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Process dynamics of starch-based microcellular foams produced by supercritical uid extrusion. II: Numerical simulation and experimental evaluation
S.H. Alavia,*, S.S.H. Rizvib, P Harriottc
a
Department of Grain Science and Industry, Kansas State University, 201 Shellenberger Hall, Manhattan, KS 66506, USA b Institute of Food Science, Cornell University, 151 Stocking Hall, Ithaca, NY 14853, USA c School of Chemical Engineering, Cornell University, 248 Olin Hall, Ithaca, NY 14853, USA Received 14 October 2001; accepted 22 May 2002
Abstract This paper presents the numerical simulation results for the process dynamics model for SCFX processing and post-extrusion drying developed in Part I. The SCFX model was written in Visual Basic, and experimental data for pregelatinized corn and potato starch based SCFX extrudates with 47% whey protein concentrate were used for validation. Predicted bubble radius (R) was 50220 mm, expansion ratio (ER) 411 and open cell fraction (fo) 0.050.27, as the drying temperature varied from 70 to 95 C. Moreover, the model predicted decrease in extrudate collapse and open cell fraction with increase in yield and failure stresses of the melt, respectively. Simulation results compared well with experimental R and fo. The model provided a good understanding of the mechanisms of bubble growth and collapse, post extrusion drying and open cell formation during SCFX processing. The model was also used to estimate the eect of various processing and material parameters on extrudate structural characteristics, and can be a useful tool in a priori design of extrudates of specic characteristics. # 2003 Elsevier Science Ltd. All rights reserved.
Keywords: Supercritical uid extrusion; Process dynamics; Modeling; Simulation results; Bubble radius; Open cell fraction; Yield stress; Failure stress
1. Introduction Supercritical uid extrusion (SCFX) patented by Cornell University (Rizvi & Mulvaney, 1992) is an innovation over traditional steam-based extrusion process for production of expanded snack foods and breakfast cereal products. In this process, pung of the starch-based melt is achieved by rst solubilizing supercritical carbon dioxide (SC-CO2) in the melt, and then inducing nucleation due to pressure drop in the nozzle, which is followed by bubble growth caused by diusion of CO2 into the nucleated bubbles. The extrudate expands further until its structure is set during postextrusion oven drying. In the rst part of this study (Alavi, Rizvi, & Harriott, 2001), the dynamics of supercritical uid extrusion and post-extrusion drying of
* Corresponding author. Tel.: +1-785-532-2403. E-mail address: salavi@wheat.ksu.edu (S.H. Alavi).
starch-based melts was discussed from macro and micro level perspectives, and a model was developed based on equations of mass, energy and momentum transport. The SCFX model was written in Visual Basic and interfaced with EXCELTM spreadsheets for input of process and material parameters and output of the process state (comprising of computed results like bubble size, expansion ratio, open cell fraction, temperature, moisture content, etc.) at each time step. The major goals of this paper were to utilize the SCFX model for: (1) understanding the various competing phenomena involved in the formation of microcellular structure during SCFX processing, (2) studying the eect of selected material and process parameters on extrudate structure, and (3) comparing simulation results with experimental data for model validation. The model described in Part 1 of this study is general and not material specic. For predicting the structural characteristics of extrudates of a specic feed formulation
0963-9969/03/$ - see front matter # 2003 Elsevier Science Ltd. All rights reserved. doi:10.1016/S0963-9969(02)00223-5
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(X), values and correlations for various mass, heat and momentum transport parameters for XwaterCO2 system would be required. The prediction accuracy of the model would depend to a large extent on the accuracy of these parameter values and correlations, but it is unpractical to conduct experimental studies to determine these parameters for each material formulation. Therefore, the approach utilized in this study was to study the behavior of a general starch waterCO2 system undergoing SCFX processing. In most cases, the material property values were obtained from literature for a similar system, and therefore the simulation results were qualitative in nature but were nevertheless very useful in meeting the objectives of this study as listed above. Some of these material properties used in the model are discussed below. 