Reuse of ornamental rock processing sludge into adhesive mortarsAbstract
Abstract The ornamental stone industry generates large volumes of sludge during its processing. The objective of this research is to evaluate the production of adhesive mortar with partial replacement of fine aggregate by this residue. Physical, chemical, and mineralogical characterizations of the materials were conducted, and formulations were prepared with varying percentages of sludge replacing the fine aggregate. Tests on fresh and hardened adhesive mortars were conducted to verify the product quality. The results indicate a decrease in the consistency index as the sludge replacement percentage increases. Formulations with 100% (dry basis) replacement of sludge showed lower tensile bond strengths and did not meet regulatory standards, whereas formulations with up to 60% residue achieved tensile bond strengths greater than 0.5 MPa, according to the curing conditions. Therefore, there is potential to use industrial solid waste in greater proportions in the production of adhesive mortars, depending on the curing method, thereby minimizing the extraction of non-renewable natural resources as raw materials for this type of construction product.
Keywords:
industrial solid waste; adhesive mortar; properties; durability
Resumo
Resumo A indústria de rochas ornamentais gera grandes volumes de lama durante seu processamento. O objetivo desta pesquisa é avaliar a produção de argamassa colante com substituição parcial do agregado miúdo por esse resíduo. Foram realizadas caracterizações físicas, químicas e mineralógicas dos materiais, e formulações foram preparadas com diferentes percentuais de lama substituindo o agregado fino. Ensaios em argamassas colantes frescas e endurecidas foram conduzidos para verificar a qualidade do produto. Os resultados indicam uma diminuição no índice de consistência à medida que o percentual de substituição por lama aumenta. Formulações com 100% (base seca) de substituição apresentaram menores resistências de aderência à tração e não atenderam aos padrões regulatórios, enquanto formulações com até 60% de resíduo atingiram resistências de aderência à tração superiores a 0,5 MPa, de acordo com as condições de cura. Portanto, existe potencial para o uso de resíduos sólidos industriais em maiores proporções na produção de argamassas colantes, a depender do método de cura, minimizando a extração de recursos naturais não renováveis como matéria-prima para esse tipo de produto de construção.
Palavras-chave:
resíduo sólido industrial; argamassa colante; propriedades; durabilidade
1 INTRODUCTION
The construction industry plays a crucial role in Brazil's economy, but it is also a major driver of environmental impacts that degrade natural areas. In Brazil, the degradation caused by the sector occurs in three distinct stages: during the extraction and production of materials, during construction, and in the disposal of waste generated by the process. Production of Portland cement, for example, is considered a potentially polluting practice due to the generation of a high volume of carbon dioxide (CO2) in the calcination phases (around 8-9%), fuel combustion, and electricity use [1]. To minimize this impact, the use of alternative raw materials, such as industrial solid waste, can help reduce the consumption of non-renewable resources and ensure the proper disposal of these co-products by the industries that generate them, for example, in the cementitious materials industry [2].
However, in addition to the cement industry, data published by the National Association of Aggregate Producers for Construction [3] indicate that global aggregate production, including sand and crushed stone, totaled 40 billion tons in 2023. The state of Rio Grande do Sul, in Brazil, alone accounts for approximately 10 million tons of sand. Ramadon [4] considers sand extraction one of the most harmful practices, responsible for pollution, alteration of watercourses, increased siltation, soil erosion, and destruction of permanent preservation areas.
Given that Brazil is ranked 3rd among the world's ceramic tile producers and 3rd among consumers [5], adhesive mortar is an indispensable product for the fixing process. Given that industrialized adhesive mortar is primarily composed of Portland cement, mineral aggregates, and chemical admixtures, it is necessary to seek alternatives to minimize the product's environmental impacts.
From this perspective, waste recycling can be a way to diversify the supply of construction raw materials, making it viable given its low market cost. Among the available waste materials is the ornamental rock processing sludge (ORPS) [6]. According to data from ABIROCHAS [7], the gross Brazilian production of ornamental rocks totaled 9,000,000 tons, mainly granite, marble, and quartzite. Of this volume, 20% to 40% is in the form of sludge, resulting from the quarrying process [8], [9].
Regarding chemical admixtures in adhesive mortars, they ensure the workability of cementitious mixtures for use in internal and external wall coverings and in floor laying. The performance of these mortars depends directly on the interaction between their components. The materials can be replaced with others of finer granulometry, provided that the particle size distribution can be adjusted and the appropriate polymers are selected to meet the mortar's needs, thus avoiding chemical and physical damage [10].
