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Review

Ozonation of Bitumen: Characteristics, Characterization, and Applications

by
Muhammad Hashami
1,2,
Yerdos Ongarbayev
1,3,*,
Dinmukhamed Abdikhan
1,3,
Erzhan Akkazin
3,4 and
Nuripa Nessipbayeva
4
1
Faculty of Chemistry and Chemical Technology, Al-Farabi Kazakh National University, 71, Al-Farabi Ave., Almaty 050040, Kazakhstan
2
Department of Chemistry, Faculty of Education, Institute of Higher Education Mirwais Khan Nika Zabul, Qalat 40xx, Afghanistan
3
Laboratory of Petrochemical Processes, Institute of Combustion Problems, 172, Bogenbai Batyr Str., Almaty 050012, Kazakhstan
4
Faculty of Natural Science and Geography, Abay Kazakh National Pedagogical University, 13, Dostyk Ave., Almaty 050010, Kazakhstan
*
Author to whom correspondence should be addressed.
Processes 2025, 13(3), 708; https://doi.org/10.3390/pr13030708
Submission received: 22 January 2025 / Revised: 24 February 2025 / Accepted: 26 February 2025 / Published: 28 February 2025
(This article belongs to the Section Chemical Processes and Systems)
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Abstract

Bitumen is a significant component used in road construction. Traditionally, it is subjected to air-blowing processes at high temperatures (220–260 °C) to enhance its viscosity, rigidity, and oxidation characteristics. However, such approaches are often energy-consuming and result in extensive environmental issues, so more efficient and environmentally friendly techniques are needed. This review evaluates the emerging novel pathways for treating bitumen, with a particular focus on the role of ozone in the air-blowing process. By examining present studies, this review emphasizes the incorporation of ozone as an oxidizing agent to address the current challenges of long process times and high temperatures in the activation process and comprehensively demonstrates the enhancement of bitumen’s mechanical properties through ozone treatment. It also highlights the minimization of toxic emissions this achieves, especially highlighting the crucial role of ozone in improving the characteristics of bitumen in relation to the global trend toward making civil construction projects more environmentally friendly. The main aim of this review is to contribute to the development of new ideas in the field of bitumen modification and to encourage further advances in road construction from the standpoint of improving efficiency and minimizing environmental impacts.

1. Introduction

Bitumen is a critically important material in road construction due to its ability to bind aggregates and ensure the durability of road surfaces. Among various treatment methods, air treatment is widely used to improve bitumen’s performance by increasing its viscosity, stiffness, and oxidation resistance, which is particularly critical for construction applications [1]. The air-blowing process involves heating bitumen to 220–260 °C and introducing air under controlled conditions, resulting in molecular changes such as polymerization and hydrocarbon oxidation. Additives such as polyphosphoric acid (PPA) grafted to silica and polyfunctional carboxylic acid have been used in air-blowing treatment, improving rheological properties such as the softening point and penetration index at low temperatures and within reduced times [2].
Recent studies have suggested that sustainability practices should become mandatory elements for road construction tasks including maintenance operations. For instance, life cycle assessments (LCAs) serve as an essential tool for evaluating environmental impacts in detailed research about decarbonization strategies [3]. This intensifies our need to find the best materials while developing better processing techniques for enhancing performance and minimizing road infrastructure emissions. Durability is one of the primary demands for construction materials which heavily depends on aging attributes, because they directly influence overall performance. Feng et al. (2016) reported that UV radiation causes changes in bitumen’s molecular structures that modify its rheological properties [4,5]. Scientific research on these natural processes enables developers to create bitumen materials that offer superior environmental resistance. Modification of materials by using difference additives and oxidizing agents and treatment methods play crucial roles in enhancing the performance of road construction materials.
Many studies have focused on air-blowing treatment using various oxidizers and additives to improve desired bitumen characteristics and reduce the release of environ-mental pollutants. Introducing ozone into the air-blowing process is an alternative approach for bitumen treatment, which addresses both environmental and performance concerns. The role of ozone in wastewater treatment has been studied mainly regarding its importance for breaking down persistent organic pollutants and lowering the toxicity of industrial effluent. Reductions of up to 70% in chemical oxygen demand (COD) and 60% in total organic carbon (TOC) make it an effective pre-treatment method for wastewater [6]. Similarly, in crude oil desulfurization, a reduction in sulfur content of up to 90% was reported upon applying ozone combined with metal chloride catalysts [7].
Ozone is an alternative oxidizer offering a more efficient and environmentally friendly solution, increasing reaction efficiency, reducing emissions, improving the mechanical properties of bitumen, and providing a sustainable alternative to traditional air-blowing methods. Air-blowing treatment conducted with O3 gas requires a proper experimental setup, as presented in Figure 1, to cope with the process parameters that are crucial to ensure the treatment quality. This process emits approximately 1.2–1.5 kg of CO2 per ton of bitumen, along with polycyclic aromatic hydrocarbons (PAHs) at concentrations of up to 0.8 mg/m3, depending on the production conditions, which poses a critical challenge for industries [8]. The energy consumption and release of hazardous byproducts such as PAHs in the air-blowing process lead to significant environmental and health risks [8,9]. This innovation is in line with global sustainable development efforts, ensuring the development of a robust and environmentally friendly road infrastructure.
Ozone is a highly reactive oxidation agent that can significantly improve the efficiency of the air-blowing process; it has been found that ozone enhances reaction rates from 20 to 30%, reducing the process time by nearly 25% compared to traditional air-blowing treatments [10]. Ozone-treated bitumen shows thermal stability and lower susceptibility to aging, with a 15% increase in oxidation resistance compared to conventionally treated bitumen. Shariati et al. reported an up to 40% reduction in PAH emissions when ozone was used as an oxidizing agent [2]. Ozone improves the mechanical properties of bitumen. For instance, ozone treatment (5–7 °C) additionally increases the softening point and reduces the penetration index by 20% compared to conventional methods, indicating improved stiffness and durability [11,12]. In addition, it promotes uniform molecular changes resulting in a 10% increase in bitumen elasticity [13]. These properties are particularly advantageous for road construction under high loads and temperatures. From an economic point of view, the air-blowing process using ozone reduces production costs by minimizing energy consumption and reducing waste treatment costs. Hajikarimi et al. reported a reduction in air-blowing costs (15–20%) when ozone is introduced [10,14].
This review highlights methodologies, findings, and limitations regarding the air-blowing treatment of bitumen using ozone gas by analyzing previous studies. It pays especial attention to studies such as those by Fernandes et al., Hussein, and Hamdoon for their innovative oxidation treatment and detailed reports on rheological modifications [15,16]. This review considers conflicting findings [12,16], such as variations in the rheological properties, critically analyzed across studies, to provide a balanced perspective. Combining the experimental findings and review-based insights allows for a comprehensive discussion of ozone air-blowing processes in bitumen treatment.