1.1. Diusion coecient for CO2 in starch melt (D) The diusion coecient of CO2 (D) in the starch melt is an important parameter which would determine the rate with which CO2 diuses into the bubble and thus the growth rate of the bubble. It is dicult to make a reliable measurement of diusivity in complex systems such as doughs. Singh, Rizvi, and Harriott (1996) studied the diusion coecient of CO2 in extruded corn meal and concluded that CO2 diusivity in a starchwater system is primarily through the absorption of CO2 in water. de Cindio and Correra (1995) made a similar assumption and used a relation based on diusion coecient of CO2 in water to predict diusivity of CO2 in dough: Xw T 9 D 1:77 10 1 m2 =s 1 Xw 298 where, Xw=moisture concentration (kg water/kg solids), T=temperature (K). From Eq. (1), at 70 C and at a moisture concentration of 0.50 kg/kg solids D is 6.81010 m2/s, which was in good agreement with the range of experimental D obtained by Singh et al. (1996) (5.77.51010 m2/s) for the same conditions. This indicated that the choice of the above equation was reasonable. 1.2. Diusion coecient for water in starch melt (Dw) Diusion coecient of water in starch melt is an important parameter which would determine the drying rate of the extrudate in the oven and also the water vapor pressure driven bubble growth during oven drying. The following relation from van der Lijn (1976) for diusion of water in maltose solution was used to model Dw as a function of moisture content (Xw) and temperature (T):
2 Other equations for Dw in starch or similar materials as a function of T and Xw were also available in literature. A comparison of Dw predicted by these equations and the reason for selecting Eq. (2) for the current study are discussed in the Appendix. 1.3. Consistency coecient (K) of starch melt Consistency coecient (K) of the starch melt signicantly aects the bubble growth rate. The dependence of K on moisture and temperature was modeled using a relation from Parker, Ollett, Lai-Fook, & Smith (1989): 4960 12:1Xw K 0:672 exp 3 Pa sn T 1 Xw 1.4. Saturation water pressure (P*) The saturation water vapor pressure (P*) is used in the model to determine the vapor pressure inside the bubble which is the primary driving force for bubble growth during the oven drying stage. Schwartzberg, Wu, Nussinovitch, and Mugerwa (1995) tted data from steam tables to obtain the following relation: 3867:44 P 1002:2 exp 9:43699 kPa 4 T 43:37 1.5. Water activity (aw) The product of water activity (aw) at the bubble surface and the saturation water vapor pressure gives the actual vapor pressure in the bubble. de Cindio et al. (1995) described the following relation for aw with moisture content for commercial our dough at a temperature of 30 C, which was also used in this study. "1 u 5 aw 1 " 1 1 u Xw where, u is the wet basis moisture content (= ) 1 Xw and the tting parameter "1=15.3. 1.6. Elastic modulus (E) of starch melt Elastic modulus of starch melt (E) tends to oppose the driving force for bubble growth and it was modeled as a function of average moisture content (Xwa) and temperature (T) based on relations from Schwartzberg et al. (1995):
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E Er exp0:1300-TkPa where, Er is a constant (10 kPa). 1.7. Flow yield stress (t0) of starch melt
Flow yield stress of the starch melt also tends to oppose the motion of the bubble wall, and was modeled based on a similar equation from Schwartzberg et al. (1995): 0 r exp0:1300 TkPa 7
where, r is a constant and was varied between 1 and 10 kPa. 1.8. Failure stress (Sf) of starch melt The tensile failure stress of the starch melt was modeled based on a similar equation from Schwartzberg et al. (1995): Sf Sm exp0:05300 TkPa 8
rotating twin screw extruder with a length to diameter ratio (L/D) of 27 was congured to operate at a screw speed of 100 rpm and dry feed rate of 9.88103 kg s1 (35.6 kg h1). A pilot scale supercritical uid system was used for injecting SC-CO2 at a ow rate of 7.6105 kg/ s into the starch melt through four valves located around the extruder barrel. Expanded samples, which were cylindrical in shape, were analyzed for bubble radius, open cell fraction and nucleation density using a scanning electron microscope. The experimental methodology is described in greater detail in Alavi et al. (1999) and Gogoi, et al. (2000).
