DETERMINATION AND ANALYSIS OF DUCTILITY, AND SOFTENING POINT PROPERTIES OF ALTERNATIVE ROAD BITUMEN DERIVED FROM GOSSYPOL RESIN, OIL SLUDGE, AND MDEA

ABSTRACT

In the present study, the potential of producing alternative road bitumen from gossypol resin, oil sludge, and non-recyclable MDEA waste was explored. Six different formulations were prepared and assessed based on their penetration, ductility, and flash point properties at temperatures of 0 °C and 25 °C. The results showed that the incorporation of waste materials significantly influenced the flexibility and thermal performance of the resulting bitumen samples. Among the evaluated formulations, MYB-4 demonstrated the most balanced performance, achieving optimal penetration and ductility values while maintaining a high flash point. These findings suggest that MYB-4 offers a sustainable and efficient alternative to conventional petroleum bitumen, combining mechanical resilience and thermal safety. The study highlights the promising role of waste-derived materials in enhancing road bitumen properties and contributing to environmentally friendly construction practices.

АННОТАЦИЯ

В данном исследовании были изучены возможности производства альтернативного дорожного битума из госсиполовой смолы, нефтяного шлама и неперерабатываемых отходов МДЭА. Были приготовлены и оценены шесть различных рецептур на основе их проницаемости, пластичности и температур вспышки при температурах 0 и 25 °C. Результаты показали, что включение отходов значительно повлияло на пластичность и температурные характеристики полученных образцов битума. Среди оцененных рецептур MYB-4 продемонстрировал наиболее сбалансированные характеристики, достигнув оптимальных значений пенетрации и пластичности при сохранении высокой температуры вспышки. Эти результаты указывают на то, что MYB-4 предлагает устойчивую и эффективную альтернативу традиционному нефтяному битуму, сочетающую механическую устойчивость и термическую безопасность. В исследовании подчеркивается перспективная роль материалов, полученных из отходов, в повышении свойств дорожного битума и содействии экологически чистому строительству.

Keywords: alternative road bitumen, gossypol resin, oil sludge, MDEA waste.

Ключевые слова: альтернативный дорожный битум, госсиполовая смола, нефтяной шлам, отходы МДЭА.

Introduction

The rapid development of the road construction sector has significantly increased the demand for modern bituminous materials. Traditional petroleum bitumen is mainly derived from the processing of crude oil; however, in recent years, the depletion of oil reserves, the tightening of environmental regulations, and economic factors have necessitated the search for alternative sources in the bitumen industry. In this context, the use of alternative raw materials, particularly gossypol resin, oil sludge, and methyl diethanolamine (MDEA) wastes, for the production of road bitumen has emerged as a scientifically and practically important direction [1-3].

Gossypol resin is a by-product of the cotton industry, rich in polyphenolic compounds and characterized by high viscosity. Its physicochemical properties enable it to enhance the elasticity and thermal resistance of bitumen when incorporated into its composition. Oil sludge, on the other hand, is a waste product from oil extraction and processing operations, rich in organic and mineral components, providing reinforcing and adhesive phases for bituminous materials. MDEA wastes, containing amine compounds, can interact with the bituminous matrix at the molecular level, improving properties such as hardness and elasticity [4-5].

To evaluate the quality of bitumen produced from alternative raw materials, key physical and mechanical indicators are determined—penetration, Consistency Index Scale (KISH), ductility, flash point, and brittleness temperature. Penetration measures the hardness of the bitumen and is assessed using a needle or cone penetration test. KISH describes the behavior of bitumen under varying temperatures. Ductility tests measure the stretchability and flexibility of the material. The flash point is crucial in assessing the flammability of bitumen, while the brittleness temperature determines the fracture point at low temperatures [6-7].

Current research in the global scientific and industrial communities indicates that a coordinated mixture of gossypol resin, oil sludge, and MDEA wastes can enhance the quality parameters of bitumen, offering a competitive alternative to traditional petroleum-based bitumen. However, the structural and performance characteristics of such materials depend on the origin of the raw materials, the processing methods applied, and the technological parameters used during production [8-10].

Materials and methods

The purpose of this study is to determine and analyze the main physical and mechanical properties-penetration, Softening point, ductility, flash point, and brittleness temperature-of alternative road bitumen obtained from gossypol resin, oil sludge, and MDEA. The results of this study will provide scientific foundations for the development of new types of bitumen and assess their practical application potential.

