Process Biochemistry 37 (2001) 125 137 www.elsevier.

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Factorial design and simulation for the optimization and determination of control structures for an extractive alcoholic fermentation
Aline C. Costa a,*, Daniel I.P. Atala b, Francisco Maugeri b, Rubens Maciel a
Department of Chemical Engineering, School of Chemical Engineering, State Uni6ersity of Campinas, P.O. Box 6066, 13081 -970, Campinas, SP, Brazil b Department of Food Engineering, School of Food Engineering, State Uni6ersity of Campinas, P.O. Box 6121, 13081 -970, Campinas, SP, Brazil Received 21 August 2000; received in revised form 13 March 2001; accepted 31 March 2001
a

Abstract The design, optimization and control of an extractive alcoholic fermentation were studied. The fermentation process was coupled to a vacuum ash vessel that extracted part of the ethanol. Response surface analysis was used in combination with modelling and simulation to determine the operational conditions that maximize yield and productivity. The concepts of factorial design were used in the study of the dynamic behaviour of the process, which was used to determine the best control structures for the process. A good choice of the operational conditions was important to enable efcient control of the process. The performance of a DMC (Dynamic Matrix Control) algorithm was studied to control the extractive process. 2001 Elsevier Science Ltd. All rights reserved.
Keywords: Response surface analysis; Factorial design; Optimization; DMC control; Ethanol

Nomenclature A b Cp D =F/V f F Fc Fc1 FE FL FLR FLS F0 Fp Fr FV Fw Dynamic matrix in the DMC algorithm Coefcients in the step-response model Heat capacity, Kcal/(kg. C) Dilution rate, h 1 weighting factor in the DMC algorithm Feed stream ow rate, m3/h Cell suspension ow from centrifuge, m3/h Cell suspension ow to treatment tank, m3/h Light phase ow rate to ash tank, m3/h Liquid outow from the vacuum ash tank, m3/h Liquid phase recycling ow rate, m3/h Liquid phase ow to rectication column, m3/h Fresh medium ow rate, m3/h Purge ow rate, m3/h Cell recycling ow rate, m3/h Vapor outow from the vacuum ash tank, m3/h Water ow rate, m3/h

* Corresponding author. Tel.: + 55-19-788-3971; fax: + 55-19-788-3965. E-mail address: accosta@feq.unicamp.br (A.C. Costa). 0032-9592/01/$ - see front matter 2001 Elsevier Science Ltd. All rights reserved. PII: S 0 0 3 2 - 9 5 9 2 ( 0 1 ) 0 0 1 8 8 - 1

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I J KdP KdT Kei Ki Ks m mp mx n NC NP p p sat i P PF PLR PV Pmax Pr r = FLR /FL rd rp rs rx R = Fr/F S SF SLR S0 Sr T TF FLR tr T0 Tr TRS TV Tw V xEi xi Xd XdF Xmax Xt = X6 + Xd X6 X6F Xc XE XF

Identity matrix Performance index Coefcient of death by ethanol, m3/kg Coefcient of death by temperature, h 1 Equilibrium constant Substrate inhibition constant, m3/kg Substrate saturation constant, kg/m3 Constant in Eq. (6) Ethanol production associated to growth, kg/(kgh) Maintenance coefcient, kg/(kgh) Constant in Eq. (6) Control horizon in the DMC algorithm Prediction horizon in the DMC algorithm Pressure, Pa Vapor pressure, Pa Product concentration into the fermentor, kg/m3 Feed product concentration, kg/m3 Product concentration in the light phase from centrifuge, kg/m3 Product concentration in the vapor phase from the ash tank, kg/m3 Product concentration when cell growth ceases, kg/m3 Product concentration in the cells recycle, kg/m3 Flash recycle rate Kinetic rate of death, kg/(m3h) Kinetic rate of product formation, kg/(m3h) Kinetic rate of substrate consumption, kg/(m3h) Kinetic rate of growth, kg/(m3h) Cells recycle rate Substrate concentration into the fermentor, kg/m3 Feed substrate concentration, kg/m3 Substrate concentration in the light phase from centrifuge, kg/m3 Inlet substrate concentration, kg/m3 Substrate concentration in the cells recycle, kg/m3 Temperature into the fermentor, C Feed temperature, C Light phase temperature, C Residence time, h Inlet temperature of the fresh medium, C Cells recycle temperature, C Total Reducing Sugars, kg/m3 Temperature of vapor from the ash tank, C Water temperature, C Reactor volume, m3 Component i concentration in the light phase, mol% Component i concentration in the liquid, mol% Dead biomass concentration into the fermentor, kg/m3 Dead biomass concentration in the feed stream, kg/m3 Biomass concentration when cell growth ceases, kg/m3 Total biomass concentration into the fermentor, kg/m3 Viable biomass concentration into the fermentor, kg/m3 Viable biomass concentration in the feed stream, kg/m3 Biomass concentration in the heavy phase from centrifuge, kg/m3 Biomass concentration in the light phase ow rate to ash tank, kg/m3 Feed biomass concentration, kg/m3