2. Materials and Methods

Bitumen production involves the distillation of crude oil, where the lighter fractions are separated, leaving behind the heavier components that form bitumen. Modifying bitumen through air-blowing and the use of additives such as silica, PPA, polymers, and ozone improves its performance. This review follows a systematic approach to provide a comprehensive, critical, and accurate analysis of the literature on the air-blowing treatment of bitumen using ozone as an oxidant, which includes a structured selection, analysis, and synthesis of relevant studies to offer valuable insights into the topic. The literature search was conducted using major academic databases including Scopus (www.scopus.com), Web of Science (www.webofscience.com), and ScienceDirect (www.sciencedirect.com) to ensure the inclusion of high-quality peer-reviewed research. Publications up to 2024 covered recent developments and also included basic research that provided historical context. Bitumen treatment, ozone oxidation, air-blowing process, bitumen modification, oxidative aging, (AND, OR) key words, and Boolean operators were used to refine the search and target studies mostly related to both ozone treatment and air-blowing processes. Inclusion criteria were established to focus on studies that directly investigated bitumen oxidation through ozone or related air-blowing processes.
As shown in Figure 2, the literature searches prioritized articles published between 2000 and 2024 that discuss ozone and air-blowing processes, specifically focusing on the analysis of rheological properties, mechanisms, and the environmental impact of treated bitumen. In addition, a theme approach was adopted to organize the literature. Studies were divided into several major themes such as the mechanisms of ozone oxidation [17,18], the rheological properties after treatment [19,20], the environmental impact and effluent management [15,21], and catalytic and additive-enhanced air-blowing [22,23].

