Revista Facultad de Ingeniería, Universidad de Antioquia, No.112, pp.

34-44, Jul-Sep 2024

Optimum design of an acetylated starch

plant from Manihot esculenta Crantz, variety
INIVIT-Y-93-4
Diseño óptimo de una planta de almidón acetilado proveniente de Manihot esculenta Crantz,
variedad INIVIT-Y-93-4
Amanda Acosta-Solares1* , Omar Pérez-Navarro1 , Ernesto Sánchez-Cabrera2 , Jorge Luis
Pérez-Díaz3
1
Department of Chemical Engineering. Faculty of Chemistry and Pharmacy. Universidad Central “Marta Abreu” de Las
Villas. Road to Camajuaní km 5 ½, 54830 Santa Clara, Cuba.
2
Aditivos y Energéticos SA de CV. Humberto Lobo 9304 Industrial park Ciudad Mitras, García, Nuevo León, México
3
Universidad de Ciencias Médicas “Dr. Serafín Ruíz de Zárate”. Aqueduct and Bypass Roads, 50200 Santa Clara, Cuba.

ABSTRACT: Considering the applicability and added value of acetylated starches,

it is necessary to find technological variants to obtain them with favorable
technical-economic results and energetic and environmental compatibility. The
CITE THIS ARTICLE AS: objective of the work is to optimize economic and dynamic indicators of profitability
A. Acosta-Solares, O. of acetylated starch production, by considering as optimization criteria the productive
Pérez-Navarro, E. capacity, the degree of substitution and the temperature of the drying air, establishing
Sánchez-Cabrera and J. L. the design of the installation in optimal conditions. Technologies adopted from the
Pérez-Díaz. ”Optimum design mechanized native starch processes were selected, and the design and development
of an acetylated starch plant of the slurry heating, acetylation, and pneumatic drying stages were proposed. A
from Manihot esculenta composite central experimental design was generated for profit (P), net present
Crantz, variety INIVIT-Y-93-4”, value (NPV), and internal rate of return (IRR), and the quadratic models obtained
Revista Facultad de Ingeniería through the Response Surface Methodology were optimized. For the evaluation of the
Universidad de Antioquia, no. indicators, the economic indexes of the process were determined, after technological
112, pp. 34-44, Jul-Sep 2024. selection, material and energy balances, and technological design. The optimum
[Online]. Available: https: operating parameters are achieved at a production capacity of 12.57 tcassava /d, degree
//www.doi.org/10.17533/ of substitution of 0.505 and 124.98 °C in the air supply to the pneumatic dryer. Under
udea.redin.20231238 these conditions, the production of acetylated starch requires larger volume acetylators
than for acetylated gelatinized starch process, but the technological requirements of
ARTICLE INFO: gelatinized pulp are eliminated, achieving remarkable energy efficiency with pneumatic
Received: September 30, 2022 drying.
Accepted: December 13, 2023
Available online: December RESUMEN: Atendiendo a la aplicabilidad y valor agregado de los almidones acetilados,
13, 2023 es necesario encontrar variantes tecnológicas para su obtención con resultados
técnico-económicos favorables y compatibilidad energética y ambiental. El objetivo
KEYWORDS: del trabajo es optimizar indicadores económicos y dinámicos de rentabilidad de la
Acetylated starch; cassava; producción de almidón acetilado, considerando como criterios de optimización la
economic and dynamic capacidad productiva, el grado de sustitución y la temperatura del aire de secado,
indicators; optimization;
Energy efficiency
estableciendo el diseño de la instalación en las condiciones óptimas. Se seleccionaron
tecnologías adoptadas desde los procesos del almidón nativo por vía mecanizada
Almidón acetilado; yuca; y se propuso el diseño y desarrollo de las etapas de calentamiento de la lechada,
indicadores económicos y acetilación y secado neumático. Se generó un diseño experimental central compuesto
dinámicos; optimización;
eficiencia energética
para la ganancia (G), el valor actual neto (VAN) y la tasa interna de retorno (TIR), y se
optimizaron los modelos cuadráticos obtenidos mediante la Metodología de Superficie
de Respuesta. Para la evaluación de los indicadores, se determinaron los índices
económicos del proceso, previa selección tecnológica, balances de materiales y energía
y diseño tecnológico.

