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An Efficient Extraction and Selective of Alumina

from Lapindo Mud
Didi Dwi Anggoro1,*, Michael David1, Shafira Kayla Alrasyid 1, Cahya Kamilla
Chaerunnisa1, and Desita Rachmawanti1
1Department of Chemical Engineering, Diponegoro University, Indonesia

Abstract. Lapindo mud, a soft clay soil found in Sidoarjo, East Java, has a
high water and mineral content. It contains 16% alumina (Al2O3), making it
a potential source of aluminum metal. The high content of silica oxide in
Lapindo mud is of particular interest to separate the oxide from the alumina
oxide. Silica oxide is insoluble in acid while aluminum oxide is soluble in
acid. The alumina extraction process was carried out using acid solvent. The
dried mud with a size of ≤100 mesh was extracted using HNO3 and HCl
solvent with concentration of 4, 6, and 8 M at temperatures of 60℃, 70℃,
and 80℃ for 100, 200, and 300 minutes. The extraction results were filtered,
then the pH of the filtrate was adjusted to 12 with 6 M NaOH. The filtrate
was filtered, thus Fe3+ was obtained as a residue. The filtrate was neutralized
to pH 8 using 6 M HCl. The filtrate was filtered to obtain NaAlO2. The
precipitate formed was washed using distilled water and dried in an oven to
obtain Al(OH)3. Al(OH)3 was then calcined at 600℃ for four hours to form
Al2O3. The results showed that acid solvent concentration, extraction
temperature, and heating time affected the mass of Al2O3 obtained.
Increasing acid solvent concentration, extraction temperature, and heating
time, increases the mass of Al2O3 obtained. The mass of Al2O3 obtained was
1.19 grams for HNO3 solvent and 1.63 grams for HCl solvent with
concentration of 8 M, extraction temperature of 80℃, and heating time of
300 minutes. The results of XRF characterization show that the Al2O3 purity
level is 42.8% and 27.3%with HNO3 and HCl solvent, respectively.

1 Introduction
The Sidoarjo Mud Flow, known as LUSI (Lumpur Sidoarjo), is the result of a mud eruption
at the drilling site of PT Lapindo Brantas in Renokenongo Village, Porong, Sidoarjo, East
Java. This mud eruption stemmed from a borehole leak during the oil and gas exploration
activities. The local community, particularly in Porong, has experienced various health,
environmental, and economic losses due to this ongoing mud flow. Comprehensive
knowledge of the characteristics of the Sidoarjo mud flow is crucial for its utilization and
management.
The Lapindo mud reported that the Lapindo mud contains oxide compounds such as
aluminum oxide, silicon dioxide, potassium oxide, titanium oxide, calcium oxide, manganese

*
Corresponding author: [email protected]

© The Authors, published by EDP Sciences. This is an open access article distributed under the terms of the Creative Commons
Attribution License 4.0 (https://creativecommons.org/licenses/by/4.0/).
E3S Web of Conferences 503, 06004 (2024) https://doi.org/10.1051/e3sconf/202450306004
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oxide, phosphorus pentoxide, sulfur oxide, vanadium pentoxide, and others [1]. in a different
study similar findings regarding the mineral composition contained in the Lapindo mud [2].
All research results regarding the composition indicate that silicon dioxide is the dominant
mineral in the Lapindo mud, followed by iron oxide and aluminum oxide. The high content
of aluminum oxide (approximately 18.27%) in the Lapindo mud can be utilized as a
supporting material for metal catalysts by separating this oxide from silica oxide [3]. The
insoluble nature of silica oxide in acid can be utilized to obtain pure alumina oxide.
Aluminum oxide is a chemical compound with the chemical formula Al2O3. The mineral
name of aluminum oxide is alumina. Aluminum oxide is a good heat and electrical insulator,
so it is widely used as an abrasive material for components in cutting tools. In addition, it is
widely used in the field of mechanical engineering to manufacture machine parts that are
resistant to fire and high temperatures. The medical field also uses it as a material for making
dental implants. This is due to its properties of high strength, hardness, wear resistance,
refractory resistance, thermal conductivity, chemical resistance and electrical strength [4].
Generally, alumina is found in a crystalline form called corundum or α-aluminum oxide.
Aluminum oxide or alumina can be obtained through an extraction process. Extraction is
a separation process that is based on the difference in solubility between two liquids. There
are many methods that can be used to carry out the extraction process, including: maceration,
soxhlet, reflux and percolation. Alumina itself can be obtained through the reflux extraction
method. The reflux extraction method is a solid-liquid extraction process at a constant
temperature. Reflux extraction is carried out by repeatedly evaporating the solvent and
continuing with condensation for a certain period of time without any loss of solvent [5]. The
principle of the reflux extraction method is that the solvent used will evaporate at a high
temperature, then be cooled with a condenser so that the solvent which was initially in the
form of vapor will condense in the condenser. There is a phase change to liquid and the
solvent falls back into the reaction container so that it will remain there throughout the
reaction [6]. This method is suitable for use on materials that are resistant to heating.
Several studies have been conducted to obtain alumina from various sources, including
Lapindo mud. From the previous research extracted Lapindo mud with HCl solvent with
various types of concentrations (1, 2, 3, 4, 5, and 6 M) for 20 minutes with and without
heating. The result shows that the highest yield was obtained in 6M HCl solvent with a yield
value without heating of 18.59% and with heating of 62.45%. The alumina that has been
obtained was then characterized by the SSA method [7].

