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Process Safety and Environmental Protection 175 (2023) 99–110

Contents lists available at ScienceDirect

Process Safety and Environmental Protection


journal homepage: www.journals.elsevier.com/process-safety-and-environmental-protection

A framework for environmental production of textile dyeing process using


novel exhaustion-rate meter and multi-layer perceptron-based
prediction model
Soohwan Jeong a, b, 1, Jonghun Lim a, c, 1, Seok Il Hong d, Soon Chul Kwon d, Jae Yun Shim d,
Yup Yoo a, c, Hyungtae Cho a, Sungsu Lim b, *, Junghwan Kim c, *
a
Green Materials and Processes R&D Group, Korea Institute of Industrial Technology, Ulsan 44413, Republic of Korea
b
Department of Computer Science Engineering, Chungnam National University, 99, Daehak-ro 76beon-gil, Yuseong-gu, Daejeon, Republic of Korea
c
Department of Chemical and Biomolecular Engineering, Yonsei University, Seoul 03722, Republic of Korea
d
ICT Textile and Apparel R&BD Group, Korea Institute of Industrial Technology, Ansan 15588, Republic of Korea

A R T I C L E I N F O A B S T R A C T

Keywords: In textile industries, a lot of wastewater are discharged which are one of the major environmental pollution
Textile industry problems, because they release undesirable dye effluents. Owing to re-dyeing procedures performed to meet
Re-dyeing customized color specifications, environmental pollution is a serious problem because of the emission of large
Right-first-time
volumes of wastewater. To solve the environmental problems caused by re-dyeing, the right-first-time (RFT) %,
Exhaustion rate meter
Multi-layer perceptron-based prediction
which is the rate at which the target quality is obtained with just one dyeing, must be increased by considering
the dyeing conditions that affect product quality. Here, this study suggests a framework for cleaner production of
textile dyeing process using novel exhaustion-rate meter (NERM) and multi-layer perceptron-based prediction
model to solve the environmental problems caused by re-dyeing procedure by controlling the exhaustion-rate
outliers. The proposed NERM measures the exhaustion-rate based on absorbance of the dyeing solution and is
composed of measuring and analysis section. The dyeing solution absorbance is metered in the measuring
component through a detector, which performs high-resolution measurement (0.3–1.5 nm full width at half
maximum) via a 25-μm slit in the 200–1100-nm wavelength range; the absorbance is then converted to the
exhaustion-rate based on Beer’s law in the analysis section. Using the NERM, an exhaustion rate dataset ac­
cording to the Na2SO4 and Na2CO3 consumption is acquired and a surrogate model that augments the exhaustion
rate data is developed. The MLP-based prediction model is then developed using the augmented data to control
the real-time exhaustion-rate outliers. As a results, the model performance as regards Na2SO4 and Na2CO3
prediction is indicated by R2 values of approximately 0.985 and 0.998, respectively, and root mean squared
errors (RMSE) of approximately 1.477 and 1.000, respectively. In addition, the effectiveness of the proposed
framework is demonstrated through application to several scenarios in which the real-time exhaustion rate
outliers are detected.

of their high stability to water, detergents, light, temperature, chem­


1. Introduction icals, soap and other parameters (Rodríguez Couto, 2009). Thus, the
wastewater from dyeing process is classified as the most polluting of all
In the textile industry, dyeing process requires considerable volumes the industrial sectors according to the increased demand for textile
of both hot water and the chemicals necessary for reactive dyeing products and the proportional increase in their production (Rahman
(Alkaya and Demirer, 2014). This process generates wastewater, which Bhuiyan et al., 2016). Therefore, dye wastewater becoming one of the
cause serious environmental pollution due to the inefficiency of the substantial sources of severe pollution problems.
dyeing process (Criado et al., 2020; D.P. Chattopadhyay, 2011). In In general, in textile industry, the exhaust method is commonly used
addition, most of these wastewater persist in the environment as a result to dye cellulose fibers with reactive dyes, because it can achieve the

* Corresponding authors.
E-mail addresses: sungsu@cnu.ac.kr (S. Lim), kjh24@yonsei.ac.kr (J. Kim).
1
Soohwan Jeong and Jonghun Lim contributed equally to this work as first authors.

https://doi.org/10.1016/j.psep.2023.05.009
Received 22 July 2022; Received in revised form 30 March 2023; Accepted 2 May 2023
Available online 8 May 2023
0957-5820/© 2023 The Authors. Published by Elsevier Ltd on behalf of Institution of Chemical Engineers. This is an open access article under the CC BY-NC-ND
license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
S. Jeong et al. Process Safety and Environmental Protection 175 (2023) 99–110

