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Article

Physical, Mechanical and Structural Characteristics of Sulfur Concrete with Bitumen Modified Sulfur and Fly Ash

by
Sergey A. Stel’makh
1,
Evgenii M. Shcherban’
2,
Alexey N. Beskopylny
3,*,
Levon R. Mailyan
1,
Besarion Meskhi
4,
Alexandr A. Shilov
1,
Alexandr Evtushenko
1,
Andrei Chernil’nik
1,
Diana El’shaeva
1,
Memduh Karalar
5,
Yasin Onuralp Özkılıç
6,* and
Ceyhun Aksoylu
7
1
Department of Unique Buildings and Constructions Engineering, Don State Technical University, Gagarin Sq. 1, 344003 Rostov-on-Don, Russia
2
Department of Engineering Geology, Bases, and Foundations, Don State Technical University, 344003 Rostov-on-Don, Russia
3
Department of Transport Systems, Faculty of Roads and Transport Systems, Don State Technical University, 344003 Rostov-on-Don, Russia
4
Department of Life Safety and Environmental Protection, Faculty of Life Safety and Environmental Engineering, Don State Technical University, 344003 Rostov-on-Don, Russia
5
Department of Civil Engineering, Faculty of Engineering, Zonguldak Bulent Ecevit University, Zonguldak 67100, Turkey
6
Department of Civil Engineering, Faculty of Engineering, Necmettin Erbakan University, Konya 42000, Turkey
7
Department of Civil Engineering, Faculty of Engineering and Natural Sciences, Konya Technical University, Konya 42075, Turkey
*
Authors to whom correspondence should be addressed.
J. Compos. Sci. 2023, 7(9), 356; https://doi.org/10.3390/jcs7090356
Submission received: 9 July 2023 / Revised: 6 August 2023 / Accepted: 23 August 2023 / Published: 25 August 2023
(This article belongs to the Section Composites Modelling and Characterization)
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Versions Notes

Abstract

:
Industrial waste usage in the technology of construction materials is currently in a relevant and promising direction. Materials made of industrial waste have a lower cost and are highly environmentally friendly. The objective of this study is to develop effective compositions of sulfur concrete based on the maximum possible number of various wastes of the local industry for this and to investigate the characteristics of this composite. Test samples of sulfur concrete were made from sulfur, fly ash, mineral aggregates and bitumen additive. The dosages of fly ash, sand and bitumen varied, while the content of sulfur and crushed stone remained constant. The following main characteristics of sulfur concrete were determined: density; compressive strength; and water absorption. Tests of sulfur concrete were carried out after 1 day and 28 days of hardening. The best values of compressive strength (24.8 MPa) and water absorption (0.9%) were recorded for the composition of sulfur concrete at the age of 28 days with the following content of components: sulfur—25%, modified with 4% bitumen of its mass; fly ash—10%; crushed stone—40%; and sand—25%. The optimal composition of modified sulfur concrete showed compressive strength up to 78% more and water absorption up to 53% less than the control composition. The characteristics of the sulfur concrete samples after 28 days of hardening differ slightly from the values after 1 day of hardening (up to 1.8%). An analysis of the structure confirmed the effectiveness of the developed composition of sulfur concrete in comparison with the control.

