This study focuses on the removal of spent engine oil (SEO) spill from the water surface using water hyacinth biomass (WHB)-based sorbents. The raw WHB was modified using extra virgin coconut oil (mainly consisting of lauric acid) to enhance the hydrophobicity and floating ability. With varying amounts of coconut oil and solvent, six diverse types of modified water hyacinth biomass (MWHB) were prepared. Among these MWHBs, an equal proportion of coconut oil and raw WHB with 10% methanol solution exhibited the highest removal of SEO reaching 96%. Various sorption kinetics and isotherm models were examined to understand the SEO sorption process on MWHB. The pseudo-second-order kinetics (R2 0.999) and both the Langmuir and Freundlich isotherm models (R2 0.992 and R2 0.999, respectively) were found to be the best-fitting models. These findings indicated a chemisorption mechanism involving the initial monolayer coverage of SEO molecules on the MWHB surface followed by the development of multilayers. The MWHB achieved a maximum sorption capacity of 4.75 g/g within 60 min. Furthermore, the reusability tests showed that MWHB maintained a sorption capacity of over 90% even after the third sorption–desorption cycle.

  • Water hyacinth biomass was applied as an eco-friendly sorbent for the removal of simulated petroleum oil spills.

  • The hydrophobicity of biomass was enhanced by modifying it with extra virgin coconut oil.

  • The most suitable models describing the oil sorption were pseudo-second-order kinetics and Langmuir and Freundlich isotherm models.

  • The sorption capacity remained above 90%, even after the third sorption–desorption cycle.

The convergence of global rapid industrialization and consumer requirements for energy resources has created an enormous demand for fossil fuels in both consumer and industrial sectors. Nonetheless, this creates environmental concerns, given the potential for oil spills in the ocean or land while transporting petroleum products (Ali et al. 2012; Liu et al. 2017). These incidents can also arise at various stages of the petroleum industry, including drilling, extraction, refining, and unintentional discharges (Gurav et al. 2017, 2021). Oil spills in the ocean have the potential to result in significant water contamination and damage to marine ecosystems (Ramirez Leyva et al. 2018; Li et al. 2020; Guo et al. 2022). The enduring consequences of such incidents may persist for many years as sediments hold residual oils (Wang et al. 2021). Hence, the pollution arising from these spills can inflict harmful consequences on the natural ecology of the aquatic environment and its living resources (Ramdhani 2023). The primary constituents of petroleum oil, namely n-alkanes, cycloalkanes, and aromatic hydrocarbons, possess mutagenic and carcinogenic potential to humans and are highly toxic to marine life and the overall ecosystem (Zhang et al. 2016; Alzahrani & Rajendran 2019). Exposure to these compounds can cause health risks affecting several systems within the human body, including the respiratory, nervous, circulatory, reproductive, immune, and endocrine systems (Udgire et al. 2015). Moreover, petroleum hydrocarbons are harmful to marine organisms, causing impacts such as habitat damage, impaired body functions, and the accumulation of these substances in food chains (Lin & Tjeerdema 2008).

In 2020, crude petroleum was ranked as the third most traded commodity, valued at $640 billion. Saudi Arabia was the main exporter, followed by Russia, the United States, Canada, and Iraq. On the import side, China was the largest buyer, with the United States, India, South Korea, and Japan being major importers. Over 50 years, from 1970 to 2020, close to 5.86 million tons of oil was spilled during shipping accidents. In 2021, the industry saw one major spill in Asia (more than 700 tons) and five medium spills across Africa, Asia, and North America (7–700 tons) (Upadhyay 2022). It has been assessed that 630 billion gallons of oil-contaminated wastewater are produced annually in the oil industries of the United States (Cherukupally et al. 2020). The oil spill of the Deepwater Horizon in 2010 stands as the largest oil spill in the history of the United States, discharging around five million barrels of oil into the Gulf of Mexico over 87 days (Follett et al. 2014). The spill had immediate environmental consequences, including the death of thousands of animals, such as turtles, birds, whales, and dolphins (McGee 2010). Additionally, it caused high concentrations of polycyclic aromatic hydrocarbons along the coast, negatively affecting wildlife (Ramseur & Hagerty 2014). Again, a study indicated that phototoxicity may still be occurring due to the presence of remaining oil (Evers et al. 2019). Another study considered the impact of an oil spill in Rhode Island, which resulted in the death of numerous birds and the need for restoration efforts (Samuelson et al. 2021). The Dalian New Port oil spill in 2010, one of China's most severe, released 35,000 tons of crude oil, resulting in long-lasting damage to the coastal and marine ecosystems. Oil slicks covered over 100 km2 of the sea and 20 km of shoreline, affecting water quality, marine life, and coastal ecosystems with persistent contamination evident even years later (Guo et al. 2022). Also, the oil spills near Sori Island and Yeo-Cheon in South Korea in 1995 released thousands of tons of crude oil, affecting over 230 km of coastline and necessitating extended cleanup operations. The Hebei Spirit spill in 2007, the country's largest, resulted in the release of about 10,800 tons of oil near the port of Daesan, impacting the same region analyzed for pollution risk in the study (Lee 2017). Several studies found that oil spills have a significant impact on global climate change. For example, research on the Deepwater Horizon oil spill revealed its impact on British Petroleum's climate change discourse, as seen in their annual reports before and after the spill (Kapranov 2017). The world is now struggling with a freshwater shortage to meet the global water demand due to climate change (Khondoker et al. 2023). Also, climate change poses challenges to the gas and oil infrastructures in coastal and offshore areas (Dong et al. 2022). Comprehending the chemical composition of petroleum hydrocarbons (PHs), their movement and deposit in the sea, and their harmful effects on marine life and ecosystems is essential to implementing efficient emergency responses and regulatory actions (Boehm 1964; Gad & Gad 2014).