RFT by increasing the compatibility of acid dyes and mononicotinic


Nomenclature acid-triazine (MNT)-type reactive dyes. In experiment, the highest final
exhaustion-rate was achieved at pH 7 or higher for MNT-type reactive
dataorigin data after preprocessing dyes, and at pH 9 or higher for monochlorotriazine (MCT)-type reactive
SMNa2SO4 surrogate model trained with dataorigin to create virtual dyes. Moreover, Shukla and Dhuri (Dhuri, 1992) experimentally inves­
data. This model describes the exhaustion-rate tigated the effect of adding leveling agents to improve the compatibility
according to the specific time (0–120 min), of mixed disperse dyes; they found that a nonionic leveling agent
temperature, Na2SO4 input, and Na2CO3 input improved the mixed disperse dye compatibility under applied depths of
SMNa2CO3 surrogate model trained from dataorigin with data of 40 1.5–4.5%. In addition, Pasha and Taylor (2013) developed a novel
min or later to augment the available data. This model 2-chloro-4-alkylthio triazinyl reactive dye with a high final
describes the exhaustion-rate according to the specific exhaustion-rate and fixation properties. The proposed dye achieved the
time (40–120 min), temperature, Na2SO4 input, and target final exhaustion-rate over a shorter period (of approximately 5
Na2CO3 input min) than conventional dyes, while exhibiting excellent compatibility
dataNa2SO4 26,896 data elements extracted using SMNa2SO4 for mixing of yellow and red dyes.
dataNa2CO3 17,612 data elements extracted using SMNa2CO3 As regards the second research focus, i.e., derivation of optimal
PMNa2SO4 this model is trained with dataNa2CO3 and describes the dyeing conditions to increase the final exhaustion-rate and to control the
Na2SO4 input according to the specific time, target color difference in the fiber dyeing process, many studies have
temperature, Na2CO3 input, and exhaustion-rate. This been performed. Kim et al. (2010) previously determined the optimal
model predicts and controls exhaustion-rate outliers dyeing conditions for Angora fibers using both reactive and acid dyes in
arising within 40 min after the start of the process order to enhance the final exhaustion-rate. The optimal dyeing condi­
PMNa2CO3 this model is trained with dataNa2SO4 and describes the tions, which yielded the highest exhaustion-rate, included a dye con­
Na2CO3 input according to the specific time, centration of 8% o.w.f. for both the reactive and acid dyes, pH 3–4 at
temperature, Na2SO4 input, and exhaustion-rate. This 110 ◦ C for reactive dyes, and pH 3–4 at 70 ◦ C for acid dyes. In addition,
model predicts and controls exhaustion-rate outliers Fakin et al. (2009) subjected fabric to surface-modifying Corona treat­
arising 40 min or later after the start of the dyeing ment and, hence, achieved their target final exhaustion-rate at a lower
process dyeing temperature and within shorter dyeing time than for
non-Corona-treated fabric. In an experiment involving the disperse
dyeing method, which is appropriate for polylactic acid fabrics, Lee and
Song (2013) derived the optimal dyeing conditions as a function of
highest final-product productivity over a short period (Iriani and temperature and time. The final exhaustion-rates for disperse red 60
Bachtiar, 2019). In the exhaust method, a neutral salt (Na2SO4) is added (DR60), disperse blue 56 (DB56), and disperse yellow (DY54) dyes
to a solution containing a dissolved reactive dye to increase the affinity increased by 12% under optimal conditions. Finally, Wahyudin et al.
between the fiber surface and the dye (Burkinshaw and Salihu, 2019). (2018) derived optimal dyeing conditions using the Taguchi method,
After sufficient adsorption of the dye by the fabric, Na2CO3 is applied to again with the aim of avoiding re-dyeing during the fiber dyeing process.
fix the dye to the fabric (Burkinshaw and Salihu, 2019). Although this The optimal dyeing conditions derived through the Taguchi method for
method is more productive than other dyeing methods, the final product the subject process were a dye concentration of 3.5%, temperature of
quality varies significantly depending on the dyeing conditions, such as 80 ◦ C, and Na2SO4 and Na2CO3 concentrations of 80 and 5.8 g/l,
the dye ratio, input timing, and Na2SO4 and Na2CO3 concentrations respectively.
(Iriani and Bachtiar, 2019). Therefore, the exhaust method often fails to However, despite many contributions to increase the RFT such as
provide the target product quality as a result of variations in the dyeing dyestuff compatibility enhancement and dyeing process optimization,
conditions, and multiple re-dyeing processes are then required to obtain several challenges still remain, which are detailed below.
the target quality. When re-dyeing is required, the overall dyeing cost
increases by 98–169% compared to a one-time dyeing process and the 1.1.1. Absence of technology to improve RFT considering color difference as
wastewater is significantly increased which is the most polluting of all well as dyeing uniformity
the industrial sectors, considering the generated volume as well as the The quality standards used to determine dyeing quality in the textile
effluent composition (Cho and Kim, 2001). Additionally, the associated dyeing process are the color difference relative to the target color and
damage to the fabric degrades the product quality. To solve the prob­ the dyeing uniformity. The color difference, as determined by the final
lems associated with re-dyeing using the exhaust method, it is necessary exhaustion-rate, has been considered for product quality evaluation in
to improve the right-first-time (RFT) %, which is the rate at which the prior studies; however, the dyeing uniformity has been neglected. The
target quality is obtained with just one dyeing, this can be achieved by dyeing uniformity is determined by the dye exhaustion-rate curve and,
considering the dyeing conditions that affect product quality. The thus, indicates the evenness of the dye distribution in the fabric. When
standards by which the final product quality is determined include the dye adsorption occurs too rapidly (rather than following the optimal
color difference and dyeing uniformity, where the color difference is the exhaustion rate curve), the dye reacts excessively quickly with alkalis
difference between the target color and the actual dyed fabric color, and during the dye-fixation reaction stage, resulting in uneven fixation and
is determined by the final exhaustion-rate; and the dyeing uniformity is dyeing. Therefore, to increase the RFT by satisfying both the color dif­
the level of dye consistency in the fabric, which depends on the dye ference and dyeing uniformity requirements, it is necessary to measure
exhaustion rate curve (Gorji Kandi and Amani Tehran, 2007; Hong et al., and control the exhaustion rate curve in addition to the final dye
2014). exhaustion-rate; however, no relevant study has yet been conducted.

1.1. Literature review 1.1.2. Impossibility of real-time control during dyeing


During the textile dyeing process, exhaustion-rate outliers may occur
To improve the RFT, prior studies have aimed to increase the due to unreacted dyes, loss of dyes, etc., and often yield unsatisfactory
compatibility of the dye itself, or to derive optimal dyeing conditions to product quality. However, real-time control of the problems associated
increase the final exhaustion-rate, which impacts the target color dif­ with exhaustion-rate outliers has been impossible to date and, thus, the
ference. As regards dye compatibility and reproducibility, Kim et al. dyeing process is often paused midway for fabric sampling. In this
(2004) previously determined the optimal pH conditions for improved approach, the operator compares the color with the target, and

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S. Jeong et al. Process Safety and Environmental Protection 175 (2023) 99–110

additional dyes, Na2CO3, or Na2SO4 are added, with these additions


being based on operator experience (Cho and Kim, 2001). If the color
difference is too large, an additional quantity of dye is measured and
added to the dyeing machine; this dye is then briefly absorbed and the
fabric is re-sampled. This process is repeated until the target standards
are met, consuming significant time and generating considerable cost.
To address these problems, a technique for real-time measurement and
control of exhaustion-rate outliers during dyeing process necessary;
however, but no fundamental solution has been proposed to date.

