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Alexandria Engineering Journal (2022) 61, 3215–3228

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Alexandria University

Alexandria Engineering Journal


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Improving the rotary kiln-electric furnace process


for ferronickel production: Data analytics-based
assessment of dust insufflation into the rotary kiln
flame
Johanna M. Romero a, Yuleisy S. Pardo a, Maricel Parra a, Andy De J. Castillo a,
Heriberto Maury a, Lesme Corredor b, Iván Sánchez c, Bernardo Rueda c,
Arturo Gonzalez-Quiroga b,*

a
Department of Mechanical Engineering, Universidad del Norte, Barranquilla 080001, Colombia
b
UREMA Research Unit, Department of Mechanical Engineering, Universidad del Norte, Barranquilla 080001, Colombia
c
Cerro Matoso S.A, Montelı´bano, Colombia

Received 30 April 2021; revised 24 June 2021; accepted 14 August 2021


Available online 26 August 2021

KEYWORDS Abstract Ferronickel contains 60–80 wt% Fe and 40–20 wt% Ni and is a feedstock for manufac-
Nickel laterite; turing stainless steel and other ferrous alloys. The primary pyrometallurgical route to produce fer-
Calcination; ronickel from laterite nickel ores is the Rotary Kiln-Electric Furnace (RKEF) process. In the
Reduction; RKEF process, minerals undergo calcination and partial reduction in a rotary kiln. Large amounts
Agglomeration; of mineral dust leave the kiln entrained in flue gases. Dust insufflation is a potential solution in
Machine learning; which dust particles enter directly into the burner flame. The aim is that the insufflated dust softens,
Data handling agglomerates, and finally joins the minerals stream that goes into the electric furnace. We applied
data analytics techniques to a 1-year operation database to assess the operation before and after
dust insufflation in an industrial rotary kiln furnace. Bootstrapping revealed statistically significant
differences in the operation with and without dust insufflation. Principal Component Analysis
(PCA) and k-means clustering were used as exploratory techniques. PCA showed subsets of vari-
ables that significantly influence the dataset variance, and k-means allowed distinguishing operation
conditions for dust insufflation with encouraging results for the calcine-to-fresh mineral and the
natural gas-to-calcine ratios. These results pave the way towards successfully implementing dust
insufflation in the RKEF process.
Ó 2021 THE AUTHORS. Published by Elsevier BV on behalf of Faculty of Engineering, Alexandria
University. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/
licenses/by-nc-nd/4.0/).

* Corresponding author.
E-mail address: arturoq@uninorte.edu.co (A. Gonzalez-Quiroga).
Peer review under responsibility of Faculty of Engineering, Alexandria University.
https://doi.org/10.1016/j.aej.2021.08.036
1110-0168 Ó 2021 THE AUTHORS. Published by Elsevier BV on behalf of Faculty of Engineering, Alexandria University.
This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
3216 J.M. Romero et al.

Nomenclature and notation

ANN artificial neural network PCA principal component analysis


ANFIS artificial neuro-fuzzy inference system PCR principal component regression
ARIMA autoregressive integrated moving average PLS partial least squares
Dc cook’s distance R2 coefficient of determination
EWMA exponential weighted moving average RKEF rotary kiln-electric furnace
KPI key performance index SVD single value decomposition
MLR multiple linear regression SVM support vector machine
MNAR missing-not-at-random y original observations
MRT mean residence time ys filtered observations using moving average filter
MSE mean squared error Ybj value of an estimate with all observations of the
MWW Mann-Whitney-Wilcoxon test dataset included
NaN not a number YbjðiÞ value when the observation i is omitted
P number of coefficients in the regression model for wt weight percentage
the Cook’s distance a smoothing coefficient for moving average filter
PC principal component