The noticeable methods used for cleaning the oil spills from water surfaces are based on physical/mechanical methods (skimmers, barriers, booms, hydrophobic meshes), chemical (dispersants or surfactants), and biological methods (microbial) (Liu et al. 2016; Doshi et al. 2018; Debs et al. 2019; Abdullah et al. 2022; Hethnawi et al. 2023). Although these methods are partly successful, searching for plant biomass-based green adsorbents is of the most significant interest from economic and ecological standpoints. Over recent years, there has been widespread utilization of advanced materials such as meshes, foam membranes, aerogels, and fabrics with modified surfaces for the effective separation of oil from water. Raffia fiber, a natural fiber abundant in eastern Africa, has shown ability as an absorbent for hydrocarbons, with higher sorption capacities observed for larger particle sizes (Silva et al. 2022). Additionally, for the removal of petroleum oil hydrocarbons, different particle sizes of activated charcoals have also been studied, resulting in the smallest particle offering the highest adsorption capacity (Ji et al. 2020). Also, inexpensive sorption materials based on raw materials derived from plants, such as vegetable waste and fruit peels, have been explored for the removal of heavy metals and petroleum hydrocarbons from water (Smyatskaya et al. 2018).

Water Hyacinth (WH) (Eichhornia crassipes), an invasive plant native to the Amazon basin, is considered one of the 10 most problematic plants because of its rapid growth and detrimental effects on aquatic ecosystems (Babatunde et al. 2023; Namasivayam et al. 2023). Furthermore, it has been found that invasive plants, including WH, enhance the methane emissions on decomposition, contributing to global warming (Zhou et al. 2022). In recent years, WH biomass (WHB) and WH biochar have been attracting researchers to utilize them as eco-friendly sorbents to remove heavy metals and other pollutants from wastewater (Priya & Selvan 2017; Gaurav et al. 2020; Amalina et al. 2022; Carneiro et al. 2022). Also, very few studies were carried out to remove petroleum oil using WHB. For instance, time-dependent capillary rise experiments were conducted to remove diesel, lubricant, and castor oil using different parts of the WH plant (leaf, stem, and root), and the stem proved to be a highly efficient sorbent among them (Rani et al. 2014). Another study was found utilizing free-floating WH plants as a sorbent for oil removal (Yang et al. 2014). The cellulose-based aerogel produced from WHB proved to be an effective sorbent for oil removal (Yin et al. 2017).

Therefore, the present research focuses on the utilization of WHB as an eco-friendly and cost-effective sorbent for the effective removal of petroleum oil spills from the water surface. To further enhance the petroleum oil sorption performance and hydrophobicity, WHB was modified using extra virgin coconut oil. Subsequently, the modified water hyacinth biomass (MWHB) was characterized and applied to remove simulated petroleum oil spills. Various isotherm and kinetic models, and analytical methods were comprehensively evaluated to deduce potential insights into the sorption process. This biomass can be used independently or with mechanical methods such as skimmers, barriers, and booms to clean the oil spill sites.

Sample collection and processing

The WH plants were collected from the San Marcos River (29°53′34.94″ N, 97°55′53.49″ W), San Marcos, TX, United States. After collection, the plant material was washed several times with running tap water, and the hairy roots were separated. The remaining plant biomass was dried for 24 h in active sunlight (4 days for 6 h each). Finally, the plant biomass was dried in an oven at 70 °C for 24 h. Spent engine oil (SEO) was collected from a local car oil changing service station. The density and viscosity of SEO were 0.88 g/cm3 at 25 °C and 1.27 Poise at 40 °C. The extra virgin coconut oil was purchased from a local general store in San Marcos, TX.