3. Bitumen

Bitumen is a complex hydrocarbon material derived from crude oil refining or found naturally in deposits. Bitumen mainly consists of high-molecular-weight aromatic and aliphatic hydrocarbons including asphaltenes, resins, and saturated alkanes [24]. The components of bitumen are presented in Table 1; they highly depend on how the crude oil is processed and from where the oil originates. Typically, it comprises asphaltenes (5–25%), which are high-molecular-weight polyaromatic compounds responsible for the stiffness and viscosity of bitumen; resins (20–40%), which are intermediate-molecular-weight compounds that provide adhesion and contribute to bitumen’s viscoelastic properties; saturates (25–45%), which are low-molecular-weight, aliphatic hydrocarbons that enhance the flow characteristics; and aromatics (20–40%), which are medium-molecular-weight cyclic compounds that influence ductility and viscosity. The rheological and mechanical characteristics of bitumen depend on its components, which influence its operational performance in various uses [25].
Bitumen is scientifically classified according to its natural origin point and method of consistency formation alongside modification approaches. Natural bitumen material, known as “migrabitumen”, emerges from petroleum detritus and exists within oil emulsions located within deposits and mineral sands [26]. Refined bitumen is produced by the distillation of crude oil and is commonly used in road construction and industrial applications. Penetration-grade bitumen is classified into grades such as 30/40, 60/70, and 80/100, based on the penetration value at 25 °C, where lower values indicate higher hardnesses. The specifications of performance-grade (PG) bitumen are indicated through PG 64–22 parameters, which describe the resistance toward temperatures between −22 °C and 64 °C during testing [27]. The properties of modified bitumen are improved through the combination of additives such as polymers, crumb rubber, and bio-oils. Polymer-modified bitumen (PMB) creates materials with increased elasticity as well as enhanced resistance against deformation [28]. The addition of CRMB to bitumen improves both the flexibility and useful life span of pavement [29]. The application of bio-oil to modify bitumen achieves two environmental benefits: enhanced sustainability and reduced environmental impact [30].
The construction industry uses bitumen for roads because it offers superior combination properties, outstanding durability, and effective resistance to weathering. The binder function of asphalt concrete mixtures enables bitumen to provide flexibility alongside load-bearing capacity; thus, it finds applications in flexible and semi-rigid pavement structures. Improvements in road sealing and skid resistance come from applying two bituminous surface treatments known as chip sealing and slurry sealing. The production temperatures for warm mix asphalt (WMA) and cold mix asphalt (CMA) differ; WMA has reduced energy utilization and greenhouse gas emissions through lower temperatures, but CMA works well in remote low-traffic locations because the asphalt is prepared under natural environmental conditions [24]. High-performance roads benefit from modified bitumen that includes PMB for better durability and rutting resistance as well as CRMB for enhanced flexibility and reduced road noise, and bio-modified bitumen provides eco-friendly construction possibilities [30]. The modern road construction sector heavily depends on bitumen because of its superior adhesive qualities along with its flexibility features. The operational performance of a modified bitumen composition can be controlled, while strategic adjustments strengthen its durability and boost its environmental sustainability and mechanical strength properties. In the future, developers of bitumen technology will seek to achieve longer-lasting pavements through transformative modifications alongside the sourcing of alternative materials for environmental benefits.

3.1. Bitumen Treatment

Treating bitumen involves modifying its characteristics to enhance its performance and durability for various applications such as road construction and roofing. Many techniques, including oxidation, polymer modification, and the addition of additives such as polyphosphoric acid, as shown in Table 2, have been studied for modifying and enhancing the performance of bitumen in many applications. These treatments increase resistance to aging, temperature fluctuations, and mechanical stress, providing durability and improved performances for a variety of applications. Bitumen is a versatile material with important properties that make it indispensable in construction. In particular, it has excellent adhesion, providing a strong bond to aggregates in road construction [31].
New cleaning and modification methods such as foam cleaning, O3, O3/H2O2, ultraviolet light in the C-band (UVC)/O3, UVC/O3/H2O2 [37], ozone, and air-blowing have been studied. These methods are used to improve the quality and properties of different types of bitumen, based on the specific application. This helps to increase its use in paving and improves its hydrophobicity. The thermal stability and hydrophobicity of these materials prevent water ingress, protecting underlying structures and functionality in a variety of environmental conditions [38]. The viscosity values are measured at 60 °C to ensure controlled spreading during application ranging from 100 to 3000 Poise. Stretchability is demonstrated by a plasticity of more than 100 cm at 25 °C, and a flash point above 230 °C ensures safe handling [38]. The penetration index, which measures hardness, ranges from 40 to 70 dmm, and a softening point of 40–60 °C ensures that plasticity is maintained at operating temperatures [39]. However, continuous exposure to UV light and oxygen can lead to aging, affecting durability. Catalysts and advanced treatment methods such as hydrocracking increase the bitumen’s resistance to oxidation, making it more suitable for long-term applications [40]. Ozone, as an oxidizer, has proven significantly effective for water [41,42] and flue gas treatment in industries over many years [43]. Furthermore, ozone has a longer lifetime in comparison to the chemical kinetic time, making it a perfect choice for pre-oxidation bitumen treatment.

3.2. Bitumen Characterization

The bitumen characterization process, especially in the context of aging effects, has been greatly improved by using advanced microscopy techniques, which can provide insight into the structure and characteristics of the material under different conditions [44,45].

