chemical engineering research and design 8 9 ( 2 0 1 1 ) 335340

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Chemical Engineering Research and Design

journal homepage: www.elsevier.com/locate/cherd

Preparation of activated carbon derived from Jatropha curcas fruit shell by simple thermo-chemical activation and characterization of their physico-chemical properties
Wimonrat Tongpoothorn, Manop Sriuttha, Phunsiri Homchan, Saksit Chanthai, Chalerm Ruangviriyachai
Department of Chemistry, Faculty of Science, Khon Kaen University, Khon Kaen 40002, Thailand

a b s t r a c t
High surface area activated carbons were prepared by simple thermo-chemical activation of Jatropha curcas fruit shell with NaOH as a chemical activating agent. The effects of the preparation variables, which were impregnation ratio (NaOH:char), activation temperature and activation time, on the adsorption capacity of iodine and methylene blue solution were investigated. The activated carbon which had the highest iodine and methylene blue numbers was obtained by these conditions as follows: 4:1 (w/w) NaOH to char ratio, 800 C activation temperature and 120 min activation time. Characterization of the activated carbon obtained was performed by using scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and nitrogen adsorption isotherm as BET. The results present that the activated carbon possesses a large apparent surface area (SBET = 1873 m2 /g) and high total pore volume (1.312 cm3 /g) with average pore size diameter of 28.0 . Crown Copyright 2010 Published by Elsevier B.V. on behalf of The Institution of Chemical Engineers. All rights reserved. Keywords: Jatropha curcas fruit shell; Activated carbon; Thermo-chemical activation; Iodine number; Methylene blue number; Physico-chemical properties

1.

Introduction

Activated carbons are the most versatile and commonly used adsorbents because of their extremely high surface areas micropore volumes, large adsorption capacities, fast adsorption kinetics, and relative ease of regeneration. The most precursors used for the production of activated carbons are organic materials that are rich in carbon (Prahas et al., 2008). Agricultural wastes are the one, which considered being a very important feed stock for activated carbon preparation because there are renewable sources and low-cost materials. With many earlier studies, an agricultural wastes such as corn cob (Tsai et al., 1998), coconut shell (Hu and Srinivasan, 1999), palm shell (Daud et al., 2000), grain sorghum (Diao et al., 2002), pistachio nut shell (Lua and Yang, 2005), olive stones and walnut shell (Martnez et al., 2006), cherry stones (Olivares-Marin et al., 2006), rice bran (Suzuki et al., 2007), jackfruit shell waste (Prahas et al., 2008) and oil palm shell (Tan et al., 2008) have

been found to be suitable precursors owing to their high carbon and low ash contents. From previous studies, the quality and characteristics of activated carbons not only depended on physical and chemical properties of the starting materials but also depended on the preparation conditions (Ahmadpour and Do, 1996; Molina-Sabio and Rodriguez-Reinoso, 2004; LilloRodenas et al., 2004). Due to successful use of Jatropha curcas oil in biodiesel production, it promotes the heavy cultivation of this plant in many countries (Sarin et al., 2007; Tapanes et al., 2008; Hawash et al., 2009; Lu et al., 2009). From this point of view, it may lead to the problem with its associated waste as J. curcas fruit shell (JS). It contains low nutrient, which is not suitable for use as an agriculture fertilizer, but it is abundant in cellulose, hemicelluloses and lignin resulting in difcult to digest or degrade. Thus, a possible solving of this waste is converting it into valueadded activated carbon, which is one of the most widely used materials because of its exceptional adsorbent properties.

Corresponding author. E-mail address: chal ru@kku.ac.th (C. Ruangviriyachai). Received 23 December 2009; Received in revised form 26 May 2010; Accepted 25 June 2010

0263-8762/$ see front matter Crown Copyright 2010 Published by Elsevier B.V. on behalf of The Institution of Chemical Engineers. All rights reserved.

doi:10.1016/j.cherd.2010.06.012

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In general, the process for manufacturing of activated carbons involves two steps, carbonization of raw carbonaceous materials in an inert atmosphere followed by the activation of the carbonized product. The activation process can be provided by two types, either by physical activation or chemical activation. However, chemical activation is now widely applied for the activation because of its lower activation temperature and higher product yield compared with the physical one (Guo and Rockstraw, 2007). Based on the literature reviewed, it was found that alkaline hydroxides (KOH and NaOH) (LilloRodenas et al., 2007) can be used to prepare the activated carbon, which gave high specic surface area in the range of 23183500 m2 /g (Macia-Agullo et al., 2004; Yoshizawa et al., 2002; Tseng, 2006). Moreover, sodium hydroxide was also shown to be more particularly interesting because NaOH activation can reduce chemical activation cost and environmental load when compared with KOH activation (Perrin et al., 2004). The aims of this work were to utilize J. curcas fruit shell, biomass waste, for the preparation of activated carbon by simple thermo-chemical activation using NaOH as an activating agent. The effects of impregnation ratio of reagent to char, activation temperature and activation time on iodine and methylene blue numbers of the activated carbon were studied in order to obtain high adsorption capacity and surface area of the product. Subsequently, the physico-chemical characteristics of the activated carbon, obtained by optimum conditions, were also determined.

