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Kinetics of Dehydroxylation and Decarburization of Coal Series Kaolinite During Calcination: a Novel Kinetic Method Based on Gaseous Products

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Kinetics of Dehydroxylation and Decarburization of Coal Series Kaolinite During Calcination: a Novel Kinetic Method Based on Gaseous Products materials Article Kinetics of Dehydroxylation and Decarburization of Coal Series Kaolinite during Calcination: A Novel Kinetic Method Based on Gaseous Products Simeng Cheng 1, Shaowu Jiu 1 and Hui Li 1,2,* 1 College of Materials Science and Engineering, Xi’an University of Architecture and Technology, Xi’an 710055, China; [email protected] (S.C.); [email protected] (S.J.) 2 Shaanxi Ecological Cement Concrete Engineering Technology Center, Xi’an 710055, China * Correspondence: [email protected] Abstract: The analysis of gaseous products reveals the characteristics, mechanisms, and kinetic equations describing the dehydroxylation and decarburization in coal series kaolinite. The results show that the dehydroxylation of coal series kaolinite arises from the calcination of kaolinite and boehmite within the temperature range of 350–850 ◦C. The activation energy for dehydroxylation is 182.71 kJ·mol−1, and the mechanism conforms to the A2/3 model. Decarburization is a two-step reaction, occurring as a result of the combustion of carbon and the decomposition of a small amount of calcite. The temperature range in the first step is 350–550 ◦C, and in the second is 580–830 ◦C. The first step decarburization reaction conforms to the A2/3 mechanism function, and the activation energy is 160.94 kJ·mol−1. The second step decarburization reaction follows the B3 mechanism function, Citation: Cheng, S.; Jiu, S.; Li, H. wherein the activation energy is 215.47 kJ·mol−1. A comparison with the traditional methods proves Kinetics of Dehydroxylation and that the kinetics method utilizing TG-FTIR-MS is feasible. Decarburization of Coal Series Kaolinite during Calcination: A Keywords: coal series kaolin; TG-FTIR-MS; kinetics; reaction mechanism Novel Kinetic Method Based on Gaseous Products. Materials 2021, 14, 1493. https://doi.org/10.3390/ ma14061493 1. Introduction Academic Editors: Coal plays a vital role in the current energy supply worldwide, especially in China [1]. Francesco Pomponi and Coal series kaolinite (CSK) is one of the foremost types of coal gangue, with confirmed Mostafa Seifan reserves of 1.673 billion tons and prospective reserves of 5.529 billion tons in China alone [2]. Worldwide, CSK is also distributed in major kaolin producing countries such as the United Received: 18 February 2021 States, Australia, the United Kingdom, Russia, the Czech Republic, Germany, and Brazil, Accepted: 15 March 2021 among others. CSK is typically abandoned as coal mine waste, resulting in serious ecolog- Published: 18 March 2021 ical and environmental pollution [3,4]. However, CSK is an ideal resource for replacing high-quality natural kaolin. Calcination is a typical method to achieve high chemical reac- Publisher’s Note: MDPI stays neutral tivity of CSK prior to further applications, such as preparation of calcined kaolin products with regard to jurisdictional claims in and metakaolin cementitious materials [5,6]. Dehydroxylation and decarburization are the published maps and institutional affil- main reactions during the calcination of CSK [7–9]. The activity of metakaolin prepared iations. from CSK depends essentially on the dehydroxylation reaction. However, the whiteness of addition agents from CSK (used in paints, plastics, coatings, and ceramics) is signifi- cantly affected by the decarburization reaction. Therefore, it is essential to characterize the dehydroxylation and decarburization reactions in CSK and to study their reaction Copyright: © 2021 by the authors. characteristics, mechanism, and kinetics. Licensee MDPI, Basel, Switzerland. The traditional thermal analysis method, based on the data of mass or heat by Thermo- This article is an open access article gravimetric analysis-Differential Scanning Calorimetry (TG-DSC), is commonly used for distributed under the terms and reaction kinetics [10–15]. The decarburization and dehydroxylation reactions in CSK are conditions of the Creative Commons synchronous, and the mass loss and exothermic heat generation are almost simultaneous. Attribution (CC BY) license (https:// Therefore, the decarburization and the dehydroxylation in CSK cannot be characterized creativecommons.org/licenses/by/ by either the mass or heat, which is a major challenge for CSK calcination. The kinetics 4.0/). Materials 2021, 14, 1493. https://doi.org/10.3390/ma14061493 https://www.mdpi.com/journal/materials Materials 2021, 14, 1493 2 of 13 calculated from TG/DSC data present the apparent characteristics of the whole calcina- tion reaction of CSK, but not the real characteristics of dehydroxylation and decarbur- ization [5,16,17]. Nonetheless, the gaseous products released by the reactions in CSK are different, which can be distinguished by detecting product release. With the development of