3. Results and discussion The model equations were incorporated in a Visual Basic code that was interfaced with EXCELTM for input of parameters and output of results such as bubble radius, expansion ratio and open cell fraction versus time. Simulations were run for about 1,000,000 time steps which corresponded to the extrusion phase and the rst few minutes of the drying phase in which most of the bubble growth takes place. The base input parameter values are shown in Table 1. 3.1. Variation in T and extrudate moisture concentration with time The spatial temperature gradients in the extrudate at various times are shown in Figs. 1 (pre-drying stage)
Table 1 Input parameters for SCFX model (parameters in bold were varied in the simulation runs) Toven Tr Sm MWD Xo Nnuc Nb N mtot mc To Ts tdry Ro den dex Ld Ld1 h n Er s,dry Kxc 358 1.0 10 1 0.01 5.00E+06 5 10 0.0073 0.5 333 300 30.0 5.00E-06 4.00E-05 1.70E-02 3.00E-03 2.31E-02 7.30E-03 15.00 0.4 10 1.16E+00 1.00E-05 K (oven temp) kPa (constt in yield stress correlation) kPa (constt in failure stress correlation) multiplying factor for water diusivity g CO2/g dry matter (initial CO2 conc.) bubbles/cm3 (nucleation density) number of tubes in macroscopic discretization number of shells in microscopic discretization kg/s (wet feed rate) (=35 kg dry/h) g water/g dry matter (feed moisture content) K (initial temp of melt) K (temp at innity) s (time for oven drying start) m (initial bubble size) kN/m (surface tension) m (nozzle entrance dia) m (nozzle exit dia) m (nozzle length) m (a nozzle dimension) W/m2 K (heat transfer coecient) ow behavior index KPa (constt in elastic mod correlation) g/cm3 (density of dry unexpanded material) m/s (mass tr coe in the oven)
where, Sm is a constant and was varied between 5 and 50 kPa. 1.9. Free convection heat transfer coecient in the oven (h) The heat transfer coecient (h) determines the ow of heat into the extrudate during oven drying, and was calculated as follows. The mean Nusselt number (Nu) in free convection over a horizontal cylinder is given by the following correlation (Geankoplis, 1993): Nu 1:09Ra0:2 9
where Ra (or Raleigh Number)=Pr. Gr Ra ranged from 100 to 1100 depending on the ambient temperature and extrudate diameter, and the corresponding values of h ranged from 12 to 17 W/m2 K. A value of 15 W/m2 K was used for all simulation runs.
2. Experimental methods Experimental results from previous studies on SCFX extrudates (Alavi, Gogoi, Khan, Bowman, & Rizvi, 1999; Gogoi, Alavi, & Rizvi, 2000) were used for comparison with model predictions. The formulation (Cornell mix) used for making the extrudates comprised of pregel corn starch (49.5%), pregel potato starch (24%), sugar (24%), salt (1%) and a dough conditioner (distilled monoglyceride, 1.5%). Thermosetting whey protein concentrate (WPC-34% protein) was added at three levels (4, 7 and 10%) and extrudates were dried at 4 dierent temperatures (22, 70, 85 and 100 C). Feed moisture was maintained at 0.50 kg/kg dry solids, and nozzle temperature at 60 C. A Wenger TX-52 co-
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Fig. 1. Radial temperature distribution inside the extrudate in the predrying stage (center: Rx=0, outer surface: Rx=5).
Fig. 3. Radial distribution of moisture concentration in the cylindrical extrudate (center, Rx=0, surface: Rx=5).
and 2 (oven drying stage), for a sample simulation run in which the extruder nozzle temperature was 333 K (or 60 C) and oven temperature was 358 K (or 85 C) (typical for SCFX conditions). The spatial moisture concentration gradients at various times are shown in Fig. 3, where the initial moisture concentration of the extrudate was 0.50 kg/kg dry matter (typical for SCFX conditions). The variation of average temperature of the extrudate (T) with time is shown in Fig. 4. In the nozzle, the extrudate remains at a constant temperature (333 K or 60 C in this case) but starts cooling and approaches room temperature (300 K or 27 C) after the nozzle exit. At 30 s, which was the time for oven drying to start, predicted T was 325 K (or 52 C). This was in accordance with experimental observation of a 10 K drop in temperature in 30 s. After the extrudate is placed in the oven, the extrudate starts heating and approaches the oven temperature of 85 C. It takes approximately, 3 min for the extrudate to reach the oven temperature.
The variation of average moisture concentration with time is also shown in Fig. 4. Moisture loss was assumed to be negligible in the pre-drying stage, while in the oven (t> 30 s), moisture concentration reduces gradually as the extrudate starts drying. As the simulation was run for only a limited number of time steps, only the initial phase of drying could be modeled. In actuality, extrudates are kept in the oven until they reach the moisture content of 0.05 kg/kg dry matter. 3.2. Variation in extrudate CO2 concentration with time The spatial CO2 concentration in the extrudate at various times is shown in Fig. 5, and the variation of average CO2 concentration with time in Fig. 6. The initial CO2 concentration based on the injection rate of CO2 in the starch melt in the extruder barrel was 0.01 kg/kg dry matter. The CO2 concentration decreases after the extrudate exits the nozzle because CO2 diuses
Fig. 2. Radial temperature distribution inside the cylindrical extrudate during the oven drying stage (center: Rx=0, outer surface: Rx=5).