Sorbent preparation

The WHB (including leaves, petioles, and stems) was chopped into small pieces with an X-ACTO wood guillotine trimmer and a kitchen knife. The chopped biomass was sieve analyzed using (1/4)″ (6.3 mm), #4 (4.75 mm), #10 (2 mm), #20 (850 μm), #40 (425 μm), #60 (250 μm), #100 (150 μm), and #200 (75 μm) size sieve screens and a pan. Particle sizes 4.75–2 mm and 2 mm–850 μm were selected to be used for the experiment in a 2:1 ratio, respectively. Preliminary sorption tests for SEO were done using varied sizes of WHB before finalizing the specific particle sizes mentioned in Section 3.1. The biomass particle sizes of 4.75–2 mm and 2 mm–0.85 μm were denoted as ‘type-1’ and ‘type-2’, respectively. Both sorbents have proven to be ‘type-II sorbent (loose)’ according to the ‘American Society for Testing and Materials, ASTM F726–17’ guideline for the dynamic degradation test and the oil sorption long and short test.

Sorbent modification

To enhance the hydrophobicity and oil sorption capacity, six types of modified biomass were designated as Mod1, Mod1′, Mod2, Mod2′, Mod3, and Mod3′. The Mod1 and Mod1′ were prepared using a 1:1 ratio of dry biomass and coconut oil, and 10 and 20% methanol in deionized (DI) water, respectively. Whereas Mod2 and Mod2′ were prepared with a 1:1.5 ratio of dry biomass and coconut oil, and 10 and 20% methanol in DI water, respectively. The Mod3 and Mod3′ were developed using a 1:2 ratio of dry biomass and coconut oil, with 10 and 20% methanol in DI water, respectively.

The extra virgin coconut oil contains about 50% lauric acid which is natural and biodegradable and helps to increase the hydrophobicity of the sorbent (Dankovich & Hsieh 2007; Zinjarde et al. 2008; Gurav et al. 2021). Therefore, six 150 ml glass beakers were added with the sieved and dried WHB along with the required concentration of coconut oil. These beakers were placed in an oven at a temperature of 70 °C for 5 h. Hand stirring was performed using a glass rod at 20-min intervals throughout this duration. Once the coconut oil was evenly dispersed, the required quantity of methanol solution was added to the beakers. The beakers were then kept in the oven at 70 °C for 1 h, with intermediate mixing. Methanol reduces surface tension and allows the coconut oil to disperse more consistently over the surface, promoting uniform coverage and minimizing clumping or uneven distribution (Navarathna et al. 2020). Then, the mixtures were filtered through a stainless-steel mesh filter and washed repeatedly with n-hexane after 20 min of soaking time. Finally, the biomass was dried in the oven at 70 °C for 24 h and preserved in air-tight containers. The SEO sorption experiments were performed with diverse types of MWHBs. To check the effect of organic solvents on the hydrophobicity of unmodified biomass (without coconut oil), the control biomass (C′) was prepared with 20% methanol solution followed by two n-hexane washes. The experimental conditions for all the types of MWHB and control biomass (C′) have been summarized in Table 1. To check the hydrophobicity, the water sorption test of raw biomass, Mod1′, and C′ was performed. Each sample weighing 0.1 g was placed in 100 ml of DI water for 1 h, and the weight difference of the biomass was considered. The Mod1′ was found to be more hydrophobic than other sorbents, hence, it was selected for further sorption experiments.

Table 1

Summary of the experimental conditions of C′ and different types of MWHB

ModificationsWHB to coconut oil ratioMethanol solutionExperimental conditions
Mod1 1:1 10% 
  • Coconut oil added WHB was incubated in the oven for 5 h at 70 °C and agitated with a glass rod at 20 min intervals.

  • After adding the methanol solution, the mixtures were kept in the oven for 1 h at 70 °C and agitated with a glass rod at 10 min intervals.

  • All the modified biomass types went through several n-hexane washes followed by 24 h oven drying and stored in air-tight containers.

 
Mod1′ 1:1 20% 
Mod2 1:1.5 10% 
Mod2' 1:1.5 20% 
Mod3 1:2 10% 
Mod3' 1:2 20% 
Control (C′) No coconut oil 20% The control WHB sample was prepared by adding 20% methanol solution to the raw biomass and following the same procedure as stated above. 
ModificationsWHB to coconut oil ratioMethanol solutionExperimental conditions
Mod1 1:1 10% 
  • Coconut oil added WHB was incubated in the oven for 5 h at 70 °C and agitated with a glass rod at 20 min intervals.

  • After adding the methanol solution, the mixtures were kept in the oven for 1 h at 70 °C and agitated with a glass rod at 10 min intervals.

  • All the modified biomass types went through several n-hexane washes followed by 24 h oven drying and stored in air-tight containers.

 
Mod1′ 1:1 20% 
Mod2 1:1.5 10% 
Mod2' 1:1.5 20% 
Mod3 1:2 10% 
Mod3' 1:2 20% 
Control (C′) No coconut oil 20% The control WHB sample was prepared by adding 20% methanol solution to the raw biomass and following the same procedure as stated above. 

