a r t i c l e i n f o abstract
Article history: Fluid bed drying and near infrared (NIR) spectroscopy are technologies widely used to dry and measure
Received 15 July 2011 moisture content and other pharmaceutical granular materials’ attributes, respectively. This work
Accepted 6 November 2012 focused on controlling a bench top fluid bed dryer using an industrial control system, the model
Available online 13 December 2012
predictive control (MPC) strategy, and NIR measurements of the moisture content of pharmaceutical
Keywords: powders. The MPC was implemented to reach the desired drying end-point while simultaneously
Fluidized bed dryer manipulating two variables: airflow and inlet air temperature. These two manipulated variables were
Model predictive control constrained based on the physical and chemical behavior of the process. The results showed that the
Process analytical technology use of the MPC with the inline NIR produced an adequate control performance and resulted at the same
Optimization
time in a reduction in energy consumption of as much as 60% in one case when compared with the
Energy reduction
current industrial practices.
& 2012 Elsevier Ltd. All rights reserved.
0967-0661/$ - see front matter & 2012 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.conengprac.2012.11.002
510 L. Obregón et al. / Control Engineering Practice 21 (2013) 509–517
the fluid bed drying process. In general, low order transfer functions airflow and temperature, this implementation will represent a
(representation of differential equations in Laplace domain) provide reduction in the cost of production. Focusing on this opportunity
simple equations that describe both the steady- and the unsteady- to reduce the consumption of energy in fluid bed drying, this
state behavior of the process variable (in this case, the powder work concentrated on: (1) developing representative transfer
moisture content) as a function of the manipulated variables, function models to capture the governing phenomena of drying,
temperature and air flow in FBD. They also provide sufficient (2) validating the use of MPC with clamped inputs and NIR as the
information to achieve optimization of a process with an adequate sensor to control a real batch fluid bed dryer with an industrial
technique (Temple et al., 2000). control system, and (3) demonstrating the real energy reduction.
Besides the modeling of the moisture content of the powders, The results will show that the MPC manipulated the airflow and
its real time measurement is essential to controlling the FBD temperature as necessary to achieve the set point (target value) of
process. As established by Wang et al. (2009), it is necessary to the moisture content with an adequate performance and reduced
have inline measurements of the powder moisture content. the energy consumption. The next section describes the equip-
Unfortunately, some process variables, such as moisture content, ment, materials, and procedures used in this research. The Results
require phenomena and technologies far more complex than section presents the NIR validation as an inline sensor, the fitted
those required by common variables, such as temperature, process model, and the controller performance with correspond-
pressure, etc. This need has prompted the development of sensors ing discussion and conclusion.
based on different fundamentals. One type of sensor (known as
soft sensor) focuses on predicting the control variable based on
readily available measurements. One example is the extended 2. Materials and methods
Kalman filter (EKF) (Li & Duncan, 2008), which uses a model of the
process, such as state space, to predict the control variable. In the 2.1. Materials
FBD, the EKF would predict the powder humidity. Although it has
been in use for some time, this technique’s performance depends The experiments were performed using lactose anhydrous NF
on the assumptions made during the development and its output Direct Tableting, similar to the one used in pharmaceutical
is just an estimate of the process variables. Due to the ever- products. This powder was granulated using only distilled water
present possibility of disturbances not accounted for during the with a pH range of 5.5–6.5 and conductivity 1.8 ms/cm. The
EKF development, the process variable estimate (and thus the distilled water was prepared on-site.
performance of the control system) can be highly inaccurate
during real operation. 2.2. Equipment
One strategy to avoid this is by using a sensor that directly
measures the process variable. Several examples include electric The process unit used for the experiments was a fluid bed dryer:
capacitance tomography (Wang et al., 2009), triboelectric probes Aeromatic AG STREA 1 model, Fig. 1. It consists of a blower with a
(Portoghese, Berruti, & Briens, 2008), microwave resonance variable speed motor that produces a steady operating range from
(Buschmuller, Wiedey, Doscher, Dressler, & Breitkreutz, 2008), 55 to 120 m3/h. The air enters through the bottom and exits through
and Near Infrared Spectroscopy (Rivera, 2004; Roggo et al., 2007). a HEPA filter at the top. It houses an electrical resistance at the
Among these techniques, near infrared spectroscopy (NIRS) pro- blower exit that enables the heating of the air. The inlet air
vides great advantages in sample analysis, such as its speed, low temperature was operated in the range from 25 to 100 1C through-
cost, and non-destructive characteristics (Roggo et al., 2007). out the entire experiment. The actual heating capacity of the
Advances in computational power have permitted the use of resistance exceeded the 100 1C but this upper limit was set in order
these large data-load sensors for inline measurements (Aditya, to protect both the unit and the powders. The power to the
Alcala , Jerez-Rozo, Muzzio, & Romañach, 2010; Liew, Karande, & resistance was manipulated by a solid-state relay.