1.2. Contribution

To address these challenges, this work proposed a framework for


cleaner production of textile dyeing process using novel exhaustion-rate
meter and multi-layer perceptron-based prediction model to solve the
environmental problems caused by re-dyeing by controlling the Fig. 1. Simplified diagram of round-type jet dyeing machine.
exhaustion-rate outliers. The aim of this study is to increase the RFT by
considering the color difference and dyeing uniformity using the sug­ wall. Moreover, the reactive dye is heated through a heat exchanger to
gested framework and, hence, to overcome the serious problems of satisfy the temperature conditions suitable for reaction of the dye. The
environmental contamination as well as excessive time consumption rotating fabric continues to absorb and react with the dye present in the
and cost. lower part of the cloth chamber.
The novel contributions are as follows: Fig. 2 shows exhaustion-rate curves over time measured for a fixed
Na2SO4 input of 10 g and added Na2CO3, where the latter varied from
1) An NERM is first developed to measure the real-time exhaustion- 0 to 20 g in 5 g increments. In general, the dyeing process consists of two
rates under various dyeing conditions; it is useful for prediction of stages. In the first stage, the fabric absorbs the dye; in the second stage,
the dyeing uniformity and color difference, which are the product the dye is fixed on the fabric through covalent bonding between them. In
quality standards. In addition, because the proposed exhaustion-rate the first adsorption stage, Na2SO4 is used to facilitate adsorption by
meter detects exhaustion-rate outliers during textile dyeing, prob­ reducing the repulsive force between the fiber surface and anionic
lems are recognized as soon as they occur. reactive dye. In the second fixation stage, the dye is fixed onto the fabric
2) The proposed MLP-based prediction model is applied to quickly and by forming covalent bonds between the fabric and dye with Na2CO3. As
accurately control exhaustion-rate outliers in various scenarios. The shown in Fig. 2, the exhaustion-rate increases after 20 min in the fixa­
results indicate that this model can suggest solutions that adhere to tion stage because the dye molecules already absorbed by the fabric
the optimum exhaustion behavior values. become fixed through covalent bonding, while the dye molecules in the
3) The suggested framework, which integrates the developed solution are also simultaneously absorbed by the fabric.
exhaustion-rate meter and the MLP-based prediction model to con­
trol exhaustion-rate outliers, contributes to RFT improvement 2.2. Dyeing wastewater
considering the color difference and dyeing uniformity. In addition,
as the proposed framework also detects and controls the real-time Textile industries are responsible for one of the major environmental
exhaustion-rate outliers during the dyeing process, re-dyeing is pollution problems, because they discharged significant dyeing waste­
prevented as appropriate and timely responses are facilitated. water. Dyeing process requires considerable volumes of both hot water
4) This study is meaningful because this work is successfully possible to and the chemicals necessary for reactive dyeing. This process generates
control the exhaustion-rate outliers and to solve environmental wastewater, which cause serious environmental pollution. In general, up
contamination of dyeing wastewater by preventing re-dyeing process to 200,000 tons of wastewater are discharged every year during the
as well as excessive time consumption and cost. Thus, it will have dyeing process, due to the inefficiency of the dyeing process (Ogugbue
great environmental and economic improvement and provide valu­ and Sawidis, 2011). The wastewater discharged from textile factories
able insight of cleaner production in textile dyeing process.

2. Process description

2.1. Dyeing process

In the experiments performed in this study, a round-type jet dyeing


machine on the pilot-plant scale was used to dye fabric-type textiles
(Iriani and Bachtiar, 2019). Fig. 1 is a simplified diagram of a round-type
jet dyeing machine, which can be applied in batch dyeing processes
including dyeing, bleaching, washing, and rinsing. The process is
fed-batch process and it allows quick dyeing under high-temperature
and high-pressure conditions and consists of a cloth guide tube, cloth
chamber, reel lifter, and heat exchanger. The dyeing process is as fol­
lows. In the cloth chamber, which is a closed tube system, the dye is
sprayed through a nozzle inside the cloth guide tube. While the nozzle
continuously sprays dye, the fabric absorbs the dye while being simul­
taneously rotated over the reel lifter owing to the injection pressure. The
turbulence generated by the dye sprayed from the nozzle facilitates
penetration of the dye into the fabric and minimizes the mechanical Fig. 2. Exhaustion-rate curves measured for 10-g Na2SO4 and 0- (red), 5-
impact on the fabric by preventing the fabric from touching the tube (green), 10- (blue), 15- (yellow), and 20-g (black) Na2CO3.

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S. Jeong et al. Process Safety and Environmental Protection 175 (2023) 99–110

