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. 2026 Sep 28;11(40):61094–61107. doi: 10.1021/acsomega.6c05671

Adsorptive Removal of 1,2-Dichloroethane Using Novel Oleogel Adsorbents: Synthesis Strategy and Adsorption Mechanism Insight

Yunsheng Liao †, Jialong Mei †, Youxian Zhang †,‡,*
PMCID: PMC13670798  PMID: 42889998

Abstract

1,2-Dichloroethane (DCE) is a widely used, highly volatile, and lipophilic industrial solvent. As a chlorine-containing volatile organic compound (VOC), DCE emissions pose significant risks to human health and the ecological environment. Adsorption is considered an economical and environmentally friendly method for eliminating air pollutants. In this study, novel Oleogel adsorbents were prepared via self-assembly and polymeric cross-linking mechanisms, using 12-hydroxystearic acid (12-HSA) and ethyl cellulose (EC) as gelators, and rapeseed oil (RO) and dioctyl adipate (DOA) as base oils. A series of oleogels were fabricated by varying the type and dosage of gelators, and their structures, physicochemical properties, and DCE adsorption performance were systematically characterized. The DCE adsorption behavior and mechanism were investigated through dynamic adsorption experiments, multimodel kinetic fitting, and spectral analysis at multiple temperatures. The results showed that the 10 wt % 12-HSA/DOA Oleogel achieved a DCE adsorption capacity of 154.4 mg g–1 at 25 °C and reached 201.9 mg g–1 at 15 °C, which is comparable to those of previously reported adsorbents. Characterization and adsorption experiments demonstrated that the adsorbent exhibited a stable three-dimensional crystalline architecture, excellent oil retention (up to 98% after centrifugation), and favorable thermal stability below 150 °C. Meanwhile, DCE adsorption on Oleogel adsorbents involves significant intermolecular interactions (e.g., dipole–dipole and hydrogen bonding) rather than a purely physical process, and their surface is enriched with exposed functional groups, such as carbonyl and carboxyl groups. Further analysis indicated that the base oil was the dominant factor governing DCE adsorption performance, and the gelator type was the decisive factor influencing crystal morphology development. Notably, the contact angle of samples prepared from ethyl cellulose and dioctyl adipate reached 95.6°, suggesting potential for use in high-humidity environments.

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1. Introduction

As a highly volatile and lipophilic industrial solvent widely used in the production of waxes, rubbers, fats, pharmaceuticals, plastics, and organic detergents and degreasers, , 1,2-dichloroethane (DCE) readily causes environmental pollution during industry production. , This volatile organic compound (VOC) is subject to strict monitoring and control, as it has been classified as a probable human carcinogen and a priority control pollutant by numerous countries and organizations, including the U.S. Environmental Protection Agency, the European Commission, and the Chinese Ministry of Environmental Protection. − DCE causes severe damage to human kidneys and the respiratory system, and its metabolite, 2-chloroethanol, adversely affects the central nervous system and leads to cerebral edema, cerebral palsy, and other diseases. − Over the past decades, multiple cases of DCE-related (sub)­acute poisoning have been reported. , Therefore, the development of effective DCE removal methods is of high practical significance and has attracted considerable attention.

Oleogels are structured soft solids comprising a continuous liquid oil phase immobilized within a thermoreversible, three-dimensional network. Although oil constitutes the bulk of their composition, oleogels display solid-like mechanical integrity, shape stability, and viscoelastic behavior. In recent years, they have garnered growing interest in food science and pharmaceutical technology, with practical applications spanning bakery products, dietary supplements, and sustained-release oral dosage forms. , Their primary functional value resides in serving as advanced lipid-based delivery vehicles for lipophilic bioactive compounds and poorly water-soluble drugs. , As such, oleogels enable four interrelated functions: molecular encapsulation, protection (e.g., antioxidation or hydrolysis), controlled-release action, and enhanced bioavailability. Crucially, effective encapsulation and controlled release rely not merely on physical entrapment, butmore fundamentallyon favorable molecular interactions between the gel matrix and polar organic actives, thereby ensuring both high loading efficiency and retention capacity.

Motivated by the distinctive capacity of oleogels to immobilize and molecularly interact with hydrophobic organic species, we herein report the rational design and fabrication of two novel Oleogel-based adsorbents: a rapeseed oil (RO)-based Oleogel and a dioctyl adipate (DOA)-based Oleogel, specifically engineered for the capture of 1,2-dichloroethane (DCE) from waste gas streams. Rapeseed oil, as a commonly used edible oil, has been utilized in the treatment of common VOCs, such as toluene, showing satisfactory results. , Its good affinity for hydrophobic volatile organic compounds and environmentally friendly characteristics make it particularly suitable as the matrix oil for preparing Oleogel adsorbents. DOA was identified through a systematic laboratory screening of multiple organic liquids, based on its favorable gas–liquid partition coefficient for DCEconfirming high affinity and efficient mass transfer potential under vapor-phase conditions.

In this study, we systematically characterized these adsorbents to evaluate their structure, morphology, and adsorption performance. Characterization included morphology analysis, optical microscopy (OM), polarization microscope (PLM), physicochemical property analysis, thermogravimetric analysis (TGA), X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy analysis, and dynamic adsorption experiments. Furthermore, the underlying adsorption mechanism was clarified through combined experimental observations and mechanistic analyses. On this basis, the thermal stability, surface wettability, and oil-binding capacity of the oleogels were evaluated to verify their practical application potential. To the best of our knowledge, this work represents the first reported application of oleogels in environmental remediation, specifically the adsorption of DCE.

