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Issue 45, 2011
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Facile synthesis of the DD3R zeolite: performance in the adsorptive separation of buta-1,3-diene and but-2-ene isomers

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Abstract

Small pore size and hydrophobic nature of DD3R make this material a unique zeolite with high potential in industrial separation applications. However, the reproducible rapid synthesis of this zeolite is still a problem. In this work, a thorough assessment of different synthetic methods revealed that synthesis reproducibility relies on two main pillars: the use of properly cleaned autoclave liners and the synthesis composition. High quality DD3R crystals are obtained when KOH is used as a cleaning agent, eliminating memory effects, and when KF is used in the synthesis as a mineralizing agent. The effect of fluoride addition is investigated by use of several characterization techniques (13C, 19F and 29Si MAS-NMR and (2D) 29Si–1H correlation spectra), while monitoring the temporal crystallization of DDR. 29Si–1H NMR reveals that template molecules accommodated within the cages are sticking to these 8-ring windows through their amine group. High quality DD3R crystals are applied in the adsorptive separation of buta-1,3-diene and but-2-ene isomers, one of the most energy intensive separations in chemical industry. Mixture separation experiments revealed that the 8-ring apertures of the DD3R cages are only accessible to trans-but-2-ene and buta-1,3-diene, while excluding but-1-ene and cis-but-2-ene molecules, resulting in shape-selective separation in the presence of C4 mixtures.

Graphical abstract: Facile synthesis of the DD3R zeolite: performance in the adsorptive separation of buta-1,3-diene and but-2-ene isomers

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Article information


Submitted
01 Aug 2011
Accepted
19 Sep 2011
First published
18 Oct 2011

J. Mater. Chem., 2011,21, 18386-18397
Article type
Paper

Facile synthesis of the DD3R zeolite: performance in the adsorptive separation of buta-1,3-diene and but-2-ene isomers

C. Gücüyener, J. van den Bergh, A. M. Joaristi, P. C. M. M. Magusin, E. J. M. Hensen, J. Gascon and F. Kapteijn, J. Mater. Chem., 2011, 21, 18386
DOI: 10.1039/C1JM13671B

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