Numerous studies have already used industrial solid waste in the production of adhesive mortars: bottom ashes from forest biomass combustion [10], sulfonated polystyrene [11], marble powder [12], granite powder [13], glass powder [14], scrap tire rubber particles [15], quarry dust [16], and marble and granite sludge [17]. However, most available studies focus on relatively low levels of cement or sand replacement, adopting a conservative approach aimed primarily at verifying the compatibility of the residue with the cementitious matrix and preserving minimum performance properties. Furthermore, investigations into the behavior of these adhesive mortars under conditions simulating real-world use are still limited, especially when incorporating high levels of industrial solid waste.
Given this context, the overall objective of this investigation is to evaluate the feasibility of recycling ornamental rock processing sludge as a substitute for natural sand in the production of adhesive mortars. The combination of these materials and the analysis of their behavior under various exposure conditions are fundamental for performance, compared with traditional residue-free adhesive mortar.
2 MATERIALS AND EXPERIMENTAL PROGRAM
To produce the adhesive mortars, CP II F–40 cement, natural fine aggregate (quartz river sand), ornamental rock processing sludge (ORPS), ethylene vinyl acetate-based polymer admixture (DA 1200 - Dairen Chemical Corporation), cellulose ether-based admixture (MKW 4000 PF 01), and water were used. ORPS waste is a mixture of ornamental rocks (granite, marble, and basalt) and was collected from a company in São Leopoldo, RS, Brazil. Sampling was performed by quartering the sludge from the collection wells. The polymers were incorporated to improve the plasticity, workability, and mechanical strength of the adhesive mortars.
The chemical and physical characterizations of the residue are shown in Table 1, and its granulometric, mineralogical, and morphological characteristics are illustrated in Figure 1. Based on these characterizations, the residue shows heterogeneity typical of commercial rocks, the absence of high percentages of oxides that could cause expansion in cementitious composites (potassium, sodium, and manganese), high crystallinity, and angular and irregular particles.
The sludge was dried in an oven at 105 ± 5 °C for 48 hours, resulting in a moisture content of 0.30%. The results of the physical characterization of anhydrous cement and sand fines (passing through sieve #150) are shown in Table 2.
The partial mass replacement percentages of fine aggregate containing ORPS were 0, 20, 60, and 100% of the fines passing through the 0.150 mm sieve. These percentages were chosen to balance the representativeness of the scenarios with experimental feasibility, avoiding an excessive number of compositions without compromising the analysis of the system's behavioral trends. The latter was developed for type AC II, using a 1:2.5 (by mass) ratio, 5% PVA, 0.4% cellulose ether, and a water/cement ratio (w/c) of 0.70. Table 3 presents the quantity of material used in the respective adhesive mortars, on a dry solid’s basis.
The used standard substrate was produced in accordance with ABNT NBR 14081-2 [18] and had the following dimensions: 250 mm x 500 mm x 20 mm. The test surface remained was exposed for 48 hours under laboratory conditions, free from any powdery material and contaminants that could impair the adhesion of the substrate.
The adhesive mortars were produced as described in NBR 14081-2 [18] and tested as recommended by current Brazilian standards. The mixing speed was slow rotation at 140 ± 5 rpm and planetary motion at 62 ± 5 rpm. The preparation and curing of the mortars occurred at a temperature of 23 ± 2°C and a relative moisture of 60 ± 2%.
The rheological characterization was carried out in the fresh state, by consistency index according to NBR 13276 [19]. The density and incorporated air content were developed according to NBR 13278 [20]. The water retention was developed according to NBR 13277 [21]. The determination of slip test was according to NBR 14081-5 [22] and the analysis of wetting power and transfer from DIN EN 1347 [23], using four samples for each test. The temperature of the analyses ranged from 29 to 32 °C under a moisture of 60 ± 2%. In the hardened state, the open time determination test was carried out according to NBR 14081-3 [24] using one sample per formulation and tensile bond strength according to NBR 14081-4 [25] at 28 days of age, using four samples per mix, totaling sixteen.
In the tensile bond strength test, the samples were subjected to 4 different climatic conditions to which adhesive mortars are exposed daily. They were tested under normal curing conditions (I), where the temperature is controlled at 23 ± 2°C and humidity at 60 ± 2%; water immersion curing (II), which remained for 7 days under normal conditions and the remaining 21 days submerged in a tank with a controlled temperature of 23 ± 2°C; oven curing (III), where for the first 14 days the samples remained under normal conditions and after this period, they remained the rest of the time in an oven at a temperature of 70 ± 2°C; and finally, curing in a hygrothermal chamber (IV), under accelerated aging by thermal exposure (heat, rain, and dew) for 14 days, based on the study by Constantino et al. [26], it consists of heating and cooling stages.
