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    Esterification Reaction

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    CCurancar meneame RESEARCH AND DesIEN 18. (2022) 416424 Content ists available ScienceDirect Chemical Engineering Research and Design = |ChemES2 journs! homepage: www.elsevier.com/locate/cherd Esterification reaction of free fatty acid in used ® cooking oil using sulfonated hypercrosslinked exchange resin as catalyst ‘Nurul Asmawati Roslan*, Sumaiya Zainal Abidin®™*, Norhayati Abdullah‘, Osarieme Uyi Osazuwa"™®, Ruwaida Abdul Rasid’, Nursofia Mohd Yunus* * Deparomen of Chemical Engineering, Colege of Engineering, Univers Malaya Fahon,Lebuvaya Tun Razak, 26209, aman, Kuantan, Pohang, Malaysia * cane for Resear in advanced Fluid Processes (FLUID CENTRE), Univers Malaysia Pahang, 26500 Cambang, Kuantan, Pohang, Malaysia * Fai of Chemical an Process Engineering Tecnology, College of Engineering Tchrloy, Universi Malaya hang Lebuhraya Tan Raa, 26900, Gambang, Ruantan, Pahang, Malaysia 4 Department of Chemical Engineering, Univers of enn, PMB 1154, Bein Cy, do Stat, Nigeria ‘esr “The production of valuable fay acd ali ester AE) commercaly known as Boles] Receved 25 June 2001 from used cooking ol (UCO) feedstock ha rece guined global interest. To cary out Received in reve form 19 this production proces, an esterification eaton i necesaty to munkze the emount of september 2021 fre fatty acid (FA) in the UCD. The purpose ofthis research work isto evalte the per ‘Accepted 1 October 2021 formance of the newly snythetzd sulfonated hypercrsliked exchange resin (SHER) for ‘valle online 22 october 2001 the exterfenton reaction, The calyt wae fe eyntesied and characterized wing var fous physicochemical analyses (Le. Fourier transform infra-red (FTIR), surface morphology, eywors: [Nz physisrption analysis and thermogravimettic analysis (TGA) and futher subjected to Used cooking ait the esterification reaction to determine the reaction kinetics, The esterification reaction Biodiesel ‘was conducted at various catalyst loading (1-8 w'), reaction temperatures (40-0 °C), and Esterifcation methanol toll molar ratios (6-241). From the characterization study, SHER was found to Free fatty acid ‘have high decomposition temperature (up to 98°C) and specie surface area (836 m? g-) Hypercroslinked exchange resins ‘Addiconaly, SHER had the capability to accommodate high number of active sites which catalyst ‘could benefit the esterification reaction. The highest FFA conversion of 97% was achieved at Kinetic 5 wt catalyst loading, 60°C of reaction temperature and 12:1 methanol toll mole ratio in 2hreaction time. Analyses of the spent catalyst revealed the presence of impurities residue ‘onthe SHER’ surface following the estericaton reaction, and the catalyst pore remained ‘evident even after several reusability cycles, Finally the Eley-Ridea, paeudo-homogeneous and Langmuir Hinshelwood:Hougen-Watson kinetic models were proposed. Due tots high activation energy; Le. 48-4) mol, the reaction was found tbe limited by surface reaction an governed by the chemical step. (© 2001 Institution of Chemical Engineers, Published by Elsevier BY Alright reserved. + corresponding autor. Email addresses: sumaiys@ump.cdu.my (S. Zaina Abidin), ruwaids@ump.edu.my (R: Abdul Raid. Inepe/doior/ 10.1016) cheré207110.020 (0253 5762/0 2021 institution of Chemical Engineers Published by Flsevier All vghts reserved Ccenacas Enon ResEARcH a Desi 10 (2022) 414-424 a5, 1. Introduction Biodieel at senewle fuel can be produced from vegetable oils or animal fats. tsa biodegradable product hat see fom sulphur and ‘considered a cleaner-buringfuelcomparedto conventional petcleum ‘ive (Chanel ta, 20%), Resides tha it hae 2 good lbrcating prop ery whereitcanlengthen the engine’ ie, enhance thefash pointand ‘he cetane umber However, the hgh production cost of equipment nd raw materiale the mor problem in the tiation of biodiot Mote than 50% ofthe overal production cost are ascribed tothe costof ‘he raw materials (ane al, 215; Kumar et al, 2017, Thus, lower ality feedstock such as Canola ol (Simsek and Us, 202), grease (Bashir tl, 202), Karaja atl ea, 2039) and used cooking ol (co) (sad eta, 2020 are lized to veduce the production cost Traditionally, biodiesel i produced through wansesterfiation reaction. The dicct usage of low-quality feedstock inthis reaction leads toincrement in pureation coat (Sori Fguero