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of Process Synthesis
In this chapter, the importance of conceptual process design during the develop-
ment of innovative process configurations is analyzed. The utilization of some
useful tools for process design is highlighted, such as mathematical modeling and
simulation. The key role played by process synthesis methodologies is empha-
sized. The two major strategies for accomplishing process synthesis are discussed.
Main trends in knowledge-based process synthesis are briefly presented as well as
the main approach to carrying out optimization-based process synthesis.
Table2.1
Steps Involved in the Development of an Industrial Process
during Its Life Cycle
Stages Features
Analysis of the chemical reaction Study of chemical synthesis
Experimental development
Selection of the best stages for the synthesis
Conceptual process design Analysis of integration possibilities
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Integration of function
Heuristic design
Superstructure design
Superstructure optimization
Process development Experimental data obtained
Test reaction and separation process
Obtain kinetic and physical data
Pilot plant
Process assessment Evaluation of cost of equipment
Definition of control schemes
Detailed engineering Plant layout
Definition and construction of equipment
Pipeline design
Energy networks definition
Utilities design
Plant operation Scheduling
Stocks handling
Preventive maintenance and repave
End cycle of life Second use possibilities
Dismantle and recycle parts
not only the designers. In this way, processing features and market demands will
be taken into account during early stages of design, when the changes are easier
and less expensive to implement. Therefore, the problems, conflicts, and change
needs can be detected in time to carry out the necessary modifications with sub-
stantially less effort than by means of sequential engineering. In this framework,
concurrent engineering applied to design implies the integration of all life cycle
steps of a process in the early stages, attaining the achievements of several goals.
Thus, the research and development activities and conceptual design have to con-
sider not only the building of a plant, its operation, control, and maintenance, but
also the achievement of technoeconomic, market, environmental, and even social
objectives. Practically, and for the case of commodities, the three first stages of
the process life cycle are accomplished in a concurrent (simultaneous) way. If the
synthesis pathways for a given product are already known, as in the case of fuel
ethanol, process design procedures are focused on the second and third stages in
Table 2.1.
In this book, these two steps are analyzed for fuel ethanol production empha-
sizing the related integrated processes. In fact, concurrent engineering elements
are considered when taking into account as evaluation criteria not only technical
indexes (yield, productivity, energy consumption), but also financial and envi-
ronmental indicators in the framework of process intensification. Financial and
environmental criteria correspond to the macro and mega scale levels of analysis
(plant and unit integration and interaction between market conditions and envi-
ronmental impact, respectively), as reported by Li and Kraslawski (2004). Just
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these two levels of analysis have been developed with more intensity in the past 15
years as a result of the globalization of the economy and worsening environment.
On the other hand, process and apparatus integration corresponds to the micro
scale level of analysis. At this level, process intensification through integrated
and hybrid processes with higher efficiency and less size has become the most
important development trend. This forced the change of the old paradigm of a
chemical process made up of a series of unit operations where the processes and
apparatus are coupled (meso scale). Finally, the nano scale (molecular design and
new materials) has become crucial for designing processes to obtain very high
value-added products.
The task of defining an appropriate process configuration requires the genera-
tion and evaluation of many technological schemes (process flowsheets) in order
to find those exhibiting better performance indicators. This task is called process
synthesis. In a process synthesis problem, system inputs (type, composition, con-
ditions, and flowrates of raw materials) and outputs (product flowrate and speci-
fications, effluent streams constraints) are given and the task consists of defining
the configuration of the process flowsheet or, in other words, the topology of the
technological scheme, which allows the synthesis of the product from the feed-
stocks entering the process. For this, at least one comparison criterion should be
established with the aim of evaluating different alternative process flowsheets
proposed in order to choose that with the better performance.
The configuration comprises the type and amount of unit processes and opera-
tions required by the overall process as well as their interconnection (intermedi-
ate, recycle, and purge streams) and the parameters of that configuration (mostly
those ones related to operating conditions: flowrates, temperatures, pressure,
compositions). Process synthesis procedures can be applied not only to the con-
ceptual design of new processes, but also to the retrofitting of existing ones. Some
approaches for process synthesis involve and apply fundamental concepts of ther-
modynamics as the starting point for generating new alternative process configu-
rations. Thus, energy consumption (calculated by enthalpy balances) of different
flowsheets can be helpful for selection of the best alternatives. In a similar way,
the concept of useful energy or exergy (widely employed in mechanical engineer-
ing) can also be employed as a criterion for selection of alternatives. Recently,
more global concepts from the ecology field, such as emergy, have been used for
choosing the best configuration of a process (see Section 2.2.5).