Heng, 2010; Shia, Cogdillb, Shorta, & Anderson, 2008). However, The bowl of the FBD where the powders were placed has a
most works with NIR still refers to offline applications; therefore, volume of 16 L with a capacity of handling a maximum of 2 kg of
there is a need to validate the technique for inline control powders. The airflow rate was set so that the fluidized powders
application. did not surpass the variable-diameter section of the bowl. If the
One of the main interests in the FBD control problem, in the powders were not restricted, the internal filter would get clogged
case of batch operation, is to reach the desired moisture content and the operation had to be stopped. The bowl has several side
(end point) as fast as possible without violating any physical ports where the NIR probe could be placed for inline measure-
constraints and thus reducing the energy consumption. This ment. In this study, the probe was placed at 10.2 cm from the
control target could be achieved using techniques such as Model bowl’s bottom. The tip of the NIR probe was placed flush with the
Predictive Control (MPC) (Abukhalifeh, Dhib, & Fayed, 2003; De bowl’s wall so that it did not affect the fluidized powders inside
Temmerman, Dufour, Nicolaı̈, & Ramon, 2009; Didriksen, 2002; the bowl. A perforated plate is placed at the bottom of the bowl to
Dougherty & Cooper, 2003; Köni, Yüzgec- , Türker, & Dinc- er, 2009), help with the distribution of the air so that fluidization problems
Generic Model Control (Li & Duncan, 2008) or Fuzzy Logic are minimized. The dryer was accessorized with two sensors to
(Atthajariyakul & Leephakpreeda, 2006). Out of these, MPC is monitor the manipulated variables: a thermocouple for tempera-
the one most used in industrial applications. It uses a representa- ture and a differential pressure for airflow.
tive model, such as low order transfer functions, to compute A Distributed Control System (DCS), Delta V 10.0 controller,
optimal changes in the inputs, gas flow rate and temperature in with several communication cards and capability for OPC com-
the case of FBD, that would reduce future errors between the munication was used for the automation of the FBD. A Dell
desired value (set point) and the measurements of the control OptiPlex 755 computer contained all the commercial software
variable, in this case the moisture content by NIR; see Section 3.2 used throughout the experiments: (1) the CDI Spec32 program,
for more details. which was used to obtain NIR spectra by the detector, (2) a
If the target end point were reached as fast as possible with Umetric software SIMCA-Pþ 12.0.1, which was used to prepare
the implementation of the optimal changes in inputs, the opera- the moisture content predicting model, (3) SIMCA Q, which used
tion would use the lowest energy possible. Since the typical the spectra from Spec32 and the model from SIMCA-Pþ12.0.1
industrial applications run the FBD in open loop or with constant to generate a table of prediction values of the moisture content,
L. Obregón et al. / Control Engineering Practice 21 (2013) 509–517 511
and (4) SynTQ Version 3.5 for additional mathematical tools and described above. The speed of response of the NIR was around
communication with the Delta V controller using the OPC 2–3 s. The actual moisture content was measured using a Sartorius
protocol. MA 35 Loss On Drying (LOD) moisture analyzer. Powder samples of
The NIR detector used, model NIR 128 Element T.E. Cooled 5 g were used to determinate the humidity of the material inside of
InGaAs Array, is from Control Development Incorporated (South the FBD. The lactose was granulated using an Erweka Gmbh type
Bend, IN). It was configured to scan with a wavelength range from SW1/S high shear granulator.
1107 to 2218 nm. This detector was connected to the computer
2.3. System integration
Next, the pre-mixed materials (2 kg in total) were placed in the Rewriting Eq. (1) in time domain one obtains (Rivera, 2006)
high shear granulator, which was operated at 400 rpm for 5 min.
