Ethanolic Extraction of Soybean Oil: Oil Solubility Equilibria and Kinetic Studies

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1 Ethanolic Extraction of Soyban Oil: Oil Solubility Equilibria and Kintic Studis Christiann E. C. Rodrigus*, Natália M. