Clean and Low-Cost Synthesis of High Purity Beta-Silicon Carbide with Carbon fiber Production Residual and a Sandstone
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Journal of Cleaner Production 238 (2019) 117875 Contents lists available at ScienceDirect Journal of Cleaner Production journal homepage: www.elsevier.com/locate/jclepro Clean and low-cost synthesis of high purity beta-silicon carbide with carbon fiber production residual and a sandstone Kaidi Sun a, Tongtong Wang a, Zhe Chen b, Wenyang Lu a, Xin He a, Weibo Gong a, Mingchen Tang a, Fangjing Liu a, Zaixing Huang a, Jinke Tang d, TeYu Chien d, Gang Tan e, * Maohong Fan a, b, c, f, a Department of Chemical Engineering, University of Wyoming, Laramie, WY, 82071, USA b Department of Petroleum Engineering, University of Wyoming, Laramie, WY, 82071, USA c School of Energy Resources, University of Wyoming, Laramie, WY, 82071, USA d Department of Physics and Astronomy, University of Wyoming, Laramie, WY, 82071, USA e Department of Civil & Architectural Engineering, University of Wyoming, Laramie, WY, 82071, USA f School of Civil and Environmental Engineering, Georgia Institute of Technology, Atlanta, GA, 30332, USA article info abstract Article history: The U.S. Department of Energy has initiated conversion of coal to solid materials, which can improve the Received 5 April 2019 coal-derived high-value product chain and decrease coal utilization related carbon dioxide emission. An Received in revised form integrated coal utilization technology was developed to respond to Department of Energy's call, which is 7 July 2019 extracting the molecules with desired molecular weight and structure in coal for carbon fiber production, Accepted 1 August 2019 then using carbon-rich residual from carbon fiber precursor extraction as carbon source to produce beta- Available online 1 August 2019 silicon carbide. For the first time beta-silicon carbide is synthesized from carbon fiber production re- Handling Editor: Baoshan Huang sidual and a sandstone. The synthesized beta-silicon carbide was characterized with multiple analytical techniques. The product exhibits good properties with its purity, density, and Vickers hardness reach the Keywords: requirements of commercial silicon carbide. Specifically, the purity of the beta-silicon carbide obtained Coal with the two inexpensive raw materials under argon atmosphere at 1600 C reaches as high as 98%. It is EtOH-SCC extraction residual the first time that the furnace-MS system was applied to analyze the gaseous products in coal-based Sandstone beta-silicon carbide synthesis process. Also, a possible synthesis mechanism was proposed and Silicon carbide confirmed with experimental results. The research further analyzed the environmental impact and proposed the possibility that the liquid wastes/byproducts generated during raw material treatment process can be recycled and efficiently reused as coagulants or desiccants when the developed beta- silicon carbide synthesis process is applied in industry. This study provides a clean and low-cost approach for reusing waste residual from coal-based carbon fiber production and sandstone powder. © 2019 Elsevier Ltd. All rights reserved. 1. Introduction and among them are carbon fiber (Yang et al., 2016) and carbide (Liu et al., 2015),. However, to the best knowledge of the authors, Coal has been used for generating electricity in power plants, integrally producing both carbon fiber and carbide with coal have which unfortunately may not be the best way to use the precious not been seen in literature. Therefore, according to the elemental natural resource (Chen et al., 2016), especially considering the fact composition characteristics of coalerich in C and poor in H, and that people are increasingly concerned about the coal combustion atom economy and energy saving principles, Fan's group proposed associated CO2 emission (Lai et al., 2018). Thus, people recently to produce both carbon fiber and carbide with high H:C and low started to pay high attention to converting coal to solid materials, H:C fractions in coal, respectively. Successful separation of the high H:C fraction from low H:C fraction in coal and preparation of carbon fiber with high H:C fraction were realized with ethanol and su- percritical CO2 (EtOH-SCC) (Liu et al., 2018) via extraction. This * Corresponding author. School of Civil and Environmental Engineering, Georgia research was focused on the utilization of the EtOH-SCC extraction Institute of Technology, Atlanta, GA, 30332, USA. E-mail address: [email protected] (M. Fan). residual and sandstone in b-SiC synthesis. https://doi.org/10.1016/j.jclepro.2019.117875 0959-6526/© 2019 Elsevier Ltd. All rights reserved. 