* Corresponding author: Amanda Acosta Solares

E-mail: [email protected]
ISSN 0120-6230
e-ISSN 2422-2844

34 DOI: 10.17533/udea.redin.20231238
Los parámetros óptimos de operación se alcanzan a una the average number of substitutions per AGU, whose
capacidad productiva de 12.57 tyuca /d, grado de sustitución maximum achievable value is 3, coinciding with the
de 0.505 y 124.98 °C en la alimentación del aire al number of available reactive hydroxyl groups [10]. AS are
secadero neumático. En estas condiciones, la producción applied as facilitators of aqueous suspensions in the food,
de almidón acetilado requiere reactores para la acetilación chemical, and pharmaceutical industries at DS less than
de mayor volumen que los del proceso de almidón 0.6. When their DS is higher than 1.5, they are used as
gelatinizado acetilado, pero se eliminan las exigencias thermoplastics. For DS between 0.6 and 1.5, they form
tecnológicas de la pasta gelatinizada, alcanzándose una highly viscous suspensions [3].
notable eficiencia energética con el secado neumático.
The characteristics of the technologies for acetylated
gelatinized starch from cassava have been addressed in a
1. Introduction study that includes the design and scale-up of equipment
[11]. This is based on experimental evaluations of process
Manihot esculenta Crantz (popularly known as cassava, conditions, kinetic studies, and thermodynamic analyses
manioc or tapioca) belongs to the Euphorbiaceae family, [2, 5, 12], which also consider direct acetylation as an
which consists of about 7,200 species. About 98 species intermediate stage. In both cases, carrying out the
of the genus Manihot have been described, of which only physical and/or chemical modification is possible and
cassava is economically relevant and cultivated. Due to convenient when the product is in an aqueous solution
its composition and, above all, its energy value and other instead of isolating it as a dry solid and dissolving it in
characteristics, such as its binding power, it is possible water afterwards. For that reason, the most common
to obtain a range of industrializable products [1]. Among technological modification situation is gelatinization
them, starch stands out for its applicability and added followed by acetylation or only acetylation as intermediate
value [2]. With the development of cassava processing steps that need to be designed through the development
industries, it is possible to obtain native starch that has of its processes.
been structurally modified by physical, chemical, or
enzymatic means, with functional properties superior to These studies show that the kinetic constant for the
those of the natural product [3]. acetylation of cassava starch of the INIVIT Y-93-4 variety
is higher when starting from gelatinized material than
As part of the physical transformations of starch, from native material. Thus, the physical modification step
gelatinization, and pregelatinization have multiple facilitates and accelerates nucleophilic substitution due
applications in the chemical and food industry [4], and to the structural fractionation involved in gelatinization
methods and technologies for obtaining precolloidal [13]. However, although these effects increase the DS,
starch have been developed on this basis [2, 5]. On the they give rise to rheological difficulties that increase the
other hand, enzymatic modifications avoid generating technological requirements of the process and do not
harmful by-products by possessing product specificity allow the gelatinized suspension to be dehydrated by
and substrate selectivity. This method has been traditional physical means, forcing the use of spray drying
successfully used to decrease the maximum viscosity [3].
and retrogradation value of starch paste [6]; however,
the cost of using enzymes is still a limiting factor for its As a consequence of the above criteria, the size of
industrial use. Finally, the different ways of chemical the acetylating units is reduced when gelatinizing prior
transformation of native starch should be highlighted to acetylation, but the energy consumption associated
for their applicability [7]. Among the most attractive is with mechanical agitation increases considerably. In
esterification catalyzed in a basic medium [8]. As evidence addition, from the rheological studies carried out for
of its use, several authors report the acetylation of physical modification [5], a very high fuel consumption
starches from different sources, where the modification of rate is derived in the spray drying process, representing
the hydrophobic behavior of the polymer makes acetylated a severe energy and environmental difficulty in producing
starches (AS) attractive for multiple industrial applications acetylated gelatinized starch. However, the feasibility
[9]. study carried out [2] showed that, despite the previous
drawbacks, the technological proposal developed allows
In a basic medium, it is possible to split the hydroxyl the production of a refined and high-value product, with
groups present in the interlinked Anhydro Glucose Units stable quality and multiple uses, obtained in processes
(AGU) present in the starch structure, releasing the with demanding technology and requirements, and
hydrogen from the C-O bonds in the C2 , C3 , and C6 reaching a satisfactory technical-economic effectiveness
positions [3]. It should be noted that the new properties [14].
will depend to a large extent on the degree of substitution
(DS) obtained. It is understood that the DS indicates