1. Introduction

Currently, one of the most important tasks of modern building science is the development of new building materials that can be manufactured using locally produced raw materials, as well as various types of waste [1,2,3]. Such types of waste include waste from the fuel and energy complex and waste from gas and oil plants. For example, with regard to the use of fuel and energy complex waste in construction technology, there are many works on the use of fly ash [4,5,6,7,8,9], slag [10,11,12,13,14,15] and microsilica [16,17,18,19,20,21,22]. As for gas and oil production, the main types of waste are oil sludge, spent proppant and sulfur. Sulfur is considered not only a problematic environmental element but also a resource component in demand in various fields of industry, agriculture, medicine and construction [23,24]. In the construction industry, of particular interest is the use of technical sulfur as a binder for the manufacture of new types of concrete [25,26], that is, cementless concrete [27,28,29].
Sulfur concrete with an optimally selected formulation has sufficiently high strength characteristics and is resistant to the aggressive environment. To illustrate this fact, in [30,31,32,33], the authors developed new compositions of sulfur concrete and assessed their resistance to aggressive influences. In [30], the authors carried out studies of sulfur concrete modified with styrene and bitumen additives for resistance to ignition and resistance to an acidic environment. The results of the experimental data confirm the effectiveness of the application of these modifying additives to increase the resistance of sulfur concrete to aggressive influences. In [31], the authors evaluated the performance characteristics of sulfur concrete used in a sewer environment in comparison with cement concrete. The conducted field studies have shown “a high specific resistance of sulfur concrete in a sewer environment with variable temperature, humidity and gases compared to concretes based on Portland cement”. In study [32], the authors evaluated the chemical resistance of modified sulfur concrete. It has been found that the strength loss of the sulfur concrete samples after soaking in a 40% H2SO4 solution was 3–6% and 0.4–1.3% with a 40% soak in an SO4(NH4)2 solution, which indicates a high chemical resistance of the developed composites. In [33], “a study was made of the durability characteristics of sulfur concrete with various types of fine aggregates”, namely beach sand, ecosand and industrial sand, which were introduced as part of the replacement of river sand. It has been established that all types of developed sulfur concrete can be used in places with high humidity and acidity.
The use of sulfur in the manufacture of concretes with various kinds of fillers and additives that increase their strength properties was studied in [34,35,36,37]. For example, in study [34], compositions of cast sulfur concrete were developed for the production of paving slabs of bricks and blocks. The best properties were recorded for products with the following formulation: 42% aggregate, 40% sand, 11.50% granulated sulfur, 1.2% bitumen-modified sulfur and 5.3% fly ash. Study [35] evaluated the strength characteristics and thermal expansion coefficient of sulfur concrete. The authors managed to develop sulfur concrete with a compressive strength of at least 50 MPa. As for the thermal expansion, it turned out to be slightly higher than that of concrete on Portland cement. The use of light catalytic cracking oil as a chemical modifier and fly ash as a filler in study [36] allows for the development of sulfur concrete of acceptable quality with a reduced environmental impact. And, in [37], the application of electrolytic manganese residues as a filler in the manufacture of sulfur concrete makes it possible to obtain a composite with excellent strength and high environmental friendliness. Also, various types of fibers can be used as reinforcing additives in sulfur concrete production [38,39]. In addition, in [38], the authors made the statement that the use of steel fiber in an amount of 0.91%, and a plasticizing additive in an amount of 2.35%, makes it possible to increase the strength characteristics of sulfur concrete by up to 15% in comparison with control samples. It should be noted that the production of sulfur concrete with high strength characteristics can be achieved not only with the application of modifying additives of various types but also through physical modification, which includes special technological solutions in the process of manufacturing this type of concrete. For example, in [39], the authors proposed a method for obtaining high-strength sulfur concrete without the chemical modifiers’ introduction. The essence of this method was to obtain a thixotropic casting mixture near the yield point of the system during vibro-laying. As a result, this method of physical modification allows for the development of sulfur concrete with a compressive strength of 94–97.5 MPa.
The relevance of this study is ensured by the high demand and, at the same time, the lack of materials in modern construction that have high-quality characteristics and are environmentally friendly and economical. There is an approach that involves the combination of technological, environmental and materials science aspects, built on providing for the maximum use of waste-free technologies in various areas of production. In this regard, this research problem will be formulated as follows. It is necessary to provide the most rational technologies that allow the use of waste from the technological and fuel and energy complex in construction. Currently, this problem has not been fully resolved, and there are large scientific and practical deficits in this area. In this regard, one of the solutions to part of the problem may be to study and expand the possibility of using sulfur concrete in construction. Such material is characterized not only by high-quality indicators but also by the function of reducing the carbon footprint and the possibility of obtaining clinker-free concrete of a more environmentally friendly type, at the same time having economic efficiency.
Analyzing the above review, it can be seen that there is a scientific deficit, expressed in the lack of a clear understanding of the relationship between the structure and properties of sulfur concrete, depending on the production and material science parameters of the components used, to determine their interdependence and the quality of the resulting sulfur concrete. Therefore, in this article, the scientific novelty is the study of the dependencies of structure formation and the production of high-quality building concrete, consisting of waste from the fuel and energy complex—fly ash and waste from the oil and gas industry—technical sulfur and mineral aggregates—sand and crushed stone, as well as obtaining new relationships between the characteristics of the sulfur concrete and prescription options. The use of these materials in construction brings environmental and economic benefits. The environmental benefit of use is that the carbon footprint and the amount of accumulated waste in residential areas and regions are reduced, which has a positive effect on the environment. The economic effect is that instead of expensive components, industrial waste is used, which reduces the cost of production.
The objective of this research is to formulate sulfur concrete using as many local industry waste materials as possible and to observe its physical and mechanical properties. Thus, the following tasks will be solved during this study:
-
The determination of the optimal sulfur content as a binder component in the composition of the sulfur concrete;
-
The selection of the optimal content of the filler in the form of fly ash;
-
The determination of the optimal dosages of the mineral aggregates;
-
The modification of the sulfur, with the help of the bitumen additive, and the selection of the most effective content of this additive;
-
The determination of the characteristics of various compositions of sulfur concrete and obtaining dependencies based on them;
-
The study of the structural features of the resulting sulfur concrete.

2. Materials and Methods

2.1. Materials

Samples of sulfur concrete of various compositions were made from the following materials:
-
Technical sulfur (TS) (Novoshakhtinsk oil products plant, Novoshakhtinsk, Russia);
-
Fly ash (FA) (Novocherkaskaya GRES, Novocherkassk, Russia);
-
Crushed sandstone (CS) (RostMed, Kamensk, Russia);
-
Career sand (S) (DON-RESURS, Kagalnik, Russia).
The main characteristics of the raw components are presented in Table 1.
Oil-building bitumen BN-50/50 (Ural Bitumen Plant, Yekaterinburg, Russia) was used as a modifying additive for sulfur. Softening temperature was 50–60 °C. The content of the bitumen modifying additive was calculated as a percentage of the mass of sulfur in the composition of sulfur-containing concrete mixtures.
The general view of raw materials for the production of sulfur concrete is shown in Figure 1.