2 Materials and Methods

2.1 Material
Lapindo mud used in this study was collected from Sidoarjo Regency, East Java, Indonesia.
The chemicals used in this study were HNO3 with purity of 65%, HCl with purity of 32%,
and sodium hydroxide.

2.2 Lapindo mud pretreatment

A schematic flow diagram of pretreatment process and extraction process of alumina from
Lapindo mud shown in Figure 1

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Fig. 1. Flow diagram of alumina extraction from Lapindo mud

The Lapindo mud was dried using an oven and then sieved to 100 mesh using hammer mill.

2.3 Extraction of alumina from Lapindo mud

The dried mud with a size of ≤100 mesh was extracted using HCl and HNO 3 solvent with
concentration of 4 M, 6 M, and 8 M at temperatures of 60oC, 70oC, and 80oC for 100 minutes,
200 minutes, and 300 minutes. The mixture was filtered, then the pH of the filtrate was
adjusted to 12 with 6 M NaOH. The mixture was then refluxed at 70 oC for 200 minutes. The
mixture was filtered, thus Fe3+ was obtained as a residue. The filtrate was neutralized to pH
8 using 6 M HCl, then the mixture was refluxed at 70 oC for 200 minutes. The mixture was
filtered to obtain NaAlO2 as a residue. The precipitate formed was washed using distilled
water and dried in an oven to obtain Al(OH)3. Al(OH)3 was then calcined at 600℃ for four
hours to form Al2O3. The purity of alumina was determined by X-ray Fluorescence and the
crystallinity of alumina was determined by X-ray Diffraction.

3 Results and Discussion

Equations should be centred and should be numbered with the number on the right-hand side.
Table 1. Yield of alumina obtained

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Variables Alumina Yield using Alumina Yield using HCl

HNO3 Solvent Solvent
4 M, 60oC, 100 minutes 2.31% 2.47%
4 M, 70oC, 100 minutes 2.63% 2.59%
4 M, 80oC, 100 minutes 3.01% 3.58%
6 M, 60oC, 200 minutes 3.3% 4.07%
6 M, 70oC, 200 minutes 6.44% 6.05%
6 M, 80oC, 200 minutes 7.63% 8.27%
8 M, 60oC, 300 minutes 7.84% 5.06%
8 M, 70oC, 300 minutes 15.77% 7.53%
8 M, 70oC, 300 minutes 20.06% 14.69%

3.1 Effect of Extraction Time on Alumina Yield

Time of the extraction process is one of the factors that will affect the alumina yield obtained.
In this study, the extraction process was carried out with two types of acid, which is HCl and
HNO3 with extraction time for 100, 200, and 300 minutes. The results showed that the longer
extraction time, the more alumina yield obtained. The result of alumina yield with time
variables are shown in Figure 2 and Figure 3.

