Recovery of free volume in PIM-1 membranes through alcohol vapor treatment

doi:10.1007/s11705-020-2001-2

Front. Chem. Sci. Eng.

2021, Vol. 15

Issue (4) : 872-881 https://doi.org/10.1007/s11705-020-2001-2

RESEARCH ARTICLE

Recovery of free volume in PIM-1 membranes through alcohol vapor treatment

Faiz Almansour¹, Monica Alberto¹, Rupesh S. Bhavsar², Xiaolei Fan¹, Peter M. Budd², Patricia Gorgojo¹(

)

¹. Department of Chemical Engineering and Analytical Science, School of Engineering, The University of Manchester, Manchester M13 9PL, UK
². Department of Chemistry, School of Natural Sciences, The University of Manchester, Manchester M13 9PL, UK

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Abstract

Physical aging is currently a major obstacle for the commercialization of PIM-1 membranes for gas separation applications. A well-known approach to reversing physical aging effects of PIM-1 membranes at laboratory scale is soaking them in lower alcohols, such as methanol and ethanol. However, this procedure does not seem applicable at industrial level, and other strategies must be investigated. In this work, a regeneration method with alcohol vapors (ethanol or methanol) was developed to recover permeability of aged PIM-1 membranes, in comparison with the conventional soaking-in-liquid approach. The gas permeability and separation performance, before and post the regeneration methods, were assessed using a binary mixture of CO₂ and CH₄ (1:1, v:v). Our results show that an 8-hour methanol vapor treatment was sufficient to recover the original gas permeability, reaching a CO₂ permeability>7000 barrer.

Keywords polymer of intrinsic microporosity (PIM) PIM-1 physical aging gas separation vapor-phase regeneration

Corresponding Author(s): Patricia Gorgojo

Just Accepted Date: 09 December 2020 Online First Date: 11 February 2021 Issue Date: 04 June 2021

Cite this article:

Faiz Almansour,Monica Alberto,Rupesh S. Bhavsar, et al. Recovery of free volume in PIM-1 membranes through alcohol vapor treatment[J]. Front. Chem. Sci. Eng., 2021, 15(4): 872-881.

URL:

https://academic.hep.com.cn/fcse/EN/10.1007/s11705-020-2001-2
https://academic.hep.com.cn/fcse/EN/Y2021/V15/I4/872

Tab.1 CO₂ permeability and CO₂/CH₄ selectivity of fresh and aged PIM-1 membranes

Fig.1 Schematic of the apparatus used for the alcohol treatment of PIM-1 membranes (alcohol is kept at constant temperature by means of a water bath) and components of the membrane cell in more detail.

Fig.2 (a) N₂ adsorption/desorption at 77 K for PIM-1 (square and circle symbols represent the adsorption and desorption data, respectively), and (b) TGA curves of PIM-1 powder and a PIM-1 membrane that has undergone methanol-vapor treatment.

Fig.3 SEM images of (a) the surface of an ethanol-treated PIM-1 membrane, (b) cross-section of as-cast PIM-1 membrane, and (c) cross-section of ethanol-treated membrane (PIM-1-EtOH-L(1)-V(120)-b).

Fig.4 FTIR spectrum of an as-cast PIM-1 freestanding membrane.

Fig.5 CO₂ permeability of freestanding PIM-1 membranes treated with (a) methanol and (b) ethanol vapor, and CO₂/CH₄ selectivity for the same membranes treated with (c) methanol and (d) ethanol vapor. Membranes were tested using a CO₂/CH₄ binary mixture (1:1, v:v) as feed at 25 °C under a transmembrane pressure of approximately 2 bar. Values are the average permeability and selectivity for 3 membranes for those showing error bars and errors are the calculated standard deviation. PIM-1 membranes were initially treated by soaking in liquid ethanol or liquid methanol and their CO₂/CH₄ separation performance was determined at different intervals up to ca. 120 d. The membranes represented by triangles in the plot were last treated with alcohol vapor (methanol or ethanol) after ca. 4 months; the last data points give their CO₂ permeability and selectivity at that stage. All the other points in between refer to an aged state of the membrane. Filled symbols are used for CO₂ permeability values and open symbols are used for CO₂/CH₄ selectivity. Squares (n,□) correspond to PIM-1 as-cast, circles (l,○) correspond to PIM-1 membranes soaked in liquid methanol, stars (★,☆) correspond to a PIM-1 membranes soaked in liquid ethanol, and triangles (????) correspond to membranes initially soaked in liquid alcohol, further aged and treated with vapor methanol or vapor ethanol after at least 114 d have passed.

Fig.6 Aging rate constant (b_P) as a function of the square of the effective gas diameter for PIM-1 membranes.

Fig.7 Robeson plot displaying the aging behavior of PIM-1 membranes PIM-1-MeOH-L(1)-V(120)-a and PIM-1-MeOH-L(1)-V(114)-b, which were initially treated by soaking in methanol, aged for ca. 4 months (120 and 114 d, respectively) and subsequently treated with methanol vapor, for the separation of CO₂/CH₄ (1:1, v:v) mixtures. Testing was done at 25 °C and approximately 2 bar feed pressure. The solid line corresponds to the revisited 2008 Robeson upper bound [45] and the dotted line represents the proposed 2019 upper bound [47]. The arrows show the aging process over the tested period and they point towards the most aged membranes.

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