thermal analysis technology, Thermogravimetric analysis-Fourier Transform Infrared Spectrometer-Mass Spectrometer (TG-FTIR-MS) technology has been widely used to detect gaseous products [18–20]. In TG-FTIR-MS, the gaseous products can be detected and identified by the FTIR detector. The release flows of gaseous products can be recorded by MS, providing an effective means for analyzing complex reactions [21]. There are several applications of TG-FTIR and TG-MS, combined for the analysis of reaction mechanisms and kinetics, but there has been no report till date on the kinetics of CSK [22–24]. Hence, it is necessary to study the mechanisms and kinetics involved in the dehydroxylation and decarburization of CSK based on the analysis of gaseous products by TG-FTIR-MS. In the present work, the TG-FTIR-MS method was used to identify and quantify the gaseous products of CSK under calcination. Three kinetic methods were used by gas product flow data instead of TG/DSC to calculate the kinetic equations. The mechanisms and kinetics of dehydroxylation and decarburization during the calcination of CSK were obtained, respectively. A comparison with the traditional methods revealed the advantages of the kinetic method by TG-FTIR-MS. The work in this paper provided a theoretical basis for the fine control of dehydroxylation and decarburization in CSK calcination. In addition, it provided guidance for the process design, energy saving, and pollutant control of green building materials and high-quality calcined kaolin products prepared by CSK. 2. Experiment and Methods 2.1. Raw Materials The CSK samples were taken from interbedded coal gangue of Junggar coalfield in Inner Mongolia, Ordos, China. A total of 30 tons of samples collected in the same batch were broken into small pieces of about 3–5 cm by a crusher. Approximately 50 kg of CSK was taken out by multi-point sampling method and broken into particles with a particle size of less than 3 mm. A ceramic ball mill was used to grind the sample into powder with a particle size of less than 80 µm. Before grinding, the powder sample was dried in an electric oven at 105 ◦C for 4 h. The raw materials were characterized by X-ray diffractometer (XRD), X-ray fluorescence (XRF), and flammability analysis. 2.1.1. XRD Analysis An X-ray diffractometer (XRD, D/MAX-2200, Japan Rigaku Corporation, Akishima City, Tokyo, Japan) was used to analyze the mineral composition of the raw material. The conditions of the instrument were Cu target Kα ray, tube voltage of 45 kV, and tube current of 40 mA. Figure1 shows the XRD patterns of the CSK. Figure 1. X-ray diffractometer (XRD) patterns of coal series kaolinite (CSK). Materials 2021, 14, 1493 3 of 13 The CSK sample largely contained kaolinite, boehmite (AlO(OH)), and calcite (CaCO3), as well as a small amount of oxidized minerals of Pb, Zr, and Ti. 2.1.2. XRF Analysis An X-ray fluorescence spectrometer (XRF, S4PIONEER, German Bruker Company, Karlsruhe, Germany) was used for elemental analysis of the raw material. The X-ray tube parameters were 4.2 kW, 60 kV (Max), and 140 mA (Max). Table1 provides the results of the XRF analysis of CSK. Table 1. Chemical composition of raw material (wt.%). SiO2 Al2O3 CaO TiO2 Fe2O3 K2O MgO SO3 P2O5 PbO Zr2O3 38.42 34.77 4.20 1.35 0.39 0.13 0.08 0.05 0.07 0.67 0.18 The primary chemical elements present in the CSK were silicon, aluminum, calcium, and titanium, along with some trace elements, such as iron, potassium, magnesium, sulfur, and phosphorus. According to the semi-quantitative calculation from Figure1 and Table1, the contents of kaolinite and boehmite in CSK are 72.82 wt.% and 19.17 wt.%, respectively. 2.1.3. Flammability Analysis The flammability of CSK was analyzed by the method specified in the Chinese Coal Industry Analysis Standard (GB/T212-2008). The analysis results are shown in Table2. The carbon content of CSK is 2.62 wt.%. Table 2. Industrial analysis results of coal series kaolin samples (wt.%). Moisture Ash Volatile Total Sulfur Total Moisture Carbon Hydrogen Nitrogen 1.00 82.8 14.74 0.03 1.06 2.62 1.53 0.07 2.2. TG-FTIR-MS Analysis A thermal analyzer (NETZSCH 409PC STA, German), infrared spectrometer (Bruker FTIR-7600, Karlsruhe, Germany), and mass spectrometer (Perkin Elemer SQ8T, Norwalk, CT, USA) were used to study the calcination of CSK. The ion source of MS was an electron bombardment source, and its working temperature was 250 ◦C. The temperature of the transmission pipeline was 280 ◦C, the electron bombardment energy was 780 eV, and the scanning mode was the full scanning mode. The test parameters were 90% N2 + 10% O2 atmosphere (similar to the composition of industrial waste gas); flow rate of 75 mL/min; heating rates of 5 ◦C/min, 10 ◦C/min, 15 ◦C/min, and 20 ◦C/min; sample mass of 6.0 ± 0.5 mg; and temperature range from ambient to 1000 ◦C. By analyzing the TG, FTIR, and MS data, the gaseous products released in the process of CSK calcination were identi- fied and quantified. The characteristics for dehydroxylation and decarburization of CSK were analyzed by analyzing the mass spectrum data of gas products.
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