2.3. Optimum conditions for the production of activated carbon

Some parameters which had effect on the activated carbon namely impregnation ratio of NaOH to charcoal (1:14:1, w/w), activation temperature (400800 C) and activation time (30120 min) were studied to determine the optimum conditions for producing this activated carbon. In this work, efciency and quality of the activated carbon were preliminarily characterized by measuring both iodine number and methylene blue number. Iodine number can be used for estimation of the relative surface area and measurement of porosity, the pores size greater than 1.0 nm in diameter. Therefore, the iodine number was measured to evaluate the adsorptive capacity of the produced activated carbon. In case of methylene blue number, it is also one of the most widely recognized probe molecules for assessing the removal capacity of the specic carbon for moderate-size pollutant molecules (1.5 nm) (Girgis et al., 2002).

2.3.1.

Adsorption of iodine

The iodine number of activated carbon was obtained on the basis of the Standard Test Method, ASTM Designation D460786 by titration with sodium thiosulphate (ASTM, D 4607-86). The concentration of iodine solution was thus calculated from total volume of sodium thiosulphate used and volume dilution factor.

2.3.2.

Adsorption of methylene blue

2.
2.1.

Experimental
Materials and preparation conditions

J. curcas fruit shells (JS) were supplied by the Ofce of Agricultural Research and Development Region 3, Khon Kaen Province, Thailand. The starting materials were cleaned with water and dried at 110 C for 48 h. The dried samples were crushed with a blender and sieved to a size smaller than 500 m. The elemental compositions and proximate analysis of the raw materials (JS) used in this study were analyzed. It was found to be 36.70, 5.43, 1.49 and 9.95% for C, H, N and ash content on dry basis, respectively. JS was prepared by carbonization and chemical activation. The dried sample was carbonized at 400 C for 1 h in a mufe furnace (Fisher Scientic, U.S.A.) in order to produce charcoal. The charcoal of J. curcas fruit shell (CJS) obtained was then subjected impregnation in NaOH solution (by weight ratio) at 70 C for 24 h. After that, it was dried in oven at 110 C for 24 h. The resulted sample was further activated in a mufe furnace at xed activation temperature and time. After cooling, the activated carbon was washed successively several times with 1 M HCl and follow hot water until the pH became neutral. The washed sample was dried at 110 C to obtain activated carbon of J. curcas fruit shell (ACJS) as the nal product.

By batch experiment, methylene blue (MB) solution was mixed with activated carbon and shaken (200 rpm) at room temperature. After the completed reaction, the solutions were ltered and the concentrations of methylene blue solution were then determined by an Agilent 8453 UV-Vis spectrophotometer (Germany) at 663 nm. The equilibrium adsorption capacities (qe ) of the activated carbon were determined based on adsorbate mass balance using Eq. (1): qe = (C0 Ce )V M (1)

where C0 and Ce are the initial and equilibrium concentrations of the dye (mg/L), respectively, V is the volume of the aqueous solution (L), and M is the mass of activated carbon used (g) (Kumar et al., 2005).

2.4. Physico-chemical characteristics of the activated carbon

The physico-chemical characteristics of activated carbon produced by the optimum conditions in this experiment were determined. These surface functional groups were analyzed by using a FT-IR spectroscopy (Perkin-Elmer, Spectrum One model Spectrometer, England). The activated carbon samples were mixed with potassium bromide and the mixture was pressed as a pellet prior to analysis. The IR spectrum was obtained by co-adding 32 scans, at a resolution of 4 cm1 over the range of 4504000 cm1 . Theirs surface of inorganic components were analyzed by a X-Ray diffractometer (Scintag 2000 system, Germany) with a germanium detector for 2 values of 1080 with scan rate of 0.03 /min. Microstructure of the sample was examined using a scanning electron microscopy (SEM, JSM-6480LV model, JEOL, Japan). Adsorptiondesorption isotherms of nitrogen at 196 C were measure with an

2.2.

