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Activated Carbon Produced by Pyrolysis of Waste Wood and Straw for Potential Wastewater Adsorption

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Activated Carbon Produced by Pyrolysis of Waste Wood and Straw for Potential Wastewater Adsorption materials Article Activated Carbon Produced by Pyrolysis of Waste Wood and Straw for Potential Wastewater Adsorption Katarzyna Januszewicz 1,*, Paweł Kazimierski 2, Maciej Klein 2,3, Dariusz Karda´s 2 and Justyna Łuczak 4 1 Department of Energy Conversion and Storage, Chemical Faculty, Gda´nskUniversity of Technology, Narutowicza 11/12, 80–233 Gda´nsk,Poland 2 Institute of Fluid Flow Machinery, Polish Academy of Sciences, 80-233 Gda´nsk,Poland; [email protected] (P.K.); [email protected] (M.K.); [email protected] (D.K.) 3 Energy Research Institute @ NTU (ERI@N), Nanyang Technological University, 50 Nanyang Drive, Singapore 637553, Singapore 4 Department of Process Engineering and Chemical Technology, Chemical Faculty, Gda´nskUniversity of Technology, Narutowicza 11/12, 80–233 Gda´nsk,Poland; [email protected] * Correspondence: [email protected]; Tel.: +48-58-347-19-31 Received: 26 March 2020; Accepted: 23 April 2020; Published: 27 April 2020 Abstract: Pyrolysis of straw pellets and wood strips was performed in a fixed bed reactor. The chars, solid products of thermal degradation, were used as potential materials for activated carbon production. Chemical and physical activation processes were used to compare properties of the products. The chemical activation agent KOH was chosen and the physical activation was conducted with steam and carbon dioxide as oxidising gases. The effect of the activation process on the surface area, pore volume, structure and composition of the biochar was examined. The samples with the highest surface area (1349.6 and 1194.4 m2/g for straw and wood activated carbons, respectively) were obtained when the chemical activation with KOH solution was applied. The sample with the highest surface area was used as an adsorbent for model wastewater contamination removal. Keywords: waste biomass; pyrolysis; activated carbon; physical and chemical activation; biochar 1. Introduction Biomass, as an effective source of energy, is one of the alternatives to fossil fuels, which can be utilised by direct burning or indirect thermal treatment. Thermal degradation processes, like pyrolysis or gasification, were designed to convert the organic matter into a variety of products including gases, oils and chars [1]. During pyrolysis, biomass is thermally decomposed in the oxygen-depleted conditions with temperatures between 300 and 1200 ◦C. This temperature range is seen as a main advantage when compared with gasification and combustion processes [2,3]. The temperature of the gasification processes is set in a range of 600–1200 ◦C (typically above 700 ◦C), whereas combustion of biomass is carried out up to 1300 ◦C[4,5]. In these conditions, biomass is decomposed into lighter chemical compounds due to several reactions, mostly of endothermic nature. As a consequence, volatile matter is generated providing liquid and gaseous products used mainly as fuels, however, by-products in the form of char are also obtained. The quality and quantity of each product are highly influenced by the temperature of the process, residence time, heating rate, and size and shape of the biomass particles [6]. Utilisation of waste biomass materials in pyrolysis process is a part of a current trend of closed cycle production to achieve more sustainable processes and products. The residue charred material formed during pyrolysis has much higher carbon content (% wt.) in comparison to the substrate, Materials 2020, 13, 2047; doi:10.3390/ma13092047 www.mdpi.com/journal/materials Materials 2020, 13, 2047 2 of 13 since moisture, volatiles, and most of the compounds with non-carbon heteroatoms are removed during the thermal treatment. Char with low commercial value formed from waste biomaterials can be activated to produce adsorbents for various industrial processes or used directly as a fuel [7]. The final surface properties and functionalities of the char are determined by the nature of pyrolyzed precursors and the type of activation process. In this regard, a variety of raw materials, as well as methods to enhance properties of the char, were investigated to produce effective and low-cost products with high sorption properties. Chars were produced from waste of wooden and non-wooden origin [8,9], including agricultural residues [10], rice husk, palm shells [11], coconut shells [11,12] , apple and cherry pulp, plum pulp and stones, and olive stones among others [13–17]. The high surface area and ability to influence the pore size and distribution during the production process makes adsorbents from waste biomass suitable for areas as different as the separation and purification of gases, water treatment, energy