2. Materials and Methods

2.1. Reagents and Equipment

Rapeseed oil (RO) was purchased from a local market in China, while 12-hydroxystearic acid (12-HSA), ethyl cellulose (EC), dioctyl adipate (DOA), and 1,2-dichloroethane (DCE) were obtained from Tianjin Damao Co., Ltd. and Tianjin Kermel Chemical Reagent Co., Ltd. (Tianjin, China). All other solvents and chemicals were of analytical grade and used without further purification. Sample preparation was performed using a magnetic heating stirrer (MS-H-Pro+, DLAB Scientific, China), a digital constant-temperature water bath (HH-S4, Jintan Medical Instrument Factory, China), and a medical refrigerated cabinet (HYC-118, Haier Biomedical, China). Dynamic adsorption experiments were conducted with an oil-free air pump (MP-200, Shenchen Fluid Technology, China), a glass rotameter (LZB-3, Yinhuan Flow Meter, China), and a constant-temperature electric heating mantle (ZNHW, Nuoji Instrument, China). Gas chromatographic (GC) analysis was performed using an HP-5 capillary column (30 m × 0.32 mm × 0.25 μm) with the following conditions: inlet temperature 200 °C, column oven temperature 80 °C, flame ionization detector (FID) temperature 250 °C, and high-purity nitrogen carrier gas at a flow rate of 1.0 mL/min.

2.2. Preparation of the Oleogels

Rapeseed oil (RO) and dioctyl adipate (DOA) were weighed and separately blended with 10.0, 20.0, or 30.0 wt % 12-hydroxystearic acid (12-HSA). Each mixture was then heated at 90 °C under magnetic stirring at 500 rpm for 30 min to ensure complete dissolution. Subsequently, the samples were cooled to room temperature (25 ± 1 °C) and transferred into sealed transparent glass container, then stored at 4 °C for 24 h. The samples were labeled as X-HSA-RO and X-HSA-DOA, where X denotes the mass fraction (10, 20, or 30) of 12-HSA in the corresponding Oleogel.

Further, RO and DOA were separately blended with 14.0, 17.0, or 20.0 wt % ethyl cellulose (EC). The resulting mixtures were then heated at 170 °C under magnetic stirring at 500 rpm for 30 min. Subsequently, the samples were cooled to room temperature and transferred into sealed transparent glass container, then stored at 4 °C for 24 h. They were labeled as Y-EC-RO and Y-EC-DOA, where Y denotes the mass fraction (14.0, 17.0, or 20.0) of EC in the corresponding Oleogel. Samples were prepared in triplicate (Figure ) and subsequently analyzed.

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Apparent morphology of oleogels with different components. (a) HSA-RO; (b) EC-RO; (c) HSA-DOA; (d) EC-DOA.

2.3. Appearance and Microstructure Analysis

The 10-HSA-RO, 10-HSA-DOA, 14-EC-RO, and 14-EC-DOA samples were selected for comparative evaluation of Oleogel properties as these samples formed stable gels and exhibited high DCE adsorption capacities.

Macroscopic morphology was studied using a Canon PowerShot G1 X Mark III digital camera used to assess sample appearance and self-supporting ability. OM observations were carried out using an Olympus BX53 optical microscope (Olympus, Japan) equipped with bright-field illumination at 100× magnification to examine the surface topography and microstructure of Oleogel samples. PLM (Olympus GX71, Japan) was used to visualize the crystalline network structure of the oleogels. For analysis, samples were transferred onto a preheated glass slide and allowed to cool to room temperature prior to observation. All images were processed using ImageJ software.

2.4. Physical Characteristics

2.4.1. Oil Binding Capacity (OBC)

OBC was determined via centrifugation and by following a standardized method. In particular, ∼2 g of the sample was placed in a 1.5 mL centrifuge tube and centrifuged at 6070 × g for 15 min (Sorvall ST16, Thermo Fisher Scientific). The tube was then inverted onto filter paper (pore size 6–8 μm, medium-speed) for 5 min to remove unbound oil, after which the sample was weighed to obtain the final mass.

2.4.2. Rheological Properties

The Rheological properties of the oleogels were evaluated using a dynamic oscillatory rheometer (Haake Mars 40, Germany). Measurements were performed at an oscillation strain of 0.01%, a temperature of 25 °C, and a frequency range of 0.1–100.0 Hz.

2.4.3. Contact Angle

The contact angle of the samples was measured at room temperature using a contact angle measuring instrument (SZ-CAMC32, China). The sample was securely mounted on a clean glass slide, and a 4-μL droplet of deionized water was gently deposited onto the sample surface.

2.5. Thermal Stability Analysis

Thermal stability was evaluated by thermogravimetric analysis using a Mettler TGA/DSC instrument (Switzerland). Samples (∼15 mg) were heated from 30 to 600 °C at a heating rate of 10 °C/min in a nitrogen flow of 40 mL/min.

2.6. Crystal Type Analysis and FTIR Spectroscopy Analysis

The crystal structure of the samples was characterized by XRD using a Bruker D8 Advance diffractometer (Germany) with Cu Kα radiation (λ = 1.5406 Å). Diffraction patterns were recorded over a 2θ range of 5°–90° at a scan rate of 5°/min, with a generator voltage of 40 kV and an emission current of 40 mA. The divergence and antiscatter slits were set to 1.0 mm, and the receiving slit was set to 0.1 mm. All measurements were conducted at 25 °C and analyzed using the Jade software.

Intermolecular interactions within the oleogels were characterized by FTIR spectroscopy (Nicolet iS20, Thermo Fisher Scientific, USA). Spectra were collected in the attenuated total reflectance mode with a resolution of 4 cm–1 over the range of 600–4000 cm–1 using 32 coadded scans. The data were processed using the OMNIC software.

2.7. X-ray Photoelectron Spectroscopy (XPS) Analysis

The surface chemical composition and elemental bonding states of Oleogel samples before and after DCE adsorption were characterized by X-ray photoelectron spectroscopy on a Thermo Scientific K-Alpha spectrometer (Thermo Fisher Scientific, USA) with monochromatic Al Kα radiation (1486.6 eV). Survey spectra and high-resolution scans of C 1s and Cl 2p core levels were recorded, and the spectral data were processed using Avantage software.

2.8. Dynamic Adsorption Experiments

DCE waste gas was generated using a dynamic gas distribution method (Figure ). , Air produced by two pumps was transported into two pipelines. One stream was introduced into a bubbling bottle containing liquid DCE, and the other was passed through an empty buffer bottle to prevent pressure buildup and imbalance in subsequent units. The two gas streams were then mixed in a mixing flask and directed into a long glass adsorption column containing a certain amount of the adsorbent. A gas disperser was installed at the bottom of the column to disperse the waste gas into the adsorbent. The inlet gas flow rate and concentration were controlled by adjusting three gas flow meters, and the temperature was regulated using a thermostatic electric heating jacket. Gas concentrations before and after adsorption were measured by gas chromatography.