DWpðtÞ ¼ K F DF air,i ðt þ K T DT air,i ðtÞÞð1et=t Þ ð2Þ
This process produced a granulation with particle sizes ranging
from 200 to 600 mm. where t is the time constant, KF is the gain associated to the
airflow effect, and KT is the gain for the effect of air temperature.
2.5. Drying procedure for process modeling The LOD measurements of moisture content of the withdrawn
samples were used to fit these three parameters. The moisture
First, the FBD was conditioned at the desired operating condi- content value of several runs along with the corresponding
tions, especially the drying temperature of 60 1C. After condition- operating conditions and time was fed to a partial least square
ing the FBD, the airflow was stopped to add 1 kg of the granulated (PLS) algorithm, which fitted the parameters in Eq. (2) to the
lactose to the bowl. The bowl with the powder was then placed raw data.
back on the FBD and the air turned back on at the desired A limitation in using Eq. (1) to describe the drying curve is that
conditions of 90 m3/h for the entire drying time. Samples of the parameters are restricted to the conditions used to generate
powders were withdrawn every 2 min as the drying process the drying curve; i.e., the gains are dependent on the initial
was progressing to measure their moisture content and prepare moisture content and the equilibrium one and the time constant
the drying curves. At the end of the drying process, all the powder on the air flow used. Although if the drying were executed at
was withdrawn from the bowl to process another fresh 1 kg of other conditions than those used for the fitting, the model would
granulated material. The sample size was maintained at the require only adjustment of the parameters for the new conditions.
smallest possible (5 g) so that the processed mass of powder did Despite this limitation, the transfer functions are adequate, as will
not change substantially as to impact the drying rate. be demonstrated later, for control purposes.
The model was developed using spectra data of the moisture 3.1. Fitted process model
content of both static and dynamic samples. The static-sample
NIR spectra provided the isolated effect of moisture content in the The fitted parameter values of t, KF and KT are presented in
NIR absorbance while the dynamic-sample NIR spectra provided Table 1. The temperature related gain is the largest, implying a
the composed effect of real factors during the drying operation on largest effect of temperature on the drying for the entire process.
the NIR absorbance. This matches the theoretical impact of temperature in the drying,
For the development of the predicting model, 20 dynamic thus supporting the fitted values. Regarding t, the mass and energy
spectra were obtained while running the FBD right before with- balances establish that this parameter would be the same for all the
drawing, at each sampling time, the 5 g sample of the powders for transfer functions. Based on this, the estimation technique was
static analysis. The withdrawn powders were used for static forced to fit equal values of the time constants for both transfer
spectra and LOD analysis. First, 20 spectra of the static powders functions, although it is understood that experimentally they could
were taken and then each sample was placed in the LOD analyzer be different. Furthermore, the fitted model balanced the prediction
to determine the sample moisture content. The data generated error between the constant and falling rate, as per the estimation
(the 40 static and dynamic spectra and moisture content of each technique; therefore, it is not capable of precisely predicting the
sample) was added to the SIMCA Pþ, which contains the Partial transition point. In spite of, it is capable of predicting most of the
Least Square (PLS) model software generator. The data was first dynamics. Further work is still necessary to develop a model that
submitted to a PCA analysis followed by a first derivative filtering. fundamentally matches better the dynamics of a FBD.
This filtered data was then fitted by the calibration model by the The nominal values in Table 1 were the result of the fit of
PLS technique to obtain the NIR calibration model. Eq. (1) to the moisture content of several runs so that the fitted
values averaged the error in LOD measurements. The fitting
2.7. Development of the low order transfer functions process produced average values of SSE¼1.8, R2 ¼0.9784, and
RMSEC¼0.67. Fig. 3 depicts the raw data of a drying curve used
Low order transfer functions (Eq. (1)) describe the steady state for validation along with the predicted values by Eq. (2) with the
as well as the dynamics of continuous processes (Temple et al., fitted parameters. As can be seen, Eq. (2) was capable of predict-
2000). During the dynamics period, the dependent variable of an ing the actual moisture content with a small prediction error.