Fig. 4. Temperature and average moisture content of the extrudate for a typical simulation run (Toven=85 C).
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stant diameter section of the nozzle (0.284t40.30), the pressure drop rate is constant as expected. After exit from the nozzle, Pf remains equal to the atmospheric pressure. PCO2 equals the product of the Henrys law constant (H) and the CO2 concentration at the bubble surface (Xc), and has a value of 4500 kPa at the time of nucleation (t$ 0.28 s). As the bubble expands, Xc decreases (Fig. 8) because of diusion of CO2 into the bubble, and the decrease of PCO2 closely follows that of Xc. After exit from the nozzle, the temperature of the extrudate decreases and thus reducing H and further decreasing PCO2. Moreover, loss of CO2 to the ambient also reduces Xc and contributes to the decrease in PCO2. 3.4. Partial pressure of water vapor in the bubble
Fig. 5. Radial distribution of CO2 in the cylindrical extrudate (center: Rx=0, surface: Rx=5).
Fig. 9 is a plot of partial pressure of water vapor (Pw), which is the main driving force for bubble growth during drying. Pw is the product of the saturation vapor pressure of water (P*) and the water activity aw at the bubble surface. aw, in turn, increases or decreases with the concentration of water at the bubble surface (Xcw). Thus variation in Pw depends both on T which determines P*, and Xcw. In the pre-drying stage Pw decreases from 17 kPa to 13 kPa because of reduction in T and Xcw, while during drying Pw increases to 45 kPa as the extrudate temperature rises. Once T reaches the equilibrium value of 358 K, Pw declines as the concentration of water at the bubble surface (Xcw) goes down. Bubble growth eventually stops when Pw is small enough to make P=0. Pw in the drying stage is an order of magnitude or more lower than PCO2 in the pre-drying stage, because of which rate of bubble growth (dR/dt) in the oven is much smaller than that immediately after exit from the extruder nozzle. 3.5. Variation of DP with time
out to the ambient. This in turn contributes partially to the reduction of partial pressure of CO2 in the bubble, and thus is one of the causes for bubble collapse, which is discussed in detail later. 3.3. Variation in uid pressure (Pf) and partial pressures of CO2 (PCO2) in the bubble Figure 7 shows the variation in Pf and PCO2, which constitute the main resisting and driving forces, respectively, for bubble growth before oven drying. Typically during SCFX processing, Pf in the extruder barrel prior to the nozzle is built up to 10,000 kPa to facilitate injection of CO2 in the supercritical phase. Predicted Pf at the nozzle entrance was 5800 kPa. From t=0.0 s (when the uid is at the nozzle entrance) until t=0.28 s, the uid pressure drop rate increases as the nozzle diameter (h) in the tapered section decreases. In the con-
P is the net force that drives the bubble growth or collapse. Figs. 10 and 11 show the variation of P with time. During bubble growth P=P(Pf+Pe+Py+2/ R). As long as the uid is inside the extruder nozzle (t< 0.30 s), the total pressure inside the bubble (P) (comprising mainly of PCO2) and the uid pressure (Pf) determine the magnitude of P, as the elastic stress (Pe), yield stress (Py) and surface tension (2/R) contributions are negligible. Bubble nucleation takes place at t=0.28 s. Thereafter, both P and Pf decrease, but the latter drops at a faster rate and thus P increases until it reaches a maximum at the nozzle exit (t=0.30 s). After the extrudate exits the nozzle, P continues to drop and thus P approaches zero and the contributions of Pe, Py and 2/R become more signicant. At t=0.47 s, P is low enough for P to become zero, and as P reduces further, P become negative, implying that the
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Fig. 7. Fluid pressure (Pf) and partial pressure of CO2 in the bubble (PCO2) vs. time for a typical simulation run. Pf=101.325 kPa after the extrudate exits the nozzle. The pressure in the barrel before the nozzle is also shown (inset on top right).
Fig. 8. Variation in CO2 concentration at the inner bubble surface (Xc) with time.