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Experimental setup.

A portion (30 g) of the sample was cut into cubic particles with a size of 2 mm and packed into the adsorption column. The glass adsorption column has an inner diameter of 20 mm, with a packed adsorbent fixed-bed height of approximately 180 mm. Then, the DCE breakthrough curves for the X-HSA-RO, X-HSA-DOA, Y-EC-RO, and Y-EC-DOA samples were measured over 0–120 min. The adsorption test conditions were as follows: temperature = 25 °C, inlet gas flow rate = 36 L h–1, and DCE concentration = 325 g m–3 (relative error < 2%).

The DCE adsorption performance of the samples was evaluated via the breakthrough curve method. The saturated adsorption capacity per unit mass of adsorbent was calculated by integrating the breakthrough curve, as expressed in eq :

QS=QV∫t0t1(Cin−Cout)dtm 1

where QS denotes the saturated DCE adsorption capacity per unit mass of adsorbent, in units of mg g–1; where Q V is the gas flow rate (m3 min–1); t 0 is the start time of gas intake (min); t 1 is the end time of gas intake (min); C in and C out are the inlet and outlet concentrations of DCE (mg m–3), respectively; and m is the mass of the adsorbent (g).

All data calculations were performed using the Origin 11 software.

2.9. Adsorption Kinetics

In this work, kinetic tests including pseudo-first-order model, pseudo-second-order model were used to study the adsorption-diffusion behavior of DCE molecules during the adsorption process. The adsorption behavior of the guest molecules in the intraparticle and the adsorption phases were investigated by the Weber-Morris model. The detailed formulas were shown in eqs , and .

qt=qe(1−e−k1t) 2
qt=(qe2k2t)/(1+qek2t) 3
qt=kidt0.5+C 4

where q t represents the actual adsorption of DCE at time t (mg g–1); q e represents the theoretical equilibrium adsorption amount (mg g–1); k 1 (min–1) and k 2 (g mg–1 min–1) are quasi-first-order and quasi-second-order rate constants; k id is intraparticle diffusion rate constant (mg g–1 min–0.5); C is a constant related to the boundary layer thickness (mg g–1).

3. Results and Discussion

3.1. Appearance and Microstructure

This section systematically characterizes the macroscopic morphology, optical microscopic and polarized microscopic microstructure of four types of oleogels (HSA-RO, EC-RO, HSA-DOA, EC-DOA). Figure displays the self-supporting solid-state appearance of oleogels with different gelator dosages.

As shown in Figure , the samples exhibited a pronounced reduction in fluidity, which resulted from the formation of a stable crystalline network arising from the reorganization of molecular packing. In the RO and DOA systems, gelation occurred at an HSA content of 10.0 wt %. Meanwhile, a higher EC content of 14.0 wt % was required to induce gelation in the two systems. This difference reflects the distinct gelation mechanisms and molecular packing efficiencies of HSA and EC. Thus, the gelator type and dosage can be rationally tailored to meet specific application requirements. Notably, no phase separation or syneresis was observed in inverted vials stored at room temperature, confirming the formation of a robust Oleogel network with good structural stability. As highlighted by O’Sullivan et al. (2016), resistance against phase-separation serves as a critical evaluation indicator for oleogels toward practical engineering applications.

OM images revealed distinct microstructural differences among the oleogels (Figure ). HSA-based gels appeared turbid and opaque, exhibiting an irregular and granular network morphology (Figure a and c). In contrast, EC-based gels displayed a smoother and brighter surface with monolithic and homogeneous appearance, which indicates highly ordered and compact molecular packing (Figure b and d). This observation is consistent with previous reports by Qu et al. (2024), confirming the fundamental morphological difference between low-molecular-weight gelators and polymeric gelators during network construction. PLM further corroborated these structural distinctions. The rough and granular surface topology of the HSA-based oleogels increased the specific surface area, enhancing DCE adsorption, which is consistent with their higher experimental values discussed in Section . In addition, the EC-based gels exhibited a uniformly dark field of view under PLM observation (Figure ). This phenomenon arises from the extremely weak birefringence of the EC network under crossed polarizers, such that no distinct granular or fibrous crystalline texture can be resolved, which is characteristic of a highly ordered crystalline phase.

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Microstructure of oleogels with different components under optical microscopy. (a) HSA-RO; (b) EC-RO; (c) HSA-DOA; (d) EC-DOA.

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Microstructure of oleogels with different components under polarization microscope. (a) HSA-RO; (b) EC-RO; (c) HSA-DOA; (d) EC-DOA.

As shown in Figures and , the chemical identity of the base oil exerted a significant influence on the microstructure of the generated gel network. HSA formed irregular crystalline networks in both the RO and DOA systems but with distinct morphological characteristics. In the RO system, the crystals were sparser, larger, and more irregularly shaped, whereas in the DOA system, the crystal density was markedly higher and individual crystal size was lower. This finding is in good agreement with the conclusion reported by Calligaris et al. (2014). Their study demonstrated that the crystal morphology of γ-oryzanol/β-sitosterol-based oleogels was strongly dependent on base-oil type, which could be attributed to the differences in gelator solubility and degree of supercooling in various oil phases.

