Xylene Permeation Transport through Composite Ba-ZSM-5/SS Tubular
Membranes: Modeling the Steady-State Permeation
Ana M. Tarditi, Eduardo A. Lombardo, and Adolfo M. Avila*
Instituto de InVestigaciones en Cata´ lisis y Petroquı ´mica (FIQ, UNL-CONICET), Santiago del Estero 2829,
3000 Santa Fe, Argentina
Steady-state single-component and ternary mixture xylene permeation fluxes through Ba-ZSM-5/SS composite
membranes were studied, as a function of temperature and pressure. The single p-xylene flux has a weak
maximum, relative to temperature (100-400 °C). The flux magnitude and its maximum location are dependent
on the extent of Ba-exchange. The o- and m-xylene fluxes steadily increase with temperature. The single
permeation behavior is well-described by a model based on the contribution of different transport
mechanisms: Knudsen flux, surface diffusion, and activated gas translation diffusion. The comparisons between
either the mixture permeation results or the pressure effect experiments and the simulated data reflect the
existing adsorbate-framework interactions that are not easily contemplated by a macroscopic model.
1. Introduction
The dimensions of zeolite pores are uniform and close to the
molecular dimensions of small hydrocarbons. Therefore, highly
selective separations can be achieved based on the molecular
sieving and the adsorption-diffusion properties of zeolites.
Therefore, zeolite membranes are capable of separating mixtures
that are difficult or impossible to separate via other means (e.g.,
xylene isomers by distillation,
1,2
azeotropic mixtures by per-
vaporation
3
). Molecules diffuse through the pores via various
mechanisms. Zeolites can be shape-selective; however, when
the interactions between the surface and the diffusing molecules
are important, adsorption or surface diffusion can dominate the
transport. It is well-established in the literature that p-xylene
adsorbs selectively on MFI from mixtures of the three isomers.
4
Therefore, not only the molecular sieving ability of the zeolites
but also their adsorption properties are important in the
separation of the xylene isomers. In fact, it has been reported
that the p-xylene flux presents a maximum, as a function of
temperature. The interplay between adsorption and diffusion
may be responsible for this maximum.
2,5
One of the most common assumptions, and a very critical
one, regarding most zeolite membrane modeling is that the
membrane is defect-free. However, most composite membranes
are not perfect. Permeation then occurs through the zeolitic
channels and nonzeolitic pores (by Knudsen diffusion and/or
viscous flow). The separation performance of zeolite membranes
is significantly dependent on the membrane quality, because
the intercrystalline space and pinholes reduce the membrane
selectivity. The quantification of these extra-zeolitic channels
is then basic information that is needed to model the transport
mechanism through zeolite membranes.
6
Thus, with the purpose
of characterizing MFI-zeolite membranes, the permeation
behavior of single xylene isomers and their mixtures have been
studied, as a function of temperature, and, in fewer cases, the
effect of pressure across the membrane also has been explored.
5,7
Moreover, note that there are no studies in the literature reporting
the xylene ternary mixture behavior through MFI-zeolite
membranes based on macroscopic gas transport models. This
is important, to understand not only the transport behavior but
also the performance of the composites. In addition, a model
description would assist in the comparison of experimental data
obtained using membranes with different characteristics and
under varying operational conditions.
The mass transport of different molecules within the zeolite
channels is not only influenced by their adsorption and diffusion
characteristics but also by other factors, such as the pore
diameters, the structure of the pore walls, the interactions
between the surface atoms and the diffusing molecules, the
configuration of the diffusing molecules, the way the channels
are interconnected, and adsorbate-adsorbate interactions. The
quantitative prediction of diffusion rates inside the zeolites with
modeling techniques is often difficult to relate to the aforemen-
tioned properties and the microscopic mechanisms. Furthermore,
the large discrepancies that often exist between diffusivities
determined through different experimental techniques
8,9
con-
tribute to the difficulty of diffusion prediction.
It is generally accepted that the generalized Maxwell-Stefan
formulation
10
offers the most convenient and the nearest
quantitative prediction of multicomponent transport through
zeolite membranes.
11
The strength of this model lies in the fact
that it intrinsically encompasses intracrystalline diffusion phe-
nomena as well as adsorption processes, facilitating the predic-
tion of multicomponent transport, based on pure component
Maxwell-Stefan diffusivities and mixture adsorption iso-
therms.
12
The objective of this study is to describe the fluxes of single
xylenes and their mixtures through Ba-ZSM-5/SS composites,
according to a steady-state permeation model that is based on
the participation of different parallel fluxes, thus contributing
to elucidate the xylene transport mechanism. To this end, the
effect of temperature and pressure gradients across the mem-
brane on the xylene permeation was studied. With this purpose,
the membrane was synthesized by secondary growth on the outer
surface of the tubular support. Its thermal stability up to 400
°C was carefully investigated, to ensure the validity of the data
obtained.
2. Experimental Section
2.1. Membrane Preparation. The tubular composite mem-
brane used in this study consisted of an MFI-zeolite layer on a
stainless steel tubular support (Mott Metalurgical, 10 mm outer
* To whom correspondence should be addressed. Tel.: +54 342
4536861. E-mail address: aavila@fiqus.unl.edu.ar.
2377 Ind. Eng. Chem. Res. 2008, 47, 2377-2385
10.1021/ie071296l CCC: $40.75 © 2008 American Chemical Society
Published on Web 02/29/2008