Fig. 9. Variation of partial pressure of water vapor (Pw) in the bubble with time.
net force tends to make the bubble collapse. As long as P is negative, the yield stress term Py acquires a negative sign, since yield stress always tends to oppose the motion of the bubble wall. As the bubble collapses its volume decreases and makes P increase until P becomes zero again and equilibrium is reached. When t > 30 s (oven drying stage), partial pressure of water vapor Pw contributes mainly to P, and as T increases so does Pw, making P positive again, although its magnitude remains relatively small.
3.6. Variation of R, R0 and W with time The variation in bubble and domain radii (R and R0 , respectively) (Fig. 12) follow closely the changes in P with time. The wall thickness W is calculated from W=R0 R. R starts increasing from Ro the initial bubble radius (=5106 m or 5 mm) when P > 0 (t=0.28 s). Before the oven drying stage, the rate of change dR/dt is proportional to RP1/n $ RP2 [Part I, Eq. (2)]. From t=0.28 to 0.30 s, P increases until it reaches a maximum and so does R, therefore, dR/dt
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Fig. 10. Variation of driving pressure (P) in the pre-drying stage. Negative value of P leads to bubble collapse.
increases and bubble growth is fast. After exit from the nozzle (t > 0.30 s) bubble growth slows down and nally comes to a stop when P reaches zero (t=0.47 s). For t=0.47 to 0.8 s, P is negative and thus R decreases or in other words the bubble experiences collapse. Collapse of SCFX extrudates after exit from the nozzle has been experimentally veried (Alavi et al., 1999). From t=0.8 to 30 s, P is zero and thus there is no change in bubble radius. For t > 30 s, P is very small but greater than zero, so R increases slowly. In this stage, dR/dt is proportional to R (P/K)2. As drying continues, R should keep increasing but with a continuously decreasing rate until P/K approaches reaches zero again because of decrease in P and increase in K, Pe and Py. When P/K $ 0, expansion stops and the extrudate structure is set. The domain radius R0 also increases with R but at a relatively slower rate, thus the bubble walls get thinner (W decreases) as it expands. Bubble radii obtained from simulation runs ranged from 46 to 223 mm depending on the processing and feed parameters, and this was in reasonable agreement with actual measured values for typical SCFX extrudates that had R ranging from 28 to 177 mm (Table 2). In general, experimental R was lower than that predicted by simulation. One reason for this anamoly is the inherent aw in measuring average bubble radius R from a two-dimensional SEM picture. In a 2-D picture, the plane of cut slices the bubbles o center and the sizes measured from the picture are in general smaller than the actual values (Campbell, Rielly, Fryer, & Sadd, 1999). The eect of various input parameters on extrudate characteristics like bubble radius, expansion ratio and open cell fraction are discussed below. 3.7. Eects of various parameters The eect of input parametersoven temperature, failure stress constant (Sm), yield stress constant ( r) and
Fig. 11. Variation of driving pressure (P) in the oven drying stage.
Table 2 Comparison of simulation results with experimental observations Simulation Drying conditions vs. bubble radius (R) Room temp. 70 C 85 C 95 C Drying conditions vs. open cell fraction (fo) Fig. 12. Variation of bubble radius (R), domain radius (R0 ) and wall thickness (W=R0 R) with time during bubble growth in the SCFX extrudate. Room temp. 70 C 85 C 95 C
a
Experimental 28
a
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multiplication factor for diusion coecient of water (Dw)was studying using the SCFX simulation model. The results are discussed below. 3.8. Oven temperature and failure stress (Sf) The eect of oven temperature Toven on bubble radius and open cell number fraction (fo) is shown in Fig. 13. Before oven drying, R was 46 mm, and during drying the nal R increased from 165 to 223 mm as the oven temperature increased from 70 to 95 . The open cell number fraction (fo) also increased from 0.06 to 0.27 as the oven temperature increased from 70 to 95 C. For a typical SCFX extrudate, the experimental value of R before oven drying and after drying at 85 and 100 C were $ 28, 117 and 177 mm, respectively (Table 2). Experimental fo ranged between 0.15 and 0.36 and also increased as the drying temperature was raised (Gogoi et al., 2000) (Table 2). Thus experimental trends for R and fo corresponded well with those predicted by the model. Formation of open cells can be explained on the basis of tensile stress experienced in the bubble wall. During drying, as the bubble wall thickness W decreases (Fig. 10), the tensile stress in the bubble wall Sw increases and approaches the failure stress (Sf) (Part I, Appendix). If the bubble does not stop expanding before Sw/Sf approaches 1 the chances of rupturing of the wall and formation of an open cell would increase. Therefore addition of a thermosetting additive to the formulation that would increase Sf should decrease the open cell fraction fo. This was conrmed from simulation results shown in Fig. 14. An increase in Sf (that can be brought about by addition of a thermosetting ingredient like whey protein concentrate or WPC) led to a lower number of open cells.
