The Influence of Sewage Sludge Content and Sintering Temperature

materials Article The Influence of Sewage Sludge Content and Sintering Temperature on Selected Properties of Lightweight Expanded Clay Aggregate Jolanta Latosi ńska 1,* , Maria Zygadło˙ 1 and Przemysław Czapik 2 1 Faculty of Environmental Engineering, Geomatic and Energy Engineering, Kielce University of Technology, Al. Tysi ˛acleciaPaństwaPolskiego 7, 25-314 Kielce, Poland; [email protected] 2 Faculty of Civil Engineering and Architecture, Kielce University of Technology, Al. Tysi ˛acleciaPaństwa Polskiego 7, 25-314 Kielce, Poland; [email protected] * Correspondence: [email protected]; Tel.: +48-41-34-24-571 Abstract: Wastewater treatment processes produce sewage sludge (SS), which, in line with environmental sustainability principles, can be a valuable source of matter in the production of lightweight expanded clay aggregate (LECA). The literature on the influence of SS content and sintering temperature on the properties of LECA is scarce. This paper aims to statistically evaluate the effects of SS content and sintering temperature on LECA physical properties. Total porosity, pore volume, and apparent density were determined with the use of a density analyzer. A helium pycnometer was uti- lized to determine the specific density. Closed porosity was calculated. The test results demonstrated a statistically significant influence of the SS content on the specific density and water absorption of LECA. The sintering temperature had a significant effect on the specific density, apparent density, total porosity, closed porosity, total volume of pores, and water absorption. It was proved that a broad range of the SS content is admissible in the raw material mass for the production of LECA. Citation: Latosińska,J.; Zygadło,˙ M.; Czapik, P. The Influence of Sewage Keywords: lightweight expanded clay aggregate; sewage sludge; sintering temperature; density; Sludge Content and Sintering porosity; water absorption; statistical model; recycling Temperature on Selected Properties of Lightweight Expanded Clay Aggregate. Materials 2021, 14, 3363. https://doi.org/10.3390/ma14123363 1. Introduction Sewage sludge is an inevitable by-product of municipal wastewater treatment. The Academic Editor: Eddie Koenders amount of sewage sludge generated in the EU is constantly growing, and prognoses indicate the continuation of this trend [1–3]. Though sewage sludge constitutes only Received: 24 May 2021 1–2% of the treated wastewater volume, the cost of its treatment and disposal reaches Accepted: 15 June 2021 Published: 17 June 2021 60% of the total cost of wastewater treatment plant operations [4]. Sewage sludge is used in agriculture for its soil-forming and fertilizing properties. However, due to the Publisher’s Note: MDPI stays neutral risk of passing heavy metals, trace organic pollutants, and pathogenic organism from the with regard to jurisdictional claims in sludge into the environment, its application is largely restricted [5–9]. Formerly common published maps and institutional affil- landfilling practice has been banned in the European Union [10,11]. The recovery of iations. energy from sewage sludge in power plants and mono-incineration plants generates wastes despite reductions in waste volume and mass and elimination of harmful substances [12]. Waste-free utilization of sewage sludge together with the reduction in natural raw material use is desirable in the context of environmental sustainability. One of the solutions is the use of municipal sewage sludge in the production of LECA. Copyright: © 2021 by the authors. Light expanded clay aggregate (LECA) is produced from natural raw materials in a Licensee MDPI, Basel, Switzerland. ◦ This article is an open access article rotary kiln by sintering at 1100–1200 C[13,14]. LECA is commonly used in civil engineer- distributed under the terms and ing, gardening, geotechnology, and environmental engineering [13–19]. This wide and conditions of the Creative Commons varied range of applications is due to its characteristic properties: regular, almost spherical Attribution (CC BY) license (https:// shape of particles, surface glazing, total porosity up to 80%, and water absorption up to creativecommons.org/licenses/by/ 20% [13,14,20]. Moreover, it is fireproof, sound-absorbing, and resistant to chemical factors, 4.0/). mold, fungi, insects, and rodents [13,14,17]. Materials 2021, 14, 3363. https://doi.org/10.3390/ma14123363 https://www.mdpi.com/journal/materials Materials 2021, 14, 3363 2 of 17 The utilization of wastes in the production of LECA started in the 1990s [21]. Natural raw material was supplemented with waste glauconite [22], waste incineration bottom ash [23], fly ash [24], washings from a granite quarry [25], digested spent bentonite clay or basalt powder [26]. The tests have shown that also municipal sewage sludge containing 40–80% dry mass (d.m.) of the organic matter promotes the formation of the porous structure of LECA [27–29]. However, the influence of sewage sludge content and sintering temperature on the properties of LECA has never been fully tested. Yan et al. [23] studied the LECA sintering process, concentrating on the effects of sintering temperature, its rise rate, and duration. They found that the temperature rise rate had the least significant effect on the LECA properties and that sintering time had the most significant effect [23]. The aim of the present experiment was to evaluate the influence of both the sewage sludge content in the range of 0–30% and the sintering temperature in the range of 1100–1200 ◦C on the physical properties of LECA, such as specific density, apparent density, closed porosity, total porosity, total pore volume, and water absorption ability. 