilhelm Schwieger, Alexandra Inayat()
Institute of Chemical Reaction Engineering, Friedrich-Alexander University Erlangen-Nürnberg, Erlangen 91058, Germany
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Abstract

The creation of intergrown layer-like zeolite crystals is one route to form hierarchical zeolites. Faujasite-type (FAU-type) zeolites are among the industrially most important zeolites and the implementation of hierarchical porosity is a promising way to optimise their catalytic and adsorptive performance. After a short general survey into routes for the preparation of hierarchical pore systems in FAU, we will review the currently existing strategies for the synthesis of FAU with layer-like morphology. Those strategies are mainly based on the presence of morphology modifying agents in the synthesis mixture. However, a very recent approach is the synthesis of layer-like FAU-type zeolite crystals assembled in an intergrown manner in the absence of such additives, just by finely adjusting the crystallization temperature. This additive-free preparation route for layer-like FAU, which appears very attractive from an ecological as well as economic point of view, is highlighted in this review. Concluding, a comparison, including powder X-ray diffraction, scanning and transmission electron microscopy, nitrogen physisorption and elemental analysis, between conventional FAU and three layer-like FAU obtained by different synthesis routes was carried out to show the structural, morphological and textural differences and similarities of these materials.
Keywords FAU      hierarchical zeolite      layer-like morphology     
Corresponding Author(s): Alexandra Inayat   
Just Accepted Date: 21 November 2019   Online First Date: 09 January 2020    Issue Date: 24 March 2020
 Cite this article:   
Bastian Reiprich,Tobias Weissenberger,Wilhelm Schwieger, et al. Layer-like FAU-type zeolites: A comparative view on different preparation routes[J]. Front. Chem. Sci. Eng., 2020, 14(2): 127-142.
 URL:  
https://academic.hep.com.cn/fcse/EN/10.1007/s11705-019-1883-3
https://academic.hep.com.cn/fcse/EN/Y2020/V14/I2/127
Fig.1  Schematic overview of proposed classification terms for zeolites with 2D-morphology.
Fig.2  Scanning electron microscopy (SEM) images of a conventional FAU-type and a conventional EMT-type zeolite. Reprinted with permission from Ref. [60]. Copyright (2001) American Chemical Society.
Fig.3  SEM images of conventional FAU crystals (top-left) and layer-like FAU synthesised in the presence of organosilanes CH3–(CH2)n–N+(CH3)2–(CH3)3–Si(OCH3)3 with different alkyl chain lengths (n = 3, 7, 11, 15 and 17). Reprinted with permission of Royal Society of Chemistry, from Ref. [73], Copyright (2015); permission conveyed through Copyright Clearance Center, Inc.
Fig.4  SEM images of examples of layer-like FAU synthesised by additive-free preparation routes from recent literature. (a) Reprinted with permission from Ref. [84]. Copyright (2016) American Chemical Society. (b) Reprinted with permission from Ref. [85]. Published by The Royal Society of Chemistry. (c) Reprinted by permission from Springer Nature, Science China Materials, Ref. [86]. Copyright (2018). (d) Reprinted with permission from Ref. [87]. Copyright (2019) American Chemical Society. (e) Reprinted with permission of Royal Society of Chemistry, from Ref. [88], Copyright (2018); permission conveyed through Copyright Clearance Center, Inc. (f) Reprinted with permission of Royal Society of Chemistry, from Ref. [89], Copyright (2019); permission conveyed through Copyright Clearance Center, Inc.
Synthesis gel composition
Al2O3 : Na2O : SiO2 : H2O		 Temp. /°C Time/ h FAU-type Surface area /(m2?g−1) Micropore volume/ (cm3?g−1) Mesopore volume/ (cm3?g−1) Ref.