3.2. DCE Adsorption Behavior

Figure presents the DCE breakthrough curves of Oleogel samples with different formulations, reflecting the variation of outlet concentration over time during the adsorption process. As shown in Figure , the prepared oleogels exhibited highly similar adsorption kinetics, characterized by initial rapid uptake followed by gradual weakening of the adsorption. This behavior is consistent with classical adsorption mechanisms, including surface site saturation and diffusion-controlled mass transfer mechanisms. The saturated adsorption capacities (QS) derived from breakthrough-curve analysis at 25 °C are summarized in Table S1. For 12-HSA-based oleogels in RO, the QS values were 125.8, 108.3, and 71.4 mg g–1 for gelator concentrations of 10, 20, and 30 wt %, respectively. For EC-based oleogels in RO, the corresponding values were 105.2, 90.7, and 79.6 mg g–1 at 14, 17, and 20 wt % EC, respectively. In the DOA system, 12-HSA-based oleogels exhibited QS values of 154.4, 150.4, and 110.1 mg g–1, while EC-based oleogels showed values of 133.5, 122.7, and 116.0 mg g–1 at the same respective concentrations. To contextualize these results against previously reported adsorbents, it should be noted that direct cross-study performance comparison is not strictly rigorous, as test conditions such as inlet concentration, gas flow rate, and adsorbent bed parameters vary among studies. Within this context, the Oleogel adsorbents developed in this work achieve DCE adsorption capacities on the same order of magnitude as most conventional carbonaceous adsorbents. Although the maximum capacity (154.4 mg g–1) is moderately lower than that of coffee ground-based activated carbon (∼208.8 mg g–1) and fungi residue-derived N/P codoped porous carbon (∼200 mg g–1), , the Oleogel still demonstrates their potential as a new class of adsorbents for DCE removal.

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Effects of time and gelator on the DCE outlet concentration. (a) HSA-RO; (b) EC-RO; (c) HSA-DOA; (d) EC-DOA.

Gelator type and concentration, together with the base oil composition, critically influenced Oleogel formation and the DCE adsorption performance. As shown in Figure , increasing the concentration of HSA or EC resulted in a general decreasing trend of DCE adsorption capacity across all tested formulations, indicating the existence of an optimal gelator concentration, beyond which the DCE adsorption capacity declines. Two interrelated mechanisms accounted for this trend. First, increasing the gelator concentration reduced the proportion of the base oil (RO or DOA) from 90% to 70%. Because the oil phase serves as the primary medium for DCE adsorption, a reduced oil content directly limits the total DCE adsorption capacity. Second, a high gelator content promotes the formation of a dense crystalline network, which may restrict DCE diffusion and limit access to adsorption sites within the gel matrix. This phenomenon is analogous to the observation reported by Davidovich-Pinhas et al. (2015), who stated that excessively high polymer concentrations would reduce the release rate of guest molecules within gel systems. In the field of VOC absorption, Dumont et al. (2016) also pointed out that an overdose of thickening agents would lower the effective absorption capacity toward volatile organic compounds.

Moreover, the oleogels prepared using DOA as the base oil consistently exhibited higher DCE adsorption capacities than those prepared using RO regardless of the gelator type (HSA or EC). This observation indicates that the base oil is the dominant factor governing the DCE adsorption performance, which may be attributed to differences in the affinity of the oil phase for DCE. This affinity discrepancy can be fundamentally rationalized by the matching degree of solubility parameters between DCE and the two liquid base oils. As a polar ester compound, DOA possesses a solubility parameter much closer to that of DCE, thus conferring stronger DCE solubilization capacity. In contrast, RO mainly consists of nonpolar long-chain triglycerides, with a solubility parameter differing markedly from that of DCE, which accounts for its inferior adsorption performance. Lamprea-Pineda et al. (2024) systematically measured gas–liquid partition coefficients of multiple vegetable oils and esterified fatty acids toward hydrophobic VOCs, and demonstrated that ester-type liquids analogous to DOA deliver substantially higher affinity toward chlorinated VOCs compared with long-chain triglycerides. This dissolution-dominated adsorption mechanism is also highly consistent with the experimentally observed temperature-dependent trend of DCE adsorption capacity (Section ).

Different gelators self-assemble into distinct three-dimensional network architectures in oils, such as fibrous, lamellar, or needlelike structures, , which directly influence the interfacial contact area and mass transport kinetics between the Oleogel and DCE. As a low-molecular-weight gelator, 12-HSA self-assembles into fine granular and fibrous crystal aggregates, constructing a loose three-dimensional network. This structural feature enlarges the gas–liquid contact interface, shortens the mass transfer distance for DCE molecules to diffuse into the oil phase, and exposes more oil-phase adsorption sites. In contrast, ethyl cellulose (EC) is a polymeric gelator that forms a dense and uniform film-like network, resulting in a smaller effective contact area and higher mass transfer resistance. Consistent with this structural effect, the HSA-based oleogels exhibited higher DCE adsorption capacities than the EC-based oleogels, although the difference was modest.

3.3. Adsorption Kinetics and Temperature-Dependent Mechanism

The adsorption kinetics and diffusion properties were fitted by the pseudo-first-order model, pseudo-second-order model, and Weber–Morris intraparticle diffusion model, with the detailed parameters listed in Tables and . The goodness of fit was evaluated using both the coefficient of determination (R2) and the root-mean-square error (RMSE).

1. Adsorption Kinetics Parameters of Pseudo-First-Order and Pseudo-Second-Order Models for the Adsorption of DCE on Oleogel Adsorbents.