2.2. Methods

The compositions of sulfur-containing concrete mixes were selected in % by weight (Figure 2 and Figure 3).
In mixtures, the proportions of fly ash varied from 0% (control composition) to 15% in increments of 5% (by weight of all dry components of sulfur concrete), the proportions of sand varied from 35% (control composition) to 20% in increments of 5% (by weight of all dry components of sulfur concrete) and the proportions of bitumen varied from 0% (control composition) to 6% in increments of 2% (by weight of sulfur).
The proportions of sulfur concrete mixtures per 1 m3 were determined (Table 2).
The following were used as industrial waste:
(a)
Technical sulfur (TS), as the main component of sulfur concrete, in an amount of 25% by weight of all dry components of sulfur concrete;
(b)
Fly ash (FA) at 0%, 5%, 10% and 15% by weight of all dry sulfur concrete components depending on the composition of the sulfur concrete mixture.
The following technology was used for manufacturing experimental and control samples. Raw materials were prepared by fractionating aggregates, washing and drying aggregates and filler to constant weight. Before the production of samples, technical sulfur was subjected to additional mechanical processing. Sulfur grinding was carried out in an Activator-4M planetary ball mill (Chemical Engineering Plant, Novosibirsk, Russia) for 1 h at 700 rpm. Modification of sulfur was carried out by introducing bitumen into it at a temperature of 125–155 °C. Modified sulfur was melted at a temperature of 125–155 °C (melting point of sulfur) to a liquid state, then it was mixed with a mixture of mineral components (fly ash, sand and crushed stone) and heated to the same temperature. The mineral components were heated to the required temperature in an oven for 2 h. The mixture was stirred for 30 min until smooth. The temperature of the mixture was maintained within 125–155 °C. The mixture was poured into heated molds and compacted on a vibrating platform for 60 s. After a day of hardening, the samples were removed from the molds.
For the manufacture and testing of fresh and hardened sulfur concrete and samples from it, the following equipment and measuring instruments were used:
-
Portable thermometer megeon 26300 (MEGEON, Moscow, Russia);
-
Cube shapes 2FK-100 (RNPO RusPribor, St. Petersburg, Russia);
-
Drying cabinet ShS-80-01 SPU (Smolensk SKTB SPU, Smolensk, Russia);
-
Laboratory vibration platform (IMash, Armavir, Russia).
An experimental research program was drawn up (Figure 4).
According to Figure 4, each series consisted of 12 samples, 6 of which were tested after 1 day of hardening and 6 after 28 days of hardening. Since there are 10 compositions, the total number of tested samples in this study was 120.
The standard deviations of the values were the following: for density, 6.20 kg/m3; compressive strength, 1.54 MPa; and water absorption, 0.21%.
Determination of compressive strength was carried out in accordance with the documents in [40,41,42,43,44,45]. The loading rate of the compressive strength was maintained in the range of (0.6 ± 0.2) MPa/s.
The density of the hardened concrete was determined according to the method in [46,47].
Determination of water absorption of sulfur concrete samples was carried out in accordance with the requirements of regulatory documents in [48,49].
Raw materials’ particle size gradations were determined using a model 201C microsizer (VA Insalt, Saint Petersburg, Russia) and a set of KSI sand and crushed stone sieves (Vibrotechnik, Saint Petersburg, Russia) according to [50,51].
X-ray diffraction was performed on an ARLX’TRA diffractometer; the characteristic radiation of a copper anode was used (wavelengths CuKα1 1.5406 Å, CuKα2 1.5444 Å). Identification of phases of serpentinites and minor minerals was carried out using the X-ray database PDF-2.
The structure of sulfur concrete samples was analyzed using an MBS-10 stereoscopic microscope (Izmeritelnaya Tekhnika, Moscow, Russia) with 10-fold magnification.