1. Introduction about 700 °C, the calcination begins. During calcination, min-
erals dissociate into oxides releasing water, as indicated by
Ferronickel, an alloy containing 20–40 wt% nickel and 60– reactions such as R1 and R2 [1].
80 wt% iron, is essential to manufacture stainless steel and 2FeOOH ! Fe2 O3 þ H2 O ðR1Þ
other alloys [1,2]. Ferronickel is vital to society’s welfare, but
its production is energy-intensive and results in significant Ni3 Mg3 Si4 O10 ðOHÞ8 ! 3NiO þ 3MgO þ 4SiO2 þ 4H2 O
environmental impact. The production of ferronickel from ðR2Þ
laterite nickel ores is mainly carried out via the Rotary Kiln-
Electric Furnace (RKEF) process [3,4]. One of the main con- R1 and R2 represent the dehydroxylation of goethite and
cerns in the RKEF process is the dust entrained in flue gases serpentine, respectively. Then, (partial) reduction starts, where
from the rotary kiln, which amounts to around 7.0 wt% of oxygen is (partially) removed from nickel and iron oxides by
the incoming fresh mineral [5]. Dust insufflation is a dust recy- CO from coal gasification [1,4]. The predominant reduction
cling and reuse technique implemented in the cement industry reactions are given by R3-R5 [1,13]. The calcined and partially
[6]. However, dust insufflation remains little explored in the reduced mineral, referred to as calcine from now on, exits the
ferronickel RKEF process. Dust insufflation has led to reduc- rotary kiln at a temperature of 800–900 °C [1,11]. Up to 40%
tions of up to 50% in NOx emission [7] and significant energy of the nickel reduces to metallic nickel [1,13], and about 5% of
savings [6]. Other dust recovery techniques applied in pyromet- the iron reduces to metallic iron [1,10].
allurgical processes are pelletizing and submerged injection
NiO þ CO ! CO2 þ Ni ðR3Þ
[8,9]. This work uses data analytics techniques to gain insight
into the operation before and after dust insufflation in the Fe2 O3 þ CO ! CO2 þ 2FeO ðR4Þ
rotary kiln furnace of a 180 t h1 RKEF ferronickel produc-
tion process. C þ CO2 ! 2CO ðR5Þ
The RKEF process was first applied commercially to treat
New Caledonian ore in the late 19th century [3]. In general, the Dust recycling has been implemented in pyrometallurgical
literature establishes three stages in the RKEF process processes such as cement, iron, and steel production. Simula-
[1,4,10,11]: I) drying or preheating in a rotary dryer, II) calci- tions of a rotary kiln furnace for clinker production showed
nation and partial reduction in a rotary kiln, and III) smelting the impact of dust injection on the flame and the temperature
in an electric arc furnace. The RKEF process is quite mature profile [14]. Results indicate risks of unstable flame and a 40 °C
and well established, has high production efficiency, and shows decrease in the temperature profile. Models were also applied
strong adaptability to the incoming ore. On the other hand, to assess the effectiveness of various NOx control techniques
high energy consumption and the generation of large amounts on three Lafarge kilns [7]. One of these kilns operated with
of by-products such as dust and slag are its disadvantages [3,4]. dust insufflation. Dust insufflation reduced flame temperature
There are three main physicochemical transformations in and, consequently, NOx emissions. These results indicate that
the rotary kiln furnace. The first one is the evaporation of free cement kiln dust takes a significant amount of heat from the
moisture. Then the thermal dissociation and removal of the flame as it increases in temperature and completes calcination.
chemically-bound water, also known as calcination. Third, On the other hand, Lou et al. [15] successfully decreased the
partial removal of oxygen from iron and nickel oxides via smelting temperature and energy consumption by controlling
reduction reactions with CO [1]. Natural gas combustion at the slag formation in a large-scale ferronickel production plant
the outlet (hot-end) of the furnace provides the energy to raise with four RKEF lines. With quaternary basicity of 0.61 and
the mineral temperature to the point required for drying, cal- 12.5 wt% FeO content, they decreased the viscosity of the slag,
cination, and reduction [12]. When the minerals bed reaches thus lowering the required smelting temperature by 86 °C. An
Improving the rotary kiln-electric furnace process for ferronickel production: 3217

invention by Darien et al. [16] presents a system for dust injec- of ANN, the adaptive neural fuzzy inference system (ANFIS),
tion that uses oxygen-enriched air for clinker production. and ARIMA. They measured model performance using the
Increasing oxygen concentration allowed faster heating and coefficient of determination (R2) and the mean square error
processing of the dust without quenching the flame or produc- (MSE), ANFIS showing the best results. These studies show
ing excessive CO emission. Likewise, Mayotte and Eleazer [17] the relevance and effectiveness of data analytics techniques
present an invention that uses oxygen enrichment in a rotary within the industrial sector.
kiln with dust insufflation. Oxygen injection allowed maintain- Current sustainable policies represent a motivation for high
ing a proper flame geometry, thus counteracting ignition delay energy-consuming industries, such as ferronickel production,
or quenching. On the other hand, Tzevelekou et al. [8] pro- to innovate in their process by reducing energy consumption
posed recycling nickeliferous rotary kiln dust by direct and pollutant emissions. Dust insufflation in the rotary kiln
reduction-smelting in an arc furnace. NiO in the slag was less furnace can potentially reduce energy consumption and envi-
than 0.03 wt%, indicating high Ni recovery. Finally, a review ronmental impacts. The benefits of dust insufflation in the
of dust injection techniques in iron and steel production and RKEF process remain unexplored and represent the knowl-
their application results is presented by Senk et al. [18]. edge gap addressed here. This work uses operation data from
The use of data analytics tools for understanding and con- a rotary kiln furnace of an RKEF industrial process before
trolling industrial processes has boomed, generally using large and after dust insufflation. A significant improvement in cal-
datasets. Clustering methods and principal component analy- cine production, and possible energy savings were found due
sis (PCA) are adequate for the exploratory analysis of data to the dust insufflation technology. An exploratory analysis
[19]. A model with a hybrid approach including clustering, of the data with dust insufflation was performed to understand
artificial neural networks (ANN), and support vector machine better the new process behavior, variance, and operating
(SVM) classification allows predicting short-term energy con- conditions.
sumption in loads sensitive to meteorological conditions, as
presented by Torabi et al. [20]. This approach resulted in 2. Methods
higher precision compared to existing models. A method based
on integrating PCA and decision trees was proposed by Sun This paper applies data analytics to gain insight into the oper-
et al. [21] to diagnose rotating machine failures. The proposed ation of an industrial rotary kiln furnace before and after dust
method has greater precision and requires less training than insufflation. The flowsheet in Fig. 1 summarizes the procedures
the back-propagation ANN. for data pre-processing, measurement of the performance
On the other hand, a study [22] compares the performance enhancement, and exploratory analysis.
of ANN, multiple linear regression (MLR), and autoregressive
integrated moving average (ARIMA) for predicting flame tem- 2.1. Data description and pre-processing
perature in a blast furnace. This study contrasted its results
against data from three months of operation and found that
ANN presented a better performance to optimize furnace effi- The industrial plant studied here uses two kilns, referred to as
ciency and stability. Similarly, a blast furnace study [23] was Kiln 1 and Kiln 2. A schematic of the process is shown in
carried out to model the permeability index. Models consisted Fig. 2a. Flue gases leave the kiln drawn by a fan located in