During the next step of the life cycle of an industrial process, process analy-
sis, the structure of the selected technological scheme is established in order to
improve the global process through its more comprehensive insight. The type of
problems undertaken by process analysis is summarized as follows: given the
process inputs and once determined the technological configuration of the pro-
cess that includes each one of the unit operations and processes involved, as well
as their parameters, find the system outputs. The analysis is aimed at predicting
how the given process behaves. It involves the process decomposition into its con-
stituent elements for the individual study of each unit performance. The detailed
features of the process (flowrates, pressures, temperatures, compositions) are pre-
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into several subproblems (Gani and Kraslawski, 2000). In this book, these sub-
problems can comprise the following jobs applied to the production of fuel
ethanol:
To undertake this task, a series of solving strategies has been proposed. They
can be classified into two large groups: knowledge-based process synthesis and
optimization-based process synthesis. The second group of strategies is oriented
to the formulation of a synthesis problem in the form of an optimization problem.
In turn, the first group of strategies is concentrated on the representation of the
design problem as well as the organization of the knowledge required by this
problem (Li and Kraslawski, 2004), i.e., it is oriented to the development of a
representation that is rich enough to allow all the alternatives to be included, and
smart enough to automatically ignore illogical options. In general, the proce-
dure of generating multiple alternative process flowsheets is carried out through
different strategies implying, for instance, the combination of heuristic rules with
evolutionary strategies for process design. Heuristic methods are particularly use-
ful when very large and complex problems are dealt with. Usually, these methods
are often based on the observation of how many other problems of the same type
are solved. Knowledge-based methods imply an evolution in the learning of the
research subject as the proposed problem is being solved. This, in turn, leads to
the generation of new and better alternatives. Nevertheless, it is impossible to
ensure that the optimal structure can be achieved when heuristic methods are
employed (Westerberg, 2004). Some approaches for knowledge-based process
synthesis mostly used in process systems engineering, as well as the most innova-
tive and perspective ones, are briefly described below.
2.2.1Evolutionary Modification
Evolutionary modification is the conventional approach for process synthesis
based on the experience of engineers and researchers. This approach condenses
this experience into a programmed set of heuristic rules intended to making deci-
sions on the process structure. Considering that this method corresponds to a trial-
and-error approximation, its main limitation consists in the difficulty of obtaining
relevant information in a way suitable for computational calculations.
2.2.2Hierarchical Decomposition
The hierarchical heuristic method is an extension of the purely heuristic approach
that entails the evolutionary modification and combines the heuristic rules with
an evolutionary strategy for process design (Li and Kraslawski, 2004). Douglas
(1988) proposed a method by which any process can be decomposed into five lev-
els of analysis for its design. This strategy has a hierarchical sequential character
considering that in each level of analysis different decisions are made based on
heuristic rules. This allows generating different alternatives, which are evaluated
from an economic point of view using short-cut models. As the method is applied
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in each one of the five levels, more information becomes available and the tech-
nological scheme of the process evolves until its completion. According to this
author, hierarchical decomposition comprises the analysis of the process in the
following levels:
Reactor
Separation and recycle system
Heat recovery system
Heating and cooling utilities
Wastewater and effluent treatment
The design begins with the reactor selection to move toward the outer surface
of the diagram by adding other layers, such as the separation and recycle system.
These heuristic methods emphasize the decomposition strategy and screening of
alternatives, which allow the fast identification of technological configurations
often located near optimal solutions (Li and Kraslawski, 2004). However, the
main drawback of these methods is the impossibility of handling the interactions
among the different levels or layers due to their sequential character. In spite
of this, the nature of this approach allows rapidly discarding many alternative
configurations not leading to good designs. In addition, the analysis by design
levels permits the utilization of process simulators with which the process flow-
sheets are completed in an evolutionary way. This methodology has been mostly
applied to chemical and petro-chemical processes. Nevertheless, the utilization
of these procedures and design schemes is less frequent in the processes of the
microbiologic industry.
2.2.3Phenomena-Driven Design
The phenomena-driven approach for process synthesis considers as a starting
point for the design, not the unit operations, but the phenomena occurring in
them at a lower level of aggregation (Gavrila and Iedema, 1996). Reactions, phase
changes, heat and mass transfer, and mixing are considered among the phenomena
included in this method. The design problem is divided (decomposed) into three
tasks: role assignment, phenomena grouping, and operating condition analysis.
The goals of these tasks can be formulated through the following questions:
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What should occur in the process in order to achieve the global design
target?
Where should it occur?
When and how should it occur?