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XLR Xr y yi Ypx Yx DH Dm k ki vmax z zm

Biomass concentration in the light phase from centrifuge, kg/m3 Cell recycling concentration, kg/m3 Controlled variable in DMC algorithm Component i concentration in the vapor, mol% Yield of product based on cell growth, kg/kg Limit cellular yield, kg/kg Reaction heat, kcal/(kg TRS) Variation in the manipulated variable in DMC algorithm Ratio of concentration of intracellular to extracellular ethanol, kg/m3 Activity coefcient of component i Maximum specic growth rate, h-1 Ratio of dry cell weight per wet cell volume, kg/m3 Density, kg/m3

1. Introduction Brazil is the world main ethanol producer as the result of a political strategy initiated in 1975 by the government to cope with the sharp increase in oil prices. Programmes in the USA in 1978 and, more recently, in Canada, followed this strategy [1]. Because of the relative stabilization of the petroleum prices at a low level, most of the incentives to the alcohol industries were withdrawn and there was a great interest in the optimization of all the stages of the ethanol production process. Nowadays, with a further increase in petroleum prices and productivity improvements attained in alcohol production there is again a good outlook for this industry. However, ethanol will only substitute gasoline as a fuel if its production becomes economically competitive. The operation of the alcoholic fermentation process in a continuous mode is desirable, since higher productivity, improved yields and better process control are attained [2]. However, the industrial implementation of a continuous process requires a previous study of the process behaviour and its use in the development of an efcient control strategy. The inuence of temperature in the kinetic parameters must be considered, as there is difculty in maintaining a constant temperature during industrial alcoholic fermentation. This is an exothermic process and small deviations in temperature (2 4 C) can dislocate the process from optimal operational conditions. As the conventional process is inhibited by ethanol, the selective extraction of this product during fermentation is essential to enhance process performance. Several schemes combining fermentation with a separation process have been developed, such as fermentation under vacuum [3,4], pervaporation [5], solvent extraction [6], ultraltration [7], fermentation combined with a ash vessel operating under atmospheric pressure [8], fermentation combined with a vacuum ash vessel [9,10] and CO2 gas stripping [11]. Silva et al. [10] have

shown that the scheme using the vacuum ash vessel presents many positive features and a better performance than an industrial conventional process [12]. Another important aspect to be considered in the optimization of the alcoholic fermentation is the development of an efcient control strategy, as it minimizes costs by maintaining the process under optimal conditions. The choice of the control structure is an important step in the development of a control strategy. In this work the performance of a continuous extractive alcoholic fermentation scheme based on that proposed by Silva et al. [10] is studied. A mathematical model considering effect of temperature on the kinetic parameters is developed based on experimental data to describe the fermentation process. Response surface analysis is used in a simulation study to determine the operational conditions that lead to high yield and productivity. The concepts of factorial design are used in the study of dynamic behavior of the process in order to choose the best control structures for efcient control of the process and the performance of a DMC (Dynamic Matrix Control) algorithm is tested to control the extractive process.