Thermogravimetric analysis

The pyrolysis behaviors of J. curcas fruit shell (JS) were determined on a Pyris Diamond TG/DTG 51 thermal analyzer (Perkin-Elmer, U.S.A.). 3 mg (0.5) of sample material was heated from 30 to 900 C at a ramping rate of 10 C/min under nitrogen gas atmosphere.

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Fig. 1 Thermal behaviors as expressed in TG (mass loss, %) and DTG (dx/dt, C1 ) curves of JS. automatic adsorption instrument (Nova-1000 Gas Sorption analyzer, U.S.A.) in order to determine surface areas and total pore volumes. Prior to the measurements, the samples were out gassed at 300 C under nitrogen for at least 3 h. The total pore volumes were estimated to be the liquid volumes of adsorbate (N2 ) at a relative pressure of 0.99. The surface area of the samples was calculated by BrunauerEmmetTeller (BET) method in relative pressure (P/P0 ) range of 0.050.30 at 196 C.

3.
3.1.

Results and discussion

Thermogravimetric analysis

In the rst part, thermogravimetric analysis is studied in order to predict their respective contributions to the chars and the subsequent activated carbons in term of weight fraction and contributions to the different porous domains (microporosity, mesoporosity, macroporosity) (Cagnon et al., 2009). Therefore, thermogravimetry provides a formation on thermal behavior of the starting JS. TG and DTG curves show the mass loss in the range 30900 C and this mass loss can be divided into several stages as shown in Fig. 1. Based on the literature survey (Cagnon et al., 2009; Girgis et al., 2002; Sentorun-Shalaby et al., 2006), the rst stage of mass loss was veried by heating the materials up to 180 C, resulting in moisture elimination. The second stage (180 < T < 375 C), which corresponds to the primary carbonization, had a greater mass loss. This stage presented the evolution of light volatile compounds occurs from degradation of cellulose and hemicelluloses. The third stage was found in the range of 375650 C indicating the decomposition of lignin, which was a structure with higher stability. Degradation of lignin takes place in a wide temperature range and lasts to higher temperature. Moreover, this stage reveals the decomposition of a portion of cellulose and residual hemicelluloses. Above 650 C, the weight loss was little indicating that the main structure of char was formed around this temperature.

Fig. 2 Effect of impregnation ratio of NaOH/CJS (w/w) (a), activation temperature (b), and activation time (c) on iodine and methylene blue numbers of ACJS.

3.2. Optimum conditions for the production of activated carbon 3.2.1. Impregnation ratio of NaOH:char

Observation of the latter has conrmed the following reaction mechanism already proposed for explaining the activation of carbonaceous materials by sodium hydroxide (Tsang, 2007): 6NaOH + 2C 2Na + 2Na2 CO3 + 3H2 (2)

With increase of impregnation ratio, the reactions became more intensive due to more activation agent being cooperated into precursor matrix, which led to pore widening. Besides, the increasing amount of NaOH used for activation may contribute to the development of internal microporous cavities, resulting in an increased surface area which was considered to be the most important factor for adsorption. The results in Fig. 2 showed that when increasing the ratio of NaOH:char at the same temperature, the highest iodine and methylene blue numbers were obtained at the impregnation ratio of 4:1. Similar impregnation ratio of the reagent to char which could give high surface area of the activated carbon was previously reported (Yang et al., 2002). Therefore, the ratio of 4:1 by weight was chosen as the optimum condition for further experiments.

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Fig. 4 The X-ray diffraction pattern of ACJS. Fig. 3 FT-IR spectra of JS, CJS and ACJS. Peaks occurring at 1411 and 1375 cm1 are all ascribed to oxygen functionalities such as highly conjugated C O stretching, CO stretching in carboxylic groups, and carboxylate moieties. Moreover, FT-IR spectra of CJS showed the decreasing of intensity of aliphatic bands around 2919 and 2850 cm1 , the IR band around 1636 cm1 assigned to stretching C O of lactonic and carbonyl groups (Ji et al., 2007), a relative intense IR band at about 1052 cm1 corresponding to CO stretching in acids, alcohols, phenols, ethers and esters (Puziy et al., 2002a,b) and the IR band located at 617 cm1 attributing to in-plane ring deformation (Ahmad et al., 2007). For FT-IR spectra of the ACJS, it showed relatively low intensity of OH band because ONa groups linked with carbon of the impregnated charcoal could be replaced by the OH groups via water washing. Furthermore, functional groups are mostly disappeared, which close to the characteristic of the commercial activated carbon used (data not shown). For these ACJS, the X-ray diffraction proles shown in Fig. 4 exhibit broad peaks and absence of a sharp peak that revealed predominantly amorphous structure, which is an advantageous property for well-dened adsorbents. However, the occurrence of broad peaks around 26 and 43 showed signs of formation of a crystalline carbonaceous structure, resulting in better layer alignment (Yang and Lua, 2006). Similar result reported was proposed by Pechyen et al. (2007). SEM photograph of the ACJS in Fig. 5 shows that the adsorbent gives roughly texture with heterogeneous surface and a variety of randomly distributed pore size. Furthermore, it contains an irregular and highly porous surface, indicating rel-

3.2.2.