3.2.1. Atomic Force Microscopy

Atomic force microscopy (AFM) provides a nanoscale resolution, allowing for analysis of bitumen’s microstructural morphology and the determination of mechanical properties such as roughness, adhesion, and stiffness and revealing changes in surface properties due to aging. The analysis of bitumen through AFM was studied in depth [46]. Figure 3 depicts AFM bitumen images that show “bee structures” that are linked to wax crystallization along with asphaltene-rich domains [46]. The structures seen in Figure 3a demonstrate a well-defined phase-separated microstructure because they stand out prominently. The decreased clarity of the structures in Figure 3b indicates morphological degradation from oxidation effects. During oxidation, bitumen molecules experience changes in their chemical bond interactions that make them more polar and lead to phase separation [47]. The literature shows that oxidation makes bee structures less distinguishable through asphaltene aggregation that weakens the elasticity of the bitumen matrix [48]. The image in Figure 3b shows reduced contrast between areas, which indicates a developing lack of microscopic detail typical of oxidative aging.
Bitumen aging levels can be evaluated using surface roughness measurements because the oxidation process forms rigid brittle structures [49]. Figure 3c shows an increased surface roughness distribution during the transition from Figure 3a [50]. The nanostructures observed in Figure 3c are thought to form through asphaltene flocculation and oxidation-induced polymerization, which produce a heterogeneous surface. Steyn (2011) established that aged bitumen develops rough surfaces because the disappearance of maltene phases exposes more asphaltene-rich domains [51].
The observed granular formations in Figure 3c support the process of oxidative cross-linking reactions that cause bitumen hardening. Atomic force microscopy analysis demonstrates that oxidative processes exacerbate phase separation, through which asphaltene molecules become concentrated as clusters [52]. The microphase distribution analysis shows that oxidative processes have driven a reorganization of small structures, which is particularly visible in Figure 3b, because asphaltene precipitation becomes more pronounced. The redistribution process serves as evidence for oxidative degradation because it transforms the bitumen matrix into networks of rigid molecules [47]. Data from atomic force microscopy are critical evidence regarding morphological changes that occur in bitumen because of oxidation. These changes become evident through the disappearance of bee structures in combination with the rising surface roughness and phase separation, which supports previously documented scientific data [46,51]. Nanoscale changes in bitumen structures result in macroscopic effects such as pavement brittleness and reduced flexibility, which affect pavement operation. Further quantitative AFM analysis, such as adhesion force mapping and phase imaging, could provide additional insights into oxidation mechanisms.

3.2.2. Environmental Scanning Electron Microscopy

Environmental scanning electron microscopy (ESEM) offers high-resolution imaging in a relatively unaltered state by allowing the material to remain hydrated. ESEM provides valuable insights into the microstructural changes in bitumen due to oxidation, allowing for a detailed analysis of phase separation, surface roughness, and porosity variations. The images in Figure 4 showed unique morphological changes. The surface in Figure 4a showed a relatively smooth appearance, indicating an unaged or minimally aged bitumen sample with well-distributed microstructures. The surface roughness increased in Figure 4b,c due to the development of more pronounced voids and micro-cracks, which was typical for oxidation-induced embrittlement [53]. Studies have suggested that oxidation reduces the asphaltene concentration and maltene level, leading to asphaltene accumulation alongside higher stiffness and diminished elasticity [44,54]. Lu et al. (2018) obtained ESEM images of aged bitumen that showed phase separation and rigid domains formed through oxidative polymerization. The surface roughness in fresh bitumen reached 150 nm, but oxidation processes could generate surface roughness in excess of 400 nm [55]. The surface images indicate such changes, which match previous research results, particularly those shown in Figure 4d, where stretchy rigid domains take over the surface area.
Mikhailenko et al. (2019) [2] demonstrated that such morphological features correlate with an increase in viscosity (from 1000 Pa·s to over 3000 Pa·s at 60 °C) and a decrease in ductility (from 40 cm to below 20 cm), further confirming oxidation effects [56]. The examination of ESEM images revealed that microvoids and fissures became more prominent, as shown in Figure 4c,d. Oxidative aging generated these voids in the bitumen structure, which impacted its stress recovery capability because they lead to more brittle behavior alongside increased crack susceptibility [54]. Pipintakos et al. (2021) demonstrated that binder oxidation causes both network stiffening and losses in interface adhesive properties at the bitumen–mineral contact point due to hardening [44].
The findings of Zhou et al. (2024) confirm that aged bitumen displays extensive voids formed through phase segregation processes combined with polymer chain breakdown, as observed through ESEM imaging [57]. The void fraction in oxidized bitumen develops from 2% in fresh bitumen to exceed 10% in heavily aged bitumen, which strongly affects mechanical behavior. Moreover, microbial degradation can increase oxidation effects in bitumen due to modifications to the chemical composition and the utilization of potential oxidizing agents in air-blowing treatment [58]. The changing structural characteristics of bitumen molecules stem from microbial activity and the corresponding acceleration of oxidative reactions that transform the overall molecular makeup of bitumen. The observed morphological variations, along with the data from Figure 4c,d, show that bitumen’s durability suffers significantly from oxidative aging through the development of structural inconsistency and an increased risk of fracture. In short, we can state that the ESEM images provide strong evidence of oxidation-induced morphological transformations in bitumen.
All the observed alterations, including a 250 nm increase in surface roughness and an 8% expansion of microvoids, together with increased phase separation, match previous research regarding oxidative aging. Bitumen requires anti-aging additives and rejuvenators to protect its long-term functionality because nanoscale changes lead to macroscopic performance decline. Confocal laser scanning microscopy (CLSM) complements these techniques by allowing the three-dimensional imaging of fluorescent components of bitumen. Bearsley et al. studied different bitumen samples and considered that they had different asphaltene fractions, which in turn produced various morphologies depending on the source of the bitumen [59]. This method provides insights into the distribution of bitumen and maltene, key components influencing the aging process. The changes in fluorescence intensity observed through CLSM highlight chemical transformations during aging, such as the growth of polar molecules [60]. Moreover, it is possible to investigate styrene–butadiene–styrene (SBS) dispersion, compatibility, and network formation using confocal laser scanning microscopy (CLSM) based on the interaction between the polymer and bitumen [61,62,63].