3. Results and Discussion

The particle size distribution of the sulfur is shown in Figure 5.
Figure 5 shows that the largest proportion of the sulfur particles, 87.1%, is in the range from 17 µm to 140 µm. The particles with a size of 2.58 µm and up to 17 µm contain 12.1%, and the number of particles larger than 140 µm is insignificant and amounts to 0.8%.
The particle size distribution of the fly ash is shown in Figure 6.
Analyzing Figure 6, it can be seen that the distribution curve of the fly ash particles can be conditionally divided into three sections. The content of the particles with a size of 2.5 µm to 8 µm is 19.4%, the largest proportion of the particles in the amount of 64.9% is in the range from 8 µm to 40 µm and the content of the particles with a size of 40 µm or more is 15.7%.
The sand particle size gradations are presented in Table 3.
The particle sizes of the crushed stone mixture of the fractions from 5 to 20 mm were distributed as follows: 50%—a fraction from 5 to 10 mm; and 50%—a fraction over 10 to 20 mm.
The XRD patterns of the raw materials are presented in Figure 7.
In Figure 7a—technical sulfur—a sulfur phase is visible and, apparently, quartz in a very small amount. In Figure 7b—quartz sand—according to the XRD results, only quartz is visible (the small “extra” tips are caused by “spurious” radiation from the device). Figure 7c—crushed sandstone—clearly shows quartz, a faint phase close to albite and a very faint phase similar to chlorite. In Figure 7d—fly ash—the profile is very dim and, apparently, there is a lot of amorphous phases and phases of quartz, and hematite and magnetite are visible.
The results of the influence of the proposed solutions, which included the use of an additional mineral filler like fly ash, and the modification of the sulfur with bitumen on the strength and physical characteristics of the sulfur concrete, are shown in Figure 8, Figure 9, Figure 10, Figure 11, Figure 12, Figure 13, Figure 14 and Figure 15. Figure 8 and Figure 9 show graphs of the dependence of the density of the sulfur concrete on the content of the fly ash and bitumen after 1 day and after 28 days, respectively.
According to the results of determining the density of the sulfur concrete samples, presented in Figure 8 and Figure 9, it can be seen that the density of the sulfur concrete samples of various compositions at the age of 1 day and at the age of 28 days varies from 2429 kg/m3 to 2445 kg/m3. The registered values of the density of the sulfur concrete compositions after 1 day of hardening varied from 2429 kg/m3 to 2438 kg/m3 (Figure 8), and after 28 days of hardening from 2430 kg/m3 to 2445 kg/m3 (Figure 9). The differences (in percent) in the density of the sulfur concrete samples after 1 day and 28 days of hardening were in the range from 0.04% to 0.62%. Therefore, based on the results obtained, it can be concluded that the recipe solutions used in this work do not significantly affect the change in the density of sulfur concrete.
Figure 10 and Figure 11 show graphs of the dependence of the compressive strength of the sulfur concrete on the content of the fly ash and bitumen after 1 day and after 28 days, respectively.
The compressive strength values of the sulfur concrete compositions after 1 day of hardening varied from 13.7 MPa to 24.6 MPa (Figure 10) and after 28 days from 13.9 MPa to 24.8 MPa (Figure 11). Following the results presented in Figure 10, it can be seen that the maximum strength value is observed for the composition of sulfur concrete type FA10/4, which is 24.6 MPa. In general, the FA5/4, FA10/4 and FA15/4 type formulations with 4% bitumen showed the best compressive strength values. Thus, for the FA5/4 composition, the compressive strength was 20.3 MPa and for the FA15/4 composition, it was 19.5 MPa. With regard to the effect of the fly ash content in the sulfur concrete compositions, the best compressive strength results were recorded for the compositions of the FA10/2, FA10/4 and FA10/6 types. Thus, the compressive strength of the FA10/2 composition was 17.8 MPa and that of the FA10/6 composition was 21.7 MPa. The lowest compressive strength of all the compositions, except for the control one, is observed in the composition of the FA5/2 type and is 14.0 MPa. The compressive strength of the FA15/2, FA5/6 and FA15/6 compositions was 15.5 MPa, 15.5 MPa and 17.3 MPa, respectively. Thus, it can be concluded that the most effective formulation solution is the use of bitumen in the amount of 4% and FA in the amount of 10%.
Figure 11 shows that the trend in the change in compressive strength of the sulfur concrete samples aged 28 days for the compositions with different contents of FA and bitumen is similar to that of the samples aged 1 day. The strength values for the samples of the sulfur concrete of the control composition and compositions of the FA5/2, FA10/2, FA15/2, FA5/4, FA10/4, FA15/4, FA5/6, FA10/6 and FA15/6 types, respectively, amounted to 13.9 MPa, 14.9 MPa, 18.0 MPa, 15.5 MPa, 20.5 MPa, 24.8 MPa, 19.7 MPa, 15.5 MPa, 21.8 MPa and 17.6 MPa. After 28 days of hardening, the compressive strength of the optimized sulfur concrete was 24.8 MPa, which is 78% higher than the compressive strength of the control composition (13.9 MPa). It should be noted that after curing for 28 days, all sulfur concrete compositions showed slight increases in compressive strength. The values of the increases in compressive strength of the sulfur concrete after 28 days of hardening in comparison with the values of the increases in compressive strength after 1 day of hardening are presented in Table 4.
The differences (in percent) in the compressive strength of the sulfur concrete samples after 1 day and 28 days of hardening ranged from 0.5% to 2.4% (Table 4).
The appearance, the nature of the collapse and the structure of the sulfur concrete samples after the collapse are shown in Figure 12.
Figure 12 shows that the presented sample of the sulfur concrete has a gray-brown tint and, on the outer surface of the sample, there is a small number of open pores-shells formed during the manufacture of the sample. The internal macrostructure of the sample, visible at the fracture, is dense and is represented by several phases: a coarse filler; a fine aggregate; and a binder component consisting of modified sulfur and fly ash.
Figure 13 and Figure 14 show graphs of the dependence of the water absorption of the sulfur concrete on the content of the fly ash and bitumen after 1 day and after 28 days, respectively.
The values of the water absorption of the sulfur concrete compositions after 1 day of hardening varied from 0.91% to 1.92% by weight (Figure 13) and after 28 days from 0.90% to 1.90% by weight (Figure 14). Figure 13 shows that the smallest value of the water absorption for the samples of the sulfur concrete composition type FA10/4 is 0.91%. In general, as in the case of compressive strength, the FA5/4, FA10/4 and FA15/4 formulations with 4% bitumen are the most effective, and the water absorption for the FA5/4 and FA15/4 formulations is 1.15% and 1.19%, respectively. Formulations like FA10/2, FA10/4 and FA10/6 with 10% FA showed water absorption values of 1.53%, 0.91% and 0.99%, respectively. The highest water absorption value was recorded for the composition of the FA5/2 type and amounted to 1.84%. And, the water absorption values of the compositions FA15/2, FA5/6 and FA15/6 are 1.66%, 1.55% and 1.50%, respectively.
Figure 14 shows that the trend of changing the water absorption of the sulfur concrete samples after 28 days for the compositions with different contents of FA and bitumen is similar to that of the samples after 1 day. The water absorption values for the samples of the sulfur concrete of the control composition and compositions of the type FA5/2, FA10/2, FA15/2, FA5/4, FA10/4, FA15/4, FA5/6, FA10/6 and FA15/6 were 1.90%, 1.83%, 1.51%, 1.64%, 1.13%, 0.90%, 1.17%, 1.53%, 0.97% and 1.49%, respectively. The decrease in the water absorption in the optimized composition (0.90%) compared to the control composition (1.90%) after 28 days of hardening was about 53%. The value of the decrease in the percentage of the water absorption of the sulfur concrete after 28 days compared with the sulfur concrete after 1 day is presented in Table 5.