Sorbent characterization

The surface morphology, microstructure, and texture of WHB and MWHB were investigated using scanning electron microscopy (SEM; JEOL JSM-6010PLUS/LA). Whereas the elemental composition of WHB and MWHB was determined using SEM–energy dispersive spectroscopy (EDS). To examine changes in the functional groups on MWHB before and after SEO sorption, Fourier transform infrared (FTIR) spectrometry was employed in the scanning range of 400–4,000 cm−1 (Bruker ALPHA II FTIR Spectrometer). The contact angle of water was measured on both WHB and MWHB using the sessile drop technique. Pictures were captured by iPhone 13 Pro, and subsequently, these photographs were examined using the ImageJ software.

SEO sorption experiments

The sorption experiments for WHB and MWHB were performed in 150 ml beakers containing 100 ml DI water spiked with 1 g of SEO and added with 0.2 g of sorbent. The beakers were positioned on a horizontal shaker platform (VWR Advanced Digital Shaker) and operated at a speed of 50 rpm for 1 h. After this period, the sorbents were separated from the beakers, placed onto aluminum foil, and dried in an oven at 50 °C for 24 h. Finally, the SEO-loaded WHB and MWHB weights were measured to calculate the sorption efficiency. All the sorption experiments were conducted at room temperature (22 ± 2 °C) and repeated three times for accuracy. The SEO removal (%) was calculated using Equation (1) (Boleydei et al. 2018), and the sorption capacity (g/g) of the sorbent (g of SEO/g of sorbent) was determined by Equation (2) (Sidik et al. 2012).
formula
(1)
Here, x is the % of SEO removal and Ci and Ca are the concentrations of initial and sorbed SEO (g/l), respectively.
formula
(2)
where Q is the sorption capacity (g/g), m is the mass of sorbent (g), Ci and Ca are the concentration of initial and sorbed SEO (g/l), and V is the volume of DI water (l).

Sorption kinetic and isotherm models

To determine the most potential mechanism of SEO sorption on MWHB, a range of kinetics and isotherm models were explored. For the kinetic study, the sorption process was analyzed over time (0–120 min), using 2 g/l of MWHB and 10 g/l of SEO. The time-dependent batch sorption data were analyzed using pseudo-first-order Equation (3), pseudo-second-order Equation (4), and Elovich Equation (5) for kinetic models. The suitability of these kinetic models was evaluated by comparing R2 values with the experimental data for validation (Gurav et al. 2023). The isotherm equations modeling for the sorption mechanism of SEO on MWHB were carried out using the Origin software.
formula
(3)
formula
(4)
formula
(5)
Here, Qe represents the equilibrium sorption capacity, while Qt stands for the sorption capacity at a specific time ‘t’. K1 and K2 denote the rate constants associated with the pseudo-first-order and pseudo-second-order kinetics, respectively. β represents the desorption constant and α signifies the initial rate of sorption. Similarly, the batch sorption data for SEO concentrations (1–10 g/l) were examined by using Langmuir Equation (6), Freundlich Equation (7), and Temkin Equation (8) for isotherm models (Gurav et al. 2023). Two grams per liter of MWHB were added to each concentration of SEO for its removal.
formula
(6)
formula
(7)
formula
(8)

Here, Qm denotes the highest achievable sorption capacity (g/g), while Kl, Kf, and Kt represent the constants linked with the Langmuir, Freundlich, and Temkin isotherm models, respectively. Ce stands for the equilibrium concentration of SEO (g/l), 1/n depicts the intensity of sorption, and A signifies an additional Temkin constant. The appropriateness of these models was ascertained by comparing the coefficient of determination (R2) against the actual experimental data, which served as a benchmark for validation. The constants and parameters within these isotherm models, such as the maximum sorption capacity and the constants associated with each model, were determined by fitting the batch sorption data to the respective equations using the Origin software.

Desorption and reutilization

To check the reusability of sorbents, sorption–desorption tests were conducted to assess the ability to regenerate MWHB. Ten milliliter of n-hexane was used to wash the sorbed SEO from 0.2 g of MWHB. After three repetitive washings, the used MWHB was dried and reused to remove 1 g of SEO. This sorption–desorption process was performed for four repetitive cycles.

Effect of raw WHB particle size on SEO removal

The dried and chopped WHB segregated into assorted sizes using a sieve was investigated for SEO removal. The particle size distribution curve of chopped and dried WHB has been depicted in Figure 1. The analysis indicates that WHB consists predominantly of four particle size ranges. Specifically, particles measuring between 6.3 and 4.75 mm, 4.75 and 2 mm, 2 mm and 850 μm, and 850 and 425 μm represented 10, 43, 29, and 10% of the sample by weight, respectively. Hence, these four sizes were selected for initial sorption experiments. 0.2 g of WHB in four different sizes (6.3–4.75 mm, 4.75–2 mm, 2 mm–850 μm, and 850–425 μm) were examined independently for the removal of 1 g SEO. The results of the sorption processes are depicted in Figure 2(a). The maximum SEO removal was 96% (4.73 g/g) for 4.75–2 mm, 95% (4.69 g/g) for 6.3–4.75 mm, 91% (4.51 g/g) for 2 mm–850 μm, and 90% (4.51 g/g) for 850–425 μm sizes of WHB, respectively.
Figure 1

Sieve analysis of chopped WHB for particle size.