2. Extractive alcoholic fermentation A general scheme of the extractive alcoholic fermentation proposed by Silva et al. [10] is shown in Fig. 1. The process consists of four interlinked units: fermentor (ethanol production unit), centrifuge (cell separation unit), cell treatment unit and vacuum ash vessel (ethanol-water separation unit). This scheme attempts to simulate industrial conditions [12], with the difference that only one fermentor is used instead of a cascade system and the ash vessel is used to extract part of the ethanol. In fact, in an industrial conventional process the usual arrangement is to have four interlinked fermentors with the measurements made at the entrance of the rst unit and at the exit of the last tank [12].

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In the cell treatment unit, the cell suspension is diluted with water, and sulphuric acid is added to avoid bacterial contamination. The ash vessel is operated in a temperature range between 28 and 30 C, which is chosen in order to eliminate the necessity for a heat exchanger. This reduces drastically the xed and maintenance costs of the process, since heat exchangers are expensive items of equipment in an alcoholic fermentation plant [12]. The associated pressure is in the range of 45.33 kPa. The process was shown to be able to maintain suitable conditions for the growth of Sacharomyces cere6isae, by maintaining a constant temperature, which may be controlled without a heat exchanger [10]. The vapourized stream leaving the ash vessel is sent to a rectication column with part of the liquid stream, while the other fraction of the liquid returns to the fermentor. This is adjusted to maintain the ethanol concentration in the fermentor in such a value that it acts as antiseptic. According to practical knowledge in industrial units, this alcohol concentration is around 40 kg/m3, which has low inhibitory effect for fermenting yeast but is highly inhibitory for most contaminating microorganisms [10].

The concentration of biomass in the cells recycle stream is xed. To maintain the concentration in a xed value, the ow rate of the water that dilutes the ferment (FW ) is adjusted. The cell recycle ow rate (Fr ) is maintained at a value xed by the cell recycle rate (R) by adjusting the ow rate of the purge (Fp ). The purge permits cell renovation and the withdrawal of secondary products accumulated into the fermentor. To be able to obtain the kinetic parameters as functions of temperature, experiments were performed at temperatures between 28 and 40 C in a system with total cell recycling by tangential microltration. The substrate used was sugar-cane molasses [13]. An intrinsic model, which takes cell volume fraction into account, was used, as suggested by Monbouquette [14]. The ethanol mass balance accounts for both intracellular and extracellular product, as suggested by the same author [15]. As the experimental data showed a loss of cell viability with an increase in the fermentation time, it was assumed that the total biomass comprises a viable (active) phase X6 and an inactive (dead) phase Xd. Assuming constant volume, the mass and energy balance equations for the fermentor using the intrinsic model are as follows: F dX6 = rx rd (X6 X6F ) viable cells: dt V F dXd =rd (Xd XdF ) dead cells: dt V d substrate: (1) (2)

3. Mathematical modelling In order to determine the feed rate and feed concentration of the fermentor, mass balances on the global process are necessary. The following considerations were made: The concentrations of substrate and product leaving the centrifuge are equal to the concentrations leaving the fermentor;



Xt SV z = F(SF S) Vrs dt

 n

(3)

Fig. 1. Extractive alcoholic fermentation.

A.C. Costa et al. / Process Biochemistry 37 (2001) 125137 Table 1 Kinetic Parameters as functions of the temperature (in C). Parameter vmax Xmax Pmax Yx Ypx Ks Ki mp mx m n KdP KdT z k Expression or value 41.47 431.4 )1.29.104exp( ) T T 2 0.3279.T +18.484.T191.06 0.4421.T 2+26.41.T279.75 2.704exp(0.1225.T) 0.2556exp(0.1086.T) 4.1 1.393.104exp(0.1004.T) 0.1 0.2 1 1.5 7.421.103.T20.4654.T+7.69 1.57exp( 41947 4.1013exp 1.987.(T+273.15) 390 0.78

129

FExEi = FVyi + FLxi

(11)

The vapour-liquid equilibrium of the ethanol-water mixture was calculated by Eq. (12), the value of p sat i was calculated by Antoines equation (the assumption was made that the light phase was a binary mixture of ethanol-water) and the value of ki was calculated using the NRTL model (Non-random Two-Liquid) [10]. p sat yi i Kei = = ki xi p (12)

Eq. (1) to Eq. (12) were solved using a Fortran program with integration with an algorithm based on the fourth order Runge-Kutta method.