2 K. Sun et al. / Journal of Cleaner Production 238 (2019) 117875 b-SiC (3CeSiC) with a zinc blende crystal structure is synthe- under Ar flow (50 ml/min) to synthesize b-SiC. A mass spectrom- sized at temperatures below 1700 C. It can be utilized in many eter (MS, HPR-20, HIDEN) was connected to the high-temperature areas, including catalysis, ceramic manufacturing, coating, milling, horizontal tube furnace (HTRH-Carbolite) to detect gaseous spe- and polishing (Chen et al., 2017). Also, b-SiC plays an important role cies generated during SiC synthesis process. During the reaction in manufacturing semiconductors, solar cells, and optoelectronics process, the gaseous products were identified and recorded by the due to its characteristics of the wide band gap, high electron molecular mass/mass number (m/z) signal of the MS. The obtained mobility, and superior thermal conductivity(Gusev et al., b-SiC products were treated at 850 C for 6 h under air atmosphere 2016),(Pang et al., 2010),(Kamble et al., 2017). to remove unreacted carbon. The schematic diagram of the exper- Currently, Acheson process (Chen et al., 2018) is the main b-SiC imental set-up for the synthesis of b-SiC is shown in Fig. 1. The flow synthesis method, which is started by mixing C-rich and Si-rich diagram of the experiment including all procedures is shown in materials in an electric resistance furnace and followed by heat- Fig. 2. ing the mixture at given temperatures for a desired period (Makkee et al., 1998). The employed coal related C-rich raw materials include 2.3. Characterization of residual, sandstone powder and b-SiC coal (Liu et al., 2015), coal tar pitch (Czosnek and Ratuszek, 2002), products and metallurgical coke (Narciso-Romero et al., 1999), while coal fl related Si-rich raw materials are coal y ash (Sulardjaka et al., 2.3.1. Chemical properties characterization of residual, sandstone fi 2011), coal gasi cation slag (Yin and Tang, 2011), and coal gangue powder and b-SiC products (Xiao et al., 2015). Other C-rich and Si-rich raw materials are acti- The elemental analysis of the residual was performed by using vated carbon and carbon black; and Si, SiO2, carbosilane and an elemental analyzer (vario MACRO cube, Elementar), and the methyltriethoxysilane, respectively. On one hand, the materials oxygen content was calculated by the subtraction method. An were successfully used for the synthesis of b-SiC. For example, the inductively coupled plasma mass spectrometry (ICP-MS, NexIon purity of b-SiC produced by coal gangue with carbon reached 350, PerkinElmer) was operated to determine the composition of 76.01% (Xiao et al., 2015). Also, b-SiC synthesized with silica fume treated sandstone powder and ash of treated residual. A nine-point e and brown coal semi-coke shows a purity of 90 91% (Anikin et al., calibration curve from 0 to 100 ng/L was created for each analysis. 2016). On the other hand, the C concentration in the C-rich mate- Residual was dried at 105 C overnight to remove moisture, then rials used in the conventional b-SiC is either too low or too high, calcined at 550 C for 6 h to obtain ash sample. For each test, 0.03 g which is not beneficial to b-SiC synthesis. Use of low C or high H:C sample was mixed with 0.24 g lithium metaborate (BLiO2) and raw materials such as coals only for b-SiC synthesis results in heated at 1100 C for 5 min in the air atmosphere. The obtained wasting a lot of valuable H, which is not desired for lowering the glass-like mixture was then fully dissolved by 5 wt% nitric acid overall cost of b-SiC. Employing high C materials with relatively low (HNO3). The dissolved solution was diluted with deionized water to activities such as activated carbon could lower b-SiC synthesis ki- obtain the testable sample for ICP-MS tests. The purity of the ob- netics, which should also be avoided for b-SiC synthesis. Thus, the tained b-SiC was determined with ICP-AES following the method of EtOH-SCC extraction residuals with reasonable H:C ratios were CAP-017P. used in this research to overcome the shortcomings of the state-of- the-art b-SiC synthesis technologies. 2.3.2. Qualitative characterization of residual, sandstone powder 2. Experiments and b-SiC products Powder X-ray diffraction (XRD) tests were performed on a 2.1. Residual and sandstone powder preparation Rigaku X-ray diffraction system using Cu Ka1 radiation (l ¼ 1.54056 Å) at 40Kv and 40 mA. The sample was placed on a The residual was obtained from EtOH-SCC extraction of Powder zero diffraction Si holder and was scanned from 10 to 90 (2q) with River Basin (PRB) coal as previously reported (Liu et al., 2018). a5 /min scanning rate at room temperature. The samples were also fi Liquid tar was used for high-value carbon fiber synthesis (Liu et al., identi ed by Fourier transform infrared spectrometer (FTIR, Nicolet À1 fl 2018). The solid residual needed to be treated prior to its use as a C iS FT-IR) with a resolution of 4 cm . A spectro uorometer (Fluo- fi resource for b-SiC synthesis for this research. The residual was rolog-3, Horiba Scienti c) was adopted to explore the photo- washed with ethanol to extract remained liquid tar and then dried luminescence (PL) of the synthesized b-SiC materials.