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Alves 2021
Alves 2021
Full-length article
A R T I C L E I N F O A B S T R A C T
Article history: Integrated simulation of manufacturing plants plays crucial role in development of sustainable processes
Available online 18 May 2021 and optimized products. However, no investigation has been reported for the whole process chain of
porcelain stoneware manufacturing. In this contribution, semi-empirical models of porcelain stoneware
processing steps have been developed and implemented into Dyssol framework. By validation based on
Keywords: industrial and lab-scale experiments, the simulation has been applied for modeling and sensitivity
Flowsheet simulation
analysis of the entire process. The simulation results are in a good agreement with experiments showing
Porcelain stoneware
that the proposed modeling strategy has high potential to be used for future digital transformation in this
Digitalization
Optimization
sector.
© 2021 CIRP.
https://doi.org/10.1016/j.cirpj.2021.04.011
1755-5817/© 2021 CIRP.
C.L. Alves, A. De Noni Jr, R. Janssen et al. CIRP Journal of Manufacturing Science and Technology 33 (2021) 473–487
Subscripts
Theory
amb Ambient
at Atomization
Every unit operation of the manufacturing plant (Fig. 1) is
boil Boiling
represented as a separate model in the flowsheet simulation. The
drop Droplet
models, applied considerations and used numerical methods and
eq Equilibrium
algorithms are described in the following subsections. The
f Feed
implemented models are based on previously validated and
gas Gas
available in the literature semi-empirical correlations. Appendices
i Size class i
A to E provide the information about the adjustment of unknown
l Liquid
model parameters that has been performed based on experimental
mill Milling
data.
p Particle
pr Product
Wet milling
slurry Slurry
During wet milling, the raw materials are mixed with water and
they are grinded in a ball mill for a specific time period to reach
desired particle size. To describe the milling process, the flowsheet
model based on correlations proposed by Tsakalakis et al. [21] and
predictability and higher efficiency by innovation in manufactur- Morell et al. [22] has been developed. In the first stage, the mass-
ing, control and measurement [2]. related specific grinding energy Em is calculated as a ratio given by
One of the central roles in Industry 4.0 plays numerical the power consumed P to the mill production mass flow m _ as seen
simulations, which have become a useful tool to optimize and in Eq. (1).
design industrial equipment as well as to evaluate operation
parameters. For numerical investigations of complex plants with P
Em ¼ ð1Þ
the connection of production steps by material and energy _
m
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C.L. Alves, A. De Noni Jr, R. Janssen et al. CIRP Journal of Manufacturing Science and Technology 33 (2021) 473–487
From known specific grinding energy, initial particle size d50;f and that the droplets have a normal size distribution with the median
known Bond work index of each single compound Wi , the particle diameter equal to the Sauter diameter. The standard
characteristic particle size d50;pr of the final product is calculated deviation is specified by the user as an input model parameter.
according to Eq. (2).
Drying of granules
0:193 0:962
Em ¼ 0:1169W i d50;f d50;pr _
m ð2Þ The modelling of spray drying chamber is challenging, given the
complexity related to the integration of the drying of the droplets
According to Morell et al. [22], the mill power consumption is a
with the interacting hydrodynamic effects as well as heat, mass
function of a no-load power (NLP) and net power (NP), as described
and momentum transfer between the solid, liquid and gas phases.
in Eq. (3). The factor k compensates the lost power, such as sound
To describe the drying process, a model based on the correlations
loss, heat transfer, etc.
proposed by Ali et al. has been developed [23]. This model
P ¼ ðNetPowerðNPÞ NoLoadPowerðNLPÞÞk ð3Þ describes the dependence of particles temperature T p , moisture
content wl , droplet radius rp and gas temperature T gas on height z
The no-load power is defined according to Eq. (4), where D is
and time. In this one-dimensional plug-flow counter-current
the mill diameter, L is the apparatus length, and f, fraction of
model a set of assumptions such as the spherical shape of droplets
critical speed.