are a mixture of dyes, metals and other pollutants and it are high in of a measuring section to measure the dye absorbance at regular time
colour, pH, suspended solids (SS), chemical oxygen demand (COD), intervals and an analysis component to analyze and display the
biochemical oxygen demand (BOD), metals and salts. Table 1 is the measured data on a monitor. The measuring section is composed of a
typical characteristics of dyeing wastewater according to difference filter, a pump, a circulation line through which the dye is circulated, a
references. lamp as a light source, and a detector. The filter removes impurities such
Table 1 shows the textile dyeing wastewater contains high environ­ as fiber particles from the extracted dye to measure the absorbance of
mental pollutants. In addition, most of these wastewater persist in the the dye itself, and the pump continuously circulates the dye through the
environment as a result of their high stability to light, temperature, circulation line. The circulate line is made of a material that allows
water, detergents, chemicals, soap and other parameters such as bleach measurement in the ultraviolet/visible range at a wavelength range of
and perspiration. Thus, the wastewater from dyeing process causes 200–750 nm. This material has high heat resistance, pressure resistance,
significant water pollution. Therefore, if the re-dyeing is required, the chemical resistance, and 0.55-mm penetration length. A pulsed xenon
wastewater is significantly increased compared to a one-time dyeing. To lamp is used as the light source to allow stable measurements over a
solve the problems associated with re-dyeing, it is necessary to improve wavelength range of 220–750 nm. The detector can measure the dye
the right-first-time (RFT) %, which is the rate at which the target quality solution at a high resolution of 0.3–1.5-nm full width at half maximum
is obtained with just one dyeing, this can be achieved by considering the using a 25-μm slit over a wavelength range of 200–1100 nm. The
dyeing conditions that affect product quality. analysis component converts the real-time spectrum of the dye
measured in the measuring section to the exhaustion-rate and displays
3. Methodology the result in real time.
The dye adsorption rate in the proposed NERM is calculated as fol­
In this section, we describe the types of dyes used in the dyeing lows. Generally, when a single dye is used for cotton fabrics, the dye
process (Section 3.1) and the NERM developed to measure the real-time concentration can be determined by measuring the dye absorbance. The
exhaustion behavior (Section 3.2). The actual data measured with this relationship between the dye absorbance and concentration is expressed
meter are applied to an artificial neural network to derive surrogate by Beer’s law as follows (Fernández-Pérez et al., 2019):
models for data augmentation (Section 3.3). Using these surrogate
A=ε×l×C (1)
models, we develop the abovementioned MLP-based prediction model to
control the exhaustion-rate outliers; this model predicts and adjusts the Where,
additional Na2SO4 and Na2CO3 input amounts in response to the specific A = Absorbance.
conditions that do not follow the optimal exhaustion-rate curve (Section ε = Molar attenuation coefficient.
3.4). Finally, the model performance evaluation is discussed (Section l = Optical path in length.
3.5). C = Concentration of the attenuating species.
The absorbance and concentration of a mixture containing n types of
3.1. Dyeing materials dye can be expressed by the following equation:

A 100% cotton fabric was used as the dyeing substrate. The neutral An = k1 × C1 + k2 × C2 + ⋯ + kn × Cn (2)
salt and alkali were Na2SO4 and Na2CO3, respectively, both of which
were extra-pure reagents. In the dyeing process, Na2SO4 was first added Where,
in 10%, 30%, 30%, and 30% proportions at 3-min intervals, and Na2CO3 k = ε × l.
was added in a single batch at the 40-min mark. Novacron Blue ECR (NB When there is no interaction between the dyes, the absorbance
ECR) was used as the reactive dye, the chemical structure of which is spectrum of the mixed dyes is calculated as the sum of the absorbance
shown in Fig. 3 (Lingeswari and Vimala, 2019). spectra corresponding to the concentration of each dye:
[An ] = [k1 ⋯kn ] × [Cn ] (3)
3.2. Novel exhaustion-rate meter (NERM)
When the dye concentration is low, it can be easily estimated from its
linear relationship with the absorbance. However, the relationship di­
The NERM was developed to satisfy the two most important factors
verts from Beer’s law when the dye concentration is high, and the in­
influencing dyeing quality, i.e., the color difference and dyeing unifor­
dividual spectrum of the n dyes combined is then applied to Eq. (3) to
mity, and ultimately, to improve the RFT. The developed NERM mea­
calculate the dye concentration at a certain point in time. Finally, the
sures the final exhaustion-rate as well as the real-time exhaustion
dye concentration at a specific time is substituted into the following
behavior of the dye, such that the RFT can be increased through optimal
equation to determine the exhaustion-rate of each dye:
control.
Fig. 4 is a simplified diagram of the developed NERM, which consists [Cn ]
[En ] = 1 − (4)
[Cn,0 ]
Table 1
Typical characteristics of dyeing wastewater according to difference references. Where,
References Ghaly et al. (2014), Kehinde and Hussein Unit
En = Total dye concentration.
Ghaly & Ananthashankar Aziz (2014) (2013) Cn = Dye concentration at specific time.
(2013) Cn,0 = Initial dye concentration.
Colour 50–2500 50–2500 - Pt-
Co
pH 6–10 6.95–11.8 5.5–10.5 - 3.3. Prediction model to control exhaustion-rate outliers
SS 15–8000 15–8000 100–5000 mg/
l
This section describes the development of the proposed prediction
COD 150–12,000 150–30,000 150–10,000 mg/
l model to control the exhaustion-rate outliers. This prediction model
BOD 80–6000 80–6000 100–4000 mg/ provides operators with guidelines to control the dyeing process when
l the real-time exhaustion rate does not follow the optimal exhaustion-
Metals and <7105 437–2242 610–2175 mg/ rate curve. Specifically, the model suggests additional Na2SO4 and
salt l
Na2CO3 inputs when an outlier which does not follow the optimal

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S. Jeong et al. Process Safety and Environmental Protection 175 (2023) 99–110

Fig. 3. Chemical structure of Novacron Blue ECR (NB ECR).

Fig. 4. Simplified diagram of developed novel exhaustion-rate meter (NERM).