Each cycle lasted 60 minutes, with 20 minutes for the temperature ramp-up (heating or cooling) and 40 minutes for stable conditions, for a total of 120 minutes per cycle. During heating, the temperature was raised from 3 °C to 38 °C, while during cooling, it was reduced from 38 °C to 3 °C. Relative humidity was controlled at two levels: 43% (minimum) and 94% (maximum). The choice of these values aimed to simulate contrasting environmental exposure conditions, representing low temperature and high humidity (humid climate) and high temperature and lower relative humidity (dry climate), to evaluate the material's behavior under representative hygrothermal variations.
3 RESULTS AND DISCUSSIONS
3.1 Fresh state
Table 4 presents the average results for the adhesive mortars in the fresh state for each formulation.
It is noticeable that the greater the replacement of the fine sand fraction by the ornamental rock processing sludge, the lower is the consistency. Among the factors that explain this phenomenon is the increase in the content of fine materials, also verified by Pereira et al. [27]. High-fineness materials tend to increase the w/c ratio due to their greater specific surface area [28]. The low sphericity and rough microstructure of ORPS require a higher water content for adequate workability. In addition, the type and granulometry of the fine aggregate directly impact the fresh and hardened state of the cementitious matrices [29].
According Carasek et al. [30], the mortar consistency shows a direct correlation with the aggregates used, particularly with respect to the angle of friction and packing factor. The second factor has a strong influence on the void index, the unit mass, and, consequently, on the material's porosity, being mainly determined by the particles' shape and geometry. Given this, a change in the consistency index behavior due to the partial replacement of fine aggregate with ORPS was already expected.
Comparing the extreme mixes, REF and 100% ORPS, the difference is 8.4% in density and approximately 59% in the incorporated air content, with one result inversely proportional to the other. For the denser mix, there is less void content and, consequently, less air. These results directly affect consistency, with a maximum difference of approximately 26%.
According to Harbi et al. [31], small particles fill the voids, increase the material's density and release the water retained in the pores. One hypothesis is that releasing this water decreases consistency, as observed for the formulation with higher ORPS incorporation. Wyrzykowski et al. [32] add that the void index directly affects the performance of the adhesive mortar in the fresh state.
The water retention allows the material to be applied in a thin layer, without reducing the amount of water needed for the hydration of Portland cement, either in the base or in the environment. The amount of water retained by the mortar results in higher bond strengths, better productivity, and greater durability, due to greater formation of hydration products and stronger bonds between the coating and the substrate. In addition, water retention affects workability by altering the interactions among constituents and, consequently, mechanical strength. Thus, it was observed that the residue had no effect on the water retention results, indicating that the amount of cellulose ether-based admixture was the main determining factor, providing plasticity and cohesion to the adhesive mortar.
Regarding the slippage of the samples, despite the reduction in the workability of the adhesive mortar as indicated by the consistency index, there were no harmful effects, and the slippage was 0 mm during 20 minutes they remained in the vertical position. This can be explained by the particle size and/or the morphology of the residue, which prevents the ceramic tile from slipping. Pereira et al. [27] explain that the less spherical the particles are, the greater the shear stress for flow.
Table 5 presents the wettability of the vitreous surface covered with the different mortars to estimate the transfer capacity over time, considering a total area of 2500 mm2.
It can be observed that the transfer capacity of the mortar decreases with exposure time and with increasing ORPS; that is, the longer the mortar's exposure time, the lower the adhesion of the ceramic piece to the mortar. In addition, it was found that within the first 10 minutes of application, the mortar already showed deficiencies in covering the tile surface. These facts are consistent with the slip values (see Table 3), and similar behaviors were also observed by Modolo et al. [10].
According to Bühler et al. [33], an upper layer forms that hardens faster than the material's interior, reducing its deformation and adhesion capacity. The formation of this layer depends on the mortar formulation, substrate type, application technique, and climate. In this investigation, given the fineness of the ORPS and the high levels of replacement, the adhesive mortars require more water for film formation and to improve wettability, corroborating the consistency data.
3.2 Hardened state
Figure 2 illustrates the values obtained in the tensile bond strength determination test under the four exposure conditions of the adhesive mortars. As can be seen, all formulations, except the 100% ORPS replacement, met the Brazilian standard in at least one analysis condition and presented tensile bond strengths at 28 days greater than 0.5 MPa.