4. Process optimization The extractive alcoholic fermentation process may be optimized using response surface methodology, which is a procedure that does not require model simplications and the explicit formulation of an objective function. The input variables considered for the optimization were the ones whose inuence on yield and productivity were determined as relevant by Silva et al. [10]. A factorial design 24 + star conguration with a central point was performed to determine two quadratic models with inlet substrate concentration (S0), cells recycle rate (R), residence time (tr ) and ash recycle rate (r) as inputs and yield and productivity as outputs. In the following simulations the fresh medium ow rate (F0) was considered constant, so that variations in residence time led to variations in the reactor volume. The reactor volume was calculated as follows: V=F.tr (13)

d product:



Xt X PV + tkPV z z =Vrp +F(PF P) dt (4) (5)

dT DHrs = D(TF T)+ dt zmCp

z and k in Eq. (3) and Eq. (4) are the ratio of dry cell weight per wet cell volume and the ratio of concentration of intracellular to extracellular ethanol, respectively. The values of the constants in the energy balance Eq. (5) are given by [10]: DH =51.76 kcal/(kg TRS); zm = 1000 kg/m3 and Cp = 1 kcal/(kg C). The kinetic rates of growth, death, ethanol formation and substrate consumption are as follows: S X rx = vmax exp(Ki S) 1 t Xmax Ks +S rd = (KdT exp(KdPP))X6 rp = Ypxrx + mpX6 rs = rx +mxX6 Yx


m

P n 1 X6 Pmax (6) (7) (8) (9)

in which tr is the residence time and the feed ow rate was calculated as: F= F0 + FLR (1R) (14)

in which FLR is the liquid phase recycle ow rate from the ash vessel and R is the cell recycle rate. Yield and productivity were dened as follows: yield= prod= F6.P6 + FLS.PLR F0.S0.0.511 F6.P6 + FLS.PLR V (15) (16)

The parameters were adjusted as functions of temperature from the experimental data and are given in Table 1. The proposed model described the dynamic behaviour of the alcoholic fermentation [13]. The dynamics of the ash tank are much faster than that of the fermentation process, so a pseudo steady state was assumed for the ash tank. The mass balances over the ash tank are given by FE =FV + FL (10)

Table 2 shows the coded factor levels and the real values for the input variables. The mathematical model was used to simulate the extractive process. The software Statistica (Statsoft, v. 5.0) was used to analyze the results. The quadratic models obtained for yield and productivity as a function of the more signicant variables were:

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Table 2 Coded factor levels and real values for factorial design S0 (kg/m3) Level +2 Level +1 Central point (0) Level 1 Level 2 280 230 180 130 80 tr (h) 2.5 2.125 1.75 1.375 1.0 R 0.5 0.425 0.35 0.275 0.2 r 0.6 0.5 0.4 0.3 0.2

Yield= 82.99 13.35.S0 2.54.S 2 +5.15.tr + 7.40.R 0 +9.14.r + 2.66.S0.tr +3.12.S0.R +5.87.S0.r (17) Prod = 14.67+ 6.44.S0 0.9.S 2 5.52.tr + 1.58.tr 2 0 4.32.R 4.9.r +0.94.S0.r 1.18.r.R (18) Table 3 depicts the analysis of variance (ANOVA) for yield and productivity. Both responses present a high correlation coefcient and the model can be considered statistically signicant according to the F-test with 99% of condence, since the calculated values were more than 17 times greater than the listed value. As a practical rule, a model has statistical signicance if the calculated F value is at least 3 5 times greater than the listed value [16].
Table 3 Analysis of variance Source of variation Sum of squares Yield Regression Residual Total Correlation coefcient F listed value: 2303.9 69.0 2372.9 0.971 Prod. 723 21.7 744.7 0.971

