The use of biomass as filler in biocomposites are becoming widespread in the present decade because its variety of advantages. Jatropha (jatropha curcas L) seed shell after separated from kernel can be used to produce carbon black because of its higher carbon content, and have the potentiality to use as reinforcement in composites. In this study, carbon black was produced from jatropha seed shell by carbonization in furnace method for 1 hour at 600oC. Thermogravimetric analysis to analyze seed shell of jatropha as raw material. The morphological properties of the carbon black were analyzed by elemental analysis by X-ray (EDX), SEM, TEM, XRD, SEM, and TEM. It was found that the yield of carbon black was 40% which included 4 different sizes ranging from 70 – 300 mesh in distribution of particle size analysis. Carbon black suggested that it could be a good filler or reinforcement in biocomposites

Amin, A. (Amri)

Aprilia, N. A. (N)

Islam, M. N. (Md)

Khalil, H. P. (H)

Aprilia, N. A. Sri

Khalil, H. P. S. Abdul

Islam, Md Nazrul

Amin, Amri

Proceedings of The Annual International Conference, Syiah Kuala University - Life Sciences & Engineering Chapter

Proceedings of The 5th Annual International Conference Syiah Kuala University (AIC Unsyiah) 2015In conjunction with The 8th International Conference of Chemical Engineering on Science and Applications (ChESA) 2015September 9-11, 2015, Banda Aceh, Indonesia100PROPERTIES OF CARBON BLACK FROM JATROPHASEED SHELL AS A POTENTIAL SOURCE OF  FILLERENHANCEMENT IN BIOCOMPOSITES1*N.A. Sri Aprilia, 2H.P.S. Abdul Khalil, 2Md. Nazrul Islam and 3Amri Amin1 Chemical Engineering Department, Engineering Faculty of Syiah Kuala University, BandaAceh, Indonesia;2 School of Industrial Technology, Universiti Sains Malaysia, 11800 Penang, Malaysia3 Engineering Department, University of Abulyatama, Lampoh Kedee, Aceh Besar, Indonesia* Coressponding author: sriaprilia@unsyiah.ac.idAbstractThe use of biomass as filler in biocomposites are becoming widespread inthe present decade because its variety of advantages. Jatropha (jatrophacurcas L) seed shell after separated from kernel can be used to producecarbon black because of its higher carbon content, and have the potentialityto use as reinforcement in composites. In this study, carbon black wasproduced from jatropha seed shell by carbonization in furnace method  for 1hour at 600oC. Thermogravimetric analysis to analyze seed shell of jatrophaas raw material. The morphological properties of the carbon black wereanalyzed by elemental analysis by X-ray (EDX), SEM, TEM,  XRD, SEM, andTEM.  It was found that the yield of carbon black was 40% which included 4different sizes ranging from 70 – 300 mesh in distribution of particle sizeanalysis. Carbon black suggested that it could be a good filler orreinforcement in biocomposites.Key words: Jatropha seed shell, carbonized particles, morphology,properties and particle size distributionIntroductionBiomass are materials renewable and abundant in the world. Reinforcement of biomass incomposite will increase mechanical properties for many application. Carbon black is veryimportant material widely used as filler in composites. Structure and configurations ofparticles influence properties of carbon black (Stabik et al., 2012). The principal uses ofcarbon black are as a reinforcing agent in rubber compounds (especially tires) and as ablack pigment in printing inks, surface coatings, paper, and plastics, Antal et al., 2003.Carbon black is a product of incomplete combustion. It is the dark component of smoke andin fact all carbon black processes start with the production of a smoke.To achieve the green composites, many researcher concern to agriculture biomass resource.Agricultural by products and waste materials used for the production of carbonized particlehave studied by several researcher include olive mill waste and sewage sludge (Gokce etal., 2009), coconut shells  (Young et al., 2010,  Li at al., 2009). jatropha hull (Xin-hui etal., 2011), jatropha fruit shell (Tongpoothorn et al., 2011, Ramakrishnan et al., 2009,Karthikeyan et al., 2008, Sricharoenchaikul et al., 2007), jatropha curcas pods(Sathishkumar et