3.2.3. Fourier Transform Infrared Spectroscopy

Fourier transform infrared spectroscopy (FTIR) spectroscopy is another important technique for analyzing functional groups on the surface of the bitumen and can characterize the chemical changes in bitumen due to oxidation and aging. The FTIR spectra presented in Figure 5 indicate the presence of bitumen functional groups and variations in these groups resulting from thermal and UV aging procedures [64]. All the significant peaks in the FTIR spectrum correspond to C-H stretching in aliphatic chains at 2920 cm−1 and 2851 cm−1, carbonyl stretching at 1695 cm−1, and sulfoxide stretching at 1030 cm−1 as well as aromatic C=C stretching at 1605 cm−1. The peak intensities together with the peak shifts demonstrate the oxidation degree and formation of aging-related functional groups. The oxidation process is confirmed by the increased carbonyl index (CI) and sulfoxide index (SI). Moreover, the ratio of carbonyl absorbance to aliphatic C-H absorbance, known as the CI, showed a 50% rise following extensive UV exposure. Additionally, in Zhang et al. (2022)’s study, it was also reported that the sulfoxide index (SI) rose by 30–60% due to aging [65].
The spectral findings for regular straight run bitumen (RSMB), RSMB–ultraviolet (RSMB-UV), and RSMB–thin-film oven test (RSMB-TFOT) indicate different chemical deterioration pathways. The TFOT treatment generated moderate growth in the carbonyl and sulfoxide peak intensity, while UV induced greater peak growth for the same components, which demonstrates advanced oxidative damage. These results correspond to Hofko et al. (2018)’s findings, which demonstrated that bitumen suffers greater chemical alterations under UV aging than thermal aging [66], confirming that the volatilization and oxidative degradation processes caused the reduction in peaks from aliphatic C-H bonds. Additional peaks observed at 1376 cm⁻1 and 1456 cm⁻1 demonstrate CH2 and CH3 deformations, which notably appear in bitumen during aging [67]. Surface oxidation introduces minimal changes to the core hydrocarbon structure because the vibrations at 722 cm⁻1 remain consistent while long-chain alkane signals stay stable.
The results from FTIR analysis support previous research findings about bitumen aging by demonstrating evidence of oxidative deterioration. Measurements of the peak changes demonstrate how bitumen’s oxidation modifies its basic chemical elements, which results in reduced durability along with diminished performance properties. The aging resistance assessment of bituminous materials relies on quantitative spectral indices named the CI and SI, which derive from their spectra. It is essential to conduct these evaluations because they help to extend the lifetime of bitumen in pavements and allow the development of optimized modified binders, which reduce oxidation impacts.