An analysis of the response surfaces plotted using Eq. (17) and Eq. (18) shows that S0, R, tr and r have opposite effects on yield and productivity, which means that the values that increase yield decrease productivity and vice-versa. It shows also that there are many combinations of values that lead to high yield and productivity. The choice of the best values for the input variables is easier if one takes advantage of previous knowledge of the process. For example, according to Andrietta and Maugeri [12], R cannot be much higher than 0.3 because otherwise it would increase the requirement for centrifuges capacity. Centrifuges are very expensive and so are their maintenance costs. Another consideration is about the reactor volume. If F0 is xed (F0 = 100 m3h), the reactor volume decreases as tr, R and r decrease. If R is xed, then, low values of tr and r that lead to high yield and productivity should be chosen. Figs. 24 show the response surfaces for yield and productivity as functions of S0 and r for tr = 1.2, 1.4 and 1.6 h, respectively. R is xed as 0.3. The surfaces are plotted together to facilitate visualization. Yield is shown as a surface area and productivity as lines. It can be observed that tr seems to have more inuence on productivity than on yield (for example, for tr = 1.2 h productivity above 26.7 kg/(m3h) and

Mean square Yield 288 4.31 Prod. 90.4 1.36

Degrees of freedom

F-value Yield Prod. 66.5

8 16 24

66.8

F8,16 =3.89 (99%)

Fig. 2. Response surface for R =0.3 and tr =1.2 h.

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Fig. 3. Response surface for R=0.3 and tr =1.4 h.

Fig. 4. Response surface for R=0.3 and tr =1.6 h.

yield above 90.7% can be reached and for tr =1.6 h the highest values for productivity and yield reached are above 22.2 kg/(m3h) and 90.7%). It can also be seen from the gures that high yield is attained for low values of S0 and r does not inuence yield much. In this way, it is possible to choose a relatively low value of S0 to maximize yield and a low value of r to increase productivity. The value of tr should be relatively low to maximize productivity and minimize reactor volume. It is worthwhile mentioning that too low values of tr, however, led to low yield. After analysis of the simulations results using the mathematical model, the following values were chosen: S0 =130 kgm3, tr =1.3 h, R = 0.3 and r =0.25. The values of yield and productivity attained were 82% and 21 kg/(m3h). Conversion was 96% and the reactor volume 257.4 m3. A simulation using the input variable values determined by Silva et al. [10], S0 =180 kgm3, tr =1.2 h, R =0.35 and r =0.4, gave yield, productivity and conversion of 81%,

22 kg/(m3h) and 96%, respectively. The volume of the reactor, however, was 339.8 m3, 32% higher than the obtained in the present work. The conversion and yield attained for the two sets of input variables were low when compared to previously published values, conversion of 99% and yield of 86.3% [16]. These values can be increased, but for a low increase in conversion and yield there is a great decrease in productivity and a great increase in reactor volume. For example, the conditions to reach conversion of 98% and yield of 86.4% (S0 = 120 kgm3, tr =1.2 h, R= 0.3 and r= 0.45) led to productivity of 15 kg/ (m3h) and reactor volume equal to 358.6 m3. The productivity of the extractive process for the conditions determined in this work or by Silva et al. [10] is much higher than that of the conventional process. Kalil et al. [16] optimized the industrial conventional process designed by Andrietta and Maugeri [12] and obtained a productivity of 12 kg/(m3h).

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Table 4 Coded factor levels and real values for factorial design S0 (kg/m3) Level +1 Level 1 143 117 R 0.33 0.27 F0 (m3/h) 110 90 r 0.275 0.225 T0 (C) 33 27

Fig. 5. Main effects of the input variables on biomass concentration.

5. Dynamic behaviour of the process To choose the best control structures for a given process, its open-loop dynamic behaviour must be investigated. The objective is to determine how the output variables change with time inuenced by changes in the inputs (manipulated variables and possible disturbances). This can be done by changing the values of the various input variables (one by one) and observing the change of the output variables with time. Another approach is the use of the concepts of factorial design. In this case, it is also possible to have information