al., 2012), Delonix Regia Seed Shell, Ferronia Seed Shell, Ipomea CarniaStem (Karthikeyan et al., 2008), olive bagasse (Demiral et al., 2011), rice husk (Wang etal., 2011) this carbon black have activated and  successfully used for the adsorptionprocesses and another application.Several researcher have studied of carbon black from biomass as a filler in biocomposites.Bioresource that used in biocomposite are bamboo (Khalil et al., 2007), coconut shell, oilProceedings of The 5th Annual International Conference Syiah Kuala University (AIC Unsyiah) 2015In conjunction with The 8th International Conference of Chemical Engineering on Science and Applications (ChESA) 2015September 9-11, 2015, Banda Aceh, Indonesia101palm empty fruit bunches (Khalil et al., 2010, 2012), carbon residue derived from woodybiomass (Pries et al., 2010), carbonized bagasse filler in rubber product (Osarenmwinda andAbode, 2010) have been investigated.The increasing areas of plantations of jatropha curcas L. in India, China, and Indonesia aswell as in South America and Africa will lead to an increased amount of jatropha curcas infuture. The shells of the seeds (hulk)  are promising to be an alternative fuel for thesecountries, because they appear as a by-product during the processing of jatropha oil andcan not used for any other application until now. The jatropha seed contains about 42%seed husks (seed shell). Analysis of the husks by (Singh et al., 2008 and Vyas and Singh,2007) showed that the husks contained 4% ash, 71% volatile matter and 25% fixed carbon.The chemical analysis of jatropha shell are 34%, 10% and 12% cellulose, hemicellulose andlignin, respectively (Singh et al., 2008). Volatile matter, ash and fixed carbon content of theshell have been shown to be 69%, 15% and 16% (Singh et al., 2008 and Jingural at al.,2010). On the other hand, the by product such as seed shell contain fixed carbon can be analternative to make carbon black as bio filler in biocomposites (Khalil at al., 2013).Two main reasons to employ particle size characterization, e.i., better control of productquality and better understanding of products, ingredients and processes. Filler from biomassis a diluent and is used primarily to lower volume cost. With use, all fillers modify certainphysical properties of the compound in addition to lowering cost. Therefore, lower cost isgenerally achieved at the expense of other desirable properties and all compounds arecompromises with various trade-offs considered and balanced by the compounder.The objective of this study was investigated to get an excellent carbon black from jatrophaseed shell as raw material filler for reinforcement in biocomposite and characterizationphysico-chemical properties of carbon black to determine elemental analysis by X-ray(EDX), SEM, TEM, XRD.Materials and MethodsProcedureJatropha curcas L seed shell originated from Aceh Province, Indonesia. The kernel weremanually removed from the seed. The seed shell were washed with distillate water toremove the foreign materials and oven dried  for 24 hours at 105 °C. The dry materialswere sieved to the particle size of 2 to 5 mm and stored in airtight container for furtherexperiment. The average proximate analysis of Jatropha seed shell represented in weightpercent, shows a moisture content of 5.68%, a volatile matter of 64.63%, fixed carbon of25.34% and ash content of 3.82%.Thermogravimetric analysisThermal degradation of jatropha seed shell was determined using a pyris Diamond TG/DTGthermal analyzer (Perkin-Elmer). The sample amount 3 mg (± 0.5) of jatropha seed shellwas heated from 30 to 800oC at a rate of 20 oC/min under nitrogen gas atmosphere.Experimental methodsCarbonization process of jatropha seed shell carry out from dry materials used in electricfurnace Gotech Testing Machines Inc. method for 1 hours at 600oC. After carbonization thesample was cooled to room temperture. The carbonized product were ground in differentgrinder. A big grinder (Mukmin Enviro) and than continue with small grinder (Retsch).Sieving process to get particle size of carbon black as a filler. Carbon black were sieved in 4size, 70-100 mesh, 100-150 mesh, 150-300 mesh, and > 300 