In the second task, the alternative designs are proposed by grouping the phe-
nomena in units and the continuous variables are described as Boolean variables
(for instance, is the rate of a phenomenon equal to zero or greater than zero?).
In the third task, the favorable conditions in the units are defined employing
ordinal relations among quantities (dR/dt > dS/dt; Gavrila and Iedema, 1996).
This method is oriented to explore innovative units and processes in order to sup-
port the creativity during the design process. However, the method is based on
an opportunistic identification and integration of the tasks as pointed out by Li
and Kraslawski (2004). This approach has been applied to very particular cases
as in the production of methyl tert-butyl ether (MTBE) by reactive distillation
(Tanskanen et al., 1995).
2.2.4Conflict-Based Approach
In the framework of the conflict-based approach, process synthesis is defined as
the process of decision making for identifying and handling the design conflicts
in order to satisfy multiobjective requirements (Li, 2004). Under this concept, a
design problem is decomposed into subproblems instead of applying a hierarchical
design. This allows for overcoming the drawback related to the interactions among
several hierarchical levels of analysis. The design problem is represented by the
conflicts among the interrelated design objectives or by the features of the techno-
logical scheme (Li and Kraslawski, 2004). Undoubtedly, this approach represents a
change of paradigm in process design, although some aspects should be developed,
such as the quantification of the conflicts and heuristic rules in function of their
contribution to the conflicts as well as the development of the solving algorithms.
which the user does not have direct access. Thus, the simulation is solved taking
into account the strict order of the units (from feedstocks to end products) mak-
ing up the process flowsheet. Main drawbacks of the optimization-based strategy
are related to the fact that the optimal configuration can only be found within
the alternatives considered in the formulated superstructure (Li and Kraslawski,
2004). Furthermore, this approach has the additional disadvantages of having a
significant mathematical complexity as well as the difficulties arising during the
definition of the superstructure of technological configurations, i.e., the difficulty
to ensure that the initial superstructure contains the best solution (Barnicki and
Siirola, 2004). In this sense only, it is possible to formulate the design problem
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Alternatives of
superstructure Selected diagram
MILP
algorithm
Start
Process model
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NLP
optimizer
Optimal
solution
Figure 2.1 Conceptual diagram of one of the algorithms most used for optimization-
based process synthesis.
algorithm, whereas the optimal values of the operating parameters are found in
the inner loop based on NLP. The best technological configuration of the process
that maximizes or minimizes the employed objective function is identified by
repeating and executing these two loops. For this configuration, the optimal val-
ues of its operating parameters are defined as well.
The solution of NLP problems is usually based either on successive quadratic
programming (SQP) or on reduced gradient methods. Among the main solu-
tion methods of MINLP problems are the branch and bound method (Gupta and
Ravindran, 1985), generalized Benders decomposition (Geoffrion 1972), and outer
approximation (Duran and Grossmann, 1986). A new trend for solving MINLP
problems is the generalized disjunctive programming whose formulation includes
the condition that one of a set of three types of constraints should be exactly satis-
fied (Lee and Grossmann, 2005; Raman and Grossmann, 1991). The three types
of constraints comprise global independent inequalities concerning discrete deci-
sions, disjunctions that are conditional constraints involving the operator OR, and
logic pure constraints involving Boolean variables (Grossmann et al., 2000).
The formulation and solution of the main types of mathematical program-
ming problems can be accomplished in an effective way using specialized com-
puter programs, such as GAMS (Generic Algebraic Modeling System; GAMS
Development Corporation, 2007). This system requires that the models and the
formulation of the optimization problem be explicitly introduced in algebraic
form. It automatically creates an interface with the solution codes for various
types of problems (solvers). This offers a great advantage because it makes its
main efforts to formulate the problem itself and not to develop methods for solv-
ing it. GAMS has a powerful set of solvers for different optimization problems
(LP, NLP, MILP, and MINLP, among others). Moreover, it makes possible the
input of indexed equations that is very useful in the case of large-sized models.
The NLP methods ensure that the global optimum can be found if and only if
both the objective function and the constraints are convex (Floudas, 1995). If this
is not the case, the location of the global solution cannot be guaranteed. The rigor-
ous or deterministic methods for global optimization ensure an arbitrarily close
approximation to the global optimum and, in addition, carry out the verification
if this approximation has been attained. These methods include the branch and
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bound method, methods based on interval arithmetic (Byrne and Bogle, 1996;
Stadherr, 1997) and generalized disjunctive programming (Lee and Grossmann,
2005), and procedures with multiple starting points in which a local optimizer
is invoked from these points (Edgar et al., 2001). In the past few years, signifi-
cant advances in the methods of rigorous global optimization have been achieved.