Fig. 1 Pre-processing, inference, and exploratory analysis procedures used to assess the rotary kiln operation before and after dust
insufflation and to understand the process variables.
3218 J.M. Romero et al.

Fig. 2 (a) Schematic diagram of the process and flue gas treatment of the two rotary kilns. Flue gases from the combustion of natural gas
in Kiln 1 pass through cyclones and a scrubber to remove particulate material. Flue gases from Kiln 2 pass through an electrostatic
precipitator to removed dust. (b) Schematic diagram of Kiln 1. Kiln 1 is 185 m long, 6.1 m in diameter, is positioned at a 2.29° inclination
angle, and its nominal rotational velocity amounts to 1.1 revolutions per minute (0.115 rad s1).

the smokestack. After leaving rotary Kiln 1, flue gases pass


Table 1 Ranges of main operation variables at the nominal
through a cyclone stage and then through a scrubber to
operating condition of rotary Kiln 1 according to operating
remove entrained dust. Dust recovered in the cyclones is fed
manuals and historical data.
back to the Kiln 1 entrance. Table 1 summarizes the typical
operating condition of Kiln 1. In rotary Kiln 2, flue gases pass Stream Value Units
through an electrostatic precipitator to remove dust. Fines Fresh mineral 170–180 th1
recovered from the scrubber and the electrostatic precipitator Reductant coal 8–10 th1
are mixed and extruded to make pellets. Pellets contain around Natural gas 118–140 Nm3 min1
25 wt% moisture and are fed back to Kiln 2 entrance. Primary air 105–140 m3 min1
In the rotary kilns, drying, calcination, and (partial) reduc- Secondary air 1370–1550 m3 min1
tion occur in a process in series, as illustrated in Fig. 2b. After
passing through a rotary dryer, the mineral enters the rotary
kiln with moisture content in the range of 9.0–9.8 wt%. In
what follows, we refer to the minerals stream leaving the rotary Recently, the company undertook a dust insufflation pro-
dryer as the fresh mineral. On a dry basis, the fresh mineral ject. The first part consists of insufflating a fraction of the dust
mainly contains Fe2O3 (18.0 wt%), NiO (2.15 wt%), and from Kiln 2 recovered at the electrostatic precipitator. The
MgO (22 wt%), and its temperature amounts to approximately dust is insufflated at the hot end of Kiln 1, as indicated by
50 °C. The reducing agent is bituminous coal with a 30–40 wt the red dash-dot-dot line in Fig. 2a. The dust insufflation sys-
% volatile content and 18–25 wt% moisture. Table 2 lists the tem uses a custom-designed lance to feed the fines right into
distance from each thermocouple to the kiln inlet. the flame, as depicted in Fig. 3. A fraction of the injected dust
Improving the rotary kiln-electric furnace process for ferronickel production: 3219

reflect the main objectives of the dust insufflation project.