The differences (in percent) of the water absorption of the sulfur concrete samples after 1 day and 28 days of hardening were in the range from 0.5% to 2.1% (Table 5).
Speaking about the variation in the compressive strength and water absorption of the sulfur concrete samples, depending on their component composition, a number of patterns can be identified. Since the content of the sulfur and coarse aggregate remained unchanged, the variation in the compressive strength and water absorption of the sulfur concrete samples was primarily associated with the amount of the bitumen and fly ash modifying additive. The main role of the modifying additive when it is introduced into the composition of the sulfur concrete is to reduce brittleness, increase strength and slow down the process of sulfur crystallization during its cooling. This is confirmed by the test results, showing that the sulfur concrete modified with bitumen has higher compressive strength and lower water absorption compared to the sulfur concrete of the control composition. The fly ash in the sulfur concrete acts as a structure former. The fine grains of the fly ash in the process of manufacturing a sulfur concrete composite are mixed with molten modified sulfur and coarse and fine aggregates and fill the voids between the particles of the aggregates, which, in turn, makes the structure more coherent and durable [52].
Also of interest is a general comparative evaluation of the effectiveness of the prescription solutions tested in this work. The variation in the characteristics of the sulfur concrete, depending on the amount of FA and bitumen, are shown in Table 6 and are presented as a percentage compared to the control composition of the sulfur concrete.
In the first few hours after preparation, the sulfur concrete gains about 70% of the maximum possible strength and 85% or more after 24 h of hardening [28].
The results of the density, compressive strength and water absorption, obtained for the samples of the sulfur concrete after 28 days of hardening, are consistent with the results of the same indicators for the samples of the sulfur concrete after 1 day of hardening. Only small increases in the compressive strength are observed, varying within 0.5–1.4%, and a decrease in the water absorption within 0.5–2.1%. A slight difference in the change in the strength characteristics of the sulfur concrete tested at an early age and after 28 days is also confirmed by the results of other experimental studies [53,54].
For a comparative assessment of the structural features of the developed compositions of the sulfur concrete, a control composition was selected, as well as a composition of the FA10/4 type with the best characteristics and a composition of the FA5/2 type with the worst characteristics. Photos of the structure of the sulfur concrete of the control composition are shown in Figure 15, the composition of the FA10/4 type in Figure 16 and the composition of the FA5/2 type in Figure 17.
Figure 15 shows that in the structure of the sulfur concrete samples of the control composition, a sufficiently large number of shrinkage cavities are observed, which directly affect its strength and water absorption. In general, sulfur envelops fine aggregate particles fairly evenly and forms a homogeneous phase boundary. Figure 16 shows a different microstructure morphology. Firstly, there are no shrinkage cavities in the FA10/4 type samples and, secondly, a dense packing of filler particles, sulfur and aggregates is visible, and sulfur itself, as a binder, fairly evenly envelops the fine aggregate particles and sticks them together. As for the composition of the FA5/2 type (Figure 17), here, shrinkage cavities are observed in the structure of the sulfur concrete. The structure of the studied sulfur concretes is in good agreement with the experimental data presented above.
Thus, the obtained results confirm the impracticality of the production of sulfur concrete without the introduction of additional additives in the form of fillers and chemical additives. The sulfur concrete of the control composition, both after 1 day of hardening and after 28 days, has a significantly lower compressive strength and greater water absorption. This is primarily due to the large number of cavities in their structure. As a rule, the main reason for the formation of these cavities is the transition of sulfur from melting to the solid state, and due to the processes of crystallization and recrystallization, these changes occur [55]. The improvement of the characteristics of the sulfur concrete can mainly be achieved by modifying sulfur with bitumen and introducing mineral filler in optimal dosages, which is confirmed by the test results. The effectiveness of these additives is also confirmed by studies by other authors [34,56].
Based on all of the above, it can be argued that the main factors that determine good results in terms of the compressive strength and water absorption of the sulfur concrete samples are such processes as the interaction of technical sulfur with finely dispersed filler FA and the combination of crystallized modified sulfur with coarse and fine aggregates, which create an organized monolithic structure, thereby providing high characteristics of sulfur concrete.
FA cenosphere is an important structure-forming mechanism-determining aspect in the formation of the qualitative structure and properties of sulfur concrete. Such fly ash at the stage of structure formation makes it possible to achieve a better distribution of the particles within the conglomerate, contribute to a more uniform and proportional pattern in both qualitative and quantitative aspects of the distribution of properties over the volume of the material and, in general, have a positive effect on the final conglomerate. Of course, as a result of the formation of good density and strength characteristics, the operational properties of the resulting conglomerate are improved. Sulfur concrete is a good material both in terms of research work and in terms of practical application for the effective and beneficial use of FA cenosphere. This is in good agreement and is based, among other things, on the following works [34,53,56].
The results obtained made it possible to solve some of the problems and eliminate some of the scientific deficits associated with the study of the characteristics of sulfur concrete, depending on the initial parameters. Determining the rational dosages of the obtained components, as well as the qualitative composition of the proposed sulfur concrete, will make it possible to use such a composite in civil engineering, taking into account the characteristics of the material but, at the same time, already having a reliable empirical base, verified theoretically and experimentally.
The conducted studies, in particular the registered values and structural analysis, showed the advantages of the practical application of the developed compositions of sulfur concrete with industrial waste in construction projects. The first advantage is the high quality of the structure and sufficient physical and mechanical performance of sulfur concrete, which allows it to be used in construction. Another major advantage is the speed of obtaining sulfur concrete products and structures in comparison with cement-based concretes. These advantages determine the prospects for using the developed composition of sulfur concrete in construction projects.
This study also showed the environmental benefits of using industrial waste in building materials. In particular, in the case of sulfur concrete, this is expressed in a decrease in the carbon footprint due to the fact that sulfur, that is, technical waste, is used as a binder. At the same time, the resulting concrete is cementless and clinker-free. This reduces the need for a binder, namely cement, the production of which leaves a significant carbon footprint and affects the environmental agenda of sustainable development.