mesh.Proceedings of The 5th Annual International Conference Syiah Kuala University (AIC Unsyiah) 2015In conjunction with The 8th International Conference of Chemical Engineering on Science and Applications (ChESA) 2015September 9-11, 2015, Banda Aceh, Indonesia102Products characterizationThe energy dispersive analysis X-ray (EDX) was used in analysis elemental of carbon black.This machine also conducted with this FE SEM. Microscopic images of carbon black wereobtained by scanning electron microscope (SEM model EVO MA10, Carl- ZEISS SMT,Germany). Transmission electron microscopy (TEM) images of carbon black of jatropha seedshell were taken by placing a drop onto a carbon film supported by a copper grid. A PhilipsCM12 instrument. The carbon black obtaining after UV cured were cut by means of amicrotome (LKB model 8800) and placed on the observation grid to get them TEM images.The diffractograms for carbon black specimens were measured by a Philips pw 1050 x-pertdiffractometer recorded using Cu k radiation (k = 1.54 A).  X-ray unit operated at 40 kVand 25 mÅ.  An X-ray diffractometer (XRD) was used to investigate the surface inorganiccomponents of the prepared carbon black. The X-ray pattern was  recorded in an angel of20o to 80o of 2θ. Distribution of particle size analysis on carbon black was used by the longBenc Mastersizer S (Malven Instruments) fitted with the Qspec Dry Powder Feeder. Sampleweight in 2 gram were prepared for this analysis. The number distributions at 10%, 50%and 90% cut-off point as well as the number mean diameter.Results and DiscussionThermal Degradation of Jatropha Seed ShellThermogravimetry analysis is study a formation on thermal behavior of the startingjatropha seed shell to form carbon black. Figure 1 show thermogravimetry  (TG) anddifferential thermogravimetric (DTG) curves of mass loss of jatropha seed shell in the range30–800 oC.Figure 1. Thermogravimetric analysis of jatropha seed shell showing weight loss and DTGplot.From this analysis show the initial weight loss coresponds to moisture removal at 100o,degradation of biomass at 200-375 oC, and degradation of lignin at >375 oC. Tongpootthornet al., 2011 and Sricharoenchaikul et al., 2008 has mentioned that the first stage of massloss was verified by heating the biomass, resulting in moisture elimination. The secondstage is primary of carbonization, in this zone had a greater mass loss of biomass. Thisstage presented the evolution of light volatile compounds occurs from degradation ofcellulose and hemicelluloses. The third stage indicating the decomposition of lignin, whichwas a structure with higher stability.Elemental composition of carbon blackTable 1 shows the major compound in carbon black from jatropha seed shell at 600oC inProceedings of The 5th Annual International Conference Syiah Kuala University (AIC Unsyiah) 2015In conjunction with The 8th International Conference of Chemical Engineering on Science and Applications (ChESA) 2015September 9-11, 2015, Banda Aceh, Indonesia103furnace methods at 1 hour by Energy Dispersive Analysis of X-Ray (EDX).Table 1. Elemental composition carbon black jatropha seed shellElement Weight% Atomic%C 74.25 81.97O 20.85 17.28K 1.57 0.53Au 3.33 0.22Carbon is a main compound in carbon black of jatropha seed shell carbonization, this isabout 74.25 weight % and 81.97 atomic %.  Carbon is main product degradation ofhemicellulose, cellulose and lignin from biomass. Oxygen is the important compound, and indetermines the properties of carbon black. Oxygen present during the carbonization processto produce carbon black.Morfology of carbon blackSurface structure of jatropha seed shell and carbon black jatropha seed shell hasinvestigated by SEM in Figure 3. The surface is not smooth and rough on the surface  shell.After carbonization of lignocellulose and attractive compound in biomass at 600oC at onehour in furnace method, the black color, sponge shape was occurred.Figure 3. Surface structure of:  a. jatropha seed shell and b. carbonized jatropha seed shellafter carbonization with magnification 200 x.Figure 4 shows the surface structure of carbonized jatropha seed shell after sizing in foursizes. This figure revealed