about the effect of the interactions between the input variables in the outputs. A two level factorial design can be used in a dynamic behaviour study, since only a preliminary investigation is necessary to determine if some factors (inputs) affect the outputs. The outputs of the extractive process are: biomass concentration in the fermentor (Xt = X6 + Xd ), substrate concentration in the fermentor (S), product concentration in the fermentor (P) and temperature in the fermentor (T). The input variables considered for manipulation are: cell recycle rate (R), inlet ow rate (F0) and ash recycle rate (r). The input variables considered as possible load disturbances are: inlet substrate concentration (S0) and inlet temperature (T0). Table 4 gives the coded factor levels and the real values for the input variables. They were calculated as variations of 9 10% around the steady state. The steady state values are as follows: S0 = 130 kgm3; R= 0.3; F0 = 100 m3h, r= 0.25 and T0 = 30 C. As the dynamic behaviour of the process is being studied, the output variables must be calculated as functions of time. Thus, for each simulation, all the output variables were calculated from 010 h. This nal time was chosen because after 10 h a new steady state had been reached in all simulations. The methodology for the calculation of the main effects as well as the interaction effects in a complete factorial design can be found in Box et al. [17]. The main effect can be interpreted as the difference (for the output variable) between the low setting ( 1) and the high setting (+ 1) for the respective input variable. A program in Fortran was developed to calculate the main and interaction effects as functions of time. Fig. 5 shows the main effects of the input variables on biomass concentration as a function of time. The interaction effects between the input variables on this output variable are negligible.

Fig. 6. (a) Main effects of the input variables on substrate concentration. (b) Interaction effects between the input variables on substrate concentration.

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Fig. 7. Main effects of the input variables on product concentration.

Fig. 8. Main effects of the input variables on temperature. Table 5 Effects of the inputs on process outputs

Table 6 Coded factor levels and real values for factorial design S0 (kg/m3) Level +1 Level 1 198 162 R 0.385 0.315 F0 (m3/h) 110 90 r 0.44 0.36 T0 (C) 33 27

Fig. 6a presents the main effects of the input variables on substrate concentration. In this case, the effects of interaction between some of the input variables on substrate are important, as seen in Fig. 6b. This means that the main effect of an input variable (factor)

on the output variable depends also on the values of the other factors. In this case, the main effects in Fig. 6a were used, but it should be clear that they are approximated mean values. Fig. 7 depicts the main effects of the input variables on product concentration, and Fig. 8 presents the main effects of the input variables on temperature. The interaction effects between the inputs on these output variables are negligible. By using the data in Figs. 58, a table of the effects of the inputs on the outputs can be constructed. In Table 5, the black area means that the input inuences the output, the white area means that the inuence is negligible and the gray area means that the input has a weak inuence on the output. Table 5 can be used to determine the best structures for an efcient control of the process. For example, F0 inuences mainly the substrate concentration and a loop that manipulates F0 and controls S can be considered decoupled from the other loops. If some disturbance deviates the substrate concentration from its set point, controlling this output through the manipulation of F0 does not affect signicantly the other output variables, which is a desirable characteristic. From Table 5 the following conclusions can be made: the biomass concentration can be controlled by the manipulation of R and disturbances in T0 have a weak inuence in this output. The best choice of manipulated variable to control the substrate concentration is F0 and disturbances in S0 and T0 affect this output. It is difcult to control product concentration with the manipulated variables considered, as they have only a weak inuence on this output. Thus, the variations in the manipulated variable necessary to control this output will probably be too large. Disturbances in S0 affect product concentration. None of the manipulations considered in this work affect temperature, which can not be controlled. In this case this is not a problem, as the proposed scheme maintains the temperature inside a desired range without the necessity of a control system [10]. Disturbances in T0 affect the temperature and disturbances in S0 have a weak inuence on this output. From the conclusions above, it can be seen that substrate concentration, which is the most important variable to be controlled in an alcohol fermentation plant, is easily controlled. However, if it is necessary to control product concentration, the operational point determined in the present work is not a good choice. A dynamic behaviour study was performed using the operational conditions determined by Silva et al. [10] for comparison. The coded factor levels and the real values for the input variables, calculated as variations of 9 10% around the steady state, are shown in Table 6. The steady state values are as follows: S0 = 180 kgm3; R= 0.35; F0 = 100 m3h, r= 0.4 and T0 = 30 C.

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In this case, two of the manipulated variables (R and r) have a strong inuence on product concentration, as can be seen in Fig. 9. The effects of the inputs on the outputs are shown in Table 7. In this table shading has the same meaning as in Table 5. From Table 7 it can be concluded that biomass concentration can be controlled by the manipulation of R. The best manipulated variable to control substrate concentration is F0, changes in S0 inuence S and changes in T0 have only a weak inuence on this output. The best choice to control P is r, as this manipulated variable has strong inuence only on this output variable, and changes in S0 inuence product concentration. None of the manipulations considered affect the temperature, which cannot be controlled. Disturbances in T0 affect the temperature.