1 : 9.6 :14.4 : 175.3–334.2 25
38
60		 24
24
48		 Y 404–757 0.14–0.30 0.16–0.19 a) [92]
Gel 1 | 1 : 1 : 10 : 140
Gel 2 | 1: 5.3 : 2.2 : 122 : 1.8 K2O
Gel∑ | 1 : 3.7 : 5.1 : 128.8 : 1.1 K2O		 G1: RT
G2: RT
G∑: 60		 48
24
72		 X 652 0.23 n.a. [90]
1 : 4.9–12 : 3.6–14 : 214–300 Ice bath
RT
60		 1
24
n.a.		 X, Y n.a. n.a. n.a. [84]
1 : 8.3 : 6.4 : 194.6–290.3 RT
100
50
100		 4
1
96
2		 X 756 0.24 n.a. [66]
1 : 31.3 : 27.5 : 531.3 RT
65		 0.33
95		 X n.a. n.a. n.a. [91]
1 : 14.4 : 9.8 : 590 RT
75		 20
16		 Y 687 0.24 0.14–0.15 [85]
1 : 13.6–36 : 3–8 : 545,5–1440 Ice bath
60		 5
24		 X, Y 544 0.26 0.13 a) [86]
1 : 10.7–18.3 : 10.4–22.6 : 815 RT
70		 2
24		 Y 729–866 0.21–0.33 0.25–0.58 a) [87]
n.a. n.a.
70		 n.a.
48		 X 541 0.26 0.11 a) [88]
1 : 4–7.3 : 3.5 : 180–300 Ice bath
RT
60		 1
24
48		 X 759–781 0.27–0.28 n.a. [89]
1 : 4 : 3 : 150–200 RT
50		 24
72		 X 445–708 0.17–0.26 0.07–0.20 This Work
Tab.1  Synthesis parameters and nitrogen physisorption analysis results for layer-like FAU zeolites prepared by the additive-free preparation route
Fig.5  Temperature profiles of additive-free syntheses of layer-like FAU, both X and Y, and for the synthesis of conventional zeolite X (reference), the different colours refer to the number of temperature steps. The dashed lines are an assumed temperature (see [88]) and duration (see [84]) due to a lack of information in the literature.
Fig.6  Comparison of different synthesis compositions of layer-like and conventional FAU, respectively. (a) H2O/Si (green), OH−/Si (blue) and Si/Al (red) molar ratios of synthesis gel compositions and resulting Si/Al molar ratios (black) of the zeolite products; (b) Ternary diagramn (Al2O3-SiO2-Na2O) with one selected synthesis gel composition of each work in comparison with the IZA verified syntheses for zeolite X and Y. The dashed areas examplify synthesis gel compositions for zeolite Y, zeolite X and zeolite A, respectively [96].
Fig.7  SEM images and correlation of H2O/Al2O3 molar ratio of the synthesis gel and particle size and 2D-crystal thickness of layer-like zeolite X from this work. The synthesis composition of these layer-like FAU was Al2O3 : Na2O : SiO2 : H2O= 1 : 4 : 4 : 150–200.
Itam Synthesis composition Aging Crystallisation
Al2O3 Na2O SiO2 H2O Additive
X-standard 1 4 3 180 – 1 d @ 25°C 3 d @ 75°C
X-TPOAC 1 3.5 3 180 0.06 TPOAC 1 d @ 25°C 3 d @ 75°C
X-Li2CO3 1 3.7 3 180 0.60 Li2CO3 1 d @ 25°C 2 d @ 75°C
X-additive-free 1 4 3 180 – 1 d @ 25°C 3 d @ 50°C
Tab.2  Molar synthesis composition and conditions for conventional FAU and three layer-like FAU
Fig.8  SEM images of a conventional zeolite X (X-standard) and three layer-like FAU, synthesised by different preparation routes.
Fig.9  (a) XRD patterns; (b) nitrogen physisorption isotherms; (c) mesopore diameter distributions (DFT) of a conventional (X-standard) and three layer-like FAU (X-TPOAC, X-Li2CO3 and X-additive-free).
Property (method) X-standard X-TPOAC X-Li2CO3 X-additive-free
Surface area (BET)/(m2?g−1) 889 452 789 708
Micropore vol. (DFT)/(cm3?g−1) 0.36 0.15 0.31 0.26
Mesopore vol. (DFT)/(cm3?g−1) 0.06 0.20 0.12 0.14
Mesopore diameter (DFT)/nm – 6–11 3–8 3–8
Si/Al molar ratio (ICP-OES) 1.39 1.43 1.37 1.38
Particle diameter (SEM)/µm 1.9 7.5 2.3 1.7
Sheet thickness (SEM)/nm – 50 65 95
Tab.3  Textural properties from nitrogen physisorption, chemical composition (Si/Al) from ICP-OES and morphological properties from SEM analysis
Fig.10  TEM images with two magnifications of three layer-like FAU, synthesised by different methods.
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