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 A. Acosta-Solares et al., Revista Facultad de Ingeniería, Universidad de Antioquia, No. 112, pp. 34-44, 2024

On the other hand, a technological proposal for AS would mass flow rate (WL ) in kg/h, and the density of the slurry
demand larger acetylators due to the speed reduction; in to be gelatinized (ρL ) in kg/m3 , was calculated by the
this case, the rheological disadvantages of gelatinization expression:
are not present. Therefore, it is possible to work the output tc × W L
VC = (1)
concentration of the concentrator centrifuges at levels ρL
higher than those of gelatinized starch, although lower
For an acetylator unit, considering a perfect mixing flow
than those of native starch via mechanized processing.
pattern, the space time (τ ) and therefore, the acetylator
According to the kinetics and product distribution reported
volume (V), was calculated by applying the design equation
for AS of low substitution degree [12], in the pneumatic
[16] shown in expression (2), for the volumetric flow rate
drying operation, an intermediate fuel consumption rate 3/h
of gelatinized slurry (v0 ) expressed
( 0 )in m , the 3initial
is estimated between the variants of native starch and
concentration of active AGU CR0− in kmol/m , the
acetylated gelatinized starch.
acetylation rate (−rRO− ) in kmol/m3 h, and the expected
monoacetyl glucose conversion X(RO− ) [11] expressed in
In view of the previous results and the fact that the direct
a fraction.
chemical modification variant has not been implemented V C 0 − · X(R0− )
with all the rigor in terms of technological design and τ= = R0 (2)
v0 −rR0−
technical-economic and environmental assessment, the
objective of the present research is to optimize economic For the battery of three continuous reactors with stirring
and dynamic indicators of profitability of acetylated starch in series, it was considered that each unit (i) has a partially
production, considering as optimization criteria the converted feed [16], where the graphic design method was
production capacity, the DS and the temperature of the applied, at a temperature of 48 ºC set at the heating stage.
drying air, establishing the design of the installation under Additionally, the concentration of monoacetyl glucose
optimum conditions. (CRAC ) was determined under the conditions previously
reported [12] and at low DS [11], where DS is considered as
the mole fraction of monoacetyl glucose substituted at C6 ,
2. Technologies taking into account the low probability of poly substitution
when acetylated for values below 0.6. Also, the kinetic
constant at the working temperature [2] was obtained to
2.1 Selection of technologies for the calculate the acetylation rate.
production of AS
The agitation parameters and conditions were determined
The characterization of technologies for the gelatinization,
by scaling up the previously reported conditions during
acetylation, and drying stages was considered, taking into
acetylation tests [12]. These tests were carried out on
account the rheology of gelatinized pastes [3, 11] and the
equipment with a volume equal to 0.004 m3 , a diameter
pneumatic drying stage for cassava flours [14]. An analysis
and height of 0.171 m, an impeller diameter of 0.085 m,
of the existing technologies for the treatment of native
and an agitation speed of 650 rpm. Geometric similarity
cassava starch [15] and of the proposals for acetylated
and constant stirrer tip speed were used as scaling criteria
gelatinization mentioned previously, made it possible to
for the acetylated gelatinized starch process [11].
select a suitable technological variant for the production
of AS directly from its native state.
An enthalpy of acetylation of native and acetylated
cassava starch of −28.4 kJ/molAS [2] was considered
2.2 Technology design for slurry heating, according to the contribution method of Joback’s groups.
acetylation, and pneumatic drying According to its composition, the heating power of Cuban
crude oil (CC) was estimated at 44,725 kJ/kg [14]. The
In the technological design of the acetylation stage, electrical power demands for heating and acetylation
recently reported methods and design equations [11] were were calculated according to the procedure established
used, which consider the determination of the volume by for jacketed vessels [17–19].
analytical and graphical means in the gelatinization and
acetylation stages. These methods were slightly modified Finally, the design of the pneumatic cylindrical duct
by replacing the gelatinizer with the slurry heater tank, dryer was based on the classical method previously
which heats the starch solution from room temperature to proposed [20], which has been currently used in the design
48 °C [5]. of this stage of the cassava flour production process [14].
Pneumatic systems were set up with a single dryer and
The capacity demanded by the slurry heater, with starch reflux up to an inlet moisture content of 30 % [2].
cylindrical geometry and flat bottom (VC ) expressed in Since drying occurs by evaporation of moisture during
m3 and considering the heating time (tC ) in hours (h), the the transport of the paste by a hot air stream, the flow