change in surface morphology of char as a function of size aftercarbonization. The surface area shows relatively smooth as well as cracked and pittedmorphology. The four sizes of carbonized particles are not different in structure.Figure 4. SEM of carbonized jatropha seed shell in size: a. 70-100 mesh, b. 100-150mesh, c. 150-300 mesh, and d. > 300 mesh.a bda bca bcProceedings of The 5th Annual International Conference Syiah Kuala University (AIC Unsyiah) 2015In conjunction with The 8th International Conference of Chemical Engineering on Science and Applications (ChESA) 2015September 9-11, 2015, Banda Aceh, Indonesia104TEM has long been employed in the study of carbon black micro-structure. TEM images ofcarbon black from jatropha seed shell is given in Figure 5. Regardless of varying averageparticle size from carbon black, some common features can be extracted from theobservations. Zhu et al, 2004 has stated in their writing that particles in the carbon blacksare commonly fused together to form aggregates so that clear boundaries among particlesare difficult to define (Figure 4a and 4b).  Aggregate is commonly the primary structuralunit for carbon black. One notable tendency is that the same aggregate appears to compriseparticles of comparable size. The particle shapes are always nearly spherical. Pores arepresent within and among the aggregates.Figure 5. TEM of carbon black from jatropha seed shell; a. Image of a particle andaggregate, b. TEM part of carbon blackXRD of carbon black jatropha seed ShellFigure 7 show X-ray diffraction patterns that were recorded in order to determine thedegree of crystallinity of the carbon black. The appearance of broad peak centered at the 2θangle of 23o in the X-ray diffractograms of carbonization. Sricharoenchaikul et al, 2008 hasindicated the presence of silica in this peak. At 2θ angle of 43o, the graphitic basal panelcould be seen in the spectrum of carbonizaion of carbon black. This is also imply byChiravoot Pechyen et al, 2007 and Wimonrat et al, 2011, which confirm the structure ofgraphitic basal plans of char crystallite in the low angle region and radial spread ofcrystalline structures in high angle region in the similar broad peak. Hence, the productcarbonization from jatropha seed shell obtain are belived to be in the form prymaryparticles of small  graphitic sheets.Figure 7. X-ray diffraction analysis of carbon black from jatropha seed shellConclusionsFour size of filler from carbon blcak jatropha seed shell was performed by furnace method ina laboratory-scale. These filler will be used to enhancement in biocomposite and havecharacterization by several technic. Carbon content from this material were 74.25 weight%and 81.7 atomic%. For these condition, carbon black products shows aggregation form,high graphite structure and according to the particle size distribution, the carbon black fromparticleaggregateabProceedings of The 5th Annual International Conference Syiah Kuala University (AIC Unsyiah) 2015In conjunction with The 8th International Conference of Chemical Engineering on Science and Applications (ChESA) 2015September 9-11, 2015, Banda Aceh, Indonesia105jatropha seed shell production in micron size. The excellent properties of the synthesizedcarbon black are predicted to expand the number of commercial processes in the future. Forwide application, to enhancement nano size in biocomposite, the carbon black from jatrophaseed shell can be  made more delicate in size to get nano size.ReferencesAbdul Khalil H.P.S, N.Z. Noriman, M.N. Ahmad, M.M. Ratnam and N.A. Nik Fuaad. 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Properties Of Carbon Black From Jatropha Seed Shell As A Potential Source Of  Filler Enhancement In Biocomposites

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Properties of Carbon Black From Jatropha Seed Shell as a Potential Source of Filler Enhancement in Biocomposites

Properties of Carbon Black From Jatropha Seed Shell as a Potential Source of Filler Enhancement in Biocomposites

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Proceedings of The Annual International Conference, Syiah Kuala University - Life Sciences & Engineering Chapter