These methods assume that special structures in these types of problems are pres-
ent, such as bilinear, linear, fractioned, and separable concave functions. It has
been demonstrated that the algebraic models always can be reduced to these sim-
pler structures if they do not involve trigonometric functions (Grossmann et al.,
2000). Floudas (2005) points out that the most important advances in determinis-
tic global optimization belong to the following categories: convex envelopes and
convex underestimators, twice continuously differentiable constrained nonlinear
optimization problems, mixed-integer nonlinear optimization problems, bilevel
nonlinear optimization problems, optimization problems with differential-alge-
braic equations, grey-box and factorable models, and enclosure of all solutions.
Other types of techniques for global optimization correspond to nonrigorous
or heuristic search methods. These methods can find the global optima, but do
not guarantee and generally are not able to prove that the global solution is found
even if they do so. However, these procedures often find good solutions and can
be successfully applied to MINLP problems. In such cases, the heuristic method
starts with a starting solution and explores all the solutions in a certain vicinity
to that starting point, looking for a better solution. The method repeats the pro-
cedure every time a better solution is found. The metaheuristic methods direct
and improve the search with a heuristic algorithm. Tabu search, sparse search,
simulated annealing, and genetic algorithms belong to this category (Edgar et al.,
2001). In particular, stochastic methods, such as simulated annealing (Kirkpatrick
et al., 1983) and the genetic algorithms (Goldberg, 1989), have gained more and
more popularity, do not make any assumptions on the form of the functions, and
require some type of discretization, and the violation of the constraints are tack-
led through penalization functions (Grossmann et al., 2000).
2.3.2 Superstructures
One of the main challenges in the optimization-based synthesis of technological
schemes is the definition of the superstructure of alternatives that contains the
best solution. Most of the works reported have been based on the hand representa-
tion of the superstructure for each particular problem without following general
rules. To generalize this procedure, the definition of the representation type for
the superstructure is needed. Among the main types of representation proposed
are the statetask network and the stateequipment network. In the first type, two
classes of nodes (states and tasks) are used for the representation; the assignment
of equipment is dealt implicitly through the model. In the second type of repre-
sentation, the states and the equipments are employed as the nodes; the tasks in
this case are treated implicitly through the model (Grossmann et al., 2000).
Other crucial aspect during optimization of superstructures consists in how
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2.3.3Hybrid Methods
Hybrid methods for process synthesis make use of mathematical programming
techniques based on optimization in combination with the knowledge-based
approach. For instance, the synthesis of heat exchange networks has been improved
by optimization employing a heuristic approach based on physical phenomena
(Gundersen and Grossmann, 1990). A method for process synthesis exploiting the
advantages of mathematical programming that uses MINLP techniques and hier-
archical decomposition maintaining the consistency of its fundamental principles
has been developed. The method consists of solving the whole technological
scheme in each decomposition level. Aggregated models (black box models)
are utilized for the subsystems that are in the lower hierarchical levels, evaluat-
ing in this way their interaction with the detailed MINLP problem of the current
subsystem that is being analyzed. The subsystems are: reaction, separation, and
heat integration (Daichendt and Grossmann, 1997). In this way, the solution of a
large-scale MINLP problem is avoided.
2.4Final Considerations
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The absolute majority of methods for conceptual process design have been devel-
oped for processes of basic chemical and petro-chemical industries. Most of these
approaches are especially oriented to the design of separation schemes, particularly
distillation trains. For this reason, there is a paramount interest in the application
of these methodologies to biotechnological processes, which are of a complex and
highly multicomponent nature. None of the described approaches can be applied
in a generic way to any type of synthesis problem, even more so in the case of
biological processes. Considering this, the application of a minimum of two strate-
gies or synthesis procedures is required to undertake the design of processes for
fuel ethanol production with a high technoeconomic and environmental perfor-
mance. In this way, a higher amount of possibilities can be covered allowing the
creativity during the design process that is the source of innovation. Therefore,
the employment of synthesis strategies that systematically compile and utilize the
accumulated knowledge around a research subject, such as fuel ethanol, directly
contributes to screening and filtering the best alternative process configurations.
Further, some of the approaches mentioned above were applied to the genera-
tion of different process flowsheets with a high technical, economic, and envi-
ronmental performance. Thus, both the hierarchical decomposition method and
optimization-based strategies were used for the main process steps needed for
ethanol production. For specific process steps, such as the synthesis of separation
and ethanol dehydration scheme, the analysis of the statics and the exergy balance
were also employed. These issues will be discussed in following chapters.
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