Table 2 Positions of each thermocouple in the rotary kiln
KPI3 and KPI4 evaluate other effects indirectly related to dust
furnace.
insufflation.
Distance from the kiln inlet, m Thermocouple All invalid measurements, such as infinity values, not-a-
Mineral number (NaN), or non-physical values, were ruled out. The
65 Tm1 datasets used here contained subsets of missing-not-at-
67 Tm2 random (MNAR) values. Please refer to Xu et al. (2015) [24]
70 Tm3 for further details on missing data classification. The percent-
78 Tm4 age of missing data for the complete dataset was 0.12%.
85 Tm5 Rather than scattered around the dataset, NaNs were consec-
94 Tm6
utive. So instead of choosing any data imputation methodol-
104 Tm7
112 Tm8
ogy, rows containing NaNs were deleted. The method works
131 Tm9 well for large data sets because it does not reduce statistical
140 Tm10 power nor induces bias in parameter estimation [25]. Using
147 Tm11 imputation methods such as interpolation and linear regres-
158 Tm12 sion could induce bias if the missing data show a pattern.
165 Tm13 The mass flow rate of fines was an additional variable in the
177 Tm14 dataset after dust insufflation. This variable presents its own
182 Tm15 dynamics because, during the studied period, the operation
Gases with fines injection was still being stabilized. Therefore, this
0 Tg1
variable was not considered during NaNs removal.
70 Tg2
The company provided a detailed report, including the
79 Tg3
94 Tg4
description, starting date, and duration of all the events that
104 Tg5 happened in the plant during the studied period. This report
112 Tg6 allowed removing measurements corresponding to scheduled
and unscheduled plant shutdowns. For the correct extraction
of shutdowns, the effect of each event on the operation was
verified. Upper and lower limits were established for the fresh
could soften and agglomerate in the burner flame. The aim is mineral flow, natural gas, secondary air, and calcine tempera-
to incorporate dust into the calcine, thus increasing the ture. Data was retained if the variables remained inside these
calcine-to-fresh mineral ratio while reducing natural gas con- limits during the declared events. If the variables crossed one
sumption. Dust insufflation can potentially lead to fines of the limits during the declared event, data was removed from
entrainment rates lower than that with pellets. Compared with the dataset. A detailed explanation of this procedure is avail-
pelletizing, dust insufflation saves water and energy (natural able as Supporting Information.
gas) as no extra moisture is fed to the furnace with the dust. Outliers were deleted considering the whole dataset rather
For this study, the dataset contains measurements from than considering only a few variables independently. The mul-
January 1st, 2020, to December 31st, 2020. Dust injection tivariate outliers are not extreme values for a variable but
started on July 9th. A total of 36 variables were registered, extreme values for a combination of variables [26]. Outliers
including the temperatures described in Fig. 2b and Table 2. have effects on measures of position or dispersion and the cor-
Table 3 lists the remaining variables available for this study. relations between variables. Cook’s distance measures how
Table 4 summarizes four key performance indexes (KPI) much the ith observation influences a parameter estimation
used to compare the operation before and after dust insuffla- when it is removed from a dataset. Cook’s distance was used
tion. Here we refer to the calcined partially reduced mineral in this research to identify multivariate outliers. A high cook’s
leaving the rotary kiln furnace as calcine. KPI1 and KPI2 distance means that the observation has a considerable weight

Fig. 3 Schematic representation of the dust insufflation system. Fines are recovered via an electrostatic precipitator and pneumatically
conveyed to the dust injection lance. A custom-designed lance delivers the fines into the burner flame.
3220 J.M. Romero et al.

Table 3 Process variables considered here to assess the effect of dust insufflation into an industrial rotary kiln furnace for ferronickel
production via the RKEF process.
N Variable description Name N Variable Name
1 Fresh mineral (partially dried) mass flow rate Ore 9 Nickel concentration in fresh mineral Ni.i
2 Coal mass flow rate Coal 10 Sum of other elements concentration in fresh mineral slag.i
3 Calcine mass flow rate cal 11 Iron concentration in the calcine Fe.o
4 Natural gas volumetric flow rate Gas 12 Nickel concentration in the calcine Ni.o
5 Injected dust mass flow rate Inj 13 Sum of other elements concentration in the calcine slag.o
6 Primary air volumetric flow rate PrimAir 14 Moisture content of fresh mineral minmoist
7 Secondary air volumetric flow rate SecAir 15 Pressure at the hot end of the kiln. CalP
8 Iron concentration in fresh mineral Fe.i

Table 4 Key performance indexes (KPI) to compare the operation before and after dust insufflation.
Name Description Units
KPI1 Calcine-to-fresh mineral ratio Dimensionless
KPI2 Natural gas-to-calcine ratio Nm3 t1
KPI3 Air (primary + secondary)-to-natural gas ratio Dimensionless
KPI4 Coal-to-calcine mass ratio Dimensionless

in the estimation, and it can be called an influencing observa- cients in the regression model, and MSE is the mean squared
tion. Eq (1) gives Cook’s distance for the ith observation (Dci ). error.
Pn  2 The exponential weighted moving average (EWMA) was
b b
j¼1 Y j  Y jðiÞ used as a noise removal method to smooth data fluctuations.
D ci ¼ ð1Þ This method was applied to all studied variables with a sliding
P  MSE
window of four samples, corresponding to two operation
Symbol Y bj represents the value of the estimate with
hours. Note that the EWMA filter emphasizes the older data
all observations included, Y bjðiÞ corresponds to the value cumulative effect, i.e., places less importance on current data
when the observation i is omitted, P is the number of coeffi- points. Accordingly, the weighting for each older data point