or neglection of heat transfer by radiation are made. The resulting
NLP ¼ 1:68D2:05 ½fð0:667LÞ0:82 ð4Þ equations which describe the main thermodynamic states are
provided in Eqs. (8) to (11). In all equations, the variables Mx , cp;x , T x
By combining the correlations proposed by Thorpe [21] and denote the mass, specific heat and temperature of component x,
Morell [22], it is possible to estimate the output particle size from respectively.
milling based on the processing time, power input, apparatus
dimensions and material properties. As a simplification, the mill is @T p dMl
Mdrop cp;drop vp ¼ ap Ap T gas T p þ hf g ð8Þ
considered perfectly cylindrical. Furthermore, it is assumed that @z dt
each solid compound is milled separately and the total grinding
energy is distributed between compounds according to their initial
volumetric fractions. Finally, the outlet stream is calculated as a @wl ð1 wl Þ2 dMl
vp ¼ ð9Þ
mixture of single compounds. @z Msolid dt
Spray drying
@rp dMl
vp ¼ ð4prliq r2p Þ ð10Þ
Spray drying is one of the most common methods for the @z dt
production of a wide variety of particulate products [23,24]. In the
scenario of the porcelain stoneware manufacturing, spray drying is
J
performed in a chamber, in which the slurry formed after wet @T gas X dM m_ slurry;j
_ gas cp;gas
m ¼ aj Ap;j þ l;j cp;vap T p;j T gas
milling is atomized as small droplets using one or several nozzles. @z dt vp;j Mdrop;j
The droplets came in contact with a co-current or counter-current
j¼1
þ 2pRapp U T amb T gas
hot gas flow and simultaneously occurring heat, mass and
momentum exchange result in the formation of granules [25]. ð11Þ
Due to the prevalent use of counter-current spray drying in the The heat absorbed by the droplet is the sum of the convective
ceramic industry, this apparatus type has been considered in this heat flux to the droplet/particle and the heat consumed by the
work. To increase flexibility during the specification of flowsheet liquid vaporization. The first term depends on the heat transfer
structure, the spray drying model is divided into two sub models to coefficient of the droplet ap , its surface area Ap and the difference
separately represent atomization and drying processes. between temperatures of the gas and the droplet. The heat
consumed in the moisture vaporization is calculated by the
Atomization product of the latent heat of vaporization hf g and the drying rate
(dM l
).
In the ceramic industry, the atomization is done without dt
additional gas phase by pumping the slurry under high pressure. Similarly, the temperature of the gas in Eq. (11) is calculated as
Therefore, the single fluid atomization model has been imple- the sum of the total heat input to the droplets by convection, the
mented. For nozzles with concentric channels, the Sauter diameter sensible heat of the evaporated vapor and heat loss to the
size of the droplets d32 can be estimated by semi-empirical environment considering the ambient temperature T amb , where U
is the overall heat transfer coefficient. In the first two terms, m _ slurry
relationships as shown in Eqs. (5)–(7). The droplet size depends on
the nozzle diameter D; liquid load lm and Ohnesorge number Z p. is the slurry mass flow, vp is the relative velocity of particles in the
" #m gas flow and Mdrop is the droplet mass.
Dp2D For simplification, Eq. (11) is solved for only one representative
d32 ¼ 2C 4 1 þ C 5 Z jp D ð5Þ
g ð1 þ lm Þ2 droplet diameter which is equal to the Sauter diameter obtained
from the atomization model. This size is adopted to perform all the
calculations and to obtain the respective size reduction due to
. moisture evaporation. Afterwards the obtained percentile of
lm ¼ m_ l ð6Þ reduction is applied for the whole distribution of granules size.