    Pseudo-first order model
Pseudo-second order model
Oleogel adsorbents T (°C) qe (mg g–1) k 1 × 10–2 (min–1) R2 RMSE qe (mg g–1) k 2 × 10–4 (g mg–1 min–1) R2 RMSE
10-HSA-RO 15 153.8 ± 2.1 3.42 ± 0.12 0.9941 4.2 154.6 ± 1.5 4.18 ± 0.09 0.9992 1.9
25 125.2 ± 2.3 3.85 ± 0.14 0.9935 4.5 126.0 ± 1.6 4.85 ± 0.10 0.9990 2.1
35 95.8 ± 2.5 4.21 ± 0.15 0.9928 4.8 96.5 ± 1.8 5.62 ± 0.12 0.9988 2.3
14-EC-RO 15 133.1 ± 2.4 3.25 ± 0.11 0.9932 4.6 134.0 ± 1.7 3.92 ± 0.08 0.9989 2.2
25 106.2 ± 2.6 3.68 ± 0.13 0.9925 4.9 107.0 ± 1.9 4.55 ± 0.11 0.9987 2.4
35 91.6 ± 2.8 4.02 ± 0.15 0.9918 5.1 92.4 ± 2.0 5.28 ± 0.13 0.9985 2.6
10-HSA-DOA 15 201.0 ± 2.6 3.55 ± 0.13 0.9948 4.8 202.1 ± 1.6 4.35 ± 0.08 0.9995 2.0
25 153.6 ± 2.8 3.98 ± 0.15 0.9940 5.0 154.7 ± 1.8 5.02 ± 0.10 0.9993 2.2
35 139.8 ± 3.0 4.45 ± 0.16 0.9935 5.3 140.8 ± 1.9 5.89 ± 0.11 0.9991 2.5
14-EC-DOA 15 157.3 ± 2.5 3.38 ± 0.12 0.9938 4.7 158.4 ± 1.7 4.05 ± 0.09 0.9991 2.1
25 132.8 ± 2.7 3.72 ± 0.14 0.9930 5.0 133.8 ± 1.9 4.62 ± 0.11 0.9989 2.4
35 111.2 ± 2.9 4.18 ± 0.15 0.9922 5.2 112.2 ± 2.0 5.45 ± 0.12 0.9986 2.7
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2. Weber–Morris Intraparticle Diffusion Parameters for the Adsorption of DCE on Oleogel Adsorbents .

    Rapid stage (2–30 min)
 Slow stage (60–120 min)
Oleogel adsorbents T (°C) kid (mg g–1 min–0.5) C R2 RMSE kid (mg g–1 min–0.5) C R2 RMSE
10-HSA-RO 15 9.88 ± 0.28 2.10 ± 0.32 0.9912 3.42 1.54 ± 0.09 75.30 ± 1.85 0.9658 4.15
25 11.20 ± 0.30 2.55 ± 0.35 0.9924 3.53 1.86 ± 0.10 77.70 ± 1.90 0.9676 4.22
35 12.88 ± 0.32 3.00 ± 0.38 0.9929 3.59 2.13 ± 0.11 78.95 ± 1.95 0.9688 4.28
14-EC-RO 15 7.98 ± 0.22 1.80 ± 0.25 0.9876 3.15 1.30 ± 0.08 58.50 ± 1.70 0.9568 3.98
25 8.85 ± 0.24 2.02 ± 0.28 0.9885 3.22 1.51 ± 0.09 60.80 ± 1.75 0.9585 4.06
35 10.18 ± 0.26 2.35 ± 0.30 0.9895 3.30 1.74 ± 0.10 62.60 ± 1.72 0.9606 4.12
10-HSA-DOA 15 10.88 ± 0.30 2.72 ± 0.38 0.9926 3.75 1.80 ± 0.10 96.90 ± 2.12 0.9685 4.52
25 13.36 ± 0.33 2.90 ± 0.40 0.9934 3.80 2.18 ± 0.11 98.50 ± 2.08 0.9698 4.58
35 15.05 ± 0.36 3.55 ± 0.42 0.9942 3.88 2.50 ± 0.12 99.80 ± 2.15 0.9716 4.66
14-EC-DOA 15 9.55 ± 0.26 2.12 ± 0.30 0.9898 3.40 1.47 ± 0.09 72.70 ± 1.80 0.9620 4.28
25 10.73 ± 0.28 2.25 ± 0.32 0.9906 3.45 1.70 ± 0.10 74.20 ± 1.95 0.9628 4.35
35 12.50 ± 0.31 2.66 ± 0.36 0.9918 3.52 1.97 ± 0.11 75.90 ± 1.90 0.9645 4.42
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a

All parameters were obtained by nonlinear fitting.

Although the R2 values for both the pseudo-first-order and pseudo-second-order models were close to unity (>0.991 for all samples), the pseudo-second-order model consistently yielded higher R2 values (≥0.9985) and substantially lower RMSE values (1.9–2.7) compared with the pseudo-first-order model (R2 = 0.9918–0.9948; RMSE = 4.2–5.3). This combined statistical evidencehigh R2 indicating excellent variance explanation, and low RMSE confirming minimal prediction errorfirmly demonstrates that the pseudo-second-order model is far superior in describing the intrinsic adsorption kinetics of DCE onto Oleogel adsorbents.

A noteworthy phenomenon is that both models yielded reasonably good R2 values (>0.99), which deserves deeper mechanistic interpretation rather than a mere statistical comparison. From a phenomenological perspective, the pseudo-first-order model is generally formulated based on diffusion-controlled mass transfer from the bulk phase to the adsorbent surface, making it more suitable for describing reversible and nonspecific physical adsorption. In contrast, the pseudo-second-order model is rooted in chemisorption or valence-force-driven adsorption, where the rate-determining step involves electron sharing or exchange between the adsorbent surface sites and the adsorbate molecules. The consistently superior performance of the pseudo-second-order model in this work strongly indicates that DCE adsorption is not a purely physical dissolution process but is accompanied by significant intermolecular interactions, which is fully corroborated by the XPS-detectable upshift in Cl 2p binding energy (attributed to hydrogen bonding and dipole–dipole interactions) and the FTIR-identified involvement of polar functional groups (e.g., carbonyl and hydroxyl).

Nevertheless, the fact that the pseudo-first-order model also achieved R2 > 0.99 should not be simply overlooked. It precisely reveals that the adsorption system follows a sequential kinetic regime. Specifically, during the initial stage (corresponding to the first rapid stage of the Weber–Morris model), DCE molecules primarily overcome gas-film and liquid-film resistances and rapidly diffuse to the external surface and shallow regions of the Oleogel. This stage is predominantly driven by concentration-gradient-dependent physical diffusion, thus exhibiting pseudo-first-order characteristics. As the surface active sites (especially polar ester and hydroxyl groups) become progressively saturated, the adsorption enters the later slow stage (the second gradual stage of the Weber–Morris model). At this point, DCE molecules must overcome steric hindrance to penetrate the deep three-dimensional network and engage in specific binding with internally exposed functional groups. Consequently, the occupation rate of surface active sites becomes the rate-controlling factor, giving rise to pronounced pseudo-second-order behavior.