et, 22) a culty in catalss recovery and reduction in yee of biodiesel (Kashyap etal, 201% Yunus etal, 2017; Roslan etal, 2019} 1m addon, this type of fedstocs ha high moisture and FA content, which ea ead to saponifcation(Abllah ct al, 2014). Moreover, the high level of FFA wil lead to hydrolysis; aside reecon will eventually raise the scoity of the mixture leading to gel formation. The gel formation fequtes additonal puiicaton steps and thus making biodiesel pro Aisin more complicated. To resalve thee problems, exterifraton reaction asa pre-weatmentstagehasbeen introduced and investigated (@hangetal, 2015). Theuilization of heterogeneous aid type catajats inthe eserication processhasbeen intensively studied asitis proven to decease the moisture and FA content in the ol while maintaining ‘high conversion of FEA. Moreover, the usage ofheterogencos ca alysts can minimize the numberof unt operations since they canbe Sepnated easy fom the reaction product (Wang et al, 2019). ‘Anideal heterogeneous aid eatalyatused in esterification reaction should have numerous strongaci sites, be cheap and have good stab ity. Asutable election ofsoldacidcatalyte could simplify the product ‘separation ab well as reduce waste generation (cuashima etal, 2009, ‘so, the solid acid eatalyt has higher thermal stability and catalytic ‘etiity when compared to solid bate esalyt. Due to this epeciic ‘apa, solid ald entalyte are widely employed in the exter ton tesction when feedrtcks that contin high FFA are ized as raw materials Heteropolyacids (Gaurav eta, 2018), 2eltes (etzer ta, 202) sulfated metal oxides Pres tl, 220) andion exchange resins (Qsazuwa and Abidin, 2020; Cadenas eta, 214) ae the mest popular acid eatalsts used in the esterification process. Amongst all hese catalyst exchange resin isknown ara versatile catalyst possesses good conosion resistant in alkaline and aic environment, ‘owing to atibutes such as very high eatin activity, ably and Felecia the eeteretion procecr Moreover, this pe of eatlyet hasbeen widely used in diferent types of reactions, sich 8 alkylation (Cadenae et al, 2014) and etherifcaion dine l, 2017), Neverthe les, til oda, designing an appropriate ion exchange resins which is Chermally stable lng fe xpan, llordable and having high reaction ‘ates lla challenge. Amodifcation ofon exchange resin in termsof ‘matrbcatrctueieequited to enhance the physiochemical properties rd subeequently promote the erterfczton reaction In earlier years in onder to explore these types of catalytic rea tons, several Kinetic models have been proposed and established, For example, Satheosh ct al (2018) examined the eeterfeation of FFA using Indian-190 catalyst. The usage of UOO as a feedstock snd methanol at alcohol was reported. The eeutions which were investigated a 58.64 °C reaction temperature was found to best ft the Langmuit-Kinshelweod-Hougen-Watson (LEW) with 134952 k mol of activation energy. The high activation energy suggests that the ratecontroling step was the surface reaction (Satheech etal (201s). Meanwhile, Konware 2016 investigated the simuancous ‘terfeation-manaesterseation reactions using a mesoporous sold cd eatalyst They found that the P-H mode well described the reac. on kinetics all the reactions (forward and reverse) followed the second-order law of kinetics, Meanwhile, Abidin etal 207) com ‘dated an FFA creation in smted CO wing RCPIGOM highly porous ion exchange resin. In the study, the Eley-Rideal (ER) model ‘vas reported tobe best in explaining the veaction Kinetics when eom- pared to pseudo:homogeneous (PH) and LHHW mode. The ress ‘Suggests that theres competng adsorption phenomenaon the surface ‘of RCPIGOM between methanol molecule ad ole cd molecules. Ton exchange resin was widely used in esterification reaction due to its ability to catalyze reaction under mild conditions (avhad and Marche 2015; note ea, 2010). The traditional on exchange esi Jsexpensve,haslow aid sie, a moderate surface area, requires eta reaction time, and ow degradation temperature fe. maximum of 120 Cor sbility (Ning nd Ni, 2017, high specific surface area of on ceachange resin ia neceasar in esterification reaction to speed up the reaction rate, increase the catalyst active site and enhance the con version of FA. n addition, thermally stable eatalyst is required 9 ‘maintain the cataljatactive site Croughout the reaction when high reaction temperate wa introdiced high thermal stabil etajet