exhaustion-rate curve arises. The MLP regression algorithm is used to ordinary linear functions, a linear estimation function, y = wT x + b,
determine the relationship between the exhaustion rate and certain must be considered. In the MLP approach, an activation function is
conditions (time, temperature, and Na2SO4 and Na2CO3 input amounts). introduced to the linear estimation function to solve nonlinear
Fig. 5 shows the development procedure of the suggested MLP-based functions.
prediction model to control the exhaustion-rate outliers. Each section Fig. 7 shows the MLP calculation process. Here, x1 …xn are input
of the figure is discussed in the following subsections. In detail, Section vectors, ω1 …ωn are weights corresponding to each input vector, and b
3.3.1 describes the overall concept of MLP application to regression represents the bias. The weighted summation based on the input vectors
analysis. Section 3.3.2 describes the data generation (Fig. 5, Step 1) and weights is applied to the activation function, f, and the result be­
through the NERM and the data preprocessing (Fig. 5, Step 2), and comes the input for the subsequent hidden layer or output unit. In the
Section 3.3.3 describes the construction process of a surrogate model MLP approach, a back-propagation procedure is usually performed by
that predicts the exhaustion rate under certain conditions using the reversely differentiating the activation function from the output layer to
preprocessed data (Fig. 5, Step 3). Section 3.3.4 explains the exhaustion- the input layer, to reduce the error between the value from the final
rate data extraction processes for numerous cases using different con­ output layer and the actual output value. The commonly used activation
structed surrogate models; the development of the prediction model to functions are ReLU, sigmoid, and tanh (Eq. (5)):
control the exhaustion-rate outliers is also described (Fig. 5, Steps 4 and
ReLU(x) = max(0, x)
5). Finally, Section 3.3.5 presents the regression model performance
indicators. 1
sigmoid(x) =
1 + exp( − x)
3.3.1. Multi-layer-perceptron (MLP) regression algorithm
MLP is a machine learning method in which computers form an exp(x) − exp(− x)
artificial neural network similar to the human brain. Recently, MLP has tanh(x) = (5)
exp(x) + exp(− x)
demonstrated superior performance in various industries by processing
not only structured, but also unstructured data related to computer Regarding the MLP experiment, we used Python 3.7.7 version, ten­
vision, voice recognition, natural language processing, signal process­ sorflow 2.1.0 version, keras 2.8.0 version, and additionally scikit-learn
ing, etc(J. J. Lee et al., 2021; Y. Lee et al., 2021; Mikolov et al., 2013; 0.23.2 version.
Roh et al., 2021; Sangeetha and Prasad, 2006; Sukanya and Sunny,
2019). 3.3.2. Data generation and preprocessing
Generally, an MLP structure consists of an input layer, hidden layer, For the experiments performed in this study, a total of 615 data
and output layer. This structure is referred to as a deep neural network points were extracted using the NERM. Four data attributes were
when there are three or more hidden layers, as shown in Fig. 6. To solve considered: time, temperature, Na2SO4 input amount, and Na2CO3 input
amount. There were time, ranging from 0 to 120 min at 3-min intervals,

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S. Jeong et al. Process Safety and Environmental Protection 175 (2023) 99–110

Fig. 5. Development procedure of suggested multi-layer perceptron (MLP)-based prediction model to control exhaustion-rate outliers.

and the temperature varied to certain set values over time. Three the corresponding data were eliminated. The remaining dataset after
Na2SO4 input amounts were considered, i.e., 10, 30, and 50 g, along preprocessing contained 41 (time) × 3 (Na2SO4) × 4 (Na2CO3) = 492
with five Na2CO3 input amounts, i.e., 0, 5, 10, 15, and 20 g. Data pre­ data elements.
processing was largely performed in two steps. In the first step, any data Data normalization was performed because the scale of each attri­
unnecessary for the regression model learning process were removed. In bute value in the dataset varied widely; that is, 0–120 min; 30–60 ◦ C;
the second step, data normalization was performed because the units 10, 30, and 50 g; 5, 10, 15, and 20 g; and 0.0–0.957% for the time,
varied by data attribute according to different value scales, which hin­ temperature, Na2SO4 input, Na2CO3 input, and final exhaustion attri­
dered the learning process. butes, respectively. Among the various normalization techniques, the z-
In the dyeing process, the Na2CO3 fixes the dye onto the fabric by score normalization method was chosen to robustly process the data in
forming covalent bonds between the two. In the experiments performed the presence of outliers. In the z-score normalization approach, the
herein, no trend was observed for an Na2CO3 input amount of 0 g; thus, mean and standard deviation of the values for the same attribute are

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S. Jeong et al. Process Safety and Environmental Protection 175 (2023) 99–110

were used. Similarly, SMNa2CO3 was constructed by taking the Na2CO3


input timing into account and using the time attribute values past
40 min in dataorigin. There were 27 (time) × 3 (Na2SO4) × 4 (Na2CO3) =
324 corresponding data elements. The MLP algorithm was used to
construct SMNa2SO4 and SMNa2CO3. As regards the MLP hyper-parameter,
the two models equally consisted of three hidden layers (h1 , h2 , h3 ), and
the unit of each hidden layer was set to 100. ReLU was used as the
activation function for h1 and h2 and sigmoid was used for h3 . Finally,
Adam was used as the optimizer function, and the mean squared error
(MSE) was set as the loss function appropriate for regression analysis.

3.3.4. Development of prediction model to control exhaustion-rate outliers


This section describes the data augmentation process (Fig. 5, Step 4)
using the SMNa2SO4 and SMNa2CO3 described in Section 3.3.3, and the
development of the corresponding prediction models PMNa2SO4 and
PMNa2CO3 to control the exhaustion-rate outliers (Fig. 5, Step 5).
Fig. 6. MLP regression structure. For data augmentation in the proposed framework, the values of the
independent data attributes (time, temperature, Na2SO4 input, and
Na2CO3 input) are subdivided to generate new independent variable
data. At this point, the Na2SO4 input and Na2CO3 input attributes must
be considered. Because these two attributes have larger intervals in the
original data compared to the other attributes, the input values for the
Na2SO4 and Na2CO3 input attributes are subdivided to generate new
input values. For the experiments performed in this work, the three
Na2SO4 input amounts in dataorigin (10, 30, and 50 g) were expanded to
41 cases with consecutive integer values of 10, 11, 12,., 50 g. Similarly,
the four Na2CO3 input amounts (5, 10, 15, and 20 g) were expanded to
16 cases with consecutive integer values of 5, 6, 7,., 20 g. The total
number of combinations of these cases was 41 (time) × 41 (Na2SO4) ×
Fig. 7. Example of weighted sum and activation function. 16 (Na2CO3) = 26,896. These data constituted dataNa2SO4 and were fed
into PMNa2SO4. The total number of data elements to be fed into
used to scale the data to a normal distribution with a mean of 0 and a PMNa2CO3, considering the Na2CO3 input timing, was 27 (time) × 41
standard deviation of 1, such that (Patro and sahu, 2015) (Na2SO4) × 16 (Na2CO3) = 17,612.
Here, dataNa2SO4 and dataNa2CO3, which were more granular than

vi =
vi − E
(6) dataorigin based on SMNa2SO4 and SMNa2CO3, indicated the exhaustion
std(E) rate for a specific time, temperature, Na2SO4 input amount, and Na2CO3
input amount. In other words, dataNa2SO4 indicates the Na2SO4 input
where E represents the values of a certain attribute, vi is the ith value amount at a specific condition (time, temperature, and Na2CO3 input
within E, and vi is the z-score normalized value of vi . In addition, E is