Fig. 4 Moving average filter applied to the fresh mineral mass flow in the rotary kiln before the dust insufflation.
Improving the rotary kiln-electric furnace process for ferronickel production: 3221

decreases exponentially [27]. For an instant t, the EWMA filter test are not adequate. Likewise, the conditions of some non-
is given by Eq. (2). parametric tests were evaluated, like the Mann-Whitney-
Wilcoxon (MWW) test for independent samples, also called
yðstÞ ¼ ayðst1Þ þ ð1  aÞyðtÞ ð2Þ
Wilcoxon rank-sum test or Mann-Whitney U test [31]. This
ðtÞ
where y is the original observation for the k instant and yðstÞ
is test does not require normally distributed data; however, it
computed using the previous filtered value, yðst1Þ . Symbol a assumes equal distributions of the two studied groups, and
represents a smoothing coefficient and varies between zero therefore, it is sensitive to heteroscedasticity [31]. That is
and one. Fig. 4 shows the result of applying the EWMA filter why the MWW test was also discarded. In this research, the
to one of the variables: ore mass flow rate entering the rotary bootstrapping method was used to compare the means. It is
kiln. similar to the randomization test, but the latter applies when
For steady-state extraction, we used the methodology pro- the randomness is caused by allocating the data in different
posed by Simon and Litt [28], later applied by Kummar et al. groups. In contrast, bootstrapping applies when the random-
[29]. This algorithm uses the standard deviation to classify data ness is due to the sampling procedure [32]. In this work, the
in a steady- or transient state. The data is divided into 6- P-value correction proposed by Davison and Hinkley was used
sample windows, corresponding to three hours of operation. [33,34].
Tree hours is the mean residence time (MRT) of the solids in
the rotary kiln according to Seaman’s model [30]. If the stan- 2.3. Principal component analysis
dard deviation of a data window is less than two reference
standard deviations, this window is assumed to be at a The principal component analysis (PCA) is a multivariate
steady-state. Only a group of relevant variables were used to analysis method that projects the data matrix to a lower-
compare standard deviations for steady-state extraction: mass dimensional space [35] proposed initially by [36]. PCA is an
flow rate of fresh mineral and natural gas volumetric flow rate. unsupervised learning method and works for exploratory anal-
Further details on the steady-state extraction algorithm are ysis of data and data visualization. This method converts the
available as Supporting Information. Fig. 5 shows results for correlations or lack thereof into a two-dimension plot. Fur-
steady-state extraction before and after dust insufflation. thermore, the generated principal components (PCs) are suit-
able for principal component regression (PCR), partial least
2.2. Bootstrapping squares (PLS), and other supervised learning methods. This
method uses Singular Value Decomposition (SVD) to obtain
For most of the variables in the dataset, the normality assump- the set of new dimensions. A complete explanation of the
tion is not met. For this reason, parametric tests such as the t- method can be found in [37].

Fig. 5 Steady-state extraction before dust insufflation for the mass flow rate fresh mineral (a and c) and natural gas volumetric flow rate
(b and d).
3222 J.M. Romero et al.