wil increase the catalyst’ regenertion and lifespan. Hence, ti ru- alt produce catalyst with high thermal tilt and specie surface area to achieve high catalytic activ “The esterification of FFA in UCD was carted out using a newy synthesized sulfonated hypercrsslinked exchange resin SHER) a the catalyst i tis current study. Recently our group has undertaken study on the production of SHER fosan etal, 2019; Rodan, 2017) SHER san synthesize by introducing a styrene a6 3 monomer vinylbensyl ‘horde (VBC) asa co-monomer, ply (N-inypyroidone (PVPS as ‘stabilizer, Titon X05 as acostablizer and and benzoyl petorde (890) as am nitsor and ethene glyco dimethacrylate (EGDMA) = 8 ‘rossinker. Based on the curent state of esterification reaction, his ‘work established the fist study of combination VBC and BPO as an comonomer and intiatorinpeporingionexchangerecinaracatalyet Besides that, ther reno stuies in regard tothe Kinetics and mecha~ istic over this typeof cataljst forthe esterification reaction There are ‘three ain pats in thie study) the yates and characterizatonsf ‘the SHER, 2) esterification reaction of SHER, and) studies onthe ea ‘on Kinetics of SHER The physicochemical properties of the SHER were ‘so evaluated using thermogravimetry analysis (TGA), Fourier tane- {erm infrared PTR) particle sie detution (PSE) Ny phyionpion, ‘elemental analysis, surface morphology, and acid capacity. The par ‘netic senatvity analysis was conducted sing one variable at atime pproach where the influence of reaction condition nach at eats Iya loading, temperature and reactant molar ratio were investigted nally ew binetes model (Le ER, PH and LIEW) were employed to cbtsn the reaction actation energy and interpret the Kinetic data 2. Materials and methods 21. Chemicals 2-propanol (995%), 01 M standatdized solution sodium hydroxide, toluene (95%), oleic acd (5%) p-aphtolbenzin, -vinylbenzyl chloride (VBC) (95%), benzoyl peroxide (BPO) (95%), ethylene glycol dimethacrylate (EGDMAVO®%), styrene(S) (99%), Triton X-305 (99%), 1,2-dichloroethane (DCE) (99%), poly {Nvinylpyrolidone) (PVP 5, ron (chloride (99%), diethyl «ther 93%) methanol MeOH) 99%), ethanel (EtOH) 29%) ace- tone (09%) nitric aci (97%), chloroform (2%) andaulfuric acid (09%) wore obtained commercially fom Sigma Aldrich. The [0 was purifed by chloroform and methanol prio to use 22. synthesls of sulfonated hypercroselinked exchange resin (SHER) ‘sulfonated hypercrosslinked exchange resin (SHER) was synthesized using non-aqueaus dispersion technique es pre- viously published in literature (Roslan et al., 2013; Roslan, 2017) This method comprises three main stages: the pro- duction of non-aqueous dispersive precursor particles, the 16 creases xcees ssesact aun Desc 180 (2022) 414-404 preparation of thehypercrosslinked particles, and the sulfona- ‘Hon of the hypercrosslinked particle. Firstly, precursor particles were prepared using non- queue dispersion polymerization (NAD) method. Ina round ‘ack, 4049 of styrene, 59 of VBC, 89 of PVP-55, 2.759 of Titon 1-205, 29 of BPO and 150 ml of ethanol were mixed, The flask ‘was equipped witha condenser and No gas was purged for 30 ‘min to initiate the polymerization reaction. The solution we ‘heated for an hour at 70°C, Algo @ solution containing 05 9 ‘of EGDMA and S g of VAC was heated tnder the No gaa low 3t 70 °C in a separated flask. This mixture was then inserted {nto the frst flasle dropwise, It was continuously heated and stirred for 24, and the resultant mixture was subsequently ‘centtfuged with methanol and ethanol at 3000 rpm. Finally, the particles were filtered using a nylon membrane filter and alrdried for overnight at 40 °C, The collected particles were Jnown as precursor paticles. ‘To prepare the hypercrossinked particles, 10 g of the pre- ‘cursor particles were applied into flask containing 40 ml of DCE. The particles were let to swell underflow of N gas for 4h. Then, 8 g of FeCl; was added, and heat was immediately Introduced into the mixture and continuously steed for 18 ‘hat €0 C. To eliminate the presence of impurities, the solid particles were retrieved and rinsed with MeOH and HNO», The collected particles were extracted using acetone, washed with ‘MeOH and diethyl ether before drying overnight was cartied out at 40°C, For the sulfonation process, 10 g of the hypercrosslinked. beads were introduced into 30 ml of anhydrous DCE and left for 1h to wet the beads. 