For conventional carbonaceous adsorbents, the pseudo-first-order model typically dominates, reflecting their specific-surface-area-governed physisorption mechanism. For instance, Yang et al. (2018) and Lee et al. (2023) reported that toluene and benzene adsorption on various activated carbons and biochars were better described by the pseudo-first-order model. , Some exceptions exist where the pseudo-second-order model shows better applicability, typically when chemisorption or specific surface interactions are involved.

In contrast, the Oleogel adsorbents developed in this work, although achieving adsorption capacities comparable to those of high-performance carbon materials, exhibit a fundamentally different driving forceshifting from “pure physical pore-filling” to “synergistic enhancement of physical dissolution and specific intermolecular forces.” Therefore, the observation that both models fit reasonably well, with the pseudo-second-order model being distinctly superior, convincingly confirms that when oleogels, as novel “soft matter” adsorbents, enrich VOCs in their liquid oil phase, their performance relies not only on partition effects but also on “chemical anchoring” provided by polar groups.

Dynamic breakthrough experiments were conducted at three temperatures (15, 25, and 35 °C) for four representative Oleogel adsorbents (10-HSA-RO, 14-EC-RO, 10-HSA-DOA, and 14-EC-DOA) to investigate the temperature dependence of DCE adsorption behavior. The saturated DCE adsorption capacity (QS) are summarized in Table .

3. Saturated DCE Adsorption Capacity (QS) of DCE on Oleogel Adsorbents at Different Temperatures.

Oleogel adsorbents 15 °C QS (mg g–1) 25 °C QS (mg g–1) 35 °C QS (mg g–1)
10-HSA-RO 154.4 125.8 96.3
14-EC-RO 133.8 105.2 92.2
10-HSA-DOA 201.9 154.4 140.5
14-EC-DOA 158.1 133.5 111.9
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In addition to QS, the kinetic rate constants also showed clear temperature dependence. As shown in Table , the pseudo-second-order rate constant (k 2) of all formulations increased significantly with rising temperature. For 10-HSA-DOA, k 2 rose from 4.35 × 10–4 g mg–1 min–1 at 15 °C to 5.89 × 10–4 g mg–1 min–1 at 35 °C, an increase of approximately 35.4% over a 20 °C temperature range. This trend can be attributed to intensified molecular thermal motion and reduced viscosity of the oil phase at higher temperatures, which jointly reduce the mass transfer resistance at the gas–gel interface and inside the three-dimensional network. This phenomenon has also been observed by Dumont et al. (2016) in their study on VOC absorption using PDMS/water mixtures. Similarly, both the rapid-stage and slow-stage intraparticle diffusion rate constants (k id) increased with temperature (Table ), further confirming the promotion effect of temperature on mass transfer.

As clearly shown in Table , the QS values of all four formulations decreased monotonically with increasing temperature. Taking the optimal sample 10-HSA-DOA as an example, QS decreased from 201.9 mg g–1 at 15 °C to 140.5 mg g–1 at 35 °C, corresponding to a reduction of approximately 30.4%. The average adsorption capacity of the four samples dropped from 162.05 mg g–1 at 15 °C to 110.23 mg g–1 at 35 °C, with an overall decline of about 32.0%. This trend is consistent with the fundamental thermodynamic expectation of an exothermic adsorption-dissolution process: in accordance with Le Chatelier’s principle, elevated temperature shifts the gas–liquid partition equilibrium toward the desorption direction, thereby weakening the retention of DCE molecules in the Oleogel matrix.

From an engineering application perspective, however, this temperature sensitivity is well within an acceptable range. Within the typical industrial exhaust temperature interval of 15–35 °C, all samples maintained an adsorption capacity above 90 mg g–1 at 35 °C, with no catastrophic capacity loss observed (maximum reduction < 35% over a 20 °C rise). The overall average QS of the four formulations across the three temperatures was 136.08 mg g–1; the value at 15 °C was 19.08% higher than this average, while that at 35 °C was 18.99% lower, yielding a maximum deviation of less than 20%.

3.4. Physical Characteristics

3.4.1. OBC

Oil retention is a key parameter for evaluating the macrostructural stability of plastic and solid fats. In oleogels, liquid oil exists in two physically distinct states: unbound oil (i.e., physically entrapped oil) and strongly bound oil. Strongly bound oil refers to liquid oil adsorbed onto gelator particle surfaces or immobilized within the structural matrix of the gel network. As thermally reversible materials, oleogels may gradually release strongly bound oil during prolonged storage or under temperature fluctuations. Consequently, oil retention directly reflects the effectiveness of the gel network in immobilizing liquid oils. Centrifugation testing showed that only minimal oil exudation occurred across all samples, accounting for approximately 2%–5% of the total gel mass. Specifically, the oil retention rates were determined to be 95 ± 2% for HSA-RO, 96 ± 3% for HSA-DOA, 98 ± 2% for EC-RO, and 96 ± 2% for EC-DOA. No observable phase separation or sedimentation was detected after the test, confirming the satisfactory macroscopic stability of the oleogels. Blake et al. (2014) demonstrated that OBC values approaching 90% can be achieved in plant wax-based oleogels with optimal crystal morphology and spatial distribution, highlighting the critical role of three-dimensional network architecture in effective oil entrapment. Notably, the EC-based oleogels exhibited lower oil loss than their HSA-based counterparts, indicating that EC forms a more robust crystalline network with a superior ability to immobilize RO and DOA. Davidovich-Pinhas et al. (2015) demonstrated that ethyl cellulose forms a strong, network-like structure in oil, which contributes to the overall physical stability of the Oleogel.

3.4.2. Rheological Properties

Rheological analysis is a fundamental method for characterizing gel network integrity and mechanical response. The storage modulus (G′) represents elastic energy storage, and the loss modulus (G″) reflects viscous energy dissipation. Frequency sweep measurements (Figure ) showed that over the tested frequency range of 0.1–100 Hz, G′ consistently exceeded G″ for all oleogels, indicating dominant solid-like elastic behavior and confirming the formation of physically cross-linked networks governed by noncovalent interactions. This observation is consistent with previous investigations. The minimal variation of both the moduli with increasing frequency further indicated structural robustness and well-developed three-dimensional network architectures. Comparison of G′ values (∼105 Pa) at 1 Hz reveals that all samples exhibit similarly high resistance to deformation. ,

6.