amount, final exhaustion rate), while dataNa2CO3 indicates the Na2CO3
the average value of E, defined as input amount at a specific condition (time, temperature, and Na2SO4
input amount, final exhaustion rate). From this perspective, PMNa2SO4
1∑ n
E= vi (7) was developed using dataNa2SO4 under specific conditions (time, tem­
n i=1
perature, Na2CO3 input, and exhaustion rate), and PMNa2CO3 was
Here, std(E) is the standard deviation of the attribute values, defined developed using dataNa2CO3. MLP-based regression was applied to
as PMNa2SO4 and PMNa2CO3. As regards the MLP hyper-parameter, three
√̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅ hidden layers (h1 , h2 ,h3 ) were established for the two models, as for the
∑ surrogate model construction. The unit of each hidden layer was set to
n
1
std(E) = (vi − E)2 (8)
(n − 1) i=1 100. ReLU was used as the activation function for h1 and h2 and
sigmoid was used for h3 . Finally, Adam was used as the optimizer
3.3.3. Construction of surrogate models for data augmentation function and MSE was set as the loss function.
A surrogate model is a small-scale extended analysis model designed
to simulate input and output properties similar to those of an actual 3.3.5. Model performance evaluation criteria
model. Surrogate models are employed when derivation of the results of The indicators commonly used to evaluate the performance of
interest is time-consuming and expensive, or when measurement is regression analysis models include the mean absolute error (MAE, Eq.
difficult, as in cases of complex computational simulation (Anand et al., (9)), MSE (Eq. (10)), root mean squared error (RMSE, (Eq. (11)), and the
2011; Hwang and Martins, 2018; Lim et al., 2021). In the dyeing process coefficient of determination (the R2 score, Eq. (12)) (Kulinich et al.,
considered in this work, the data acquisition is limited by the high time 2019; Kwon et al., 2021, 2020; J. Lee et al., 2021; Y. Lee et al., 2021).
and financial costs generated by measurement of the exhaustion rate When y is the real value, ̂ y is the value predicted from the regression
under specific conditions (time, temperature, Na2SO4 input, and Na2CO3 analysis, and n is the number of data points, each indicator can be
input). defined as follows.
Therefore, surrogate models were constructed for data augmenta­ ∑
n
tion. First, surrogate model SMNa2SO4 was constructed as a Na2SO4 yi|
|yi − ̂
prediction model to predict the exhaustion rate depending on the spe­ MAE = i=1 (9)
n
cific operating conditions (time, temperature, Na2SO4 input, and
Na2CO3 input). The data obtained after preprocessing, labeled dataorigin, Note that MAE is the most intuitive error indicator because it cal­
culates the mean as an absolute value following addition of the

105
S. Jeong et al. Process Safety and Environmental Protection 175 (2023) 99–110

differences between the predicted and real values of the model. molecules already absorbed by the fabric were becoming fixed through
covalent bonding, while the dye molecules in the solution were also

n
(yi − ̂y i )2 being simultaneously absorbed by the fabric. This process is referred to
MSE = i=1
(10) as “secondary exhaustion.” Section 4.2 describes the surrogate model
n
constructed using the data measured by the proposed NERM.
Here, MSE is obtained by calculating the mean following addition of
the square of the differences between the predicted and real values of the
model, which can be considered as the mean of the area of the differ­ 4.2. Performance of surrogate model for data augmentation
ences. Given this difference from MAE, the presence of an outlier yields a
large MSE value. This section reports the performance evaluation of the surrogate
√̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅ model constructed using the MLP-based regression analysis described in
√∑
√n Section 3.3.3. The training and test datasets were split at a 0.75:0.25
√ (yi − ̂y )2 ratio to build the regression model, and RMSE and R2 were used as

RMSE = i=1 (11) performance indicators. To demonstrate the MLP performance, well-
n
known regression analysis methods, i.e., lasso, ridge, and support vec­
As apparent from the equation, RMSE is the square root value of MSE tor regression, were applied to identical datasets. Each model was sub­
and, thus, its interpretation is simplified by reconverting the unit of the jected to 100 regression experiments and the training and test data were
error indicator to that of the real value. Although similar to MAE, RMSE randomly varied each time. The performance of each regression model
is more robust. This is because, for MAE, the total sum is divided by n; was compared in terms of R2 and RMSE. Table 2 lists the mean and
√̅̅̅
however, for RMSE, the total sum is divided by n. Thus, a penalty is standard deviation values obtained for the 100 experimental results for
applied in the case of a large error. each model.

n From Table 2, the MLP regression exhibited the highest performance
y i )2
(yi − ̂ and the smallest error, with MAE, MSE, RMSE and R2 values of 0.007,
SSR SSE
2
R = = 1− i=1
= 1− ∑ n (12) 0.001, 0.016 and 0.994, respectively.
SST SST
(yi − y)2 Fig. 9 shows a comparison between the actual exhaustion-rate values
i=1
of dataorigin (x-axis) and the predicted values obtained from the MLP-
Here, the total sum of squares (SST)is expressed as y − y and indicates based regression model (y-axis). The solid red line is the y = x trend­
the total deviation, the regression sum of squares (SSR) is expressed as line. The values generally fall on this line, indicating the high perfor­
y − y and indicates the deviation described by the regression equation,
̂ mance of the MLP regression model.
and the error sum of squares(SSE) is expressed as y − y and indicates the Fig. 10 shows the exhaustion-rate behaviors over time for different
deviation that is not described by the regression equation. The other Na2CO3 and Na2SO4 input amounts, where the solid lines ( − ) indicate
performance indicators can vary widely in value depending on the data the actual values and the triangles () indicate the predicted values from
scale, making performance evaluation based on absolute values difficult; the SMNa2SO4 surrogate model. Fig. 10(a)–(d) correspond to the cases for
however, R2 indicates the performance of a regression model in relative which the Na2CO3 input amounts were 5, 10, 15, and 20 g, respectively.
values and, thus, the interpretation is intuitive. It is apparent that the regression-based surrogate model was in good
agreement with the exhaustion behavior over time. Hence, the surrogate
4. Results & discussion model defined using the actual dataset can be considered reliable.