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A. Acosta-Solares et al., Revista Facultad de Ingeniería, Universidad de Antioquia, No. 112, pp. 34-44, 2024

arrangement was in parallel [21]. The heat associated A 2k full factorial design was generated for the factorial
with the solid drying demands was determined through portion of the CCD, a central point in the cube, and 2k
the energy balance, considering the sensible heat for axial points at a rotational distance α = 1.681 from the
paste heating and the latent heat required for moisture center of the design for a total of 15 runs, the results
evaporation. of which were plotted using OriginPro 2022 software.
Through regression analysis, the models were adjusted
for P, NPV, and IRR, which allowed obtaining the quadratic
3. Optimization equations that establish the dependence of the evaluated
responses with the independent factors for a significance
3.1 Modeling and optimization of project level of 5%. Optimization of the obtained surfaces was
economic indicators performed by means of chord analysis according to the
methodological bases and the heuristic procedure of the
The profit (P) associated with the production of AS was Response Surface Methodology for separate and multiple
determined from the total production costs and total sales responses [23].
of the main product AS and the by-product bran (dry fiber).

The net present value (NPV) and the internal rate of Estimated AS sales prices as a function of DS
return (IRR) [3, 14], were considered dynamic profitability Starch in its native state can be used primarily
indicators. These were determined based on the as a thickener and adhesive in the paper, textile,
productive capacity of the project (X1 ) expressed in pharmaceutical, and especially in the food industries
tcassava /d, the conversion achieved in the process (X2 ) [24]. Its prices, in the international market, have a high
expressed as DS, and the air feed temperature to the oscillation depending on the source, purity, and other
pneumatic dryer (X3 ). For this analysis, 15 years of the factors. The range of greatest stability in these prices
useful life of the project was estimated with a discount has been between 500 and 1,200 USD/t [25, 26], and is
factor of 10 %, and an installed capacity utilization of 50 % currently in the order of 700 to 900 USD/t [27].
was considered for the first year, 80 % for the second year,
and 100% from year 3 onwards [14]. However, these products have functional limitations
that limit their use in certain applications, mainly in
The investment and production costs of the process aqueous suspension and freezing, due to insolubility
were estimated using a classic methodology [22]. The at room temperature, retrogradation, and instability to
basic raw material, cassava roots, was considered to thermal and pH changes [28, 29].
be purchased at wholesale prices from a network of
agricultural producers set up for the project and valued at For these reasons, modified materials such as AS,
0.07 USD/kg. The rest of the raw materials and materials, which have much better functional behavior than the
including the esterifying agent, pH regulating and cleaning native material with multiple specific and highly effective
agents, as well as energy and natural resources, were food and industrial applications [30–32], are higher priced
valued at current updated international prices and were in the market. Given the above and the fact that DS
determined through material and energy balances. represents the advance of the chemical modification of
this material, an estimate was made of the probable price
A central composite experimental design (CCD), developed of AS, as a function of its DS. For this purpose, a list of
with Statgraphics Centurion XV. II. software, was used prices of AS from cassava, potato, and cereals for different
to determine the statistical models of the behavior of purity levels, applications, suppliers, etc., was obtained.
the economic indicators selected as a response to be The aforementioned relationship was obtained through
evaluated with the (k = 3) factors, capacity, DS, and drying multiple online consultations with different suppliers
air temperature. A range of variations of production [27, 33]. As a result, the extreme values were discarded,
capacity between 8 and 12 tcassava /d was considered, with and the following polynomial regression equation was
a maximum agricultural capacity of the region selected for obtained for a regression coefficient (R2 ) equal to 85.8%,
installation of the plant of 13.36 tcassava /d. For DS, a range which relates the price of AS (PAS ) in USD to DS:
of values was considered between 0.2, which is usable for
food applications, up to 0.5, at the limit of low values [2], PAS = 800 + 1.6 × 103 DS + 1.43 × 104 DS 2 −
but very useful as facilitators of aqueous suspensions. For (3)
5.95 × 104 DS 3 + 5.42 × 104 DS 4
drying air, a temperature range between 150 °C and 225
°C was considered, with a maximum permissible of 260
°C with drying times of up to 3 seconds, to avoid product
deterioration [2].
4. Results and discussion