storage and catalysis, among others [18–21]. Activation processes increase porosity, enhance surface areas and modify chemical properties by introducing a variety of surface sites such as carboxylic, phenolic, hydroxylic and carbonyl groups [22]. The most important reason for the use of different technics of activation is to increase a partially blocked porous surface by using agents to remove the trapped products of incomplete pyrolysis. The activation can be either physical or chemical in nature. In the first attempt, the material is exposed to high temperatures (800–900 ◦C) and treated with steam or CO2 in a nitrogen or argon atmosphere. Thermal treatment is a basic method of improving the sorption parameters of the char, which also forms new functional groups on the surface [18]. Oxidation with agents mainly increases the amount of surface functional groups [23], but at the same time, accompanied by temperature, expands the porous structure of the material by removing trapped gases and oils (products of pyrolysis process) and oxidises existing functional groups. Steam, as an activation agent, increases the hydrophilicity and changes the properties of the char by taking part in the generation of additional oxidation agents like CO and CO2. Physical treatment with CO2 is often preferred over steam due to its low reactivity, which makes the process easier to control, thus obtaining more uniform porosity [24]. For the chemical activation of char, KOH, ZnCl2, NaOH, H3PO4 and K2CO3 impregnation can be applied, accompanied by high temperatures. By using this method, the hydrophilic properties of biochar can be improved and the N/C and H/C (aromaticity) ratio increased [18]. Chemical activation with alkaline reagents, especially KOH, is widely used, providing materials with very high surface area and defined micropore size distribution [25]. This process is usually performed at high temperatures, e.g., 650–950 ◦C[26]. The activation mechanism can be described by the following reactions: dehydratation (2KOH = K2O + H2O); water–gas reaction (C + H2O = H2 + CO); water–gas shift reaction (CO + H2O = H2 + CO2); and carbonate formation (K2O + CO2 = K2CO3)[26]. Above 700 ◦C metallic potassium is formed due to reduction by carbon or hydrogen. The comparison of two typical alkaline activation agents, KOH and NaOH, revealed that in the similar condition of activating the process the biomass samples prepared with NaOH had lower surface area and micropore volumes than those with KOH [27]. However, the chemical activation process must be followed by an additional treatment to eliminate chemicals used [28]. Nevertheless, the main challenge in the production of activated carbon (AC) is development of the economically justified method to obtain products with given surface properties using low cost materials [29–32]. In this regard, the aim of this study is to compare different technics for increasing the surface area and porosity of the biochar obtained from waste beech wood and wheat and rye straw pellets. Both raw materials are by-products of agriculture and the wood industry. For example, in Poland, the overproduction of straw in relation to agricultural demand reaches about 10 million tons per year, which is equivalent to around 6 million tons of coal [33]. The additional valuable utilization method of waste straw could be pyrolysis and valorization through its activation. Additionally, the mode of action of the activated carbon with the highest surface area was determined as a potential adsorbent for the removal of model contaminant—Rhodamina B (RhB) from aqueous solutions. Materials 2020, 13, x 3 of 15 Materialsas a potential2020, 13, 2047adsorbent for the removal of model contaminant—Rhodamina B (RhB) from aqueous3 of 13 solutions. 2.2. MaterialsMaterials andand MethodsMethods 2.1.2.1. MaterialsMaterials TwoTwo types types of of biomass biomass fromfrom thethe PolishPolish locallocal market,market, woodwood andand straw,straw,were were chosen chosenas assubstrates substrates forfor pyrolysispyrolysis andand biocharbiochar production.production. TheThe pelletpellet strawstraw andand woodwood chipschips werewere usedused asas examplesexamples ofof agriculturalagricultural waste.waste. Typically, thethe strawstraw pelletspellets areare aa heterogeneousheterogeneous mixturemixture ofof variousvarious wastewaste straw,straw, likelike wheatwheat andand rye.rye. ThisThis pelletpellet isis commonlycommonly usedused inin PolishPolish agricultureagriculture andand isis commerciallycommercially available,available, thereforetherefore suchsuch biomass was was chosen chosen for for the the experiment experiments.s. The The beech beech wood wood residues residues in the in form the formof chips of chips with a particle size distribution of about 3 2 2 cm and mixed wheat and rye straw pellets with a particle size distribution of about 3 × 2× × ×2
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