_g
m
The droplet drying rate dMl =dt varies through three different
drying stages. In the first drying stage, the residence time is smaller
Z p ¼ mslurry =ðgrDÞ1=2 ð7Þ than the surface drying time tsd , the drying rate is calculated by
Eq. (12). The surface drying time is taken as the time which is
where C 4 , m, j and C 5 are the semi-empirical constants, which have needed to reduce the moisture concentration at the surface to a
been determined based on experimental data [26]. It is assumed 90% of the equilibrium moisture content. The drying rate on this
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C.L. Alves, A. De Noni Jr, R. Janssen et al. CIRP Journal of Manufacturing Science and Technology 33 (2021) 473–487
stage depends on the saturated humidity of the gas Y sat , the current content compared to smaller ones [27] and as a consequence the
gas humidity Y, mass transfer coefficient b and the surface area of granules reveal different mechanical behavior. This can negatively
the droplet/particle given by its radius rp . influence the quality of conformed green bodies and lead to
formation of zones with different densities. Consequently, to avoid
dMl
¼ 4pr2p bðY sat YÞ ð12Þ this problem, one of the main goals during storage is to ensure
dt
complete moisture homogenization among the grains.
Once the surface is dry (t > tsd ), the drying rate is limited by the Industrially, the silos are fed centrally which means that the
internal diffusion of moisture to the surface. In this period, the rate atomized powder is directed through conveyor belts to the top of
calculated as: the silo, where it is dumped inside. This feeding system is adopted
2 !0:2 3 in the model and it is also assumed that there is no moisture
dMl t tsd evaporation during storage.
¼ 106 rp exp418:9 17:7 5 ð13Þ
dt 106 rp To describe moisture homogenization during the storage a mass
transfer model is developed. For particles from each size class i, the
The third drying stage starts when the particle temperature variation of the moisture W l over time is calculated according to:
reaches the boiling point of the slurry T boil. In this case the drying
@W l;i 2
rate is calculated according to Eq. (14), where dT boil
is the variation of ¼ bpdi W l W l;i ð15Þ
dw l @t
the boiling temperature of the slurry in relationship with the
moisture content. where di is the diameter of granules from size class i, b is the mass
transfer coefficient and W l is the average moisture content in the
dMl ap 4prp 2 T gas T p silo. The mass transfer coefficient has been fitted according to
¼ ð14Þ
dt hf g ðð1 wl Þcp;solid þ wl cp;liq Þð1 wl ÞdT boil
dwl
experimental data [26] (s. Appendix B).
To perform the calculation of moisture homogenization the total
For the implementation of the spray drying model, the spray storage time t stor is discretized into smaller time steps Dt and in
tower has been discretized through a height into a set of layers. In the each time step the predictor-corrector scheme is applied to ensure
first iteration, the output gas temperature has been assumed to be the conservation of mass. It is ensured that at any arbitrary time
equal to the initial temperature of granules. Using this assumption, point the summarized liquid mass flow which leaves wet granules
the calculations have been performed from the top to the bottom of m_ l;giv is equal to the summarized mass flow that is received by more
the tower. The numerical calculation of the derivatives in Eq. (8) to _ l;rec . In the predictor step, the change of the moisture
dry granules m
(11) is made by the finite difference method for every height layer.
content from the particles of size class i is calculated according to
Finally, the calculated gas temperature at the bottom of the tower is
Eq. (15). If the value calculated is negative it is summed to the
compared with the known value of inlet gas temperature. If there is a
received mass flow m _ l;rec, otherwise it is summed to the given mass
substantial deviation between these temperatures, the assumed
flow m _ l;giv. Afterwards, the overall mass flow of transferred liquid
value of the outlet gas temperature is slightly increased and the
calculations are repeated. The average number of iterations needed m_ l is determined as the minimum value between the absolute
to reach convergence is about 12 iterations. values of the received and given mass flow. This condition assures
The final moisture distribution over the different particle sizes that the liquid mass transferred between granules is conserved. In
classes has been calculated based on two assumptions. Firstly, it is the corrector stage the normalization of equations to describe
assumed that the moisture content of each granule is proportional time-dependent moisture change is performed. Fig. 2 illustrates
to its size. The second assumption is that the moisture evaporation the main flowchart of the developed calculation algorithm.