Figure 1

Sieve analysis of chopped WHB for particle size.

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Figure 2

(a) SEO sorption experiments for different particle size WHB and (b) removal of different concentrations of SEO with 0.2 g of blended type-1 and type-2 WHB.

Figure 2

(a) SEO sorption experiments for different particle size WHB and (b) removal of different concentrations of SEO with 0.2 g of blended type-1 and type-2 WHB.

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The result justified that WHB with different particle sizes ranging 6.3 mm to 425 µm could remove more than 90% of SEO. However, on using large particle size (6.3–4.75 mm) WHB, only the lower surface was exposed to SEO slick, whereas the upper part of WHB remained unexposed due to large particle size and floating nature. As a result, 100% SEO removal with a 6.3–4.75 mm particle size of WHB was not achieved. On the other hand, particles ranging from 850 to 425 μm were extremely small, making their separation after SEO sorption more challenging.

Based on the particle distribution diagram (Figure 1), type-1 and type-2 WHB were found in greater quantity and the SEO sorption capacity was more than 90% for each. Therefore, these two types of WHB were used in a 2:1 ratio. Also, a sorbent size of 1–2 mm can perform better removal of oil (Boleydei et al. 2018). A blend of one portion of type-2 and two portions of type-1 WHB samples was prepared for further experiments. Two grams per liter of blended WHB was used to remove 5, 10, 15, and 20 g/l of SEO as reported in Figure 2(b). The removal of 5, 10, 15, and 20 g/l of SEO was 90% (2.21 g/g), 95% (4.66 g/g), 94% (6.95 g/g), and 88% (8.73 g/g) with 2 g/l of blended WHB. Due to the high amount of SEO (15 and 20 g/l) used in the experiment responsible for increasing the thickness of the oil spill in the beaker containing water, a good amount of SEO removal was observed due to the availability of more surface area for interaction between WHB and SEO. However, high SEO concentration in the reaction beaker could also attach more SEO on the inner wall beaker resulting in a huge loss of SEO. Hence, 10 g/l was used for further experiments and analysis.

SEO sorption using coconut oil-modified WHB

Different types of MWHB (Mod1, Mod1′, Mod2, Mod2′, Mod3′, and Mod3′) were used to remove 10 g/l SEO using 2 g/l of MWHB. As depicted in Figure 3(a), Mod1, Mod1′, Mod2, Mod2′, Mod3, and Mod3′ removed 95% (4.71 g/g), 96% (4.75 g/g), 96% (4.95 g/g), 96% (4.87 g/g), 96% (4.77 g/g), and 96% (4.75 g/g) of SEO, correspondingly. Though all MWHBs (except for Mod1) demonstrated over 95% SEO removal, Mod1′ (1:1 ratio of WHB and coconut oil and 20% of methanol solution) was chosen for the batch sorption, kinetics, and isotherm studies due to its eco-friendly nature. The hydrophobicity test results are shown in Figure 3(b). The graph indicated that the modified biomass possesses the lowest water sorption capacity (11%), indicating greater hydrophobicity as compared to the untreated (14%) and control (21%).
Figure 3

(a) SEO sorption with different types of modified biomass (Mod1, Mod1′, Mod2, Mod2′, Mod3, and Mod3′), and (b) hydrophobicity test of raw, control, and modified biomass.

Figure 3

(a) SEO sorption with different types of modified biomass (Mod1, Mod1′, Mod2, Mod2′, Mod3, and Mod3′), and (b) hydrophobicity test of raw, control, and modified biomass.

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Sorbent characterization

Contact angle

Water drops on WHB and MWHB are shown in Figure 4. According to the analysis with the ImageJ software, the contact angle of water on WHB was measured as 79.56°, whereas the MWHB contact angle was enhanced to 103.5°.
Figure 4

Water contact angle measurement. (a) Water drops on WHB and (b) water drops on MWHB.

Figure 4

Water contact angle measurement. (a) Water drops on WHB and (b) water drops on MWHB.

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The lauric acid and other fatty acids in coconut oil demonstrated higher hydrophobic properties and the ability to form molecular interactions with the sorbent surface, contributing to an increased contact angle and enhancing the hydrophobicity of the sorbent (Navarathna et al. 2020; Gurav et al. 2021). The materials with contact angles beyond 90° were considered more hydrophobic as reported in lauric acid-modified Douglas fir biochar (Navarathna et al. 2020). Enhanced hydrophobicity helps the sorbent to float which could help the easy recovery of sorbent from the water surface after petroleum oil sorption. Besides, the carboxylic acid groups present in fatty acids could interact with oleophilic alkyl chains in petroleum oil that help higher SEO sorption.