3.3. Ozonation of Bitumen

Treating bitumen through air-blowing using ozone as an oxidizing agent requires a precise experimental setup and controlled conditions to ensure optimum modification. A high-temperature reactor equipped with an ozone generator capable of producing ozone at a concentration of 20–50 ppm is employed. An air compressor equipped with a fixed air-to-ozone ratio is used along with a stainless-steel reactor vessel that can withstand temperatures from 200 °C to 300 °C. Temperature and pressure sensors are integrated for accurate monitoring, and an effluent treatment system removes byproducts such as nitrogen oxides (NOx) and sulfur oxides (SOx). The bitumen feedstock, usually vacuum column residue, is pre-characterized in terms of properties such as penetration, softening point, and viscosity [68]. The experimental process starts by preheating the bitumen to a constant temperature of 240 °C under inert conditions. Ozone gas is then introduced into the reactor through a diffuser for uniform dispersion, while hot air is continuously supplied at a controlled flow rate of 1–5 L/min. Maintaining a 10:1 ratio of air to ozone is critical to achieve uniform oxidation, depending on the desired rheological modifications, with reaction times varying from 2 to 4 h [19,22]. During this process, samples are extracted at 30 min intervals to monitor changes in penetration, viscosity, and softening point, highlighting the importance of optimizing the temperature and air flow to prevent thermal degradation while simultaneously improving oxidation efficiency.
Ozone is a triatomic allotrope of oxygen that has the formula O3, a strong oxidizing agent that is highly reactive and, therefore, can readily cleave chemical bonds. This can occur through electrophilic modes such as interactions with unsaturated hydrocarbon preservatives to produce oxygen-rich products such as carboxylic acids and peroxides [69,70]. For instance, it can easily open up aromatic rings in wastewater, lowering the chemical oxygen demand (COD) and enhancing biodegradability [71]. In the mechanism of bitumen ozonation, this improves polarity, leading to products that are less biotoxic with more potential for industrial applications [72]. In addition, ozone is known to possess antimicrobial activity as well as controlled reactivity, which makes it well-suited to both chemical and biochemical usage [73,74]. According to the investigation of Boczkaj et al. (2017), ozonation enables better removal of biotoxic compounds and higher biodegradability compared to other oxidation processes [75]. In the treatment of wastewater from the production of bitumen, ozonation improved the reduction in COD by 40–50% and that in total organic carbon (TOC) by up to 80%. Moreover, the results showed a great enhancement in biodegradability because the biochemical oxygen demand over 5 days or chemical oxygen demand (BOD5/COD) ratio increased by more than 0.4 in the ozonated samples, demonstrating that ozone is more efficient in degrading other complex hydrocarbons into harmless and environmentally friendly compounds than other emerging advanced oxidation processes (AOPs), stressing its applicability in minimizing adverse environmental effects in industries [75]. In Figure 6, the Criegee mechanism is highlighted, which has a higher selectivity of addition products during indane or indene ozonation at higher conversions. First, 1,3-dipolar cycloaddition occurs to form 1,2,3-trioxolane (Figure 6(1)), which is followed by C–C bond fragmentation to further form a carbonyl-peroxide intermediate (Figure 6(2)). The intramolecular reaction in indene gives rise to ozonides, and further oxidation leads to intermolecular reactions with carbonyls, where dimeric ozonides are formed (Figure 6(3)). This mechanism is consistent with that in other studies carried out on asymmetric olefins and carbonyl-containing reaction mixtures [76].
There are a variety of methods and raw materials for bitumen improvement, demonstrating remarkable differences in reductions in time and temperature, and effectiveness for a wide range of purposes and applications. The ozone treatment of bitumen through oxidation benefits the process by accelerating the material’s development, particularly lowering production temperatures. As observed in Table 3 and Figure 7, the combination of ozone treatment and catalysts such as FeCl2 provides the most efficient bi-product in petroleum-derived asphalt flux through its ability to reduce the processing time by 78%, along with a 57% reduction in temperature, as Table 3 and Figure 7 illustrate.
The rheological characteristics of bitumen show a 30% improvement after employing this method, which results in improved performance and durability. The combinatory treatment for aged bitumen with UV and ozone exposure resulted in a 25% increase in resistance against aging. Ozone proved more effective than other treatments for accelerating bitumen’s modification without causing damage to its structural elements. The ozone oxidation process can replace conventional air-blown methods because it establishes a sustainable environmental solution through efficient energy usage and effective optimization of bitumen’s characteristics.
Through this process, bitumen production is made more economically sustainable and environmentally friendly while simultaneously improving its overall performance. Despite all the above advantages, the control and scalability of the reaction are the main remaining ozone-related problems to address. Current studies lack a comprehensive evaluation of the economic feasibility and long-term environmental impact of ozone processes and their integration into air-blowing systems. Uncontrolled oxidation in bitumen treatment leads to unwanted hardening and embrittlement, which reduces its long-term stability [79]. Exposing bitumen to prolonged ozone oxidation results in a 50% increase in material hardness, which reduces its flexibility and increases its tendency to crack. There are cost-effectiveness limitations of large-scale ozone application due to the high operational expenses that cannot be overcome because of the intensive energy requirements. Industrial-based ozone bitumen treatment consumes 15 to 20 kWh of energy to process one ton of material, resulting in higher operational expenses [80]. The environmental impact of secondary oxidation byproducts is another area that requires further investigation, as their potential contribution to volatile organic compound (VOC) emissions may offset some of the sustainability benefits. VOC emissions during the ozone oxidation of bitumen have been observed to increase by 10–15%, necessitating additional treatment strategies [81].
Optimizing the ozone treatment performance for bitumen remains an unaddressed problem in current research. Additional research is required to enhance catalytic systems for bitumen enhancement through improving the prevention of side reactions and optimizing performance. Current research lacks investigation into how environmental factors affect ozone oxidation efficiency, particularly humidity variations and temperature fluctuations [82]. Future investigations should focus on combining ozone with air-blowing techniques to optimize oxidation efficiency while minimizing emissions, exploring new catalysts for better control and addressing gaps in our understanding of aging mechanisms under realistic conditions. There is a need to develop hybrid treatment approaches that combine ozone oxidation with other chemical modifiers to balance reactivity and stability in bitumen processing, an important aspect that needs to be studied in detail. Additionally, investigating sustainable energy sources for ozone generation could address the high energy demands of this technology. Implementing renewable energy solutions, such as solar or wind-powered ozone generators, could potentially reduce energy consumption by 30% [83]. Upon addressing these challenges, ozone oxidation treatment could become a more viable and environmentally friendly method for enhancing bitumen’s properties while minimizing negative side effects.