4. Conclusions

In this study, effective compositions were developed based on local industry waste, and the characteristics of sulfur concrete were studied. The optimal content of sulfur as a binder component in the composition of sulfur concrete has been determined. The optimal content of fly ash in sulfur concrete has been selected. The optimal dosages of mineral aggregates are determined. Sulfur was modified with the help of bitumen additive and the most effective content of this additive was selected. The physical and mechanical characteristics of various compositions of sulfur concrete are determined and dependences are obtained on their basis. The structural features of the obtained sulfur concrete have been studied. Based on the results of this study, the following conclusions can be drawn:
(1)
The optimal composition of modified sulfur concrete after 28 days, which showed the best compressive strength (24.8 MPa) and water absorption (0.9%), contains 25% sulfur modified with 4% bitumen by weight, 10% fly ash, 40% crushed stone and 25% sand.
(2)
The optimal composition of the modified sulfur concrete made it possible to increase the compressive strength up to 78% and reduce the water absorption to 53%.
(3)
The characteristics of the sulfur concrete samples after 28 days of hardening differ slightly from the values after 1 day of hardening: density—up to 0.6% more, compressive strength—up to 1.7% more and water absorption—up to 1.8% less.
(4)
The formulation solutions considered in this study do not significantly affect the change in the density of sulfur concrete. The density of all compositions, including the control one, varied from 2429 kg/m3 to 2445 kg/m3.
(5)
The structure of the sulfur concrete samples of the control composition contains a sufficiently large number of shrinkage cavities, which directly affect its strength and water absorption. In this case, the sulfur evenly envelops the fine aggregate particles and forms a homogeneous phase boundary. There are practically no shrinkage cavities in a sample of the sulfur concrete of the optimal composition, the packing of filler particles, sulfur and aggregates is dense, and sulfur itself, as a binder, fairly evenly envelops the fine aggregate particles and sticks them together.
The practical significance of the results obtained lies in the development of the optimal formulation of the sulfur concrete mixture and the choice of rational dosages of the components, as well as the type and characteristics of these components proposed for implementation in practice. The experimental results obtained made it possible to create an empirical basis for the development on the basis of a new line and nomenclature of a building composite material of a fundamentally new quality and composition.
Continuation of this research is planned in the direction of using other types of waste from thermal power plants and metallurgy in sulfur concrete, such as slag, microsilica and dust, as well as dolomite flour, and determining the long-term properties of sulfur concrete.

Author Contributions

Conceptualization, S.A.S., E.M.S., A.N.B. and A.A.S.; methodology, S.A.S., E.M.S., Y.O.Ö., C.A., D.E. and A.C.; software, A.A.S., D.E., A.N.B., Y.O.Ö., A.E. and C.A.; validation, A.A.S., S.A.S., E.M.S. and L.R.M.; formal analysis, A.E., S.A.S. and E.M.S.; investigation, S.A.S., E.M.S., A.N.B., A.C., D.E., Y.O.Ö., C.A. and B.M.; resources, B.M.; data curation, S.A.S., E.M.S. and A.C.; writing—original draft preparation, S.A.S., Y.O.Ö., C.A., M.K., E.M.S. and A.N.B.; writing—review and editing, M.K., S.A.S., E.M.S. and A.N.B.; visualization, S.A.S., E.M.S. and A.N.B.; supervision, B.M. and L.R.M.; project administration, B.M.; funding acquisition, A.N.B. and B.M. All authors have read and agreed to the published version of the manuscript.

Funding

This research received no external funding.

Institutional Review Board Statement

Not applicable.

Informed Consent Statement

Not applicable.

Data Availability Statement

This study did not report any data.

Acknowledgments

The authors would like to acknowledge the administration of Don State Technical University for their resources and financial support.

Conflicts of Interest

The authors declare no conflict of interest.