Fig. 2. Effect of extraction time on alumina yield for HCl solvent

Fig. 3. Effect of extraction time on alumina yield for HNO3 solvent

Based on Figure 2 and 3 above, the result indicates that the highest alumina yield was
achieved at extraction time 300 minutes, for both HCl and HNO 3, which was 20.06% and
14.69%, respectively.
Previous research conducted [8], shows a directly proportional relationship. Where the
longer the extraction time, the greater the alumina yield obtained. Another study conducted
by [9] also showed that alumina recovery increased with increasing extraction time. At an

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extraction time of 15 minutes, the aluminum obtained reached 63.51%. Meanwhile, at an

extraction time of 30 minutes, the aluminum obtained reached a maximum value of 87.89%.
The extraction rate increases significantly at the beginning of time, then slows down and
finally remains constant after reaching a certain time. This shows that the alumina obtained
has reached its maximum amount.
In this study, the highest alumina yield was achieved at 300 minutes of extraction time
for both HCl and HNO3, with respective yields of 20.06% and 14.69%. This indicates that an
increase in extraction time influences the extraction rates and alumina yield obtained.

3.2 Effect of Acid Concentration on Alumina Yield

Acid concentration plays a significant role in extracting alumina from Lapindo mud. In this
study, the alumina extraction process was carried out using two types of acid, HCl and HNO 3,
at concentrations of 4 M, 6 M, and 8 M. The results of alumina yield obtained with acid
concentration variables are shown in Figure 4 and Figure 5.

Fig. 4. Effect of HCl concentration on alumina yield

Fig. 5. Effect of HNO3 concentration on alumina yield

Based on Figure 4 and 5, the result indicates that increasing the acid concentration
increases the yield of alumina. In this study, the highest alumina yield was achieved at acid
concentration of 8 M, for both HCl and HNO3,which was 20.06% and 14.69%, respectively.
Based on previous studies, an increase in acid concentration can enhance the yield of
alumina. Concentration of H+ ions affected the solubility of Al atoms. The higher the acid

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concentration, the higher H+ ions are contained [10]. It is also assumed that the diffusion rate
of Al3+ ions from solid to solution increase with an increase in concentration and diffusion of
hydronium ions [8]. According to [11], the alumina yield increases because of the acid being
predominant at this stage, therefore increasing the conversion of aluminum ions (Al 3+) to
alumina (Al2O3). Based on the level of reactivity to alumina silica, HCl is more reactive than
HNO3. Alumina silica is easily soluble in HCl, both at low concentrations and high
concentrations, while alumina can only react with HNO 3 at high concentrations [12].

Al2O3 (s) + 6HCl (l) → 2AlCl3 (aq) + 3H2O (l) (1)

Al2O3 (s) + 6HNO3 (l) → 2Al(NO3)3 (aq) + 3H2O (l) (2)

In this study, the highest alumina yield was achieved at acid concentration of 8 M for both
HCl and HNO3, with respective yields of 20.06% and 14.69%. This indicates that an increase
in acid concentration influences the recovery of alumina from Lapindo mud, leading to
increased extraction rates and improved process efficiency.

3.3 Effect of Extraction Temperature on Alumina Yield

The extraction process of alumina from Lapindo mud is influenced by temperature. In this
study, the extraction process was carried out with two types of acid, which is HCl and HNO 3
at temperatures of 60oC, 70oC, and 80oC. The influence of the extraction temperature on the
yield of obtained alumina are shown in Figure 6 and Figure 7.

Fig. 6. Effect of extraction temperature on alumina yield for HCl solvent

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Fig. 7. Effect of temperature on alumina yield for HNO3 solvent

Based on Figure 6 and 7 above, the result indicates that the highest alumina yield was
achieved at extraction temperature of 80oC, for both HCl and HNO3, which was 20.06% and
14.69%, respectively.
From the results obtained, it is evident that an increase in extraction temperature leads to
a higher yield of alumina. The findings indicate a positive correlation between temperature
elevation and the enhanced recovery of alumina from Lapindo mud. As the temperature
increases, the extraction rate also rises, indicating a direct influence of temperature on the
process efficiency. The significant increase in dissolution rates at higher temperatures is
attributed to the exponential relationship between temperature and the constant in the
Arrhenius equation, a factor used in calculating the activation energy [13].
Previous studies have shown that elevating the extraction temperature, regardless of the
acid used (HCl or HNO3), can effectively augment the alumina yield. High temperatures
boost the kinetic energy of reactant particles, resulting in more energetic and frequent
collisions, thereby accelerating the overall reaction rate. Additionally, temperature alterations
influence the solubility of specific compounds present in Lapindo mud. Increased
temperatures enhance solubility, accelerate the diffusion rate between extraction
components, and facilitate particle movement, potentially enhancing the overall extraction
yield [14].
In this study, the highest alumina yield was achieved at 80 oC for both HCl and HNO3,
with respective yields of 20.06% and 14.69%. This indicates that an elevation in extraction
temperature notably influences the recovery of alumina from Lapindo mud, leading to
increased extraction rates and improved process efficiency. Overall, these findings
underscore the pivotal role of temperature in enhancing alumina yield and its profound
impact on the extraction process from Lapindo mud, as indicated by previous studies.