The output of a SISO (Single Input Single Output) system can be computed from its step response model, (bi ), as follows:
NP + 1

yol,i = y meas + 0

(bi + 1 k b1 k )(Dmk )old

(19)

k=0

in which yi is the value of the output y at sampling time i (in the future); Dmk is the change in the manipulated variable at sampling time k (in the past) and y meas is the 0 measured value of y at the actual sampling time. The DMC algorithm minimizes the square of the deviation between the predicted output in closed loop and the set-point values at NC future sampling periods by solving the constrained least squares minimization problem: J= % (y set point ycl,i )2 + f
i=1 NP NC 2

% [(Dmk )new]2

(20)

k=1

6. Dynamic matrix control The basic concepts of the DMC algorithm were originally presented by Cutler and Ramaker [18] and can be found in Luyben [19]. This control algorithm has great potential for industrial application [20]. The basic idea is to use a time-domain step-response model of the process to calculate the future changes in the manipulated variables that will minimize some performance index.

in which J is the performance index to be minimized; Dm is the vector of the NC future changes in the manipulated variable to be calculated; f is the suppression factor or tuning parameter, which penalize the objective function for changes in the inputs Dm; NP is the prediction horizon and NC is the control horizon. The minimization of Eq. (20) using the least squares method results in the following equation (Dm)new = [A TA+ f 2I] 1A Ty in which: y= y set point yol (22) (21)

Matrix A in Eq. (21) is the dynamic matrix and is composed by the step-response coefcients. The DMC controller has three parameters that can be adjusted to good performance of the controller: NP, NC and f. In this work the DMC algorithm was implemented in a Fortran program. In the following tests with the DMC control, the operational conditions used were the determined in the present work and the steady state conditions are given by: Xt = 30.1 kgm3, S= 5.4 kgm3, P =37.7 kgm3, T= 33.4 C.

6.1. Case 1. Substrate concentration control by manipulating F0

Fig. 9. Main effects of the input variables on product concentration. Table 7 Effects of the inputs on process outputs

This control structure was chosen based on the dynamic behavior study results. As the inlet ow rate (F0) inuences strongly only the substrate concentration, it is a good variable to be manipulated to control that output variable. In the rst test of the performance of the controller, step changes of 9 20% were made in the inlet substrate concentration (S0). Fig. 10 shows the open-loop response and the result when the DMC controller is used. The controller maintained the controlled variable near

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to the set-point value in the presence of the load disturbances considered. The performance of the DMC controller for the servo problem was tested by making a step change of 9 50% in the set-point value. Fig. 11 presents the results for the controlled variable when the process is operated with the DMC controller. It can be seen that the DMC controller presented good performance for the servo problem.

6.2. Case 2. Product concentration control by manipulating R

According to Table 5, the ash recycle rate (r) is the best choice of manipulated variable to control product concentration, as it inuences only this output variable. However, as this inuence is weak, the manipulated variable whose inuence on product concentration is the strongest was chosen (see Fig. 7), the cells recycle rate (R). This manipulated variable was chosen only to determine if product concentration can be controlled, but it is not a good choice, since it has a strong inuence on biomass concentration (see Table 5). Then, the variations made in this manipulated variable to control product concentration would affect much the biomass concentration. Also, according to Andrietta and Maugeri (1994), the value of this manipulated variable can not be much higher then 0.3 because otherwise the needs on industrial centrifuges capacity would be increased. Step changes of 9 20% were made in S0. Fig. 12a and 12b show the behaviour of the controlled and manipulated variables, respectively. It can be seen from the gures that, in the case of the positive step change, the DMC controller was able to return the substrate concentration to the steady state. For the negative step change, however, R reached a lower restriction (it was

Fig. 10. Substrate concentration against time for step change of 920% in feed substrate concentration.

Fig. 11. Substrate concentration against time for change of 950% in the set point.