overdamped stable process varies monotonically from an initial
steady state to a new one. On the other hand, in batch processes 3.2. Model predictive control implementation
the dependent variable always changes from one value to
another; therefore, the batch FB drying could be seen as the 3.2.1. Controller
dynamics period of the continuous drying operation. The specific The Model Predictive Controller (MPC) actions were based on
assumption is that the continuous FB drying process is suddenly the control performance index in Eq. (3),
closed to the powders but the drying gas continuous flowing
T
causing the humidity content to decrease down to the equili- J ¼ Eðkþ 1Þ Q Eðk þ1Þ þ DUðkÞT RDUðkÞ ð3Þ
brium state. The low order transfer function will no longer be a
function of the inlet or outlet conditions but rather a function
Table 1
solely of the variables affecting the drying phenomenon: airflow Nominal fitted process model parameters.
rate and temperature. Eq. (1) represents such a phenomenological
model where the humidity content (Wp) is affected only by the Parameter Value
airflow rate (Fair,i) and air inlet temperature (Tair,i)
KF 0.0768
K F K T KT 0.0987
WpðsÞ ¼ F ðsÞ þ T ðsÞ ð1Þ t
ts þ 1 air,i ts þ 1 air,i 491 s
L. Obregón et al. / Control Engineering Practice 21 (2013) 509–517 513
where
2 3
k1 0 ... 0
6 k2 k1 & ^ 7
6 7
6 7
6
6 k3 k2 & 0 7
7
6 7
K ¼6 ^ & & k1 7
6 7
6 7
6 ^ ... ^ ^ 7
6 7
4 5
kp kp1 ... kðpm þ 1Þ
kn ¼ ð1etn =t Þ K F K T
The minimization of J at each sampling time produces optimal 3.3. NIR calibration model
control moves, DU(k), of the airflow and temperature for the batch
FBD application that when implemented minimize the error. The development of the calibration model based on static and
Eq. (5) is the un-constrained analytical solution of the control dynamics data followed Section 2.6. However, the complete
performance index equation to compute the optimal control description of the development of the model will be the subject
moves of a separate paper. Fig. 4 is included though to demonstrate the
o o accuracy of the NIR in predicting the actual moisture content. The
DUðkÞ ¼ ðK T Q K þ RÞ1 K T Q E^ ðkþ 1Þ ¼ K c E^ ðk þ 1Þ ð5Þ
diagonal line represents the real values while the symbols
where Ê 1(kþ1) is the error between the reference and the represent the predicted values. The average error of prediction
predicted trajectories of the moisture content and K is the was 0.25% with an average deviation of 0.04% plus, as it will be
dynamic matrix with a p rm dimension. shown later, it was adequate for control purposes.
Eq. (5) was used to compute the optimal values, which were
subjected to the following two physical constraints: (1) air flow over 3.4. Control performance
120 m3/h must be avoided so that the air did not carry the powders
to the filters at the exit of the FBD as flows below 40 m3/h so that 3.4.1. Control performance with nominal process parameters
the FBD did not shutdown, and (2) temperatures (over 85 1C) must Fig. 5 depicts the predicted moisture content of four different
be avoided since almost all pharmaceutical ingredients degrade at runs under closed loop, and Fig. 6a and b depicts the air flow and
those temperatures. The industrial control system allowed the temperature profile implemented for Runs ]1 and ]2, respec-
implementation of these two physical constraints only as clamped tively. The final predicted moisture content at any given time is
values, which is a limitation of the technology rather than the an average of the last three predictions including the current one.
technique. The implemented physical constraints read This was implemented to further decrease the scattering of the
prediction.
(1) 40 rF air ðtÞ r120
(2) T air ðtÞ r85 Table 2
Nominal values of the MPC tuning parameters.
Parameter Value
Fig. 6. (a) Inputs: setpoints computed by the MPC (top) and process values applied through the PIDs (bottom), nominal model, Run ]1. (b) Inputs: setpoints computed by
the MPC (top) and process values applied through the PIDs (bottom), nominal model, Run ]2.
Table 3
Non-nominal value of the MPC tuning
parameters.
Parameter Value
KF 0.05
KT 0.04
t 0.3
Q1 2.43 10 05
Q2 1.15 10 05
R 0.3
4. Conclusions
Acknowledgment
The authors appreciate the support of Pfizer Co., the NSF-ERC for
Structured Organic Particulate System (EEC-0540855) and INDUNIV,
a local consortium of industry, government and academia.
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