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Figure 1. Raw materials: (a) sulfur; (b) sand; (c) crushed stone; and (d) fly ash.
Figure 1. Raw materials: (a) sulfur; (b) sand; (c) crushed stone; and (d) fly ash.
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Figure 2. Control composition of sulfur-containing concrete mix.
Figure 2. Control composition of sulfur-containing concrete mix.
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Figure 3. Composition of sulfur-containing concrete mixes with different content of bitumen modifier 2%; 4%; and 6%: (a) FA 5%; (b) FA 10%; and (c) FA 15%.
Figure 3. Composition of sulfur-containing concrete mixes with different content of bitumen modifier 2%; 4%; and 6%: (a) FA 5%; (b) FA 10%; and (c) FA 15%.
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Figure 4. Experimental research program.
Figure 4. Experimental research program.
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Figure 5. Sulfur particle size curve.
Figure 5. Sulfur particle size curve.
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Figure 6. Fly ash particle size distribution curve.
Figure 6. Fly ash particle size distribution curve.
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Jcs 07 00356 g007aJcs 07 00356 g007bJcs 07 00356 g007c
Figure 7. XRD patterns of raw materials: (a) sulfur (green); (b) sand (red); (c) crushed sandstone (dark blue); and (d) fly ash (purple). Used PDF-2 database cards: 1—quartz (PDF: 46-1045); 2—sulfur (PDF: 08-0247); 3—albite (PDF: 09-0466); 4—chlorite (PDF: 29-0701); 5—hematite (PDF: 33-0664); and 6—magnetite (PDF: 19-0629).
Figure 7. XRD patterns of raw materials: (a) sulfur (green); (b) sand (red); (c) crushed sandstone (dark blue); and (d) fly ash (purple). Used PDF-2 database cards: 1—quartz (PDF: 46-1045); 2—sulfur (PDF: 08-0247); 3—albite (PDF: 09-0466); 4—chlorite (PDF: 29-0701); 5—hematite (PDF: 33-0664); and 6—magnetite (PDF: 19-0629).
Jcs 07 00356 g007aJcs 07 00356 g007bJcs 07 00356 g007c
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Figure 8. Dependence of the density of sulfur concrete on the content of FA and bitumen at the age of 1 day (0, 2, 4, 6—bitumen content, % by weight of sulfur).
Figure 8. Dependence of the density of sulfur concrete on the content of FA and bitumen at the age of 1 day (0, 2, 4, 6—bitumen content, % by weight of sulfur).
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Figure 9. Dependence of the density of sulfur concrete on the content of FA and bitumen at the age of 28 days (0, 2, 4, 6—bitumen content, % by weight of sulfur).
Figure 9. Dependence of the density of sulfur concrete on the content of FA and bitumen at the age of 28 days (0, 2, 4, 6—bitumen content, % by weight of sulfur).
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Figure 10. Dependence of the compressive strength of sulfur concrete at the age of 1 day on the content of FA and bitumen (0, 2, 4, 6—bitumen content, % by weight of sulfur).
Figure 10. Dependence of the compressive strength of sulfur concrete at the age of 1 day on the content of FA and bitumen (0, 2, 4, 6—bitumen content, % by weight of sulfur).
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Figure 11. Dependence of the compressive strength of sulfur concrete at the age of 28 days on the content of FA and bitumen (0, 2, 4, 6—bitumen content, % by weight of sulfur).
Figure 11. Dependence of the compressive strength of sulfur concrete at the age of 28 days on the content of FA and bitumen (0, 2, 4, 6—bitumen content, % by weight of sulfur).
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Figure 12. Determination of the compressive strength of sulfur concrete: (a) sample before testing; (b) the sample under test; and (c) a fragment of the destroyed sample.
Figure 12. Determination of the compressive strength of sulfur concrete: (a) sample before testing; (b) the sample under test; and (c) a fragment of the destroyed sample.
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Figure 13. Dependence of change in water absorption of sulfur concrete at the age of 1 day on the amount of FA and bitumen (0, 2, 4, 6—bitumen content, % by weight of sulfur).
Figure 13. Dependence of change in water absorption of sulfur concrete at the age of 1 day on the amount of FA and bitumen (0, 2, 4, 6—bitumen content, % by weight of sulfur).
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Figure 14. Dependence of change in water absorption of sulfur concrete at the age of 28 days on the amount of FA and bitumen (0, 2, 4, 6—bitumen content, % by weight of sulfur).
Figure 14. Dependence of change in water absorption of sulfur concrete at the age of 28 days on the amount of FA and bitumen (0, 2, 4, 6—bitumen content, % by weight of sulfur).
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Figure 15. Photographs of the structure of sulfur concrete of the control composition: (a) without marking; and (b) marked (–, phase boundaries; –, shrinkage cavities).
Figure 15. Photographs of the structure of sulfur concrete of the control composition: (a) without marking; and (b) marked (–, phase boundaries; –, shrinkage cavities).
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Figure 16. Photographs of the structure of sulfur concrete composition type FA10/4: (a) without marking; and (b) with marking (–, phase boundaries; –, zones of dense packing of filler particles and gluing of sulfur binder with sand particles).
Figure 16. Photographs of the structure of sulfur concrete composition type FA10/4: (a) without marking; and (b) with marking (–, phase boundaries; –, zones of dense packing of filler particles and gluing of sulfur binder with sand particles).
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Figure 17. Photos of the structure of sulfur concrete composition type FA5/2: (a) without marking; and (b) marked (–, phase boundaries; –, zones of dense packing of filler particles and gluing of sulfur binder with sand particles; –, shrinkage cavities).
Figure 17. Photos of the structure of sulfur concrete composition type FA5/2: (a) without marking; and (b) marked (–, phase boundaries; –, zones of dense packing of filler particles and gluing of sulfur binder with sand particles; –, shrinkage cavities).
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Table 1. Characteristics of raw components.
Table 1. Characteristics of raw components.
Component NamePropertyActual Value
TSBulk density (kg/m3)1347
Sulfur mass fraction (%)99.95
Ash content (%)0.02
Mass fraction of organic substances (%)0.01
Mass fraction of acids in terms of sulfuric acid (%)0.002
Mass fraction of water (%)0.018
FABulk density (kg/m3)1180
Na2O0.65
MgO2.49
Al2O324.2
SiO248.45
K2O1.25
CaO7.3
TiO20.92
MnO0.069
Fe2O39.88
V2O50.02
Gr2O30.01
Stotal0.26
CO20.1
P2O51.71
Cu0.012
Zn0.019
Loss on ignition at 950 °C2.66
CSParticle size (mm)5–20
Bulk density (kg/m3)1385
Apparent density (kg/m3)2567
Resistance to fragmentation (wt %)12.0
The content of lamellar and acicular grains (wt %)8.4
SFineness modulus1.65
Bulk density (kg/m3)1462
The content of dust and clay particles (%)0.14
Content of clay in lumps (%)0.11
Organic and contaminant contentNo
Table 2. Mix proportioning.
Table 2. Mix proportioning.
Composition TypeConcrete Mixture Proportion per 1 m3
TS (kg/m3)FA (kg/m3)CS (kg/m3)S (kg/m3)Bitumen (kg/m3)
C60509688470
FA5/260512196872612.1
FA10/260524296860512.1
FA15/260536396848412.1
FA5/460512196872624.2
FA10/460524296860524.2
FA15/460536396848424.2
FA5/660512196872636.3
FA10/660524296860536.3
FA15/660536396848436.3
Table 3. Sand particle size gradations.
Table 3. Sand particle size gradations.
Residues on Sieves (%)Sieve Diameter (mm)
2.51.250.630.3150.16<0.16
Partial3.67.98.210.868.41.1
Total3.611.519.730.598.9
Table 4. Increase in compressive strength of sulfur concrete after 28 days of hardening in comparison with sulfur concrete after 1 day of hardening.
Table 4. Increase in compressive strength of sulfur concrete after 28 days of hardening in comparison with sulfur concrete after 1 day of hardening.
CompositionCFA5/2FA10/2FA15/2FA5/4FA10/4FA15/4FA5/6FA10/6FA15/6
Compressive strength growth (%)1.42.41.10.61.00.81.01.30.51.7
Table 5. Values of reduction in water absorption of sulfur concrete after 28 days of hardening in comparison with sulfur concrete after 1 day of hardening.
Table 5. Values of reduction in water absorption of sulfur concrete after 28 days of hardening in comparison with sulfur concrete after 1 day of hardening.
CompositionKFA5/2FA10/2FA15/2FA5/4FA10/4FA15/4FA5/6FA10/6FA15/6
Water absorption reduction (%)1.10.51.31.21.81.11.71.32.10.7
Table 6. Changes in the characteristics of sulfur concrete (∆) depending on the amount of FA and bitumen.
Table 6. Changes in the characteristics of sulfur concrete (∆) depending on the amount of FA and bitumen.
Characteristics of Sulfur ConcreteThe Content of FA (% wt) in the Composition of the Sulfur Concrete Mixture
51015
Bitumen Additive Content (% by Weight of Sulfur)
246246246
Density after 1 day (kg/m3)−0.04−0.120.08−0.120.120.250.040.21−0.08
Density after 28 days (kg/m3)0.250.080.450.4100.290.290.490.62
Compressive strength after 1 day (MPa)2.248.011.729.979.658.412.442.326.3
Compressive strength after 28 days (MPa)7.247.511.529.578.456.811.541.726.6
Water absorption after 1 day (MPa)−4.2−40.1−19.3−20.3−52.6−48.4−13.5−38.0−21.9
Water absorption after 28 days (MPa)−3.7−40.5−19.5−20.5−52.6−48.9−13.7−38.4−21.6
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MDPI and ACS Style