4.1. Exhaustion-rate measured by NERM


4.3. Performance of prediction model to control exhaustion-rate outliers

Fig. 8 shows the exhaustion-rate curve measured by the NERM


The ultimate goal of this study was to provide users with a method to
proposed in this study for 30-g Na2SO4 and 20-g Na2CO3. The curve
identify the additional Na2SO4and Na2CO3 input amounts required
increases rapidly in the initial 12 min, corresponding to the period when
when the dyeing process does not conform to the optimal exhaustion-
the Na2SO4 was divided and injected to increase the affinity with the
rate curve. As discussed in Section 3.4, the dyeing process consists of
reactive dye. The Na2CO3 was introduced at the 20-min mark to fix the
two stages: exhaustion and fixation. In the proposed framework, MLP
dye to the fabric through covalent bonding. As apparent from the curve,
regression is applied to define a model that predicts the additional
the exhaustion-rate increased after 20 min; this was because the dye
Na2SO4 and Na2CO3 input amounts required in each stage. In the
experiment performed here, the training and test datasets were split at a
ratio of 0.75:0.25 for learning and evaluation, and RMSE and R2 were
used as evaluation indicators. Hence, the high performance of the two
obtained prediction models, PMNa2SO4 and PMNa2CO3, was
demonstrated.
Fig. 11 shows a comparison of the actual Na2SO4 input amounts (x-
axis) under specific conditions (time, temperature, Na2CO3 input, and
final exhaustion) and the Na2SO4 input amounts obtained from the
prediction model (y-axis), i.e., PMNa2SO4. The solid red line is the y = x
trendline and the RMSE and R2 values of the PMNa2SO4 were 1.447 and
0.985, respectively, based on the re-scaled values.
Fig. 12 compares the actual Na2CO3 input amounts under specific
conditions (time, temperature, Na2SO4 input, and final exhaustion) and
the Na2CO3 input amounts obtained from the prediction model, i.e.,
PMNa2CO3. The RMSE and R2 values of PMNa2CO3 were 0.100 and 0.998,
respectively, based on the re-scaled values. Thus, both models exhibited
high performance, indicating that they are sufficiently reliable to pro­
Fig. 8. Exhaustion-rate curve measured using proposed NERM for 30-g Na2SO4 vide operators with guidelines on exhaustion-rate outliers during the
and 20-g Na2CO3. dyeing process.

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S. Jeong et al. Process Safety and Environmental Protection 175 (2023) 99–110

Table 2
Performance of each model.
Regression model MAE MSE RMSE R2

Lasso regression 0.068 ± 0.005 0.013 ± 0.003 0.110 ± 0.015 0.726 ± 0.040
Ridge regression 0.068 ± 0.006 0.012 ± 0.003 0.273 ± 0.020 0.723 ± 0.037
Support vector regression 0.125 ± 0.025 0.105 ± 0.045 0.066 ± 0.017 0.902 ± 0.035
MLP regression 0.007 ± 0.002 0.0001 ± 6.06E − 05 0.016 ± 0.006 0.994 ± 0.004