Activation temperature

Activation temperature was shown to have remarkable effects on both surface area and the nature of porosity. Increase in activation temperature signicantly increases in both microand mesopore developments, resulting in the increase of both iodine and methylene blue adsorptive capacities of the activated carbon. This might due to the diffusion rate of water molecules to the interior of carbon, which was higher at higher temperature to develop a wide range of pore network as reported previously (Kumar et al., 2006). Moreover, more volatile compounds are released at higher temperature, which leads to open the carbon structure and gives rise to more surface area. From the results as shown in Fig. 2, it illustrated that the highest iodine and methylene blue numbers of the activated carbons were obtained at 800 C. Additionally, the yields of activated carbon obtained by varying activation temperature from 400 to 800 C were not signicantly different (in the range of 40.0542.75%). Thus, at 800 C was chosen as the optimum activation temperature.

3.2.3.

Activation time

The effect of activation time on iodine and methylene blue number is illustrated in Fig. 2. It was show that increasing of activation time resulting in the increase of the iodine and methylene blue numbers. The results present that 120 min is the suitable length of time for activation because it gave the highest iodine and methylene blue numbers of product with a maximum value of 1138.13 mg/g and 499.17 mg/g, respectively. This trend is expected because some volatile compounds which were in the inner part of particle could evaporate more with long activation. The reason is that heat penetrated deeper inside of particles than at short time, so the porosity development at long time was higher than at short time resulting in the increase of iodine number.

3.3. Physico-chemical characteristics of the activated carbon

It is generally accepted that pore structure development is inuenced by many factors including inorganic impurities and internal structure of carbon. FT-IR spectra as shown in Fig. 3 present the development of surface textures of the JS, CJS and ACJS. According to the literatures, it was found that JS presents the IR band around 3398 cm1 assigned to OH vibrational stretching of hydroxyl groups. Peak at 1636 cm1 is the characteristic of the C O stretching vibration of carbonyl groups.

Fig. 5 SEM photograph of ACJS.

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Table 1 Surface area, pore volume and pore size parameters of JS, CJS and ACJS. Parameters JS
BET surface area, SBET (m2 /g) Total pore volume, Vtot (cm3 /g) Average pore diameter () 9.0 0.037 163.7

Samples CJS
288.4 0.225 39.44

ACJS
1873.0 1.312 28.00

addition, since there is high adsorptive capacity and surface area of this activated carbon, therefore, it can be employed as low-cost adsorbent and considered as an alternative one to commercial activated carbon. Accordingly, this would contribute for solving many current-day environmental pollution problems.

Acknowledgements
The authors thank Khon Kaen University for all supporting facilities and gratefully acknowledge the nancial support from National Research Council of Thailand and Rajamangala University of Technology Issan, Khon Kaen campus. We also special thank Ofce of Agricultural Research and Development, Khon Kaen province and Nakon Ratchasima Field Crops Research Center, Nakon Ratchasima province for their material supports of J. curcas fruit. The Center of Excellence for Innovation in Chemistry (PERCH-CIC), Commission on Higher Education, Ministry of Education is gratefully acknowledged for some chemicals.

References
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4.

Conclusion

Value-added high surface area activated carbons can be produced by simple thermo-chemical activation of J. curcas fruit shell with NaOH as an activating agent. The activated carbon which has the highest iodine and methylene blue numbers was obtained by using 4:1 impregnation ratio of NaOH:charcoal (by weight) at 800 C activation temperature for 120 min of activation time. As the results illustrated that the activation temperature also exhibited a signicant inuence on development of the pore structure which caused increasing of an adsorption capacity of the activated carbon. Under these optimum conditions, the activated carbon which has specic area over the acceptable range for commercial activated carbons (5001500 m2 /g) (Amaya et al., 2007) and a good decolorizing carbon which fullls at least 200 mg/g removal capacities for dye (Attia et al., 2008) were obtained. Moreover, the carbon possesses a larger apparent surface area (SBET = 1873 m2 /g) and higher total pore volume (1.312 cm3 /g) when compared with other data reported (Namasivayam et al., 2007; Pechyen et al., 2007; Sricharoenchaikul et al., 2008). In

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