occurred by a drying front and all granules have the same dry layer
thickness. Pressing
Storage The most widely applied shaping method for stoneware is dry
pressing due to the low costs and high productivity. The granules
During storage, the granules obtained from spray drying are after storage are compacted in a rigid cavity by applying pressure in
collected and stored in industrial silos with 10–13 m height. The only one axial direction through a rigid punch forming the green
large granules formed after spray drying have higher moisture tile. The main process control parameter is given by the bulk
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C.L. Alves, A. De Noni Jr, R. Janssen et al. CIRP Journal of Manufacturing Science and Technology 33 (2021) 473–487
density of the tile, which can be translated by porosity content. The mathematical solution of this equation can be derived by
There exist several correlations to describe influence of applied several conventional (thin layer equations, Fourier’s equations)
pressure on the porosity [28,29]. One of the most widespread and non-conventional approaches like neural networks [37]. In
models used is the semi-empirical one proposed by Bal’shin et al. this contribution, thin layer equations have been adopted. Such
[28]. Here the porosity of the tile e depends on the density of the lumped parameter model addresses the thin layer drying as only
atomized powder rat, applied pressure p and parameters A2 and B2 , layer of sample particles or slices and due to the thin structure of
as it is shown in Eq. (16). layers, the temperature distribution can be assumed as uniform
rat [32].
e¼1 þ C 2 d50;mill ð16Þ Henderson et al. [39,40] used the thin layer approach and
A2 lnp B2
derived the analytical solution given in Eq. (18). This model has
The second term, with an additional parameter C2 and which also been used in finite element method calculations [41].
considers the influence of median particle size obtained after
!
milling d50;mill , has not been considered in the original model of W l ðtÞ W l;eq p2 Def f t
Bal’shin. This modification is proposed based on experimental data ¼ A1 exp ; ð18Þ
W l ð0Þ W l;eq A2
and previous work of the authors [30,31].
where W l ð0Þ is the initial moisture content of tile considered to be
Drying homogeneous in the entire geometry and W l ðtÞ is the average
moisture content in the tile at a time t. W l;eq is the equilibrium
The main goal of the drying process is to reduce the moisture moisture content, at which the tile is neither gaining nor losing
content of the tile from 6 to 8% to approximately 1%. This is made in moisture. W l;eq depends on the material, relative humidity and air
industrial convective dryer through hot gases circulation. It is temperature and is assumed to be 104 for porcelain tile [42,35].
generally agreed in the literature that the moisture distribution The parameters A1 and A2 are geometric constants which depend
within a grain over time is controlled by diffusion as stated by on the geometry of the green body. Considering the thickness of
Fick’s law given by Eq. (17) [32–38], where Def f is the effective green body L, Eq. (18) can be rewritten as:
diffusivity parameter.
W l ðtÞ W l;eq pDt
@W l ¼ 1 8=p2 exp ð19Þ
¼ rðDef f rW l Þ ð17Þ W l ð0Þ W l;eq L2
@t
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C.L. Alves, A. De Noni Jr, R. Janssen et al. CIRP Journal of Manufacturing Science and Technology 33 (2021) 473–487
Table 1 Table 2
Two different compositions of the raw materials. Main process parameters of all units for processing of Composition 1.
where k and n are the frequency and time factors accordingly, Ea is To describe particle size distribution (PSD) for both composi-
the activation energy, R is the gas constant, T is the temperature, t is tions the equidistant grid from 0 to 5 mm containing 1000 size
the time and e0 is the porosity of the green body obtained after classes has been applied for process simulation. The PSD of all raw
pressing. The values of n, Ea and k have been estimated based on components has been described as a normal distribution with
previously obtained experimental data. However, since experi- given median d50 and standard deviation s.
ments have been performed for constant heating rate, the Table 2 summarizes the main process parameters for the
correlation given in Eq. (21) is firstly applied to estimate unknown porcelain manufacturing of Composition 1 that are used for
parameters and only afterwards Eq. (20) is used for modeling of the flowsheet simulation.
manufacturing process. The Composition 1 and corresponding process parameters
provided in Table 2 have been defined based on the data obtained
nRk Ea
e ¼ e0 exp tn exp ; ð21Þ from the Brazilian porcelain factories: “Eliane Revestimentos
d50;mill Ea RðT 0 þ btÞ
Cerâmicos” and “Cecrisa Revestimentos Cerâmicos”. The experi-
where T 0 is the initial temperature and b is the heating rate. A mental data which have been used to estimate unknown model
detailed description of procedure to find unknown model
parameters is provided in Appendix E.