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 A. Acosta-Solares et al., Revista Facultad de Ingeniería, Universidad de Antioquia, No. 112, pp. 34-44, 2024

4.1 Technologies for the production of AS Table 1 Niveles de las variables independientes

Mechanized native starch technology [2] can be used Levels

Independent variables
-1.681 -1 0 1 1.681
for the initial and final stages of this process. It uses a
Production capacity
sequence of washing-shelling, grinding, fiber separation, 6.636 8.000 10.000 12.000 13.363
X1 (tcassava /d)
purification, concentration, and dehydration of the starch DS X2 0.097 0.200 0.350 0.500 0.602
by vacuum filtration, and drying. For fiber separation, Temperature
124.43 150.00 187.50 225.00 250.56
X3 (ºC)
sieving centrifuges are used, and for purification and
concentration of the slurry, plate, and disc centrifuges are
used.
the estimated capacity of the acetylators and, therefore,
in the associated investment and operating costs. These
In the technological proposal for AS, this technology
effects suggest the existence of optimal values in the
can be adopted (assimilated), and the new slurry heating
considered intervals for X1 , X2 and X3 . It should be
and acetylation stages can be inserted into it. Heating
noted that the energy consumption rate per ton of cassava
and acetylation can be carried out in jacketed equipment
processed is very advantageous with respect to the
with agitation systems suitable for the rheology of
process of gelatinization prior to acetylation [3]. At the
the non-gelatinized suspension, which is much less
upper limit of the design for acetylated gelatinized starch,
demanding than that of the gelatinized material [5]. In
spray drying demands a rate of 0.22 tcc /tcassava [3], while
the case of AS, unlike acetylated gelatinized material, it is
for higher values of production and air feed temperature
possible to use the typical mechanical paste dehydration
at the upper limit of the design for AS, compared to the
processes used in the native starch process, and therefore,
previous process, pneumatic drying demands a rate of
the same pneumatic drying method is also applicable.
0.045 tcc /tcassava according to the values reported in Table
At this stage, air heating is ensured by indirect heat
2.
exchangers, using CC combustion as an energy option
when renewable options are not available. Figure 1 shows
Figure 2 shows the results of the estimation of the
the flow diagram for the slurry heating, acetylation,
total investment required, caloric energy costs, total
and pneumatic drying stages, where the first two are
production costs, and the economic indicators considered
highlighted, given their incorporation into the mechanized
in the optimization: P, NPV and IRR; valuing production
native starch process. Where W identifies water stream;
according to the DS achieved as shown in Equation 3.
HW, hot water; CS, concentrated slurry; GS, gelatinized
slurry; SH, sodium hydroxide; HA, hydrochloric acid; SP,
The results depicted in Figure 2 confirm the trend of
starch paste; A, air; S, starch; RS, recirculated starch;
increasing investment with increasing capacity and DS
H-AIR, hot air; RA, recirculated air; CC, Cuban crude; and
and decreasing heat energy cost with decreasing drying
ES, exhaust steam.
air temperature.

4.2 Behavior of project economic indicators 4.3 Optimal operational parameters

The three coded levels of the optimization parameters The second-order mathematical models (quadratic)
(X1 , X2 and X3 ) generated in the CCD are shown in Table relating the economic optimization indicators to the
1. independent variables (X1 , X2 and X3 ), obtained for the
applied design are shown in Equations 4, 5 and 6.
The results of the estimation of the main design
parameters of the main equipment of each stage and P = −507, 772 + 526254 × X1 + 1.82 × 106 × X2 +
the energy demand are shown in Table 2. The sizing of the
7752 × X3 − 2385 × X12 + 168781 × X1 × X2 −
heater corresponds to the application of Equation 1, that
of the acetylator to Equation 2, and that of the pneumatic 254 × X1 × X3 − 2.63 × 106 × X22 − 1505 × X2 ×
dryer following previously reported and applied methods X3 − 0.88 × X32
[14, 20]. The energy consumption and indexes refer to 20 (4)
hours of daily operation during 300 days per year.