3.4 XRF Analysis of Alumina and Lapindo Mud

XRF analysis was conducted to identify the major element and minor element from alumina
and Lapindo mud. The element from alumina and Lapindo mud was obtained from the
collision of atoms on the surface by X-ray. The results of XRF analysis of alumina and
Lapindo mud are presented in Table 2 below.

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Table 2. XRF analysis results

Element Lapindo Mud Alumina with HCl Alumina with
Solvent HNO3 Solvent
Al2O3 16.2% 27.3% 42.8%
SiO2 36.9% 0.074% 0.273%
Fe2O3 7.20% 0.0137% 0.0256%
Na2O 0.879% 19.0% 1.66%
SO3 0.931% 0.256% 0.272%
Cl 0.544% 19.3% 0.759%
K2O 1.47% 0.120% 0.0348%
CaO 2.06% 0.0183% 0.0188%
Zno 0.0124% 0.0216% 0.0157%

Table 2 shows that the XRF analysis results in changes of the relative weight of the
elements between Lapindo mud and alumina samples. The Al 2O3 element contained in
Lapindo mud was 16.2%, which is lower than the samples from the alumina extraction. The
sample from the alumina extraction with HCl solvent had 27.3% of Al 2O3 element, while
with HNO3 solvent had 42.8%. Al2O3 element has increased due to impurity elements that
do not dissolve during the extraction process, so impurity elements are left behind as residue
. Apart from that, some elements experienced a significant loss. This can happen because
Al2O3 can dissolve in acid solvent and other elements can not dissolve in acid solvent [15].
Based on the XRF analysis, it can be seen that the best type of acid solvent between
hydrochloric acid (HCl) and nitric acid (HNO 3) that can be used in extracting alumina from
Lapindo Mud is HNO3. Nitric acid solvent has good selectivity. In addition, the regeneration
process is very effective, so it can reduce acid usage by up to 90% [16]. Nitric acid reacts
with alkalis, basic oxides, and carbonates to form salts. Because it has oxidizing properties,
nitric acid does not release its protons in reactions with metals and the resulting salts that are
in a higher oxidized state. This causes the extraction results have high alumina element due
to the large amount of impurities left in the residue.

3.5 XRD Analysis of Alumina

XRD analysis was conducted to determine the crystallinity of sample from the alumina
extraction with HCl and HNO3 solvent. The crystallinity of alumina was obtained by using
crystallinity index. The results of XRD analysis of alumina are presented in Figure 8 below.

Fig. 8. XRD analysis results

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Figure 8 shows that in the XRD analysis result pattern high peaks at 2θ angles for each
sample. There are highest peak at 31° for alumina with HCl solvent and at 66° for alumina
with HNO3 solvent. It can be seen that the peaks of alumina with HCl solvent looks sharper
and narrower shows that it has high crystallinity. Moreover, the peaks of alumina with HNO 3
solvent looks wider and slopes shows that it amorphous. Alumina with HNO 3 solvent has
more reactivity because amorphous has wider surface area and unstable [17].

4 Conclusion
Extraction of alumina from Lapindo mud using acid solvent was successful. Optimum
conditions were obtained at acid concentration of 8 M at extraction temperature of 80 oC and
extraction time for 300 minutes, resulting alumina yield of 20.06% for HCl and 14.69% for
HNO3. Extraction time is one of the factors that will affect the alumina yield obtained because
the longer the extraction process, the extraction process will be more perfect. The acid
concentration also plays a significant role in extracting alumina from Lapindo mud. The
higher acid concentration, resulting in increase of H+ ions contained and increase of diffusion
rate of Al3+ ions from solid to solution. The alumina yield also increases because the acid
being predominant at this stage. The extraction process of alumina from Lapindo mud also
influenced by temperature. Higher temperature resulting in increased solubility, accelerating
rate of diffusion between components, and accelerating particle movements. Alumina from
extraction using HCl and HNO3 solvent had a purity of respectively 27.3% and 42.8%. XRD
results showed that highest peak for alumina from extraction using HCl and HNO 3 solvent at
31°and 66° respectively.

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