SEM and EDS analysis

Figure 5 shows the morphological characteristics of SEM images of WHB and MWHB. Image (a) reveals the stem of the WHB has a honeycomb-like spongy structure. Images (b) and (c) were the images of WHB and MWHB at different magnifications. The diameters of WHB and MWHB pores range from 84 to 216 μm and 47 to 207 μm, respectively. The elements present on the surface of WHB and MWHB were investigated by EDS. Figure 6 illustrates that the major elements present on the WHB surface were carbon (C) and oxygen (O). The mass of C increased from 47.66 to 57.66%, whereas the mass of O decreased from 44.18 to 36.86% after modification with coconut oil. Some other elements (chlorine, potassium, calcium, magnesium, and aluminum) were also detected in minor quantities in WHB and MWHB. When fatty acids react with hydroxyl (OH) groups in cellulose, hemicelluloses, and lignin of WHB, an esterification reaction takes place. This reaction considers OH components in the biomass to react with alkyls from the lauric acid, resulting in a non-polar layer on the MWHB surface that repels water (Sidik et al. 2012). Esterification typically involves the removal of water (which contains oxygen) as the hydroxyl groups (OH) from cellulose, hemicellulose, and lignin with the acid groups (COOH) of the lauric acid to form esters. This reaction effectively removes some of the oxygen that was originally part of the hydroxyl groups in these biological molecules, thus reducing the overall oxygen content and increasing the carbon content of MWHB (Ahmad et al. 2005).
Figure 5

(a) SEM image of WHB, (b) WHB at different magnifications, and (c) SEM image of MWHB.

Figure 5

(a) SEM image of WHB, (b) WHB at different magnifications, and (c) SEM image of MWHB.

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Figure 6

EDS analysis showing the surface elemental composition of (a) WHB and (b) MWHB.

Figure 6

EDS analysis showing the surface elemental composition of (a) WHB and (b) MWHB.

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FTIR analysis

Figure 7 shows the FTIR spectra of WHB, MWHB, and MWHB after the sorption of SEO. The FTIR spectra of the biomass showed O–H stretching at 3,300 to 3,400 cm−1 which justifies the presence of lignin and cellulose in the WHB structure (Rani et al. 2014). Two distinct peaks were noticed at 2,852 and 2,922 cm−1, which can be recognized as the signature of C–H bonds stretching in different ways within the CH3 and CH2 groups.
Figure 7

FTIR spectra of WHB, MWHB, and MWHB after SEO sorption.

Figure 7

FTIR spectra of WHB, MWHB, and MWHB after SEO sorption.

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Additionally, an identified peak at 1,742 cm−1 can be linked to the stretching of the C=O bond, typically found in carbonyl groups. Moreover, a peak that appeared at 1,598 cm−1 was associated with the C=C bond stretching, a characteristic often seen in aromatic compounds present in both the sorbent and the SEO. Nevertheless, the MWHB displayed further intense peaks at 2,922 and 2,852 cm−1, which are associated with the stretching of C−H bonds in CH2 and CH3 groups, signifying the integration of fatty acids from coconut oil into WHB (Navarathna et al. 2020; Gurav et al. 2021, 2023). Furthermore, the appearance of a new peak at 1,742 cm−1, associated with the stretching of the carbonyl groups present in fatty acids, was noted, indicating an enhancement in hydrophobic properties of MWHB (Sidik et al. 2012; Gurav et al. 2021). Furthermore, wide peaks were observed at 1,153 and 1,006 cm−1. These are believed to be due to the stretching of the C−O−C and C−O within lignin, and those within cellulose and hemicellulose, respectively (Pandey & Pitman 2003). Additional peaks in MWHB were identified at 1,317 cm−1 (related to CH3 bending) and 1,153 cm−1 (indicating C=O stretching). Hence, the presence of saturated C−H, C−C, CH2, CH3, and C=O groups on MWHB suggested the biomass possessed increased hydrophobic and oleophilic properties (Yin et al. 2017; Ribeiro et al. 2000; Oliveira et al. 2020; Gurav et al. 2021, 2023).

Nevertheless, the peak intensity at 2,923 and 2,853 cm−1 for C–H justifies asymmetric stretching in CH3 and CH2 groups in alkane hydrocarbons was increased after SEO sorption on MWHB. Two new peaks appeared at 1,461 and 1,377 cm−1 after the SEO sorption was detected. The peak at 1,461 cm−1 can be attributed to the asymmetric bending mode of CH3 groups, which are abundant in petroleum hydrocarbons. Similarly, the peak at 1,377 cm−1 revealed the presence of symmetric C–H bending in SEO (Sidik et al. 2012).

Sorption kinetics model

Various kinetic models, including the pseudo-first-order, pseudo-second-order, and Elovich models, were examined to identify the step that controls the rate of sorption of SEO (10 g/l) onto MWHB (2 g/l). The sorption of SEO onto MWHB displayed a rapid initial sorption rate, reaching 92.2% (4.57 g/g) removal within the first 2 min (Figure 8(a)).
Figure 8

Sorption kinetics of the (a) time-dependent sorption process, (b) pseudo-first-order, (c) pseudo-second-order, and (d) Elovich models.

