AUTONOMOUS UNIVERSITY OF COAHUILA

SCHOOL OF CHEMISTRY
Design of Experiments

Case Study: Optimization of a Hybrid Distillation-Vapor Permeation Process on

Propylene/Propane System Using Response Surface Methodology

The rising demand for propylene and propane makes the recovery a widespread concern.
Because propylene's relative volatility to propane is close to 1, conventional distillation
necessitates the column as high as 90 m and a reflux ratio larger than 10, resulting in
high-energy consumption and high cost. An energy-efficient distillation-membrane
hybrid process has developed rapidly in recent years. Compared with single-column
separation, the hybrid distillation-membrane process could decrease the number of stages
and reflux ratio of distillation, so it is a potential separation process for propylene and
propane mixtures. Studies of different separation problems have shown that significant
reductions in operating costs (often in the order of 20-50%) may be obtained using the
hybrid distillation-membrane process (Pettersen et al., 1996).

The response surface methodology (RSM) is a mathematical statistics method

dealing with designing experiments and developing predictive models for simulation
and optimization that characterize the system's responses. In this study, RSM was
used to observe the interaction of input variables where all factors were varied
simultaneously over a set of experimental runs. RSM is widely used in chemical
engineering, biology and other science and technology fields (VanHoof et al., 2004;
Ravikumar et al., 2005).

This study used RSM to achieve the optimal process conditions of a hybrid distillation-
vapor permeation on the propylene/propane system. The process is shown in Figure 1.

Experience has shown that this process is affected by different parameters such as
Distillate pressure (kPa), Reflux ratio, Membrane Pout (kPa), Side-draw flow (kmol/h),
Distillate rate (kmol/h), Feed temperature (ºC), Residue column tray, Side-draw column
tray. Previous batches demonstrated that the most critical factors affecting the process
are: Reflux ratio (F1), column side-draw rate (F2) and distillate rate (F3). Further batches
were carried out to analyze these factors at different levels, presented in Table 1.

Table 1. Levels and factors analyzed for the distillation-vapor permeation.

Level
Factor
Low Intermediate High
Reflux ratio (F1) 8.5 8.75 9
Column side-draw rate (F2, kmol/h) 2900 3025 3150
Distillate rate (F3, kmol/h) 755 765 775

The target response to optimize is the composite indicator, a combination of three

independent responses: propylene purity overhead, propane purity bottom, and total cost.
The objective is to minimize the composite indicator. The results are presented in
Table 2.

Please analyze the provided data and determine the following:

 Which factors influence the response and what types of effects are significant?
 What are the factors' levels likely to provide the optimum?
 What would be the response at optimum levels?

References

Pettersen Torbjern, Andrew Argo, Richard D. Noble, Carl A. Koval, 1996, Design of
combined membrane and distillation processes. Seperation Technology, 06, 175-187.

Ravikumar K., K. Pakshirajan, T. Swaminathan, K. Balu, 2005, Optimization of batch

process parameters using response surface methodology for dye removal by a novel
adsorbent, Chemical Engineering Journal, 105, 131-138.

VanHoof Veerle, Liesbet Van den Abeele, Anita Buekenhoudt, Chris Dotremont, Roger
Leysen, 2004, Economic comparison between azeotropic distillation and different hybrid
systems combining distillation with pervaporation for the dehydration of isopropanol.
Separation and Purification Technology, 37, 33-49.
Table 2. Obtained results from 27 batches evaluated at different conditions.

Factors Composite indicator

Replicate Replicate Replicate
F1 F2 F3
1 2 3
8.50 2900 755 30.05 32.91 33.78
8.75 2900 755 43.12 44.88 43.59
9.00 2900 755 53.31 53.45 48.40
8.50 3025 755 38.90 37.56 38.12
8.75 3025 755 48.13 49.61 48.02
9.00 3025 755 57.95 58.26 52.92
8.50 3150 755 32.18 38.63 38.62
8.75 3150 755 50.81 50.76 48.61
9.00 3150 755 57.89 59.49 53.60
8.50 2900 765 1.20 2.20 1.17
8.75 2900 765 20.42 19.76 16.58
9.00 2900 765 32.15 33.92 26.99
8.50 3025 765 7.54 8.83 7.50
8.75 3025 765 26.90 26.47 23.00
9.00 3025 765 38.69 40.71 33.50
8.50 3150 765 11.25 11.88 9.99
8.75 3150 765 29.56 29.60 25.58
9.00 3150 765 40.13 43.92 36.17
8.50 2900 775 17.90 18.01 18.92
8.75 2900 775 40.90 41.16 39.93
9.00 2900 775 67.12 60.91 55.94
8.50 3025 775 29.30 26.62 27.24
8.75 3025 775 43.16 49.85 48.34
9.00 3025 775 69.12 69.68 64.44
8.50 3150 775 30.15 31.65 31.72
8.75 3150 775 53.21 54.96 52.91
9.00 3150 775 76.89 74.87 69.10