These results show the tendency to increase the volume N P V = −3.92 × 106 + 332656 × X1 + 1.26 × 107 ×
required in the equipment and the energy demand for X2 + 2, 4143 × X3 − 1, 0529 × X12 + 1.17 × 106 × X1
drying when the capacity increases. Additionally, there is
a tendency to reduce the size of the dryer and the energy × X2 − 1793 × X1 × X3 − 1.83 × 107 × X22 − 1, 0169×
demand when the drying air temperature increases. On X2 × X3 − 5.5 × X32
the other hand, the increase in DS leads to an increase in (5)

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A. Acosta-Solares et al., Revista Facultad de Ingeniería, Universidad de Antioquia, No. 112, pp. 34-44, 2024

Figure 1 Flow diagram for the slurry heating, acetylation, and drying stages in the AS process. Source: Adapted from [2].

optimize the evaluated responses show similar behavior

in the three cases. This is beneficial for the subsequent
IRR = −30.12 + 5.38 × X1 + 159.53 × X2 + 0.005× establishment of optimization criteria for the three
responses simultaneously.
X3 − 0.126 × X12 + 4.583 × X1 × X2 − 0.0017 × X1 ×
X3 − 163.77 × X22 − 0.022 × X2 × X3 + 1.95 × 10−5 × To maximize P, NPV and IRR, the optimization of separate
X32 responses suggests operating with values of production
(6) capacity and DS close to or equal to the upper limit of the
In the statistical evaluation of the degree of adjustment to CCD. As for the influence of the drying air temperature,
the results of the design, the analysis of variance indicated these indicators benefit the lower limit of the study range.
that the adjusted models are significant for a p less than It should be noted that the values of the factors that
0.05. In all cases, the sum of squares of the pure error optimize the evaluated responses show similar behavior
was small with respect to the sum of squares of the total, in the three cases.
indicating good reproducibility at the central point [34]. This is beneficial for the subsequent establishment
Regarding the regression coefficient R2 , the adjusted of optimization criteria for the three responses
models explained the variability of the response in 99.92% simultaneously.
for Equation 4, 99.91% for Equation 5, and 99.95% for
Equation 6, with a good correlation with the source values This analysis achieved high desirability and allowed
and a good fit for their optimization. the establishment of the optimal operating parameters of
the AS production plant, at a production capacity of 12.57
With the fitted quadratic models, the optimization of the (tcassava /d) , DS = 0.505 and 124.98 °C in the air feed to
separate responses and the optimization of the multiple the pneumatic dryer, reaching a profit of 1,420,000 USD/y,
responses were performed, which are shown in Table an NPV of 9,090,000 USD, an IRR of 82.51 %.
3. The minimum and maximum levels of the factors
correspond to the extremes of the design represented in 4.4 Technological design in optimal
Table 1. This analysis made it possible to determine the
conditions
configurations of these factors (X1 , X2 and X3 ) that cover
the desired characteristics for the responses (P, NPV and The design is based on the previously defined optimum
0
IRR) simultaneously. conditions, a CR0− = 1.323kmol/m3 (at 20 % w/w),
isothermal operation at 48 °C and an AS concentration
To maximize P, NPV and IRR, the optimization of separate (CAS ) at the reactor outlet of 2.20 × 10−2 = kmol/m3
responses suggests operating with values of production [2]. Table 4 summarizes the results of the material and
capacity and DS close to or equal to the upper limit of the energy balance under these conditions.
CCD. As for the influence of the drying air temperature,
these indicators benefit the lower limit of the study range. The above results confirm that fuel consumption is
It should be noted that the values of the factors that significantly lower than for the production of acetylated

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 A. Acosta-Solares et al., Revista Facultad de Ingeniería, Universidad de Antioquia, No. 112, pp. 34-44, 2024

Table 2 Results of the sizing of the main equipment and energy demand in AS production

Experimental Factors Design Parameters Energy

Volume (m3 ) demand
Run
Capacity DS Temperature Acetylator Drying
Heater CC (tcc /y)
X1 (tcassava /d) X2 X3 (◦ C) (Battery) chamber
1 8.000 0.500 150.00 0.30 19.17 6.61 73.7
2 10.000 0.350 250.56 0.37 20.93 2.72 147.5
3 13.363 0.350 187.50 0.50 27.97 4.95 144.7
4 10.000 0.602 187.50 0.37 29.37 6.47 124.2
5 12.000 0.200 150.00 0.45 16.69 5.43 93.6
6 8.000 0.500 225.00 0.30 19.17 3.48 108.5
7 8.000 0.200 150.00 0.30 11.12 5.48 62.4
8 12.000 0.500 150.00 0.45 28.76 6.55 110.6
9 6.636 0.350 187.50 0.25 13.89 3.73 71.8
10 12.000 0.500 225.00 0.45 28.76 3.46 162.8
11 10.000 0.350 124.43 0.37 20.93 5.95 68.6
12 8.000 0.200 225.00 0.30 11.12 2.85 91.1
13 10.000 0.350 187.50 0.37 20.93 3.72 108.3
14 10.000 0.097 187.50 0.37 10.42 4.71 92.8
15 12.000 0.200 225.00 0.45 16.69 2.86 136.7