8 ml of sulfuric acid was then added {nto the reaction ask. The lution was heated rapidly to60'C and continuously stired under N, gus flow before the resulting beads were allowed to cool and washed with distilled water. Post particle recovery, the particles were dried at 40 “Cusing a ‘vacuum filtration process for 12h, The particles produced in this stage fs known as SHER. 23. Characterzations of the SHER ‘The Nz physisorption analysis were conducted to identify specific surface area, pore diameter and pore volume of the catalyst, Elementar Germany analyzer was used to deter- ‘mine the percentage of carbon, Ha, Nz and sulphur content of the resin, Titration techniques was employed to calculate ‘the ion exchange capacity (IEC) ofthe resin. The decompo sition temperature of the synthesized catalyst was analyzed by 0500 thermogravimetre analyzer Fourier transform infra~ red (FTIR) analysis was performed forthe synthesized catalyst to identify the existence of functional groups. To determine the size distribution of the synthesized catalyst, Malvern ‘Mastersizer 2000 was used, The fresh catalys's surface mor- phology was viewed using CARL ZEISS scanning electron microscopy (SEM) analyzer, while the surface morphology and sulphur content ofthe spent catalysts was obtained using the {leld-emission scanning electron microscopy-energy disper- sive X-ray spectroscopy (FESEM-EDX). 24, Used cooking oil (UCO) preparation ‘To prepare the simulated UCO, 100 g of cooking ofl and 6 g of oleic acid were mixed and stirred for min Standard titration method (ASTM D374) was employed to calculate the samples acid value. The ald value of ol used was about 12 mg KOH and the Fra content was 6% 25. Free fatty acid esterification in UCO A 500 ml reaction flask fitted with @ temperature controller snd condenser was used during thie study. UCO and methanol were added, stirred and heated in the flask. The catalyst was Added once the solution reached the desired temperature, The esterification reaction were investigated for 8h. Samples were periodically taken to obtain the acid value. The percentage of FFA (XFFA) is determined using E4. 1. x-¥ FPA = xc x 282 0 ‘where C= concentration ofthe titration solution, X = volume ofthe titration solution (mi) and ¥ = volume of blank (ml) and w= the oll mass ( ‘reusability study ofthe SHER was conducted todetermine the catalyst life span. The SHER was washed with methanol in the ultrasonic bath until all UCO was removed and a colour Jess solution was obtained. The conductivity of the solution was recorded and the process continues until the conduct ity ofthe solution was approximately the same withthe wash solvent used. (Conductivity of methanol: 023 wS m~). The SHER was filtered and dried in an oven at 100 ¢ for 6h. 2.6. Kinetic modeling studies ‘The effect of temperature towards the FFA conversion was employed to determine the reaction kinetics. ER, PH and LitHW second-order kinetic models were utlizedin tis study to ithe kinetic experimental data Several assumptions made to adopt these kinetic models are: 1} a reversible hetero- geneous process was presumed to be the reaction, 2) nom existence of FAMEat time, t=0,3) the reaction mixture volume remained the same throughout the reaction, 4) The perfor- mance of the catalyst was deemed tobe the same for all resin sites 5) relative to the catalyzed reaction, the reaction rate for reaction without the presence of catalyst was negligible 3. Results and discussion 3.41, Catalyst characterizations The detalls discussion on FTIR, morphology or surface struc- ture, TGA and Nz physisorption analyses of SHER were presented in this section, 3.4.1. Fourier transform infra-red (FTIR) analysis “The FTIR spectra shows in Fig, 1 was employed to determine the functional group presence in the eynthesized catalyst, “The presence of 0-H bond (3000 em” and above is because of the presence of moisture inthe sample which was likely adsorbed from the surrounding air during the preparation of ground resin and moulding of the potassium bromide (KBr) tablet Hence, due to its hygroscopic nature, SHER adsorbed moisture and consequently formed O-H bond. A sharp peal ‘around 1000-1250 cm indicates S=0 vibration of the sul- fonic acid group. A peak stretching around 1171 em!