Stel’makh, S.A.; Shcherban’, E.M.; Beskopylny, A.N.; Mailyan, L.R.; Meskhi, B.; Shilov, A.A.; Evtushenko, A.; Chernil’nik, A.; El’shaeva, D.; Karalar, M.; et al. Physical, Mechanical and Structural Characteristics of Sulfur Concrete with Bitumen Modified Sulfur and Fly Ash. J. Compos. Sci. 2023, 7, 356. https://doi.org/10.3390/jcs7090356

AMA Style

Stel’makh SA, Shcherban’ EM, Beskopylny AN, Mailyan LR, Meskhi B, Shilov AA, Evtushenko A, Chernil’nik A, El’shaeva D, Karalar M, et al. Physical, Mechanical and Structural Characteristics of Sulfur Concrete with Bitumen Modified Sulfur and Fly Ash. Journal of Composites Science. 2023; 7(9):356. https://doi.org/10.3390/jcs7090356

Chicago/Turabian Style

Stel’makh, Sergey A., Evgenii M. Shcherban’, Alexey N. Beskopylny, Levon R. Mailyan, Besarion Meskhi, Alexandr A. Shilov, Alexandr Evtushenko, Andrei Chernil’nik, Diana El’shaeva, Memduh Karalar, and et al. 2023. "Physical, Mechanical and Structural Characteristics of Sulfur Concrete with Bitumen Modified Sulfur and Fly Ash" Journal of Composites Science 7, no. 9: 356. https://doi.org/10.3390/jcs7090356

APA Style

Stel’makh, S. A., Shcherban’, E. M., Beskopylny, A. N., Mailyan, L. R., Meskhi, B., Shilov, A. A., Evtushenko, A., Chernil’nik, A., El’shaeva, D., Karalar, M., Özkılıç, Y. O., & Aksoylu, C. (2023). Physical, Mechanical and Structural Characteristics of Sulfur Concrete with Bitumen Modified Sulfur and Fly Ash. Journal of Composites Science, 7(9), 356. https://doi.org/10.3390/jcs7090356

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