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C.L. Alves, A. De Noni Jr, R. Janssen et al. CIRP Journal of Manufacturing Science and Technology 33 (2021) 473–487
Fig. 4. (a) Counter-current spray drying configuration scheme (b) Profile of the gas temperature and granules moisture during spray drying.
parameters and to validate models have been obtained from new Table 3
Comparison between experimental data and simulation results.
experimental measurements and previous contributions
[26,30,31,44,45]. This data has also been derived for the above- Unit operation Property Experiments Simulation
mentioned factories with same process conditions. For almost all Wet milling Particle diameter (d50) [mm] 11.23 11.3
models of single unit operations industrial data has been used. Spray drying Granules temperature [ C] 60 58.2
However, due to the difficulties of obtaining and adjustment of Gas output temperature [ C] 100 100
Moisture [%] 7 7
sintering parameters for industrial kiln, the model parameters of
Granule diameter (d50) [mm] 311 307
Eq. (20) have been estimated based on data of a laboratory scale Storage Moisture [%] 6.5 7
kiln (Electric furnace Jung LT 3). In this case, the simulation of Pressing Porosity [%] 33 32.9
sintering in the lab-scale kiln has been performed with Eq. (21) and Drying Moisture [%] 0.3 0.31
compared with experimental data. Afterwards, adjusted model Sintering Porosity [%] 3.5 3.49
parameters have been used in Eq. (20) for industrial sintering times
and temperatures.
A porcelainized stoneware Composition 2 for anorthite is based
on data from Taskiran et al. [46] and has been used to validate Appendix A, the simulation results are in good agreement with
models for wet milling and sintering. The process parameters have experimental data.
been also taken from Taskiran et al. [47]. Appendix F describes in Existing literature suggests that flowsheet process simulations
details the process parameters and considerations made for the can be computationally expensive and potentially inaccurate.
simulations. These problems are given by the high dimensional equations
systems that are often highly nonlinear, ill-conditioned and poorly
Results and discussion structured [48,49]. These issues are often directly related to the
robustness of numerical algorithms, which may hinder transfer of
Process simulation research advances to final software products and, as a conse-
quence, strongly limit their industrial applicability. These matters
The entire plant has been simulated in steady-state mode and could be overcome in this study and an industrial application can
simulation results have been compared to the experimental data. be foreseen. The overall calculation time needed to perform
In Fig. 3 the particle size distributions at different stages of the flowsheet simulations in Dyssol and to reach steady-state is in the
manufacturing process are shown. The initial raw materials with range of 4 s.
median size of 60 mm have been milled that lead to reduction of With the proposed flowsheet model, it is possible to analyze the
median particle size to 10.1 mm. Due to the different material influence of parameters of single unit operations parameters not
strengths, the components milled differently attaining different only locally, but through the whole process chain. Fig. 5 shows the
sizes. The average diameter of feldspar decreased from 100 to 16.4 influence of specific parameters on the entire manufacturing
mm. The average diameter of clay diminished from 22 to 4 mm and process.
of kaolin from 32 to 4.9 mm. Within the spray drying process, The material properties that have a major influence on the
granules with average diameter of 307.1 mm are formed. entire process behavior are the particle size obtained after milling,
In Fig. 4 (a) and (b), the schematic representation of counter- the moisture of granules and green tile porosity. Based on that, a
current spray dryer and thermodynamic properties in it are shown. sensitivity analysis is carried out at different case studies where
It can be observed that the gas temperature and moisture are non only one of the following parameters is modified at the same time:
linearly dependent on the vertical position. The droplets injected at
the top of the dryer contact humid gas with relatively low Milling time
temperatures, leading to moderate drying rates. At the bottom of Pressure applied during pressing
the chamber, where the pre-heated droplets contact the high- Sintering time and temperature.
temperature inlet gas, the higher evaporation rate can be observed.