2.4. k-means clustering dust insufflation. Fig. 6a shows the difference in the calcine-
to-fresh mineral ratio with and without dust insufflation,
The k-means method classifies data into smaller groups or reflecting an increase. This result is a first indication that dust
clusters proposed by Hartigan and Wong algorithm [38]. A insufflation promotes the incorporation of dust into the
cluster is a group where all samples feature some similarity calcine.
and are different from samples in another cluster. This algo- xKPI2 represents the ratio between natural gas volumetric
rithm owes its popularity to its simplicity, robustness, and effi- flow rate and calcine mass flow rate. The means difference
cient implementation [38]. For this unsupervised learning before and after dust insufflation for KPI2 was 1.431. The
method, k is the number of clusters. The first step is to define P-value for the bootstrapping test was 1  104 indicating a
the number of clusters and then locate random centroids for statistically significant difference between the compared data-
those clusters. Then, assign to each centroid the data closest sets. As inferred from Fig. 6b, there was a decrease in the nat-
to it. Finally, recalculate the centroids with the average of each ural gas-to-calcine ratio. According to these results, dust
cluster. These steps repeat until the cluster assignments stop insufflation can potentially lead to energy savings in the rotary
changing or reaching the maximum number of iterations. kiln. The partially calcined and dried dust requires lower
Elbow and silhouette methods were used to determine the opti- energy for calcination and reduction.
mum value for k. The bootstrapping method also showed a significant differ-
ence before and after dust insufflation for KPI3, i.e., the air-to-
3. Results and discussion natural gas volumetric flow ratio. A decrease in KPI3 after
dust insufflation is evident (Fig. 6c). By reducing the airflow
entering the furnace, the superficial velocity and the dragging
The comparison of results for the datasets before and after
of fines also decrease. This outcome could lead to enhanced
dust insufflation revealed statistical differences. Results show
conditions for incorporating the agglomerated dust into the
salient differences in material streams and mineral tempera-
calcine stream. Note that this hypothesis is consistent with
tures. Likewise, we identified the groups of variables contribut-
the results for KPI1.
ing the most to the total variance after dust insufflation. After
On the other hand, the distributions for KPI4, i.e., the coal-
dust insufflation, three main operating conditions were distin-
to-calcine mass flow rate ratio, do not show a significant
guished using k-means clustering, thus gaining insight into the
change in shape and scattering before and after dust insuffla-
improved process. One of these operating conditions showed
tion (Fig. 6d). Therefore, using only the bootstrapping results
encouraging results in terms of the KPIs defined in Table 4.
to compare this indicator is correct. Bootstrapping showed a
positive difference between before and after dust insufflation
3.1. Performance enhancement with dust insufflation (Table 5).
The thermocouple Tm15 is located at 3 m from the end of the
The reader is referred to the Supporting Information to see the rotary kiln. Fig. 6f shows a different shape for the distribution
normality and bootstrap distribution plots for all the relevant of this variable. For this temperature, when analyzed after the
variables studied in this section. Table 5 summarizes the means intervention, there are two separated operating conditions.
difference of these variables and the P values from the boot- One of them coincides with the values it had before dust insuf-
strapping test. The means difference for KPI1 is 0.053, which flation, but the other has considerably higher values. This tem-
is a value practically outside of the bootstrapping distribution perature could be associated with calcine quality and with the
(S3 1 in the Supporting Information). For this mean differ- extent of reduction reactions. Li (1999) [39] shows that for tem-
ence, a P-value of 1  104 was obtained, which allows reject- peratures in the range of 710–740 °C, when the CO/CO2 ratio
ing the null hypothesis. This result indicates a statistically falls between 2 and 3, the nickel recovery achieves the maxi-
significant difference in the dataset’s values before and after mum values. Therefore, although this temperature shows a sta-
tistically significant change, it stays within a range [39] that
would not compromise calcine quality. This temperature
Table 5 Bootstrapping results for the most relevant variables impacts energy consumption for the next stage in ferronickel
and the key performance indexes (KPIs). P-values were production, corresponding to the smelting-arc furnace. The
calculated using Eq. 3. increase in the calcine temperature at the end of the rotary kiln
could reduce energy consumption in the electric arc furnace
KPI/Variable Mean difference Relative change (%) P-value
[11]. The electric furnace smelting stage requires high energy
KPI1 0.053 6.31 0.0001 consumption. In fact, some techniques such as controlling slag
KPI2 1.431 2.65 0.0001 formation have been evaluated to reduce energy consumption
KPI3 0.086 0.71 0.0001
in ferronickel production [15].
KPI4 0.005 8.04 0.0001
Fresh mineral 2.413 1.38 0.0001
Tm13 is the closest thermocouple to the flame; therefore, it
Coal 1.178 13.39 0.0001 registers the highest mineral temperatures. The means differ-
Gas 2.949 2.24 0.0001 ence for Tm13 was 21.9 °C, and the P-value from the bootstrap-
Calcine 7.042 4.80 0.0001 ping test was 1  104 reflecting a statistically significant
Primary air 1.786 1.34 0.0001 difference for the means of the variables. This result indicates
Secondary air 22.280 1.53 0.0001 that the lateritic mineral possibly achieved higher temperatures
Tm13 21.867 2.15 0.0001 after dust insufflation. Fig. 6e shows different peaks for the
Tm15 9.007 1.23 0.0001 distributions before and after dust insufflation. Besides, a
Tg6 13.518 1.48 0.0001
bimodal distribution is evident after dust insufflation. Two dif-
Improving the rotary kiln-electric furnace process for ferronickel production: 3223

Fig. 6 Density probability plot and box plot with data points for (a) the calcine-to-fresh mineral ratio (KPI1), (b) natural gas-to-calcine
ratio (KPI2), (c) air (primary + secondary)-to-natural gas ratio (KPI3), (d) coal-to-calcine mass ratio (KPI4), (e) Tm13 and (f) Tm15 . Fig. 2b
and Table 2 give the position of thermocouples in the rotary kiln.

ferent groups are obtained from the bimodal distribution, atures above 1100 °C, the fines are expected to reach higher
which could correspond to two different operating scenarios. temperatures due to their passage through the flame. The fines
The temperature for one of these scenarios is considerably injected into the burner have residual carbon (1% wt. approx-
higher than the temperature without dust insufflation. This imately), which is necessary to reduce the oxides. Therefore,
increase in the maximum mineral temperature could positively the dust injection process may promote the formation of rings
contribute to the reduction process in the rotary kiln. How- in the reduction zone of the rotary kiln.
ever, it could also lead to crusts due to the sintering of metal The region between 50 m and 150 m in length of the furnace
particles. does not show evidence of a noticeable change in the temper-
On the other hand, at temperatures above 900 °C, nickel ature profile before and after dust insufflation, as shown in
and iron oxides fuse with SiO2, forming non-reactive silicates Fig. 7. Unstable combustion and mineral cooling were
[1]. These are low melting point complex compounds, which reported for a clinker rotary kiln after dust insufflation [6].
gradually deposit on the refractory surface of the rotary kiln Here, the dust-to-calcine mass ratio did not exceed 0.25, and
[40,41]. This phenomenon is known as accretion or ring forma- the minerals and gases temperature profiles before and after
tion. Ring formation can also be due to the presence of dust insufflation resemble each other.
carbon-containing fines at high temperatures (1200–1400 °C) In the temperature region 800 °C-880 °C, there are notice-
[41,42]. Although, in this case, the ore does not reach temper- able differences between the temperature averages before and
3224 J.M. Romero et al.