(a) (b)

Figure 2 Results of the determination of economic indicators for the production of AS. a) Main cost elements; b) Response
variables to be optimized

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A. Acosta-Solares et al., Revista Facultad de Ingeniería, Universidad de Antioquia, No. 112, pp. 34-44, 2024

Table 3 Results of the optimization of dynamic profitability indicators in AS production

Optimization of separate responses

Capacity Temperature
Factors DS X2
X1 (tcassava /d) X3 (◦ C)
Optimization for P Optimum value = 1,550,000 USD/y
Optimum value 12.82 0.602 124.43
Optimization for NPV Optimum value = 10,500,000 USD
Optimum value 13.36 0.501 124.43
Optimization for IRR Optimum value = 89.38%
Optimum value 13.34 0.602 124.43
Optimization of multiple responses (desirability: 0.9804)
Optimum value 12.57 0.505 124.98
Responses P (USD/y) NPV (USD) IRR (%)
Optimum value 1,420,000 9,090,000 82.51

gelatinized starch [11], mainly due to the use of the and allows it to be selected to perform the reaction. Table
mechanical dehydration method of pneumatic drying. 5 shows the geometrical characteristics and agitation
conditions for these units, resulting from the scale-up
A residence time in the heater set to 0.6 h guarantees criteria applied.
the heating of the slurry. For this design parameter, a
WL equal to 863.50 kg/h and a ρL of 1,050 kg/m3 [2], Table 6 shows the results of determining the electrical
the VC resulted in 0.5 m3 , when applying Equation 2 for power and heat transfer demands for the heating and
a 10% overdesign. From the full kinetic expression for acetylation stages.
starch acetylation [2], the kinetic constant at 48 °C yielded
a value of 3.67 × 10−3 moll min , obtaining the reaction In all cases, the available lateral surface area satisfies the
rate expression as a function of active AGU concentration heat transfer demand in these units. It should be noted
(CRO− ) and acetic anhydride concentration (CAA ), that the low heat transfer requirements in the acetylator
expressed as: units are supported by the moderate acetylation enthalpy
values.
−rR0− = 3.67 × 10−3 (CR0− ) × (CAA ) (7)
The results of the pneumatic dryer design are shown
The conversion to mono acetyl glucose at the optimum in Table 7. A gas velocity of 25 m/s, considered in the
C
DS is X(RO−)f = 1 − CRO−
0 = 0.505 and was calculated design, allows for overcoming the fluidization velocity
RO−

with C(RO−)consumed = CRAc = 0.668 kmolm3 . At the reactor

and guarantees the entrainment condition [14, 20]. As
exit, a CAA = 2.20 × 10−2 kmol m 3 was reached, and the the drying duct demands a high length/diameter ratio, its
acetylation rate resulted in −rRO− = 5.29 × 10−5 mkmol spatial distribution was proposed in the form of vertical
3 min

according to Equation 7. With these results, a τ = 210 h forks.

[16] was calculated for an acetylator unit, so it is obtained
that the volume of the equipment V = 165.2m3 . T, drying gas temperature; t, temperature of AS
paste, which at the inlet is a mixture of wet paste
The above result demonstrates that direct acetylation and recirculated dry AS (tm ); ∆Tm, driving force as a
of native starch requires high acetylator volumes, so it is function of temperature differences; G1 , relative mass
not possible from a practical point of view to implement flow between gas and solid; Ua , volumetric heat transfer
a single acetylator approach. This situation is because coefficient; VC , drying chamber volume; and subscripts
the kinetic constant is about 17 times lower when not 1 and 2 denote the input and output of the equipment
gelatinized prior to acetylation [12]. However, a battery respectively.
of perfect mixing reactors in series requires a smaller
volume than a single reactor [16, 19]. The technological requirements of the optimal variant
demand a pneumatic dryer with a duct of 2.52 m3 , a
Applying the graphical design method, the volume of standardized diameter of 0.3 m, and a length of 35.66
each acetylator unit is Vi = 11.63 m3 , and the volume m, spatially located in a bank of 3 U-shaped forks with a
of the system of three acetylator units in series is length of 5 m and 5.56 m occupied by the accessories and
V = 34.90 m3 . The size of the acetylator battery is 21% of the rest of the duct up to the cyclone separator.
the size of a stand-alone reactor, which corresponds to the
trend of such behavior for positive order reactions [16, 19]