2. Materials and Methods 2.1. Materials The clay was collected from the deposit in Budy Mszczonowskie (Mszczonów, Poland), formerly exploited by the LECA production plant. The sewage sludge, stabilized and dewatered, was from the mechanical–biological wastewater treatment plant located in Sitkówka–Nowiny (Sitkówka-Nowiny, Poland). The wastewater treatment plant receives sewage from the Kielce metropolitan area. 2.2. Experiment Parameters According to the Rotatable Plan In order to increase the effectiveness of the regression function, a rotatable plan was adopted for two independent variables: sewage sludge content (x1), and sintering temperature (x2; Figure1). The experiment covered five independent repetitions at every point of the plan. Figure 1. Points determined according to the rotatable plan: x1—sewage sludge content % d.m.; ◦ x2—sintering temperature C. The sewage sludge content (0–30% d.m.) and the sintering temperature (1100–1200 ◦C) were established based on the authors’ own former test results [27,28] and the literature data [30,31]. Insignificant coefficients of the multiple regression function were eliminated with the Backward method (the elimination method) for the level of significance p < 0.1. Materials 2021, 14, 3363 3 of 17 The quadratic model of the multiple regression was used for the adopted rotatable plan [32]: yj = a0 + a1 · x1 + a2 · x2 + a11 · x12 + a12 · x1 · x2 + a22 · x22 (1) where x1 is sewage sludge content; x2 is sintering temperature; a0, a1, a2, a11, a12, a12, and a22 are coefficients for independent variables estimated with the least-squares method; and yj represents dependent variables representing specific density, apparent density, total porosity, closed porosity, total volume of pores, and water absorption. The significance of coefficients in Equation (1) were verified with an F-test [32]: N − K − 1 R2 F = · (2) K 1 − R2 where R is coefficient of multiple correlation; and N is number of coefficients of the regression function (i.e., a1, a2, a11, a12, a12, a22). 2.3. The Conditions of Forming and Sintering Procedures The raw clay was dried until it reached the air-dry state, ground in a disk-screw grinder, and pulverized in a mortar to fractions <1.0 mm. The sewage sludge was dried at 105 ◦C until the air-dry state and pulverized in a mortar to fractions <1.0 mm. Raw masses were prepared (150 g) with a variable sewage sludge content (Figure1). The sewage sludge and clay were mixed with distilled water until the mixture reached a plastic state. The content of mixing water was 27–31%. After that, cylindrical pieces 10 mm in diameter and 10 mm high (Figure2) were made with a hand press. The samples were air-dried at room temperature of ~20 ◦C and then in a laboratory drier (WAMED, Warsaw, Masovian, Poland) at 105 ◦C for 2 h. The drying shrinkage of the S7 sample (0% sewage sludge) was 12%, while that of S1–S6 and S8–S10 samples was from 11 to 13%. Figure 2. Dried S1–S10 samples. Materials 2021, 14, 3363 4 of 17 The dried samples were sintered in a laboratory furnace (Nabertherm GmbH, Lilien- thal, Germany) in an oxygen atmosphere at preset temperatures (Figure1). The time of sintering was 60 min, including 10 min at the maximum temperature. After sintering, the samples remained in the furnace until they cooled down to 100 ◦C. 2.4. Methods The oxide composition of clay was tested with the use of an X-ray fluorescence spectrometer (XRF; PANalytical, Almeo, Netherlands). The characteristics of sewage sludge were established according to [33–38]. The phase compositions of the sewage sludge, clay, and S1–S10 samples were determined with Debye–Scherrer–Hull X-ray powder diffraction. An Empyrean diffractometer was used for this purpose (PANalytical, Almeo, The Netherlands). The test was conducted in the range of angles 6–70 ◦2θ with the use of a Cu lamp and an X’Celerator strip detector. The results were processed using the HighScore Plus program (v.4.7., PANalytical, Almeo, The Netherlands). Qualitative analysis was based on the ICDD PDF-2 database. Data from the Crystal- lography Open Database (COD) were used for quantitative analysis, which was performed with the Rietveld method on the basis of the qualitative analysis. Total porosity, total pore volume, and apparent density were determined with the use of a GeoPycTM 1360 density analyzer (Micromeritics, Norcross, GA, USA).

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