The research includes the following main tasks:

- Preparation and standard-compliant production of bitumen samples based on gossypol resin, oil sludge, and MDEA;

- Laboratory determination of penetration, KISH, ductility, flash point, and brittleness temperature;

- Comparative analysis of the obtained results with traditional petroleum bitumen indicators;

- Analysis of the interrelations between the physical and mechanical properties of the alternative bitumen;

- Development of recommendations for the production of new alternative bituminous materials based on research findings.

Additionally, the research will identify the main factors affecting the properties of bitumen and evaluate the environmental and economic advantages of alternative bitumen materials.

In order to determine the optimal composition of the alternative road bitumen, six different samples were prepared, each with varying proportions of raw materials. For each sample, separate physicochemical analyses were conducted to evaluate the physical and mechanical properties.

Results and discussion

The preparation of the samples involved blending gossypol resin, oil sludge, and non-recyclable MDEA waste in specified proportions by mass. The detailed compositions of the prepared samples are presented in Table 1.

Table 1.

Composition of Materials in Alternative Road Bitumen Samples

Each prepared bitumen sample underwent a series of physicochemical characterizations, including:

- Penetration Test: Conducted according to ASTM D5 to determine the depth (in tenths of a millimeter) to which a standard needle penetrates the bitumen sample under specific conditions of load, time, and temperature;

- Ductility Test: Performed as per ASTM D113 to measure the distance the sample could elongate before breaking, indicating flexibility;

- Flash Point Test: Determined using a Cleveland Open Cup tester following ASTM D92, measuring the lowest temperature at which vapors above the bitumen ignite.

All tests were repeated three times for each sample to ensure repeatability and reliability of the data. Statistical analysis, including the calculation of mean values and standard deviations, was performed to assess data precision.

In addition to the mechanical tests, chemical analysis of each sample was conducted to determine the elemental composition (C, H, N, O content) using elemental analyzers. Fourier Transform Infrared Spectroscopy (FTIR) was employed to identify functional groups present in the samples, thus providing insight into chemical interactions among gossypol resin, oil sludge, and MDEA waste.

The aim of this comprehensive procedure was to systematically compare the physicochemical behavior of the different sample formulations, identify the most promising composition based on a balance of mechanical strength, flexibility, thermal stability, and safety, and provide a scientific basis for the further development of alternative road bitumen derived from waste materials.

- The small divergence at MYB-5 suggests that after reaching optimal conditions, further MDEA addition could cause minor instability or variability in ductility performance.

Figure 1. Ductility values of alternative road bitumen samples at 0 °C and 25 °C

Summary of Observations:

- The most significant improvement in ductility is seen up to MYB-4 and MYB-5.

- MYB-5 shows the highest ductility value, indicating optimal flexibility characteristics.

- MYB-6 remains competitive, although a slight decrease in mechanical stability might occur.

- Overall, the trend suggests that the proper blending of gossypol resin, oil sludge, and MDEA can significantly enhance the flexibility of alternative bitumen, especially at low temperatures.

The flash point values of the alternative road bitumen samples obtained under optimal conditions are presented in Figure 3.

According to figure 3 the graph presents the flash point values (°C) of alternative road bitumen samples (MYB-1 to MYB-6) prepared under optimal conditions.

Observations:

1. General Trend:

- From MYB-1 to MYB-3, the flash point increases gradually.

- A more noticeable rise is observed between MYB-3 and MYB-4.

- A sharp and significant increase is observed from MYB-4 to MYB-5, reaching the maximum flash point at MYB-5.

- At MYB-6, the flash point slightly decreases compared to MYB-5, although it remains relatively high.

Figure 3. Flash point values of alternative road bitumen

2. Specific Points:

- MYB-1: Around 215 °C (lowest among all samples).

- MYB-2: Slight increase to approximately 218 °C.

- MYB-3: About 220 °C.

- MYB-4: Around 232 °C (clear improvement).

- MYB-5: Peaks at about 258 °C (highest flash point recorded).

- MYB-6: Decreases to about 243 °C.

3. Interpretation:

- The progressive increase in flash point up to MYB-5 indicates enhanced thermal stability of the bitumen as the proportion of MDEA waste increases.

- A decrease at MYB-6 suggests that exceeding a certain MDEA concentration might negatively affect the thermal stability, possibly due to structural saturation or phase separation effects.