41
 A. Acosta-Solares et al., Revista Facultad de Ingeniería, Universidad de Antioquia, No. 112, pp. 34-44, 2024

Table 4 Summary of material and energy balance for AS

Production AS (t/d) 5.697

By-product Bran (Dry fiber) (t/d) 1.508
Raw Cassava roots (t/d) 12.569
materials NaOH at 50 % w/w (t/d) 0.003*
and key HCl at 35 % w/v (t/d) 0.119*
streams Acetic anhydride (t/d) 1.135
Water for technological use 19.869
Water
Utilities (m3 /d)
CC (t/d) 0.313
Fuels
Fuel consumption rate (tCC /tAS ) 0.055
Discarded roots (t/d) 0.375
Solids Sand (t/d) 0.589
Waste
Shell and husk (t/d) 0.037
Liquids Centrifuge effluent (m3 /d) 27.520
Process Losses (t/d) 0.124
losses Yield based on cassava (%) 45.32
* Consumption includes chemical cleaning agents.

Table 5 Dimensions and fundamental parameters of the slurry Table 7 Basic dimensions of the pneumatic dryer in the
heater and acetylator applying scale-up ratios for agitation production of AS under optimum conditions

Acetylator Parameter Value

Dimension Heater
unit Pasta fed (30% humidity) 2,152.56
Volume (m3 ) 0.5 11.63 Recirculated starch (kg/h) 1,595.00
Diameter and height (m) 0.86 2.45 Dry AS (kg/h) 285.12
Impeller diameter (m) 0.43 1.21 Energy demand (GJ/h) 0.6
Agitation speed (rpm) 130 46 T1 (°C) 124.98
T2 (°C) 78.00
Table 6 Results of the determination of power and heat transfer tm1 (°C) 28.26
requirements for AS production t2 (°C) 62.00
∆Tm (°C) 56.09
Results G1 (kg/s m2 ) 5.0
Calculated parameters Heater Acetylator Ua (J/s m3 K) 1,287.96
units VC (m3 ) 2.52
4
Reynolds mixing 4.09·10 1.20·105 Duct diameter (m) 0.30
Agitator power (kW) 1.39 12.45 Duct length (m) 35.66
Pellicular heat transfer Number of forks 3
4,071.59 1,547.48
coefficient (kJ/hm2 C)
Pellicle coefficient referred to the
4,056.59 1,545.51
outside diameter (kJ/hm2 C)
acetylating a suspension of native starch.
Total clean heat transfer
2,032.03 773.25
coefficient (kJ/hm2 C)
Total clean heat transfer The optimal operating parameters of the plant for
1,196.27 610.85 obtaining this product are encouraging economic
coefficient (kJ/hm2 C)
0.85 (U1) indicators. They are achieved at a production capacity
Required heat transfer 1.61 0.24 (U2) of 12.57 tcassaval /d, DS of 0.505, and 124.98 °C in the air
area (m2 ) 0.07 (U3) supply to the pneumatic dryer.

Under optimum conditions, 5.997 t/d of AS with a DS

5. Conclusions of 0.505 is produced. As equipment for acetylation, this
production demands a slurry heater of 0.5 m3 and a
The production of AS can be carried out in technological battery of three acetylating units in series of 35 m3 in
processes based on the schemes reported for acetylated total. For drying, with 124.98 °C in the gas feed to the
gelatinized starch, maintaining the principle of adopting pneumatic dryer, a 2.52 m3 duct with a standardized
the stages of native starch by mechanized means, diameter of 0.3 m and a length of 35.66 m is required,
eliminating the gelatinization stage, and directly where an energy efficiency significantly higher than that of

42
A. Acosta-Solares et al., Revista Facultad de Ingeniería, Universidad de Antioquia, No. 112, pp. 34-44, 2024

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