Fig. 12. (a) Product concentration against time for step changes of 9 20% in S0. (b) Cells recycle rate against time for step changes of 9 20 in S0.

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Fig. 13. (a) Product concentration against time for step changes of 9 20% in S0. (b)- Flash recycle rate against time for step changes of 9 20 in S0.

assumed that R cannot be lower than 0.05) and the product concentration did not return to the steady state. As the dynamic behaviour study has shown, the inuence of R on S is weak, and, for the negative step change in S0, the variation in R necessary to return the controlled variable to the steady state was too large. Tests were made using the other manipulated variables (F0 and r) to control the product concentration and in all the cases the control algorithm failed in the case of the negative step change.

6.3. Case 3. Product concentration control by manipulating r (operational conditions determined by Sil6a et al. [10])
As the dynamic behaviour study showed that it is possible to control product concentration if the operation point is that determined by Silva et al. [10], the performance of the DMC controller was tested for the same disturbances considered above. In this case, the manipulated variable chosen was r, as it inuences strongly only this output (see Table 7), which is a desirable characteristic. Fig. 13a and 13b show the behavior of the controlled and manipulated variables. In this case the DMC controller was able to return the product concentration to the steady state for the positive and negative step changes.

7. Discussion Despite many advantages of using ethanol produced from biomass as a fuel (it is a high-energy, clean burning and totally renewable liquid fuel), it will only substitute gasoline if its production is economically competitive. Thus, there is an increased interest in the optimization of all the steps of ethanol production.

One way to improve the productivity of a product inhibited fermentation such as ethanol production is the continuous removal of the product as it is formed. Several attempts have been made to achieve simultaneous separation of ethanol using various product removal methods [2]. The fermentation process coupled with a vacuum ash vessel proposed by Silva et al. [10] and studied in this work presented a high productivity (2122 kg/(m3h)) when compared to the industrial conventional process proposed by Andrietta and Maugeri [12]. This process was optimized by Kalil et al. [16] and presented a productivity of 12 kg/(m3h). A key to the successful design, optimization and control of an appropriate industrial process is a thorough understanding of the systems dynamics. A mathematical model based on fundamental mass balances and kinetic equations using experimental parameters described as functions of the temperature has been used to investigate the inuence of operational variables on yield and productivity, using the method of factorial design and response surface analysis. Under the determined conditions the productivity attained was 21 kg/ (m3h) and the yield was 82%. The reactor volume was 254.7 m3. The operational conditions determined by Silva et al. [10] led to productivity and yield of 22 kg/(m3h) and 81%, respectively. The volume of the reactor, however, was 339.8 m3, 32% higher than that obtained in the present work. In both cases the productivity was higher and the reactor volume was lower than in an industrial conventional process [12,15]. Yield and conversion, however, were lower. Higher yield and conversion, of 86.4% and 98%, respectively, can be obtained, but productivity decreases to 15 kg/(m3h) and the reactor volume increases to 358.6 m3. The industrial operation of the extractive fermentation process requires the development and implementation of an efcient control strategy, able to keep the

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main process variables in its set points in spite of load disturbances and/or set point changes. The DMC controller has great potential for industrial application, because this algorithm is considered robust and easily implemented [20]. To choose the best structures for an efcient control of the alcoholic fermentation, its dynamic behaviour has been studied. The factorial design methodology was successfully used to achieve this goal. It was shown that the operating conditions have a strong inuence on the performance of the control algorithm. If the extractive process is operated at the conditions determined in this work, substrate concentration is easily controlled by the manipulation of F0. Product concentration, however, cannot be controlled in at least one situation (disturbance of 20% in S0). The operation of the extractive process at the conditions determined by Silva et al. [10], in spite of requiring a higher reactor volume, enables the control of both substrate and product concentrations. This shows the importance of the study of the dynamic behavior of the process before designing an industrial plant. The methodologies used in this work (factorial design and response surface analysis combined with simulation) were adequate for the optimization and determination of control structures for the extractive ethanol fermentation. They can be applied to any other fermentation process, independently of the number of variables, provided that a representative mathematical model is available.

Acknowledgements The authors acknowledge FAPESP (process number 98/09198 6) and CAPES for nancial support.

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