Fig. 14 illustrates two scenarios in which outliers deviating from the


optimal exhaustion-rate curves occurred 40 min after the start of the
dyeing process. The corresponding conditions are listed in Table 5.
Table 5 lists the dyeing conditions, optimal exhaustion rates, and
outliers for the two scenarios in Fig. 14. In Scenario 3, dyeing proceeded
normally along the optimal exhaustion-rate curve for the first 54 min,
after which the exhaustion rate decreased to 0.75 rather than increasing
to 0.849 as expected. Similarly, after dyeing proceeded normally in the
first 78 min of Scenario 4, the exhaustion rate decreased to 0.82 rather
than increasing to 0.917. When these outliers occurred, the conditions
(time, temperature, Na2SO4 input amount, and current final exhaustion)
of each situation were fed into PMNa2CO3 to predict the Na2CO3 input
amount and to determine the appropriate additional Na2CO3 amount.
Table 6 lists the attribute values fed into PMNa2CO3 for each scenario,
the predicted Na2CO3 input amounts, and the additional Na2CO3
amounts required when the exhaustion-rate outliers occurred. For Sce­
nario 3, when the exhaustion rate dropped to 0.75 under the conditions
Fig. 9. Plot of predicted vs. actual exhaustion-rate values. listed in Table 5, PMNa2CO3 determined the Na2CO3 input amount to be
9.896 g. Therefore, conformance with the optimal exhaustion-rate curve
4.4. Application could be achieved by introducing an additional amount of 10.104 g. For
Scenario 4, when the exhaustion rate dropped to 0.82, PMNa2CO3
This section presents examples of exhaustion-rate outlier manage­ determined that the Na2CO3 input amount was 6.174 g and that an
ment achieved by applying the PMNa2SO4 and PMNa2CO3 models devel­ additional amount of 3.826 g was required to conform to the optimal
oped in this study. Note PMNa2SO4 was used in the first 40 min, whereas exhaustion rate. These results demonstrate that the PMNa2SO4 and
PMNa2CO3 was used after 40 min PMNa2CO3 developed in this study can be used to provide guidelines for
Fig. 13 illustrates two scenarios in which an outlier deviating from scenarios in which the exhaustion-rate outliers deviate from the optimal
the optimal exhaustion-rate curve occurred in the first 40 min from the exhaustion-rate curve.
start of the dyeing process. The conditions corresponding to these sce­ Table 7 lists the attribute values fed into PMNa2CO3 for each scenario,
narios are listed in Table 3. In each plot, the solid yellow line represents the predicted Na2CO3 input amounts, and the additional Na2CO3
the optimal exhaustion-rate curve, the blue dotted line represents the amounts required when the exhaustion-rate outliers occurred. For Sce­
ongoing dyeing process along the optimal exhaustion-rate curve, and the nario 3, when the exhaustion-rate dropped to 0.75 under the conditions
red star represents the exhaustion-rate outlier. listed in Table 5, PMNa2CO3 determined the Na2CO3 input amount to be
Table 3 lists the dyeing conditions, optimal exhaustion rates, and 9.896 g. Therefore, conformance with the optimal exhaustion-rate curve
outliers found in the two scenarios shown in Fig. 13. In Scenario 1, could be achieved by introducing an additional amount of 10.104 g. For
dyeing proceeded normally along the optimal exhaustion-rate curve for Scenario 4, when the exhaustion-rate dropped to 0.82, PMNa2CO3
the first 21 min; then, the exhaustion rate decreased to 0.58 rather than determined that the Na2CO3 input amount was 6.174 g and that an
increasing to 0.682 as expected. Similarly, after dyeing proceeded nor­ additional amount of 3.826 g was required to conform to the optimal
mally in the first 24 min of Scenario 2, the exhaustion rate decreased to exhaustion-rate. These results demonstrate that the PMNa2SO4 and
0.55 rather than increasing to 0.702. When these outliers arose, the PMNa2CO3 developed in this study can be used to provide guidelines for
conditions (time, temperature, Na2CO3 input amount, and exhaustion scenarios in which the exhaustion-rate outliers deviate from the optimal
rate) of each scenario were fed into PMNa2SO4 to predict the Na2SO4 exhaustion-rate curve.
input amount and to determine the appropriate additional Na2SO4
amount (Table 3). 5. Conclusion
Table 4 lists the attribute values fed into PMNa2SO4 for each scenario,
the predicted Na2SO4 input amounts, and the additional Na2SO4 In this study, we proposed a framework for cleaner production of
amounts required when the exhaustion-rate outliers occurred. For Sce­ textile dyeing process using novel exhaustion-rate meter and multi-layer
nario 1, under the conditions of 21 min, 30 ◦ C, 10-g Na2CO3 input perceptron-based prediction model to solve the environmental problems
amount, and a 0.58 exhaustion rate, the Na2SO4 input amount was caused by re-dyeing by controlling the exhaustion-rate outliers. This
determined to be 25.877 g based on PMNa2SO4. In that case, it was study makes two major contributions to the literature. First, the NERM
possible to attain conformance with the optimal exhaustion-rate curve was developed to measure the real-time exhaustion rate as well as the
by adding 24.123 g of Na2SO4 [i.e., 50 g (initial Na2SO4 input) – final exhaustion rate under various dyeing conditions. This meter is
25.877 g (the amount used for dyeing)]. Similarly, for Scenario 2, under useful to predict and control the dyeing uniformity and color difference,
the conditions of 24 min, 30 ◦ C, 20-g Na2CO3 input amount, and a 0.55 which are the relevant product quality standards. In addition, because
exhaustion rate, the Na2SO4 input amount was determined to be the NERM also detects real-time exhaustion-rate outliers during textile
11.051 g based on PMNa2SO4. In that case, conformance with the optimal dyeing, these outliers can be controlled immediately. Second, in this
exhaustion-rate curve could be achieved by adding 18.949 g of Na2SO4 work, the proposed MLP-based prediction model was applied to predict
(i.e., 30 – 11.051 g). and control various exhaustion-rate outliers quickly and accurately.

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S. Jeong et al. Process Safety and Environmental Protection 175 (2023) 99–110

Fig. 10. Actual and predicted using SMNa2SO4 values for real-time exhaustion behaviors for different Na2CO3 and Na2SO4 input amounts.

Fig. 11. Plot of predicted vs. actual values for Na2SO4 inputs. Fig. 12. Plot of predicted vs. actual values for Na2CO3 inputs.

Through this model, solutions that conform to the optimum exhaustion economic improvement and provide valuable insight of cleaner pro­
behavior can be suggested directly; thus, proper and immediate control duction in textile dyeing process. In this work, the outliers which
is possible and the need for re-dyeing is prevented. Thus, since the re- incurred according to the Na2CO3 and Na2SO3 input amounts is only
dyeing procedure is prevented through the suggested framework by considered. However, the other operating conditions such as dye ratio in
increasing right first time %, it will have great environmental and the dyeing solution, input time of Na2CO3 and Na2SO3, etc. are also

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S. Jeong et al. Process Safety and Environmental Protection 175 (2023) 99–110

Fig. 13. Abnormal scenarios due to insufficient Na2SO4 (Table 2).

Table 3
Conditions for scenarios of Fig. 13.
Table 5
Classification Scenario 1 Scenario 2
Conditions for scenarios of Fig. 14.
Time (min) 21 24
Classification Scenario 3 Scenario 4
Temperature (℃) 30 30
Na2SO4 input (g) 50 30 Time (min) 54 78
Na2CO3 input (g) 10 20 Temperature (℃) 59 60
Optimal exhaustion rate 0.682 0.702 Na2SO4 input (g) 10 30
Exhaustion-rate outlier 0.58 0.55 Na2CO3 input (g) 20 10
Optimal exhaustion rate 0.849 0.917
Exhaustion-rate outlier 0.75 0.82

Table 4
Na2SO4 inputs determined from PMNa2SO4.
Table 6
Classification Scenario 1 Scenario 2
Na2CO3 inputs determined from PMNa2CO3.
Time (min) 21 24
Classification Scenario 3 Scenario 4
Temperature (℃) 30 30
Na2CO3 input (g) 10 20 Time (min) 54 78
Exhaustion-rate outlier 0.58 0.55 Temperature (℃) 59 60
Predicted Na2SO4 input (g) 25.877 11.051 Na2CO3 input (g) 20 10
Suggested additional Na2SO4 amount (g) 24.123 18.949 Exhaustion-rate outlier 0.75 0.82
Predicted Na2SO4 input (g) 9.896 6.174
Suggested additional Na2SO4 amount (g) 10.104 3.826

Fig. 14. Abnormal scenarios due to insufficient Na2CO3 (Table 4).

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interests or personal relationships that could have appeared to influence Kwon, H., Oh, K.C., Choi, Y., Chung, Y.G., Kim, J., 2021. Development and application of
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National University Research Grant, 2022 and the Korea Institute of jksct.2013.37.7.952.
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