Fig. 14. Predicted open cell number fraction (fo) vs. time in SCFX extrudate at three dierent values of failure stress constant, Sm: 5, 10, 50 kPa (Oven temperature=85 C).
3.9. Role of yield stress in minimizing bubble collapse Thermosetting additives can also be used to increase the yield stress of the uid, thus increasing the contribution of the yield stress term Py in the force balance equation [Part I, Eq. (2)] and reducing the driving force for bubble collapse. Fig. 15 shows the eect of the yield stress coecient ( r) on bubble collapse. For r=1 kPa, R reached a maximum of 74 mm and then reduced to 47 mm due to bubble collapse. When r was increased to 10 kPa, no collapse was observed and R (=63 mm) was higher than that for the earlier case. This result was also conrmed qualitatively from experimental results (Alavi et al., 1999). Prior to oven drying, SCFX extrudates exhibited a reduction in R from over 80 mm to 30 mm. But on addition of
Fig. 13. Predicted bubble radius (R) and open cell fraction (fo) in SCFX extrudate vs. time at dierent oven temperatures, Toven: 70, 85 and 95 C (Sm=10 kPa).
Fig. 15. Predicted bubble radius (R) versus time in SCFX extrudate for two dierent values of yield stress coecient (Tr) showing the eect of thermosetting additive on reduction of extrudate collapse.
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Fig. 16. Eect of diusion coecient of water on predicted average moisture content and bubble radius in SCFX extrudate (multiplying factor, MF: 0.2, 1.0 and 5.0).
7% WPC to the feed formulation R only reduced to 73 mm, thus indicating that thermosetting WPC helped in reducing collapse plausibly due to an increase in yield stress of the starch melt. 3.10. Diusion coecient of water The above simulation results are to an extent qualitative in nature as some input parameters like viscosity, diusion coecient for water, mass transfer coecient, elastic modulus, surface tension, yield stress and failure stress were either taken from literature values reported for other similar materials (corn starch, wheat dough, etc.) or were adjusted to make the nal cell size close to experimental values. Experimental determination of all these parameters would not only be time consuming but also redundant as some of these parameters do not aect the results signicantly. For example, the diusion coefcient of water in starch Dw was estimated to be the equal to Dw in maltose (Schwartzberg et al., 1995). Fig. 16 shows that even if this estimation was not accurate, though higher values of Dw led to faster drying as expected, the nal bubble radius is not aected signicantly.
results of bubble radius (R) and open cell fraction (fo) of extrudates exhibited a good qualitative match with experimental measurements. A closer correspondence between simulation and experimental results for both R and fo can be achieved if three-dimensional imaging techniques are used for analyzing the cellular structure of extrudates. The model also proved useful in understanding several phenomena involved in SCFX processing, including bubble growth and collapse, role of postextrusion drying and the mechanisms by which collapse and open cell formation can be reduced. Moreover, the model can be used to estimate the relative signicance of various processing and material parameters in aecting the extrudate structural characteristics. In the future, the mechanisms of bubble nucleation and non-porous skin formation need to be incorporated into the model, and also more accurate measurements of important parameters like melt viscosity, mass transfer coecient in the oven, etc. need to be done. Also, simulation runs need to be a carried out on a much faster CPU in order to fully model the oven drying stage in a reasonable time-frame. Also this SCFX process dynamics model can be integrated with a model that can predict mechanical properties of extrudates with their structural characteristics. Such an integrated model can be very useful in a priori design of products with unique texture.
Acknowledgements The authors would like to thank the United States Department of Agriculture for providing the funding for this project, and Wenger Manufacturing, Inc. for their assistance through the Cornell-Wenger Extrusion Program.