In Table 3, various properties such as moisture, porosity and In the real process, the moisture obtained after spray drying will
median particle size are listed. Overall, it can be seen that after the depend on various properties, such as diameter of particle
adjustment of model parameters which are described in detail in obtained after milling. However, this is not considered in this
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C.L. Alves, A. De Noni Jr, R. Janssen et al. CIRP Journal of Manufacturing Science and Technology 33 (2021) 473–487
Sensitivity analysis
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C.L. Alves, A. De Noni Jr, R. Janssen et al. CIRP Journal of Manufacturing Science and Technology 33 (2021) 473–487
intervals lead to higher porosity of the green body after pressing. sintering at 1225 C can be seen in Fig. 8 (b). Detailed information
With decreasing particle size, the attractive forces and interparti- on the chemical composition of this formulation and processing
cle friction is increased leading to enhanced agglomeration of parameters is provided in Appendix F.
particles [50]. Strong agglomeration compromises the fluidity of A good agreement between experiments and simulation has
the particles in the die during conformation and it leads to the also been obtained considering Composition 2 with an average
formation of large pores and, thus, higher porosity. Contrary to this, difference value of 1.25 microns. However, it can be observed that
the opposite influence of milling time on porosity of the final longer milling times result in a higher discrepancy of experimental
product can be observed. According to Carter et al. [51] the kinetics and numerical results. Moreover, for the same sintering tempera-
of sintering is governed by the reactant particle size. On the one ture, the porosity after sintering decreased with higher milling
hand, fine particles mostly promote the reaction because of the times.
decreased distances. On the other hand, the growth of the solid- Overall, the good agreement between experimental data and
state reaction product in powder systems essentially occurs at simulation results for different compositions and processing
particle contact points. Thus, the combined effect of reactant conditions allows to forecast outcomes of individual processing
particle size and degree of green body particle contacts (variation units and of the final product, without the need of expensive
in green porosity) directly affects the porosity after sintering. The experimentation or trial and error approaches.
increased contact among particles created by agglomeration, leads
to smaller tile densities [52,53]. Therefore, to increase the density Pressure variation during pressing
of the tiles, it is mandatory that the green bodies possess low green The properties of the final porcelain tile strongly depends on
density and homogenous packing of particles. the microstructure of the green body [54]. Fig. 9 illustrates the
The same conclusion has been drawn for different porcelain effect of applied pressure on the porosity of the green tile. A good
compositions. Taskiran et al. [46,47] developed a porcelainized agreement has been obtained after to the adjustment of A2 and B2
stoneware composition based on anorthite and performed an model parameters (Eq. (16)) for granules with different moistures,
extensive detailed experimental study of the influence of milling as seen in Appendix C. The good match between experiments and
time on the sintering behavior. The data obtained by experiments simulation is confirmed by the R2 value of 0.99.
according to the study of Taskiran et al. [47] and simulation of The porosity of the green body decreases when higher
Composition 2 (s. Table 1) for different milling time is presented in pressures are applied or when the moisture of the granules is
Fig. 8 (a). The influence of the milling times on the porosity after increased. The moisture favors the formation of intergranular
Fig. 8. Comparison between the experimental study of Taskiran et al. [48] and new simulations.
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C.L. Alves, A. De Noni Jr, R. Janssen et al. CIRP Journal of Manufacturing Science and Technology 33 (2021) 473–487
Fig. 10. Correlation between the porosity of the green body and sintered tile for Fig. 11. Comparison of the evolution of porosity on the tile for different sintering
different pressures applied during pressing. times and temperatures. Experimental data from Gómez et al. [43].
