2.1. Materials
To comprehensively assess the impact of Refuse-Derived Fuel (RDF) on the ceramic mass and experimentally validate its potential to enhance the thermal insulation properties of clay blocks, a meticulous laboratory simulation of the entire production process was conducted. The objective was to investigate the effects of RDF incorporation from the initial processing of raw clay material to the final firing of the samples, accompanied by essential tests on the fired specimens. While the laboratory tasks adhere to standard clay material testing procedures, the unique nature of the RDF additive necessitated a modified approach.
Three distinct mixtures were formulated and evaluated in this study. The first mixture, designated as "TZ," consisted solely of plain clay material. The second mixture, labeled "TZRDF10," combined clay material with 10% raw RDF, while the third mixture, identified as "TZRDF10 P," integrated clay with 10% processed RDF. In all mixtures, the requisite amount of water was added to facilitate uniform blending. It's noteworthy that the clay material utilized in all three cases originated from the same quarry to isolate the impact of RDF exclusively. The clay material, sourced from CHALKIS S.A. in the Vasiliko Evia region, has been employed for tile production at the factory for over two decades and falls under the classification of inorganic clay with moderate plasticity, according to ISO 14688-2:2017.
The chemical composition of the clay was determined and is detailed in
Table 4. The analysis was conducted using Atomic Absorption Spectrometry (AAS), adhering to ISO 26845:2016 standards. Furthermore, the granular characteristics of the TZ material were examined in accordance with ASTM D422-63 (2007), as it can be seen in
Table 5. The clay's average density, assessed following ASTM D698-12, stands at approximately 1781 Kg/m
3. Upon transportation from the manufacturing site to the laboratory, the clay exhibited an average moisture content of 8.15%.
Table 3 provides a comprehensive overview of the fundamental characteristics of the TZ material [
10]. In accordance with ISO 14688-2:2017 classification, TZ can be described as an inorganic clay with a medium level of plasticity.
The RDF employed in this study was procured from one of the largest waste management companies in the Mediterranean. Differentiating between raw and processed RDF was crucial, primarily due to their influence on the production process. The physical attributes of the acquired non-hazardous RDF are detailed in
Table 6. Furthermore,
Table 7 presents the metal content, while
Table 8 offers insights into the presence of halides and sulfur. Lastly,
Table 9 provides an analysis of the organic content, as indicated by the Total Organic Carbon (TOC) measurement [
11].
Raw RDF refers to its original form when added to the mix, whereas processed RDF undergoes grinding and shredding before integration [
12]. This differentiation was deemed necessary due to the heterogeneous nature of RDF, comprising biodegradable materials, primarily paper and plastics, with occasional wood and varying types of plastic pieces, ranging from soft bag fragments to rigid components from packaging or even razor handles. The inclusion of processed RDF was chosen to ensure more consistent results and to address any potential issues arising from the raw form.
The laboratory procedures encompassed both quality control, focusing on material properties and the extrusion process, and technological control, which involved tests simulating factory conditions and processes. Quality control included the calculation of calcium carbonate content (calcimetry) and grain size estimation (granulometry) and was conducted solely on the pure clay material mixture, as RDF addition did not affect these results. Technological testing comprised the calculation of Pfefferkorn plasticity, the manufacture of specimens in a high-pressure press under vacuum, evaluation of the drying cycle, determination of bending strength for dried specimens, assessment of re-absorption capacity in dried specimens, evaluation of specimen properties and density calculation for dried specimens.
This comprehensive methodological approach allowed for a rigorous examination of how RDF incorporation impacts each stage of the brick manufacturing process and its potential for enhancing the production environment in a brick plant [
13]. The results obtained from these tests form the basis for drawing meaningful conclusions regarding the utilization of RDF in ceramic mass, particularly in the context of environmentally friendly brick production.
In the course of these experiments, silica sand was employed in conjunction with RDF, with the primary objective of reducing the size of the RDF particles through the use of a hammer mill. Silica sand primarily consists of two main elements: oxygen and silica. More specifically, silica sand is primarily composed of silicon dioxide (SiO
2). Quartz, a crystalline mineral constituted by silicon dioxide, is known for its chemical inertness and relatively high hardness, rating 7 out of 10 on the Mohs hardness scale [
14]. The selection of this particular type of sand, denoted as ZK, was driven by its finer texture and its absence of unwanted additives, making it a preferable choice over sea sand or sandy clays All the tested materials can be seen in
Figure 2.
One notable challenge encountered in this process arises from the composition of RDF, which predominantly includes plastic and paper materials. These components, owing to their lightweight nature, cannot be effectively ground within the hammer mill, especially given the elevated temperatures generated inside the mill. Furthermore, the RDF particles are unable to pass through the metallic screen with a 2mm mesh size. To overcome this issue and facilitate the study, a 1:1 mixture of RDF and sand was adopted, streamlining the grinding process for the RDF component. The grain size of the sand can be seen in
Table 10.
2.2. Methods
The initial phase of this study involved the drying of all the aforementioned materials in a laboratory electric dryer of the SCN/400/DG model, maintaining a temperature of 105°C for a duration of twenty-four (24) hours. Subsequently, the clay and sand materials were subjected to preliminary crushing using a jaw crusher, specifically model A92, featuring jaws with a 2mm clearance. In the case of the clay material and the RDF-sand mixture, intended for the formulation of mixture no.3 (TZRDF10 P), these materials underwent further processing through a laboratory hammer mill, designated as Mod. HM/530 Series. This mill utilized a 1mm mesh screen to facilitate the comminution process.