4. Conclusions

The addition of ozone to the air-blowing process in bitumen treatment leads to the production of new road construction materials, marking a revolutionary achievement. Ozone treatment offers dual advantages: it enhances the bitumen’s mechanical properties and its oxidation and has a substantially reduced environmental impact compared with conventional methods. Ozone-based bitumen modification enables sustainable development and it reduces both energy usage and radiation intensity while decreasing dangerous compound emissions including polycyclic aromatic hydrocarbons (PAHs). Scientific evidence demonstrates that ozone functions efficiently as a modern chemical oxidizer to transform concentrated oil substances, thus demonstrating suitability in bitumen modification research. The developing technological requirements have made bitumen ozonation gain considerable improvement potential. The combination of ozone treatment solutions with advanced oxidation technologies utilizing either UV-ozone systems or catalyst-assisted ozonation processes would improve reaction efficiency together with selectivity outcomes. Optimizing process parameters may further refine bitumen properties for broader industrial applications.
The use of ozone modification with bitumen will establish itself as critical for sustainable road construction because it both improves asphalt structural performance and reduces carbon emissions. The evaluation of economic benefits in energy savings and operational cost reductions will determine the widespread application potential of this method. Studying bitumen stability after ozone treatment requires deeper investigation together with methods to reduce secondary oxidation products during research. Future studies should focus on optimizing application techniques and evaluating long-term performance, ensuring that ozone-driven solutions transform infrastructure with a reduced carbon footprint.

Author Contributions

Conceptualization, M.H. and Y.O.; methodology, M.H.; software, M.H.; investigation, D.A., E.A. and N.N.; resources, M.H. and Y.O.; writing—original draft preparation, M.H.; writing—review and editing, Y.O.; visualization, M.H.; supervision, Y.O.; project administration, Y.O.; funding acquisition, Y.O. All authors have read and agreed to the published version of the manuscript.

Funding

This research was funded by the Science Committee of the Ministry of Science and Higher Education of the Republic of Kazakhstan, grant No. BR21882255, “Development of new methods for heavy oils, oil residues, oil sands processing, residue oxidation with modifiers to expand bitumen production”.

Data Availability Statement

The data that support the findings of this study are included within the manuscript.

Conflicts of Interest

The authors declare no conflicts of interest.