-1226 cm represents the asymmetric SOs, Meanwhile, the peaks present between 1000 em"! and 1120 em-! was indicative of symmetric $03. To further confirm the present of SO, X-ray 022) 41424 a7 ii women Fig. 1~ FTIR spectra of SHER, Photoelectron Spectroscopy (XPS) analysis was also conducted and presented in Supplementary File. 3.1.2. Morphology and surface structure ‘The morphology/surface structure of the resin represents in Fig. at 25x and 5000x magnifications, respectively were ana lyzed using SEM. The images in fig. 2a clearly shows the formation of uniform spherical shapes for synthesized SHER, ‘while 2b represent the morphology on the catalyst’ surface at lower magnification (5000), showinghighly porous surface of the SHER. 3.43. Thermogravimetric analysis (TA) TGA thermogram of the SHER catalyst is shows in Fig. 3.1m the frststage, the elimination of water adsorbedby the SHERis observed (below 150°), Decreasing peaks were demonstrated atthis stage due to SHER's inability to adsorb additional mois ture and this beahviour further confirm in the FTIR analysis (Geferto Fig. 1), where the result indicates lew intensity ofthe (O-H bond, Furthermore, decomposition of sulphate species from the surface of the SHER occurred in the second stage between 300 °C and ~500 °C. From the TGA analysis, SHER has an excellent temperature resistivity due to the ability of this resin to withstand up to 358 C before decomposing. The polymer structure degradation was shown atthe final stage where total weight loss was occurred around 500 °C-780 °C. 3.14. No hysisorption analysis The BET surface area obtained for SHER was 636 m? specific poe volume ofo.52em° g-? and an average pore diam: eter of 28.2 A. The adsorption-desorption behavior of SHER obtained from the Np physisorption analysis was presented in supplementary data. Initially, when the relative pressure Increases, the amount of Np adsorbed also increased and then plateaued, The result shown that capillary condensation of Np take place within the catalyst’ pore. The isotherm shows Fig. 3~ TGA curves of SHER catalyst SSS ‘Appearance ‘Sphere and opaque eee High Polymer srsctre Functional group acroporous plyeyrene sulfoi acid Degre of eufonstion (x) =a ‘Tempertare lt (2) =e Ton exchange capacity(mmolg) 50 Perea ue mental Ari 0 Carbon ns nyoen sa 2 pysrpion Analysis BET surface are mg) 6 Specifepore volume (em? g) 082 ‘Average pote diameter (A) m2 4 linear trend at approximately P/Py less than 0.2, which sug {gests monolayer adsorption of Nz on the pores of the SHER. AtP/P, greater than 0.20, an upward trend was obtained. At this stage, Nz molecules with multiple layers were developed Based on the IUPAC classification, the isotherm ofthe parti cle showed the catalysthavingpores that were classified inthe ‘mesoporous range type V. Mesoporous isotherm typelIV and V indicates the multilayer adsorption ofthe mesoporous struc ture by the existence of the hysteresis loop accompanied by capillaty condensation, The activities of adsorption and des corption are significantly linked to this loop of hysteresis. The hysteresis loop for this sample was an Hi type loop ascribed to the porous materials consisting of agglomerates withanarrow pore size distribution 245. Summary on the SHER properties ‘The characterizations of the SHER were summarizesin Table 1. Fig. 2~ Surface morphology of SHER ata) 25x magnification and b) 5000x magnification. a8 creases xcees 3.2. Esterifeation offre fatty acid 3.2.1. Mass transfer resistance ‘To ensure the reaction is controlled by surface reaction during the measurement of the apparent reaction kinetics, the mass ‘transfer resistance external and internal) mustbe minimized ‘The experimental design was divided into two pars (Le difer- ‘ent stirring speed and different range of particle size) Tostudy the presence of extemal mass transfer resistance, the exper- Jmental work was conducted at various stirring speed, and the findings were further verified usingMears Criterion theory. Meanwhile, different range of particle size was manipulated to examine the internal mass transfer resistance, and theo- retical verification was conducted using Weisz Prater Criterion theory. 