The materials were meticulously weighed according to their respective mixing ratios, taking into account their prevailing moisture content. Subsequently, these materials were thoroughly blended according to the specific formulation for each mixture. This blending process occurred within a kneading mixer, where the requisite amount of water was carefully introduced. The addition of water was meticulously controlled until achieving an optimal plasticity index, determined through the Pfefferkorn's test.
The Pfefferkorn plasticity method hinges on the observation of the sample's deformation in response to the calibrated plate's descent onto the underlying test body, shaped with the aid of an auxiliary shaping tool [
15]. This test employs two distinct reading scales, one measuring the deformation in millimeters, and the other determining the deformation in line with the Pfefferkorn theory. For our study, the Pfefferkorn plasticity tester employed was Ceramic Instruments 01CI4540, and we adopted the calculation method described by Andrade et al [
16]. It is crucial to emphasize that the amount of water added is unique to each premixture and is contingent upon the clay material's absorbent properties and the specific extrusion process employed for a given type and final product.
The uniformly blended mixture for each test underwent extrusion through a vacuum-extrusion process to form rectangular samples of standardized dimensions [
17]. The laboratory extruder, specifically the HANDLE KHS-Type: PZVM8b model, was employed for this purpose. The wet material, post-mixing, was loaded into the feeding chamber, equipped with an upper porch for material input, followed by a pre-extruder mixer incorporating a screw mixer responsible for propelling the material through an air vacuum chamber and out of the extruder's outlet,
Figure 3. The extrusion process was carefully monitored, including pressure levels, through a pressure gauge. The extruder's outer section allowed for the incorporation of interchangeable molds, facilitating the production of extruded products in various sizes and shapes. All the extruded samples were solid, lacking any hollow spaces within their mass, and conformed to a standardized size of 120 × 20 × 20 mm (length × width × height). Notably, the vacuum pressure applied during the extrusion process remained consistent and uniform across all tested mixtures, consistently registering at 0.8 kp/cm2. The plasticity, as assessed by the Pfefferkorn method, fell within the range of 0.7 to 0.9 for all mixtures, achieved by carefully adjusting the water content. In total, each test involved the construction of fifteen (15) individual samples. Consequently, across all three (3) mixtures examined, a total of 45 samples were meticulously prepared (3 mixtures × 15 samples).
2.3. Drying procedure
The drying process for all extruded specimens was conducted systematically within a laboratory electric oven of SCN/400/DG type. This drying cycle comprised three distinct phases [
18], each demanding meticulous attention to address potential issues related to the samples, as can be seen in Figure 5.
The initial "humidity" phase was characterized by maintaining a high ambient humidity within the dryer, an essential step to keep the surface pores of the bricks open. This phase is particularly critical, as any mismanagement may result in the development of cracks, deformations, or fragility in the bricks.
Subsequently, during the "shrinkage critical point phase," it was imperative to ensure that the drying shrinkage was completed before the temperature increased significantly for the final drying phase. It was crucial to manage the temperature rise gradually to prevent any cracking issues.
In the last phase, the primary objective was to minimize the remaining body humidity within the bricks as much as possible. All regulations and settings during these phases were tailored to the specific production mixture and its unique behavior.
The initial focus of the drying process was to keep the surface pores of the samples open to facilitate the gradual loss of humidity from the internal body. This phase represented the most critical juncture. In the subsequent phase, as the temperature rose and dryer humidity decreased, any mishandling could lead to the occurrence of cracks, deformations, or increased fragility in the bricks. The dried samples resulting from this carefully orchestrated drying process are illustrated in
Figure 4.
2.4. Drying sensitivity of samples
Drying sensitivity assessment for the formulated mixtures involved the individual application of Bigot's curve method [
19]. Under controlled conditions, the test samples were exposed to a temperature of 25°C within the laboratory dryer, with the humidity level maintained at a stable 75% inside the dryer. Bigot's curve, a graphical representation, illustrated the fluctuations in water content relative to linear shrinkage over a 24-hour period.
Bigot's curve method divides the drying process into two distinct phases. The initial phase, characterized by a constant and rapid drying rate, is indicated by a high linear correlation coefficient. This phase remains consistent until the critical point is reached. Subsequently, in the second phase, the drying rate gradually decreases, and shrinkage approaches its conclusion [
20].
The laboratory dryer, a crucial component of this study, was equipped with the necessary instruments to analyze the drying shrinkage behavior of the green brick samples. Comprising three essential sections – the tunnel dryer unit, the air preparation unit, and the control system incorporating measurement sensors and data acquisition – the dryer had a volume of approximately 125 cm3 and was thoughtfully insulated to minimize heat loss to the surroundings.
Within the air preparation unit, an adjustable centrifugal fan and an adjustable electrical heater played key roles. The centrifugal fan drew drying air from the ambient surroundings. The temperature of the drying air was precisely controlled through a PID-regulated system (Jumo Dtron 304). The drying air, initially passing through an electrical heating zone, then flowed over the sample, maintaining a parallel trajectory to the surface of the sample positioned on a wire mesh. The distance between the hot air inlet and outlet within the tunnel dryer unit was 75 cm, with a 35 cm separation from the air inlet to the sample holder.
To establish steady-state testing conditions, the air fan and electrical heater were initially engaged. Subsequently, a green brick sample was placed on the metallic carrier. Throughout the experiments, the humidity level of the drying air was meticulously monitored. Relative humidity within the dryer was measured every 5 minutes using a humidity sensor (TMI Orion—CeriDry), adhering to the precise measurement procedures and methodology outlined by Makrygiannis and Karalis [
21]. The drying sensitivity level was determined by the CSB index, an indicator of drying sensitivity according to Bigot. The classification of sensitivity levels is presented in
Table 11.