Some factors could explain the decrease in values of this mechanical property, mainly under oven conditions and hygrothermal exposure. Researchers attribute it to the following factors: high temperatures increase the porosity of the cementitious matrix [34], the higher degree of water saturation in the pores degrades the mechanical properties of the composites [35], the polymeric film that penetrates the pores of the substrate can be destabilized due to thermal sensitivity [36], high temperature increases the expansion rate of the cementitious paste, which produces high internal stresses and generates microcracks [37], as well as the change in the glass transition of the polymers negatively impacting temperature variations [38].
Furthermore, according to Carasek et al. [39], high levels of fines impair the adhesion of mortars. This can occur in two ways: very fine particles can penetrate the pores of the substrate and fill the space of the hydrated cement products, or pores smaller than those of the substrate can prevent the mortar from being drawn into the substrate. In general, the decreases in strength with increasing ORPS content corroborate the studies by Buyuksagis et al. [12] and Pereira et al. [27].
Table 6 presents the analysis of variance (ANOVA) for the different curing types and formulations investigated. Based on the results, there is a significant difference between these variables and between their interactions, with a significance level of 95% (p < 0.05). Additionally, applying Tukey's test, it was found that the hygrothermal condition differentiates the behavior in relation to the other conditions, but homogenizes the formulations among themselves, belonging to the same homogeneous group; the ambient and submerged conditions do not show significant differences; and high substitutions (60–100% ORPS) increase the differences in relation to REF.
Regarding the open time determination test, Figure 3 shows that partial replacement of fine aggregates with ORPS directly affects the test. Póvoas [40] reports that this method measures the time required for the adhesive mortar to lose water, due to suction from the base or evaporation into the environment. This loss occurs soon after mortar is applied to the substrate, thereby reducing its adhesion strength.
However, it was observed that the 20% ORPS and 60% ORPS mortars reached tensile adhesion strengths after 20 minutes, meeting the normative requirements for AC II. The gains in mechanical strength over the open time were 126% for 20% ORPS and 78% for 60% ORPS, compared to the minimum value of 0.5 MPa. The percentage variations for the formulations were -2.59% with 20% ORPS, -23.28% with 60% ORPS, and -99.93% with 100% ORPS, compared to the REF adhesive mortar. This gradual reduction in performance may be related to the agglomeration of residue particles around the cement particles [41]. It is believed that due to the smaller hydrated cementitious area required to ensure adhesion, there is an increase in matrix porosity and, therefore, lower strength is expected.
Despite the numerical results of the tests above, it is fundamental to understand the behavior of adhesive mortars in relation to failure or rupture patterns. It was observed that the system rupture occurred predominantly in the mortar layer and at the interface between the adhesive mortar and the ceramic tile, regardless of the curing condition. Despite this, up to 60% ORPS was sufficient to ensure mortar anchorage to the ceramic substrate, due to its surface porosity. Figure 4 illustrates the rupture mode of the investigated samples.
This behavior was also verified by [42] when using basalt rock powder in the production of adhesive mortars. The results of the open time and tensile strength tests decreased with the substitution of fine aggregate by waste.
According to Scartezini and Carasek [43], the substrate is primarily responsible for tensile bond strength, since its high surface roughness either confers or does not confer tensile bond strength to the mortar. Complementarily, Oliveira et al. [44] point out that the roughness (including peaks and valleys) and topography of the ceramic substrate, as well as the interface area between the ceramic substrate and the cementitious matrix, directly affect the adhesive properties between these materials. Almeida et al. [45] finally report that the adhesive mortar/ceramic tile interface is where the most significant principal stresses are concentrated when evaluating the thermal action in facade coatings.
4 CONCLUSIONS
This research investigated the total or partial replacement of fine aggregates with ornamental rock processing sludge in the production of adhesive mortars, under different exposure conditions, to simulate real environmental conditions. Based on the results obtained, it can be concluded that:
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The formulation with up to 60% ORPS proved ideal for ensuring tensile bond strength in ambient and submerged curing, as well as adequate open time, meeting Brazilian standards;
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Adhesion decreased with increasing temperature under curing conditions in the oven and hygrothermal chamber;
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The formulation with 100% ORPS showed the lowest tensile bond strength under all investigated conditions;
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High levels of ORPS require more water to form the spreading film.
Finally, it is recommended that future studies focus on the effects of waste on microstructural analysis under harsh environmental conditions, on life cycle assessment, and on the life cycle cost of this cementitious material, to complement the understanding of the behavior observed in this investigation.
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Correspondence
Corresponding author:Bianca Carlin Cadore. E-mail: biancadore96@gmail.comConflict of interest:
Editors:
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