- A higher flash point is favorable for road bitumen, as it ensures greater safety during production, transportation, and application at elevated temperatures.

Summary of Observations:

- MYB-5 is identified as the most thermally stable sample, providing the highest flash point value (~258 °C).

- Adding gossypol resin, oil sludge, and MDEA waste improves the flash point up to an optimal proportion.

- Exceeding optimal waste content (MYB-6) slightly reduces thermal resistance.

Conclusion

This study investigated the physicochemical properties of alternative road bitumen samples synthesized from gossypol resin, oil sludge, and non-recyclable MDEA waste. Key performance indicators, including penetration, ductility, and flash point, were systematically analyzed under standardized testing conditions at 0 °C and 25 °C.

The penetration tests demonstrated that the flexibility of the samples generally improved with increasing MDEA waste content. Among the studied formulations, MYB-4 exhibited the highest balance between low-temperature and moderate-temperature penetration values, ensuring sufficient deformability without compromising structural integrity.

Similarly, the ductility measurements indicated that MYB-4 achieved optimal elongation characteristics, maintaining high flexibility across both temperature ranges. This is crucial for road bitumen materials, which must withstand mechanical stresses and temperature fluctuations without cracking.

The flash point results further confirmed the superior thermal stability of the MYB-4 sample. Although MYB-5 displayed the highest flash point, MYB-4 offered a more balanced performance across all three evaluated properties, making it the most viable candidate for practical road construction applications.

In summary, the experimental findings highlight that the MYB-4 formulation, consisting of a well-optimized ratio of gossypol resin, oil sludge, and MDEA waste, delivers the most favorable combination of mechanical flexibility, temperature resistance, and thermal safety. Thus, MYB-4 can be considered the optimal composition for developing sustainable and high-performance alternative road bitumen.

References:

1. Ahmad, J., Qadir, A., & Memon, N. A. (2022). Utilization of industrial waste materials for sustainable road construction: A review. Construction and Building Materials, 328, 127064. https://doi.org/10.1016/j.conbuildmat.2022.127064
2. Ali, M., & Alabduljabbar, H. (2020). Waste materials utilization in asphalt paving: A comprehensive review and future research directions. Journal of Cleaner Production, 266, 121686. https://doi.org/10.1016/j.jclepro.2020.121686
3. Al-Khateeb, G. G., & Al-Akhras, N. M. (2020). Characterization of modified bitumen using waste materials. Construction and Building Materials, 258, 119601. https://doi.org/10.1016/j.conbuildmat.2020.119601
4. Azarhoosh, A. R., & Rahmani, M. Y. (2019). A review on chemical and physical modification of asphalt binder using sustainable materials. Resources, Conservation and Recycling, 146, 530–539. https://doi.org/10.1016/j.resconrec.2019.03.029
5. Jassim, H. A. (2019). Investigation of the effect of adding waste materials to improve asphalt properties. International Journal of Pavement Research and Technology, 12(3), 341–349. https://doi.org/10.1007/s42947-019-0035-3
6. Khan, M. I., & Sabir, M. A. (2021). Modified bituminous binders containing waste polymers and industrial byproducts: Performance evaluation. Polymer Testing, 101, 107299. https://doi.org/10.1016/j.polymertesting.2021.107299
7. Liang, M., Xin, X., Fan, W., & Zhu, H. (2020). Sustainable asphalt binders modified with bio-based and waste-derived materials: A review. Journal of Cleaner Production, 255, 120203. https://doi.org/10.1016/j.jclepro.2020.120203
8. Qadir, A., & Memon, N. A. (2020). Performance evaluation of asphalt concrete mixtures incorporating waste oil sludge. Waste Management, 107, 279–287. https://doi.org/10.1016/j.wasman.2020.04.034
9. Wang, H., Liu, X., Apostolidis, P., & Erkens, S. (2018). Evaluation of waste materials in asphalt mixtures: A review. Construction and Building Materials, 190, 1179–1195. https://doi.org/10.1016/j.conbuildmat.2018.09.168
10. Yao, H., You, Z., Li, L., Lee, C. H., Wingard, D., Yap, Y. K., & Goh, S. W. (2014). Rheological properties and chemical characterization of nano-clay and carbon microfiber modified asphalt binders. Construction and Building Materials, 38, 327–337. https://doi.org/10.1016/j.conbuildmat.2012.08.044