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Figure 1. A graphitic diagram of the setup for the ozone air-blowing treatment of bitumen.
Figure 1. A graphitic diagram of the setup for the ozone air-blowing treatment of bitumen.
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Figure 2. Number of publications per year (2000–2024) on the oxidation of bitumen via air-blowing and ozone treatment. Data were retrieved from Scopus using the term “bitumen oxidation” in article titles, abstracts, and keywords.
Figure 2. Number of publications per year (2000–2024) on the oxidation of bitumen via air-blowing and ozone treatment. Data were retrieved from Scopus using the term “bitumen oxidation” in article titles, abstracts, and keywords.
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Figure 3. AFM topographical images (all 40 × 40 µm2) of binder AAK-1 as a function of film thickness: (a) 1 µm film (z-scale = 350 nm), (b) 0.1 µm film (z-scale = 90 nm), and (c) 0.01 µm film (z-scale = 300 nm) [46] (Reproduced with permission from Xiaokong Yu, Advances in Colloid and Interface Science, Elsevier, 2015).
Figure 3. AFM topographical images (all 40 × 40 µm2) of binder AAK-1 as a function of film thickness: (a) 1 µm film (z-scale = 350 nm), (b) 0.1 µm film (z-scale = 90 nm), and (c) 0.01 µm film (z-scale = 300 nm) [46] (Reproduced with permission from Xiaokong Yu, Advances in Colloid and Interface Science, Elsevier, 2015).
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Figure 4. Microstructures visualized by ESEM for B120N, (a) deposited without smearing and (b) deposited by smearing, and for SBS polymer modified bitumen, (c) undeformed and (d) after being elongated. GSE images [53] (Reproduced with permission from Xiaohu Lu, Fuel, Elsevier, 2018).
Figure 4. Microstructures visualized by ESEM for B120N, (a) deposited without smearing and (b) deposited by smearing, and for SBS polymer modified bitumen, (c) undeformed and (d) after being elongated. GSE images [53] (Reproduced with permission from Xiaohu Lu, Fuel, Elsevier, 2018).
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Figure 5. FTIR spectra of the RSMB before and after aging [64] (Reproduced with permission from Zhengang Feng, Construction and Building Materials, Elsevier, 2021).
Figure 5. FTIR spectra of the RSMB before and after aging [64] (Reproduced with permission from Zhengang Feng, Construction and Building Materials, Elsevier, 2021).
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Figure 6. Criegee mechanism of ozonation applied to indene [76] (Reproduced with permission from Hendessi Sima, Ozonation of oilsands bitumen, ACS, 2016).
Figure 6. Criegee mechanism of ozonation applied to indene [76] (Reproduced with permission from Hendessi Sima, Ozonation of oilsands bitumen, ACS, 2016).
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Figure 7. Significant effects of ozone-based oxidation on bitumen treatment: Reduction in processing time and temperature for different bitumen formulations under oxidative conditions.
Figure 7. Significant effects of ozone-based oxidation on bitumen treatment: Reduction in processing time and temperature for different bitumen formulations under oxidative conditions.
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Table 1. Components of bitumen and their related functions.
Table 1. Components of bitumen and their related functions.
ComponentPercentage (%)Component CompoundsFunctionRefs.
Asphaltenes5–25%Polycyclic aromatic hydrocarbons (PAHs)Provide stiffness and viscosity[24,25]
Resins20–40%Polar aromatics, heterocyclic compoundsImprove adhesion and viscoelastic properties
Saturates25–45%Alkanes, cycloalkanesEnhance flow characteristics
Aromatics20–40%Alkylated aromatic hydrocarbonsInfluence ductility and viscosity
Table 2. Different metal separation purification methods for bitumen treatment.
Table 2. Different metal separation purification methods for bitumen treatment.
BitumenTreatment MethodTreatment AgentSeparated Metals, (%)Ref.
VNi
Oil sand bitumenUltrasound-assisted extractionConcentrated HNO3 acid40–50<20[32]
Petroleum bitumenCavitation1 M HCl60–8020–40[33]
Heavy oil/bitumenHigh-pressure treatmentAlkane solvents10–205–10[34]
Petroleum resinsAcid treatmentPolyfunctional carboxylic acid [35]
Bitumen emulsionAcid treatmentPPA [36]
Table 3. A comparison of air-blowing treatments using different oxidants.
Table 3. A comparison of air-blowing treatments using different oxidants.
Bitumen SourceOxidizing AgentAdditiveReduction in Time (%)Reduction in Temp. (%)Improvement in Properties (%)Refs.
Air-blown bitumen (vacuum residue)AirPPA-grafted silica2915Reduction in carbon footprint (CO2 emission analysis): 35%[2]
Industrial-grade bitumen (penetration grade 60/70)AirWaste polymer additives (WEVA)1510Elastic modulus (MPA): +56%; ductility (cm): +20%; viscosity (Pa·s): +15%[77]
Petroleum-derived asphalt flux (soft asphalt)OzoneCatalysts (e.g., FeCl2)7857Complex shear modulus G* (kPa): +30%[16]
Aged bitumen (UV-exposed road asphalt)UV/ozoneNone3525Oxidative aging index reduction (carbonyl/sulfoxide ratio): −25%[78]
Polymer-modified asphaltAirRecycled waste additives105Softening point (°C): +15%[19]
Industrial bitumen (penetration grade 50/70)AirSilica and PPA1530Durability (fatigue resistance cycle): +18%; tensile strength (MPa): +12%[10]
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Hashami, M.; Ongarbayev, Y.; Abdikhan, D.; Akkazin, E.; Nessipbayeva, N. Ozonation of Bitumen: Characteristics, Characterization, and Applications. Processes 2025, 13, 708. https://doi.org/10.3390/pr13030708

AMA Style

Hashami M, Ongarbayev Y, Abdikhan D, Akkazin E, Nessipbayeva N. Ozonation of Bitumen: Characteristics, Characterization, and Applications. Processes. 2025; 13(3):708. https://doi.org/10.3390/pr13030708

Chicago/Turabian Style

Hashami, Muhammad, Yerdos Ongarbayev, Dinmukhamed Abdikhan, Erzhan Akkazin, and Nuripa Nessipbayeva. 2025. "Ozonation of Bitumen: Characteristics, Characterization, and Applications" Processes 13, no. 3: 708. https://doi.org/10.3390/pr13030708

APA Style

Hashami, M., Ongarbayev, Y., Abdikhan, D., Akkazin, E., & Nessipbayeva, N. (2025). Ozonation of Bitumen: Characteristics, Characterization, and Applications. Processes, 13(3), 708. https://doi.org/10.3390/pr13030708

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