32.2. Effect of external mass transfer resistance ‘The FFA conversion obtained using different stirring speed from 150 to 450 rpm was investigated to study the influence of ‘external mass transfer. From the results presented inthe sup- plementary data, itcan be concluded that there is «negligible difference in the stiring speed for the final FFA conversion. ‘The Mears Criterion (Cy) was utilize to verify the insignif- ‘cant presence of external mass transfer resistance as shown in q.2. Tax Re xn un ex Co oa ® ‘Where, =rate of reaction, Cag = bulle concentration of limit- ingreactant, Ke = mass transfer coefficient n = reaction order, y= bulk density catalyst and R= catalyst radius In this current study, all Cy values found are <0.15. This val~ ‘uesshow that therate of diffusion ofthe reactants through the layer of fui was extremely fast. tt can therefore be concluded that the reaction rate and FFA conversion are not affected by the stirring speed, hence, can be neglected. Taking the energy ‘consumption into consideration, string speed of 150rpm was adopted forthe subsequent experimental work, The values of (Cyat diferent string speed is surmmarized inthe supplemen- tary data 42.3, bffect of internal mass transfer resistance Different ranges of PSD (250-450 mm, 3-895 jum and 600-850, tam) were selected to study the influence of internal mass transfer. The detailed results on the mass transfer limitation ‘were presented in supplementary data, The result shows a similar pattern of reaction rate and FFA conversion using a selected range of PSD. Weisz Prater Criterion (Cyp) equation represented n Eq. 3 was used to verify the presence of internal ‘mass transfer resistance theoretically mrant _ Cue= eae @ were 14 = tection rt, ge = catalys densiy, Re = cat Iya radius, Gy = concentration of limiting reactant and Day fective ditfusiviy, ‘The calculated values of Cyp obtained for all particle size range were less than 1, These values indicate minimal resis- ‘tance to the pore's internal ciffasion; therefore inthe selected range of PSD, the internal diffusion can be neglected, The details value of Cy» was tabulated in supplementary data. | .ofitye ° "| oxay (6 f2/s alt a fg. mone of xalyt nding onthe FA conversion. (ot 150 rpm, 12:1, and 60 “C reaction condition: 3.24, Effect of catalyst toading A fixed reaction conditions (150 rpm, 60°C, and 12:1 M rato, the influence of catalyst loading on FFA conversion was con: ducted by manipulating the amount of SHER loaded into the reactor from 1 to 8 wit, The results presented in Fig, 4 show that the resction rate increases with an increment in loading of SHER. in addition, the time required to achieve the equi Nbrium point is reduced. In accordance with lnerature (Wang ft al, 20148), and from Fig 4, the best catalyst loading is 5 ‘we to obtain an FFA conversion of 97%. This is attributed to the increased in the number of the active site with increas ing the catalyst loading. The high actve site available during the reaction will contribute to the high contact rate or mass transfer between reactant and catalyst. Hence, subsequently Increased the FFA conversion and reaction rate. However, fut: ther increase in catalyst loading (Le. >$ wes) only helps to Improve the reaction rate, but the final conversion remains the same. This is probably due tothe high availabilty of active site ‘butan insufficient amount of reactants and therefore reduced the FFA conversion. Moreover, the nsignificantincreasein FFA conversion algo resulted from the mass transfer limitation at high catalyst loading. Hence, 5 wt of SHER is selected for further experimental work, 3.25. Effectof reaction temperature Im selecting the reaction temperature, the boiling point of methanol needs tobe considered to avoid the les of methanol (vaporization of methanol) throughout the esterification reac- tion, Various reaction temperatures (40, 45, 50, 55, and 60°C) ‘were evaluated to investigate the best reaction temperature, From Fig 5, the conversion and the rate of reaction increase ‘when the reaction temperature increases. The introduction of higher reaction temperature resulted in an increase in the number of energy collisions, hence, increased the rate of reac- tion and reaction conversion (shatia etal, 20203; Li et a, 2014; Baja et al, 2010a; Thinnakorn and Techeikuna, 20149) 1 the fist 60 min, all temperatures show a sharp rise in FFA conversion, indicating a high rate of reaction taking place at the beginning of the reaction. in the second phase (approx- imately 60-180 min), the reaction rate gradually decreases. Finally, in the third phase (about 60-180 min), a relatively steady conversion of FFA iz achieved as the reaction moves towards the equilibrium stage. No further increase in FFA con- Ccenacas Enon ResEARcH a Desi 10 (2022) 414-424 419 | SRT RSeerey em

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