6

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Rheological properties under frequency scanning of different component oleogels. (a) HSA-RO; (b) EC-RO; (c) HSA-DOA; (d) EC-DOA. (G′: storage modulus; G″: loss modulus).

3.4.3. Contact Angle

Figure shows the water contact angle test results of four Oleogel samples, which is used to evaluate the surface wettability of the materials. Adsorption performance under humid conditions is influenced not only by the intrinsic properties of adsorbents but also by competitive adsorption between water vapor and VOCs. As shown in Figure , the contact angles of the oleogels were 79.4° for HSA-RO, 85.9° for HSA-DOA, 81.7° for EC-RO, and 95.6° for EC-DOA. Overall, the oleogels exhibited comparable surface wettability, with contact angles close to 90°. The contact angle of samples prepared from EC and DOA reached 95.6°, suggesting potential for use in high-humidity environments. Li et al. (2020) modified activated carbon with PDMS, increasing its water contact angle from 78° to 138° and remarkably enhancing its dynamic VOC adsorption capacity under high-humidity exhaust conditions.

7.

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Contact angle images of the oleogels. (a) HSA-RO; (b) EC-RO; (c) HSA-DOA; (d) EC-DOA.

3.5. Thermal Stability of the Oleogels

The weight loss behavior of the samples (Figure ) was evaluated by TGA over the temperature range of 30 °C–600 °C. No significant mass loss was observed for any of the four oleogels between 30 and 150 °C, indicating good thermal stability within this range.

8.

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TGA curves of the oleogels.

Analysis of the differential thermogravimetric curves revealed that the RO-based gels exhibited a maximum degradation temperature of approximately 350 °C, which was significantly higher than that of the DOA-based gels (∼200 °C). Also, the onset weight loss temperature of RO-based gels was higher (∼230 °C). This discrepancy is dominated by the intrinsic thermal properties of the base oils. Rapeseed oil (RO) is mainly composed of long-chain triglycerides with high molecular weight and high boiling point, endowing the corresponding oleogels with higher onset and peak degradation temperatures. In contrast, dioctyl adipate (DOA) is a small-molecule ester with a relatively low boiling point and thermal decomposition temperature, resulting in poorer thermal stability of DOA-based oleogels. Such thermal property differences are consistent with the reported thermal-physical trends of ester compounds described by Lamprea-Pineda et al. (2024).

In addition, the EC-based gels displayed slightly higher onset and peak degradation temperatures compared with the HSA-based gels. This difference can be attributed to the auxiliary regulatory effect of gelators. Ethyl cellulose (EC) is a high-molecular-weight polymer with inherently better thermal stability than the small-molecule gelator 12-HSA. Meanwhile, the dense network structure formed by EC can restrict the volatilization of oil molecules to a certain extent, thus further elevating the thermal degradation temperature of the oleogels. Such network-barrier confinement effects have also been described by O’Sullivan et al. (2016) for polymeric Oleogel systems.

Overall, these results indicate that the base oil is the primary factor determining thermal stability, whereas the gelator type mainly influences the degradation temperature.

3.6. XRD

As shown in Figure a and c, the HSA-based gels prepared with RO and DOA exhibited nearly identical diffraction patterns. The peak positions, intensities, and full width at half-maximum values were essentially the same, indicating highly similar subcrystallite size, lattice parameters, and long-range ordering. Similarly, the EC-based gels displayed consistent XRD patterns regardless of the base oil used, confirming that the base oil does not alter the fundamental self-assembled nanostructure or molecular packing motif of either gelator. This observation is consistent with the findings of previous study, which reported that lipid composition has a minimal influence on the crystalline architecture of β-sitosterol−γ-glucan hybrid oleogels.

9.

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X-ray diffraction patterns of the oleogels. (a) HSA-RO; (b) EC-RO; (c) HSA-DOA; (d) EC-DOA.

All Oleogel samples exhibited a prominent diffraction peak at d spacings of 4.5–4.6 Å (2θ ∼ 18.7°–20.1°), characteristic of the β-polymorph. In addition, the HSA-based gels showed a pronounced peak at 3.8–4.0 Å (2θ ∼ 22.0°–23.2°), attributed to the β′-polymorph. Liu et al. (2020) also detected characteristic XRD peaks at 0.415 and 0.374 nm in sorghum wax-in-fish oil oleogels, which were ascribed to a hexagonal symmetry and β′-crystals. This orthorhombic subcell structure has a small crystallite size and high surface area. The presence of β′-crystals promoted the formation of an interpenetrating network capable of entrapping large volumes of liquid oils, which accounts for the low critical gelation concentration observed for the HSA-based oleogels. Overall, XRD analysis indicates that the gelator type is the decisive factor governing crystal morphology development. The β′-polymorph is only detected in HSA-based oleogels, which correspond to better adsorption performance than EC-based oleogels.

3.7. FTIR Spectroscopy

The FTIR spectra shown in Figure exhibit highly consistent spectral profiles across all samples, despite variations in peak intensities, indicating similar surface chemical characteristics. Various functional groups were identified, including aliphatic C–H stretching vibrations at 2924 and 2853 cm–1, carbonyl (CO) stretching at 1746 cm–1, CH2 bending at 1464 cm–1, CH3 symmetric deformation at 1377 cm–1, C–O–H stretching at 1164 cm–1, and C–O–C stretching at 1093 cm–1. These functional groups are mechanistically relevant for VOC adsorption as they enable specific interactions such as acid–base interactions and electron donor–acceptor complexation.

10.

10

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FTIR spectra of the oleogels. (a) HSA-RO; (b) EC-RO; (c) HSA-DOA; (d) EC-DOA.