bonding. Tanaka et al. [55] showed that more intensive local considered for the analysis ranging from 3 h, 12 h, 24 h, 48 h and 96
particle rearrangement might occur with higher moisture content, h. The comparison between experiments and simulation can be
enhancing the particle packing in the green body. seen in Fig. 12. A good agreement has also been obtained with R2
The influence of pressure applied during conformation on final value of 0.95 with an average difference of 0.3 %. Considering both
tile porosity has been investigated in the interval between 40 and compositions, it is possible to analyze different processing
50 MPa. This is a common range of pressures applied for the parameters and outcomes from units through the developed
stoneware conformation in the industry [3,54,56]. The influence of models. In the case of the second composition, the optimal milling
pressure on porosity of the green tile prior to sintering as well as on time is 48 h and sintering temperature is 1200 C, that allows to
the end porosity of the tile are shown in Fig. 10. It can be inferred reach almost zero porosity. Further milling and higher sintering
that an increase in pressure leads to almost linear decrease in both temperature would lead to inefficient utilization of energy in the
properties. Nevertheless, the absolute porosity reduction on process. This conclusion has been drawn by Taskiran et al. [47] with
sintering is approximately 10 times smaller than the reduction extensive experimental work. The same outcome has been derived
of porosity after pressing. This behavior is consistent with the well- by the simulation with according processing parameters for the
known fact that the final density is essentially influenced by the milling and sintering units.
sinterability of the system, e.g. by particle size and phase Considering the Composition 2 proposed by Tsakarian et al. [47],
composition. The simulation, thus, allows to forecast the porosity the blowing effect has occurred in temperatures higher than 1240
after sintering for specified conditions.
C but not as significant as in the Composition 1. Consequently, the
influence of the blowing effect is more significant for this
Time and temperature variation during sintering composition, justifying the higher divergence from simulations.
The reduction of porosity during sintering depends on several The simulation for Composition 2 overestimates the porosity for
variables such as temperature, time, initial density and particle size milling times above 12 h. This is caused due to discrepancies which
[43,57]. Firing temperature and time are determining factors in already appear in the wet milling and propagates through the
obtaining appropriate technical properties of porcelain stoneware. whole process chain.
Experimental data obtained by single burn conventional sintering The sintering model implemented here has been developed for
for Composition 1 has been used to analyze the behavior of this unit. alumina solid-state sintering considering only open porosity and
In the experiments the fixed heating of 50 C/min until 450 C, disregarding the effect of liquid phases during sintering. It is
followed by a rate of 30 C/min until the plateau was used. Four
different plateau holding time intervals of 3, 5, 10 and 15 min as
well as different plateau temperatures in the range of 1120 C and
1260 C was considered [30]. The model is applied during the
isothermal period to compare the sintering model proposed by
Gómez et al. [43]. The minimum porosity achieved by experiments
and simulations is equal to 0.054 %. A good agreement with R2
value of 0.94 is obtained considering the different conditions of
holding temperatures and times, presenting slight discrepancy at
temperatures above 1180 C as seen in Fig. 11. This is caused due to
the fact that the feldspar develops a liquid phase at low
temperatures about 900 C [3,58]. Due to the high amount of
this component, there is a high amount of liquid (ca. 50–60 %)
leading to a blowing effect. This justifies the increase of closed
porosity observed in the experiments for all sintering times
evaluated for temperatures higher than 1180 C.
Considering the analysis carried by Tsakiran et al. [47], the
sintering process for Composition 2 has been evaluated for test
samples on temperatures ranging from 1160 to 1325 C with 25 C Fig. 12. Comparison of simulations and experiments of sintered tile porosity for
intervals and soaking time of 3 h. Different milling times have been different milling times based on data of Tsakiran et al. [48].
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C.L. Alves, A. De Noni Jr, R. Janssen et al. CIRP Journal of Manufacturing Science and Technology 33 (2021) 473–487
supposed that there is a direct correlation of the sintering without the need for extensive experimentation or trial and error
mechanism with the values of the time factor parameter (n), approaches. This offers the potential to perform sensitivity
which may lead to the different values found. However, the analysis throughout the process chain, to determine optimal
development of a sintering model for porcelain tiles including parameters and as a consequence to make step towards process
these aspects is beyond the scope of this work. It is envisioned that sustainability.
a microscale calculations approach like the discrete element
method can allow to include these aspects [59,12]. Declaration of interests
Conclusion and outlook The authors declare that they have no known competing
financial interests or personal relationships that could have
An integrated flowsheet process model for porcelain stoneware appeared to influence the work reported in this paper.