Fig. 7 Mineral and gasses temperature profiles before and after dust insufflation. See Table 2 for the location of the thermocouples.
Upper and lower limits for the temperature bands are defined with the standard deviation of each thermocouple. The standard deviation
of Tm13 (at 165 m from the kiln entrance) is three times higher for the case with dust insufflation.

after dust insufflation. Besides, the temperature in this range is Results show a first PC (PC1) that explains 42% of the vari-
the only one that is lower for the scenario with dust insuffla- ance and a second PC (PC2) that accounts for 9.5% of the
tion. Kinetic studies on the thermal decomposition of lateritic variance. The first ten PCs explain 85.9% of the variance.
minerals identify an exothermic recrystallization event in this Table 6 shows the variables associated with PC1 and PC2.
temperature region [43–46]. Therefore, there is no mass loss PC1 includes the highest temperatures for the gasses and inter-
but rather a crystalline rearrangement. Using thermogravimet- mediate temperatures for the mineral. On the other hand, PC2
ric analysis (DTA-TG), published studies [43–46] found 876, also includes minerals concentration in the calcine and fresh
830, 821, and 820 °C, as the temperatures for the exothermic mineral, secondary air volumetric flow rate, and some of the
recrystallization event. kiln’s highest temperatures. These variables explain a signifi-
cant share of dataset variability. PC3 and PC4 are linear com-
3.2. Exploratory analysis and operating conditions binations of the remaining temperatures, gas volumetric flow
rate, mass flow rates of fresh mineral, insufflated dust and coal,
PCA allowed identifying the two components that better and the primary air volumetric flow rate.
explain the variance of the after-dust-insufflation dataset. Fig. 8 illustrates the contribution of each variable to the
PCs. Positively correlated variables point in the same direc-
tion, and negatively correlated variables point in opposite
Table 6 Contributions of each variable to the first (PC1) and directions. Only the variables with the highest contribution
second (PC2) principal components. to PC1 and PC2 appear in Fig. 8a and Fig. 8b, respectively.
All temperatures in the chart point to the left, but contrary
PC1 PC2
to the rest, Tm10 , Tm13 , Tm14 and Tm15 point to the top of the
Variable Contribution, % Variable Contribution, % chart. Tm7 and Tm13 are essentially uncorrelated, while Tm14
Tm4 5.79 Ni:o 9.70 and Tm15 reflect a similar result. These results are consistent
Tg3 5.66 Tm15 9.03 with the relative distance between these thermocouples. Con-
Tm8 5.63 Tm14 7.91 versely, the correlation between Tm13 and Tm15 , much closer
Tm3 5.63 Feo 7.61 thermocouples, is 0.395. On the other hand, the correlation
Tg4 5.55 SecAir 6.95 between Tm8 and Tg6 located at the same distance from the kiln
Tg2 5.48 Tm13 6.90
furnace entrance, amounts to 0.836.
Tm5 5.34 Tm7 4.86
Similarly, steady-state KPIs data after dust insufflation
Tm1 5.23 slagi 4.48
Tg6 5.20 Slago 4.39 allowed identifying different operating conditions. Graphical
Tg5 5.13 Tm10 3.82 exploratory analysis cast light on the difference between the
generated clusters. Within the set of variables studied here,
Improving the rotary kiln-electric furnace process for ferronickel production: 3225

Fig. 8 Contribution of variables to the variance of the after-dust-insufflation dataset for (a) PC1 and (b) PC2. Positively correlated
variables point to the same side. Negatively correlated variables point to opposite sides of the plot. SA: secondary air. Table 2 and Fig. 2
describe gas and mineral temperatures. Table 3 describes the other variables in the figure.