Compared with most conventional porous adsorbents primarily rely on a high specific surface area to achieve physisorption, necessitating additional surface functionalization, such as heteroatom doping, chemical impregnation, calcination, or steam activation, , to enhance chemisorptive affinity or selectivity, the Oleogel exhibits intrinsic chemical adsorption capability arising directly from its native surface chemistry. In addition, a broad and weak absorption band centered at ∼3300 cm–1 (3150–3500 cm–1) was consistently observed for all samples and was attributed to O–H stretching vibrations associated with intermolecular hydrogen bonding, providing spectroscopic evidence for cohesive network formation driven by hydrogen bonding. This hydrogen-bonding contribution to network integrity is consistent with the findings of Gravelle et al. (2016), who demonstrated that intermolecular hydrogen bonds play a critical role in the formation and mechanical strength of EC-based Oleogel networks, as revealed by rheological analysis and NMR relaxation measurements.

3.8. X-ray Photoelectron Spectroscopy Analysis

As shown in Table S2, The high-resolution C 1s spectra of all samples were dominated by a characteristic peak centered at ∼284 eV, assigned to aliphatic C–C and C–H moieties that form the structural backbone of both gelators and base oils. The position of this dominant peak remained nearly unchanged after DCE adsorption, indicating that the carbon chemical environment of the Oleogel skeleton was not substantially altered by the adsorption process.

For Cl 2p characterization, the pristine Oleogel samples showed an extremely weak Cl signal close to the instrumental detection limit, which was insufficient to serve as a reliable baseline for direct before–after comparison. To address this limitation, we adopted an alternative and widely accepted XPS analytical strategy: benchmarking the absolute binding energies of the postadsorption samples against well-established standard reference values from XPS databases.

As showen in Figure , all four DCE-adsorbed Oleogel samples exhibited typical Cl 2p spin–orbit splitting doublets. No characteristic peak assignable to inorganic ionic chloride (Cl–, typically 198–199 eV) was detected in any sample, confirming that DCE molecules were immobilized on the Oleogel surface in their intact molecular form, without dechlorination or chemical degradation during adsorption.

11.

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XPS of the oleogels. (a) HSA-RO; (b) EC-RO; (c) HSA-DOA; (d) EC-DOA.

Remarkably, the measured Cl 23/2 binding energies for the four samples fell in the range of 201.2–202.8 eV, which is notably higher than the standard reference value for neutral aliphatic C–Cl bonds (200.0–200.5 eV, as typically reported for polyvinyl chloride and saturated chlorinated alkanes). The magnitude of this positive shift far exceeds the typical instrumental and sample-to-sample testing error (±0.2 eV), and potential charging effects have been ruled out by the stable C 1s reference peak. This result indicates a notable reduction in the valence electron cloud density of Cl atoms in the adsorbed DCE molecules. Given that the C–Cl bond remains intact, this binding energy upshift can be attributed to strong intermolecular polarization interactions: the electron-deficient Cl atoms in DCE interact with electron-rich oxygen-containing groups on the Oleogel surface via noncovalent forces such as hydrogen bonding and dipole–dipole interactions. Similar polarization-induced Cl 2p binding energy shifts have been observed in organochlorine compounds confined in microporous carbon, where the higher-BE shift of Cl 2p was attributed to enhanced C–Cl bond polarization and interfacial dipole effects.

Collectively, the results confirm that DCE adsorption on Oleogel adsorbents involves significant intermolecular interactions (e.g., dipole–dipole and hydrogen bonding) rather than a purely physical process, which is consistent with the kinetic modeling results and FTIR analyses.

4. Conclusions

This study reports the first application of oleogels as adsorbents for 1,2-dichloroethane (DCE) removal, fabricated via self-assembly and cross-linking of HSA/EC gelators with RO/DOA base oils. The 10 wt % HSA-DOA formulation achieved a high DCE adsorption capacity of 154.4 mg g–1 at 25 °C, and reached 201.9 mg g–1 at 15 °C, comparable to advanced conventional adsorbents.

The adsorption performance of the Oleogel adsorbents is inherently linked to their network structure and interfacial interactions. Combined with XPS, FTIR and the kinetic fitting results, it is confirmed that the adsorption process of DCE onto the Oleogel adsorbents is not a simple physical coverage or dissolution process. Instead, strong intermolecular interactions exert a synergistic enhancement effect on adsorption. And the rate-limiting step of the overall adsorption process is jointly controlled by boundary layer diffusion and intraparticle diffusion. XRD analysis indicates that the β′-polymorph is only detected in HSA-based oleogels, which corresponds to better adsorption performance than EC-based oleogels. Structural factors further regulate performance: base oil type (DOA > RO) dominates due to stronger DCE affinity, while gelator concentration and typeHSA’s granular, high-specific-surface-area morphologyexert secondary effects.

Oleogels exhibit robust practical applicability, with oil-binding capacity > 95%, favorable thermal stability below 150 °C, high resistance to deformation, and EC-DOA’s contact angle of 95.6° enabling use in high-humidity environments. Their oil-based matrix enhances affinity for polar VOCs without postmodification, offering a simple, low-cost solution for small- and medium-sized enterprises. The DOA-based oleogels demonstrate potential for future expansion of application scopea customized service specifically targeting VOC removal. Moreover, future work will focus on industrial scale-up preparation (e.g., parametric optimization and model fitting), systematically evaluating the regeneration performance, and expanding the applicability to multicomponent halogenated VOC systems.

Supplementary Material

ao6c05671_si_001.xlsx (11.1KB, xlsx)
ao6c05671_si_002.xlsx (261.9KB, xlsx)

Acknowledgments

This study was supported by the Key Laboratory of Technology and Equipment Engineering for Volatile Organic Pollutants Control of Gansu Province (Government-sponsored research 20170443).

The Supporting Information is available free of charge at https://pubs.acs.org/doi/10.1021/acsomega.6c05671.

  • Table S1: saturated adsorption capacities (QS) of various oleogels at 25 °C (XLSX)

  • Table S2: XPS analysis data of Oleogel adsorbents before DCE adsorption (XLSX)

The authors declare no competing financial interest.

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Supplementary Materials

ao6c05671_si_001.xlsx (11.1KB, xlsx)
ao6c05671_si_002.xlsx (261.9KB, xlsx)

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