Appendix. Diusivity of water in starch and similar materials Several equations have been proposed in literature for diusivity of water (Dw) in starches and comparable materials as a function of temperature (T) and moisture concentration (Xw), some of which are discussed here. de Cindio et al. (1995) used diusivity data for commercial our dough from earlier studies to obtain the following equation by a tting procedure. Xw T logDw 16 72:38 log A1 298 1 9:34Xw This equation was used to model diusion of water during leavening of dough, and was found to predict moisture concentration in qualitative agreement with industrial experience. Karathanos, Vagenas, and Saravacos (1991) experimentally measured water diusivity in dough samples
4. Conclusions A process dynamics model was developed for modeling expansion and post-extrusion processing of starchbased supercritical uid extrudates, at both microscopic and macroscopic levels. The model had several simplifying assumptionsinstantaneous nucleation, nucleation density as an input parameter instead of being a function of the pressure drop rate in the nozzle, and various material properties approximated from literature. Despite these assumptions and the need for further renement and testing of the model, the predicted
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(prepared from native granular starch powder containing 98% amylopectin) at dierent temperatures, moisture concentrations and pressures (P). Their data matched previously reported results, and the following equation was obtained by tting. lnDw 10:882 2851 0:3122lnP 1:5111Xw T A2
solids) using the above three Eqs. (10)(12). Although the three equations predicted Dw of the same order of magnitude ($ 1010 m2/s), it diered by a factor of up to 7 at any temperature, depending on the equation used. The equation proposed by van der Lijn (1976) was selected for this study as it predicted intermediate values of Dw, and has been used successfully for prediction of moisture distributions in starches in previous studies. References
Alavi, S. H., Rizvi, S. S. H., Harriott, P. (2001). Process dynamics of supercritical uid extrusioninduced pung of starch-based melts. I: model development. Alavi, S. H., Gogoi, B. K., Khan, M., Bowman, B. J., & Rizvi, S. S. H. (1999). Structural properties of protein-stabilized starch-based supercritical uid extrudates. Food Research International, 32, 107 118. Campbell, G. M., Rielly, C. D., Fryer, P. J., & Sadd, P. A. (1999). Reconstruction of bubble size distributions from slices. In G. M. Campbell, C. Webb, S. S. Pandiella, & K. Niranjan (Eds.), Bubbles in food. St. Paul, MN: American Association of Cereal Chemists. de Cindio, B., & Correra, S. (1995). Mathematical modeling of leavened cereal goods. Journal of Food Engineering, 24, 379403. Geankoplis, C. J. (1993). Transport processes and unit operations (3rd ed.). Engelwood Clis, NJ: Prentice Hall. Gogoi, B., K., Alavi, S. H., & Rizvi, S. S. H. (2000). Mechanical properties of protein-stabilized starch-based supercritical uid extrudates. International Journal of Food Properties, 3(1), 3758. Karathanos, V. T., Vagenas, G. K., & Saravacos, G. D. (1991). Water diusivity in starches at high temperatures and pressures. Biotechnology Progress, 7, 178184. Parker, R., Ollett, A.-L., Lai-Fook, R., & Smith, A. C. (1989). The rheology of food melts and its applications in extrusion processing. In R. E. Carter (Ed.), Rheology of food, biological and pharmaceutical materials. London: Elsevier Science. Rizvi, S. S. H., & Mulvaney, S. J. (1992). Extrusion processing with supercritical uids. US Patent 5120559. Schwartzberg, H. G., Wu, J. P. C., Nussinovitch, A., & Mugerwa, J. (1995). Modelling deformation and ow during vapor-induced pung. Journal of Food Engineering, 25, 329372. Singh, B., Rizvi, S. S. H., & Harriott, P. (1996). Measurement of diffusivity and solubility of carbon dioxide in gelatinized starch at elevated pressures. Industrial Engineering and Chemistry Research, 35, 44574463. van der Lijn, J. (1976). Simulation of heat and mass-transfer in spray drying. PhD thesis, Agricultural University of Wageningen, The Netherlands, (pp. 7780) [as referred in Schwartzberg et al., 1995].
Schwartzberg et al. (1995) used a correlation for diffusivity of water in maltose, proposed in an earlier study (van der Lijn, 1976), to predict moisture distribution in popcorn during vapor-induced pung. Experimental moisture concentration data from this study was in agreement with predicted values. D 1:35 21:61548 T1:194 3:68Xw 10 exp T1 18:98Xw
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A3 Fig. A1 compares predicted Dw versus temperature (at a constant moisture concentration, Xw=0.50 kg/kg
Fig. A1. Predicted water diusivity (Dw) versus temperature (at constant moisture concentration, Xw=0.50 kg/kg solids) using various correlations from literature.