Figure 8

Sorption kinetics of the (a) time-dependent sorption process, (b) pseudo-first-order, (c) pseudo-second-order, and (d) Elovich models.

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This rapid initial sorption is more likely attributed to the accessibility of numerous available surfaces, functional groups, and vacant pores on the surface of MWHB. However, as time progressed, the sorption rate gradually decreased, reaching equilibrium after 75 min and achieving a maximum SEO removal of 96.3% (4.77 g/g). It was observed that as the sorption time was extended from 2 to 75 min, the amount of SEO uptake increased. Beyond 75 min, the rate of sorption remained constant, suggesting that the surface of the MWHB was completely covered with SEO, therefore equilibrium was reached. To ensure that a complete equilibrium condition was achieved, the observation was continued for 120 min. It was noted that approximately 60 min was the effective time for the sorption of SEO, hence, 60 min was the ideal contact time set for later experiments. The R2 values and the linear-fit graphs for all the kinetic models are shown in Figure 8(b)–(d) and Table 2. The sorption process of SEO on MWHB was effectively described by the pseudo-second-order model (R2 > 0.999), which aligns with the findings from previous research on petroleum oil sorption (Sidik et al. 2012). This model suggests that the step that limits the rate of sorption involves a chemical interaction between the hydrophobic tails on MWHB and the sorbate surface (Cheu et al. 2016; Boleydei et al. 2018; Khamizov 2020; Yasid et al. 2022).

Table 2

Kinetic and isotherm parameters for the sorption of SEO on MWHB

ModelParametersValue
Kinetic Pseudo-first order Qe 0.361 
K1 −0.0006 
R2 0.908 
Pseudo-second order Qe 4.774 
 22.793 
K2 1.144 
R2 0.999 
Elovich α 21.182 
β 96.535 
R2 0.940 
Isotherm Langmuir Qm 4.998 
K1 5.622 
R2 0.992 
Freundlich 1/n 0.723 
Kf 8.816 
R2 0.999 
Temkin A 1.359 
Kt 50.948 
R2 0.865 
ModelParametersValue
Kinetic Pseudo-first order Qe 0.361 
K1 −0.0006 
R2 0.908 
Pseudo-second order Qe 4.774 
 22.793 
K2 1.144 
R2 0.999 
Elovich α 21.182 
β 96.535 
R2 0.940 
Isotherm Langmuir Qm 4.998 
K1 5.622 
R2 0.992 
Freundlich 1/n 0.723 
Kf 8.816 
R2 0.999 
Temkin A 1.359 
Kt 50.948 
R2 0.865 

Sorption isotherm model

The distribution pattern of SEO molecules at the MWHB sorbents was assessed using isotherm models (Langmuir, Freundlich, and Temkin) after acquiring the equilibrium data shown in Figure 9.
Figure 9

(a) Batch isotherm sorption experiments, (b) Langmuir, (c) Freundlich, and (d) Temkin isotherm models.

Figure 9

(a) Batch isotherm sorption experiments, (b) Langmuir, (c) Freundlich, and (d) Temkin isotherm models.

Close modal

Among these models, both Langmuir and Freundlich isotherms proved to be the most suitable for describing the sorption of SEO, as evidenced by higher regression coefficient values (R2) of 0.992 and 0.999 (Table 2). The Langmuir isotherm model suggests that the sorption of SEO onto the MWHB surface occurs as a homogeneous monolayer process. This implies that the SEO molecules were evenly sorbed on the active surfaces of MWHB susceptible to holding only one kind of sorbent on each side, and all these sites possess equipotential energy levels. According to the Langmuir analysis, the maximum sorption capacity (Qm) reached 4.99 g/g for MWHB, whereas the experimental value was 4.75 g/g. Furthermore, the Freundlich model justified that the sorption process might have occurred in a heterogenous multi-layer after the monolayer sorption mechanism (El-Hassouni et al. 2013; Senturk et al. 2016; Boleydei et al. 2018). However, a higher precision, with an R2 value (>0.999), suggests that the Freundlich isotherm model is a more accurate description of how SEO attaches to the MWHB. MWHB sorbent might have a heterogeneous surface with a non-uniform distribution of active sites, capable of sorbing SEO droplets in a multi-layer fashion. With a Kf value of 8.816, it is understood that higher Kf values correlate with higher sorption capacity. The literature supports that attachment is effective when the n value is between 1 and 10, and a higher n value means higher sorption intensity. Here, the n value is 1.38, indicating a favorable attachment of oil to the MWHB. On the other hand, the Temkin model showed a lower R2 value of 0.865, which suggests that it does not fit the experimental data as well, pointing to a less satisfactory model for describing the isotherm model (Sidik et al. 2012).