KPIs are those functions that better reflect the impact of dust only with steady-state values. For better representation, points
insufflation on the rotary kiln operation. Therefore, KPIs were were connected with a dashed line in Fig. 10. Different zones
used in the clustering algorithm instead of the entire dataset. were evident, indicating three main operating conditions dur-
Three were the optimum number of clusters determined via ing dust insufflation.
the elbow and silhouette methods. These plots are available The first zone encompasses the first 250 samples, represent-
for the interested reader as Supporting Information. Fig. 9 ing ~ 5 days of operation. In this zone, C2 predominates, with
shows a graphical representation of the clusters as a function an average of 0.87 for KPI 1, a value slightly higher C3, but
of PC1 and PC2. Using only the four KPIs in the PCA still lower than C1, which showed averages of 0.85 and 0.93
method, the explained variance of PC1 and PC2 are 61% for KPI1, respectively. The average mass flow rate of insuf-
and 28.7%, respectively. flated dust for C2 was 3:7th1 , which is the lowest of the three
Clusters C1, C2, and C3 contain 411, 233, and 256 samples, clusters. The second zone includes from sample 250 to 750
i.e., the three clusters have comparable sizes indicating no clus- approximately, representing ~ 11 days of operation. In this
ter of outliers. Table 7 summarizes each cluster content by pro- zone, C1 predominates, exhibiting the higher KPI1 and lower
viding the minimum, mean, maximum, and standard KPI2, with averages of 0.93, 50.9, respectively. Therefore, this
deviation. Mean values in C1 are smaller than those in C2 operating condition was the one with the highest efficiency
and higher than those in C3, except for the calcine, which during the dust injection. The increase in calcine production
affects KPI1, KPI2, and KPI4. According to the calcine-to- is the salient difference, with an increase of 6.31% and
mineral ratio (KPI1) and the natural gas-to-calcine ratio 9.07%, compared to C2 and C3, respectively. This operating
(KPI2), C1 is a cluster with promising results. condition features the highest mass flow rate of injected dust,
KPIs data were plotted sequentially in Fig. 10 to verify that with an average of 6:9th1 . In the third zone, which goes from
clusters correspond to different operating conditions rather sample 750 to 900, C3 predominates and corresponds to
than random data. Note that at this point, we are working approximately three operation days. The average KPIs for this
cluster resemble those of C2, with differences no greater than
5%. Within these two clusters, the most different variable is
the mass flow rate of injected dust, being 5:6th1 and 3:7th1 for
C3 and C2, respectively.
It is relevant to compare the conditions in C1 and C3, con-
sidering the characteristics of each cluster. Both present a sim-
ilar dust injection rate, and the main operating variables do
not show significant differences either. Despite this, C1 pre-
sents a notable increase in calcine-to-fresh mineral compared
with C3. A plausible explanation for these results is that the
difference in the calcine-to-fresh mineral ratio is not due to
one variable’s effect but to the interaction of several. Uncon-
trolled variables may impact KPI1, such as the angle of injec-
tion of fines or the agglomeration rate. Determining the factors
that explain the difference in KPI1 between C1 and C3 is
beyond this paper’s scope.
To summarize, C2 does not show a significant change with
respect to the operation without dust injection; therefore,
Fig. 9 Graphical representation of clusters as a function of potential benefits are not observed in this operation scenario.
principal components PC1 and PC2. Results correspond to the In C1, there is a reduction in the mass flow rate of dust bypass-
after-dust-insufflation dataset. ing the cyclones and a noticeable increase in the calcine-to-
3226 J.M. Romero et al.

Table 7 Minimum (Min), mean, maximum (Max), and standard deviation (SD) for data in each cluster. Results correspond to the
after-dust-insufflation dataset.
C1 C2 C3
Min Mean Max SD Min Mean Max SD Min Mean Max SD
Mineral 162.8 171.5 175.1 3.5 165.0 173.9 175.1 2.8 165.0 171.7 175.1 2.7
Coal 9.0 10.1 11.3 0.5 8.4 9.5 10.8 0.4 9.4 10.2 11.5 0.4
Natural gas 128.9 135.6 140.8 2.9 121.6 132.3 137.8 3.3 123.0 134.1 140.3 2.5
Calcine 147.6 159.9 172.6 4.5 132.9 150.4 163.2 5.1 123.8 146.6 157.9 6.0
Injection 0.0 6.9 10.0 2.6 0.0 3.7 8.0 2.1 0.0 5.6 10.0 2.9
KPI1 0.868 0.932 1.007 0.026 0.795 0.865 0.933 0.025 0.707 0.854 0.902 0.035
KPI2 46.9 50.9 54.7 1.4 47.8 52.8 57.9 1.6 51.2 54.9 64.2 2.0
KPI3 11.5 11.9 12.5 0.2 12.0 12.4 13.0 0.2 11.5 11.9 12.7 0.2
KPI4 0.056 0.063 0.071 0.003 0.056 0.064 0.072 0.003 0.065 0.070 0.078 0.002

Fig. 10 Values of (a) the calcine-to-fresh mineral ratio (KPI1), (b) natural gas-to-calcine ratio (KPI2), (c) air (primary + secondary)-to-
natural gas ratio (KPI3) and (d) coal-to-calcine ratio (KPI4) for the different clusters. Results correspond to the after-dust-insufflation
dataset.

fresh mineral ratio. Finally, in C3, the low incorporation of analytics techniques bootstrapping, PCA, and k-means cluster-
injected dust is evident, consistent with the KPI1 values and ing to a one-year operation database from a large-scale rotary
the increase in dust mass flow rate at the outlet of the cyclones. kiln with and without dust insufflation. The data-treatment
Further details on the dust mass balance are available in the process was divided into three stages: pre-processing, infer-
Supporting Information. ence, and exploratory analysis. The data distribution and
knowledge about process variables were crucial to choose
4. Conclusions proper statistical methods for the pre-processing stage. This
stage started discarding the NaNs and plant shutdowns. Sub-
The benefits of dust insufflation in the RKEF ferronickel pro- sequently, we removed multivariable outliers and reduced
duction process were studied in this paper. We applied the data noise with the exponential moving average filter. Finally, the
Improving the rotary kiln-electric furnace process for ferronickel production: 3227

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