Katholieke Universiteit Leuven

Faculty of Bioscience Engineering

Department MS
Centre for Surface Chemistry and Catalysis
Kasteelpark Arenberg 23, B-3001 Heverlee (Leuven), Belgium

LEUVEN

E-mail: ivo.vankelecom@biw.kuleuven.be; Tel.: (32) 16/32.15.94; Fax: (32) 16/32.19.98

High throughput equipment for membrane based gas separations

Asim Laeeq Khan, Subhankar Basu, Angels Cano-Odena and Ivo F.J Vankelecom*
Introduction
High throughput (HT) synthesis and screening is a powerful tool for rapid preparation and processing of a large variety of materials. The discovery process of new materials can indeed
be reduced considerably by their synthesis and performance-testing in a HT way. Such techniques have been used over the years in pharmaceutical and biotechnological research.
Membrane technology is an attractive area for HT exploration. Membranes for gas separation (GS) purposes are typically screened in a standard single gas permeation cell. Mainly due
to the more complicated, hence expensive, on-line analysis, the more interesting mixed gas selectivities are very scarce in literature. High throughput (HT) screening equipment will
allow to screen a large number of membranes in a single run. This study reports the first application of such HT in gas separation (GS). A HT gas separation (HTGS) system was
designed and fabricated, allowing on-line selectivity and permeability analysis of 16 membranes simultaneously with variable mixed gas feeds.

2. Reproducibility of the set-up

1. HTGS Set-up

The reproducibility of HTGS was evaluated by testing commercial PolyAn

(Germany) and lab-made PSf membranes. The lab made membranes were
prepared by phase inversion process using NMP/THF and water as solvents and
non-solvent respectively. The mean, maximum and the minimum values, standard
deviation, and relative standard deviation for each run were analyzed.

Fig 6. Reproducibility test of

HTGS with
PolyAn membranes.
Fig 1. Schematic diagram of the HTGS set-up

Table 1 Statistical analysis of permeability and mixed gas selectivity obtained with the HT-module, for (a) PolyAn
membrane and (b) Lab-made PSf membrane
CO2/CH4 (50/50)
Permeance (cm3 (STP)/cm2-bar-s) x 10-4

Fig 2. Various connections to the set-up

CO2/N2 (50/50)
Selectivity

Permeance (cm3 (STP)/cm2-bar-s) x 10-4

CO2

Selectivity

CO2

CH4

N2

Average

5.26

0.422

12.60

6.40

0.25

24.97

Minimum

4.25

0.32

10.11

5.95

0.25

24.00

Maximum

5.91

0.57

13.29

6.76

0.27

27.57

Standard deviation

0.439

0.0629

0.88

0.204

0.0158

1.05

Relative standard
deviation

8.35

14.90

6.95

3.19

6.14

4.19

Average

8.61

2.77

3.11

9.74

1.89

5.18

Minimum

8.19

2.43

2.85

9.5

1.8

4.77

Maximum

9.12

3.12

3.57

9.95

2.03

5.49

0.296

0.194

0.21

0.220

7.07 x 10-6

0.22

3.44

6.98

6.79

2.26

3.75

4.24

PolyAn

PSf membrane

Standard deviation
Fig 4. Sixteen membrane positions

Relative standard
deviation

Fig 3. Gas separation module

3. Reliability of the HTGS

Mixed gas permeance and selectivity experiments for the commercial PolyAn membrane at different
feed gas concentrations were compared between the HT and the single cell module. The effect of
different temperatures and pressures was also studied (Fig. 5, 6 and 7).
Both set-ups show a similar decrease in
selectivity by increase in CO2 feed concentration.

Operating pressure had no effect on CO2/CH4

selectivity for either equipment.
The decrease in selectivity with temperature was
in the same order of magnitude for HTGS as for the
conventional single cell permeation unit.

Fig 5. Effect of different feed concentration and set-up comparison

4. Conclusions
A HTGS setup was designed, aiming at a rapid and accurate
assessment of membrane performance permitting the parallel
screening of 16 membranes.
The reliability of the equipment was tested and compared with the
results obtained with a standard single cell permeation module and
those from an industrial supplier.
The reproducibility of the equipment was tested with a commercial
(PolyAn) and a lab-made PSf membrane. The HTGS results for the
commercial membrane were in excellent agreement with those tested
by conventional single gas permeation cell.
The relative standard deviation of CO2/CH4 and CO2/N2 separations
was highly encouraging proving the effectiveness of this HTGS
equipment to increase the pace of membrane development by
providing a fast quality check in industrial membrane manufacturing.

Acknowledgements

Fig 6. Effect of operating temperature

Fig 7. Effect of operating pressure

The authors wish to thank MIP-project, I.A.P.-P.A.I. and G.O.A grants,

Departament dUniversitats, Recerca i Societat de la Informaci (DURSI)
Generalitat de Catalunya, K.U.Leuven for support in the frame of the
CECAT excellence and the Flemish Government for the Methusalem
funding and the Federal Government for an IPA grant.