The maximum sorption capacity of different petroleum oils on different types of sorbents is shown in Table 3. The results shown in the table imply that this study could be compared with many of them that used natural sorbents with minimal surface modification. It could be said that the surface area and hydrophobicity of sorbents play a crucial role in the sorption process. Higher sorption capacity requires sorbent modifications with a high dose of hydrophobic agents and complicated technologies. The enhanced sorption of oil onto the hydrophobic surface areas of MWHB is illustrated in Figure 10.
Table 3

Comparison with other oil sorption studies

SorbentType of petroleum oilSorption capacity (g/g)Reference
Extra virgin coconut oil-modified MWHB Spent engine oil 4.75 This study 
Oleic acid-grafted sawdust Crude oil 6.4 Banerjee et al. (2006)  
Cocoa pods Crude oil 3.97 Onwuka et al. (2018)  
Ammonium sulfate-modified biomass Crude oil 4.20 Eze et al. (2019)  
Ipomoea batatas peel Motor oil 3.87 Akpomie & Conradie (2023)  
Lauric acid-treated oil palm leaves Crude oil 1.2 ± 0.12 Sidik et al. (2012)  
Silk cotton fiber Diesel 58.5 Oliveira et al. (2020)  
Cellulose-based aerogel from WHB Different types of oil 60.33–152.21 Yin et al. (2017)  
Kapok fiber Diesel oil 19.6 Ali et al. (2012)  
Sugarcane bagasse Diesel oil 10.5 Ali et al. (2012)  
Rice husks Diesel oil 2.6 Ali et al. (2012)  
Carbonized rice husks Different types of oil 5.5 Angelova et al. (2011)  
SorbentType of petroleum oilSorption capacity (g/g)Reference
Extra virgin coconut oil-modified MWHB Spent engine oil 4.75 This study 
Oleic acid-grafted sawdust Crude oil 6.4 Banerjee et al. (2006)  
Cocoa pods Crude oil 3.97 Onwuka et al. (2018)  
Ammonium sulfate-modified biomass Crude oil 4.20 Eze et al. (2019)  
Ipomoea batatas peel Motor oil 3.87 Akpomie & Conradie (2023)  
Lauric acid-treated oil palm leaves Crude oil 1.2 ± 0.12 Sidik et al. (2012)  
Silk cotton fiber Diesel 58.5 Oliveira et al. (2020)  
Cellulose-based aerogel from WHB Different types of oil 60.33–152.21 Yin et al. (2017)  
Kapok fiber Diesel oil 19.6 Ali et al. (2012)  
Sugarcane bagasse Diesel oil 10.5 Ali et al. (2012)  
Rice husks Diesel oil 2.6 Ali et al. (2012)  
Carbonized rice husks Different types of oil 5.5 Angelova et al. (2011)  
Figure 10

Proposed mechanism of the enhanced sorption of oils onto hydrophobic surface areas of MWHB.

Figure 10

Proposed mechanism of the enhanced sorption of oils onto hydrophobic surface areas of MWHB.

Close modal

Reutilization of modified biomass

Evaluating the reusability of sorbents was an essential step in the development of a cost-effective and environmentally friendly technology to prevent further pollution when disposing of spent biomass (Gurav et al. 2021). While the sorption efficiency of MWHB decreased with each cycle of sorption and desorption, it is noteworthy that the sorbent still maintained an excellent performance, with a sorption efficiency of over 90% even after the third sorption–desorption cycle as shown in Figure S1 (Supplementary Data). This indicates effective reusability characteristics for the sorbent. The decrease in the sorption capacity with each cycle might be attributed to SEO components that were not fully removed during the treatment with n-hexane (Kim et al. 2020). Similarly, the decline in performance could be linked to a loss in the fatty acid content on MWHB. The carboxylic acid groups on fatty acids actively participate with the oleophilic C–H (alkyl) chains, therefore loss of fatty acid composition could be another reason for the decrease in sorption performance (Cai et al. 2019; Ji et al. 2020; Gurav et al. 2021).

Among the different MWHBs, the MWHB produced using an equal portion of extra virgin coconut oil and WHB followed by treatment with 10% methanol solution demonstrated a higher hydrophobicity and SEO sorption. The best-fit sorption kinetics and isotherms indicated a chemisorption mechanism involving initial monolayer coverage of the MWHB surface followed by multi-layer coverage with SEO. Due to the increased hydrophobicity of MWHB, a higher sorption capacity was observed as compared to raw WHB. Furthermore, reusability testing of MWHB demonstrated over 90% sorption efficiency even after the third sorption–desorption cycle, highlighting its excellent reutilization properties. Therefore, modifying WHB with extra virgin coconut oil could offer an inexpensive and sustainable approach for treating water contaminated with petroleum hydrocarbons. In real-scale applications, floating MWHB could be retrieved using other mechanical techniques such as fishing nets (smaller pore size than biomass), booms, or skimmers.

All relevant data are included in the paper or its Supplementary Information.

The authors declare there is no conflict.

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