manufacturing process has been developed and applied for
simulation of an entire plant. Semi-empirical models of all Acknowledgments
relevant processing steps, such as milling, spray drying, pressing,
sintering, etc. have been developed and implemented to the We gratefully acknowledge the financial support of the German
flowsheet simulation framework Dyssol. The unknown model Research Foundation (DFG). Project-ID: 418788750 (DFG DO 2026/
parameters were adjusted based on the lab-scale or industrial 6-1), of the DAAD (Pro Bral 57447192) and of CAPES-DFG program
experimental data. (PIPC 88881.207634/2018-01).
The proposed flowsheet model has been successfully used to
consider interdependencies between single unit operations in the Appendix A. Parameters adjustment
whole process chain and to analyze the influence of main process
parameters. It was shown how milling time, pressure applied The presented above semi-empirical models of different
during pressing and sintering parameters influence process state transformation steps starting with wet milling and ending with
or final product properties. Overall, it was shown that simulation sintering containing a set of unknown parameters. These
results are in a good agreement with experimental data parameters were adjusted according to the experimental data
considering different compositions and processing parameters. using a generalized reduced gradient and the Levenberg-
Furthermore, the flowsheet simulation and Dyssol demonstrated Marquardt algorithm. The estimated model parameters for all
to be effective in establishing a digital twin of ceramic fabrication, unit operations are listed in Table A1. Table A2 shows additional
allowing to forecast outcomes during the processing sequence material properties and model parameters used for calculations.
Table A1
Parameters of the models fitted to the experimental data.
Table A2
Additional material properties and model parameters used for calculations.
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C.L. Alves, A. De Noni Jr, R. Janssen et al. CIRP Journal of Manufacturing Science and Technology 33 (2021) 473–487
Fig. B2. Time-dependent evolution of moisture distribution among granules with Fig. C2. Dependency of parameter B2 on the moisture of granules and pressure
different size during storage. applied during pressing.
Table C1
Experimental data sets for different moisture of granules and pressures applied [31].
Parameter set Moisture of granules – Factory A [%] Moisture of granules – Factory B [%] Pressure – Factory A [MPa] Pressure – Factory B [MPa]
1 7.7 6.7 19.02 36.28
2 6.5 6.0 15.49 24.91
3 6.9 6.4 17.26 30.69
4 8.1 7.1 20.69 42.07
5 7.5 47.66
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C.L. Alves, A. De Noni Jr, R. Janssen et al. CIRP Journal of Manufacturing Science and Technology 33 (2021) 473–487
Table D1
Experimental data from several Brazilian factories.
Factory Gas temperature [K] Residence time [s] Tile thickness [mm] Moisture input [%] Moisture output [%]
1 473.15 2700 10 6.5 0.5
458.15 3900 9 6.5 0.5
2 523.15 1500 12 7 0.3
3 408.15 1320 11 7.2 0.39
398.15 1620 9.8 7 0.38
The diffusivity constant in Eq. (18) has been estimated based on 1 0.072172 69504.69
experimental data of the factories listed in Table D1. The values 3 0.159797 58995.61
Aiming to obtain the model parameters (n, k and Ea) used in Eqs.
(20) and (21), experiments with optical dilatometry have been
Fig. D1. Dependency of estimated diffusivity constant on temperature.
performed. The dataset of expansion has been obtained applying
Fig. E1. Comparison between experimental data and simulation results for samples with median particles size of 7.5 and 5 mm for heating rates: (a) 10 C/min, (b) 30 C/min
and (c) 50 C/min.
485
C.L. Alves, A. De Noni Jr, R. Janssen et al. CIRP Journal of Manufacturing Science and Technology 33 (2021) 473–487
Table E1
Values obtained for the parameters k, n and Ea with respective conditions and quality of the sintering model fit.
different constant heating rates (10 C/min, 30 C/min and 50 C/ [8] Gültekin, E.E., Topateş, G., Kurama, S., 2017, The Effects of Sintering Tempera-
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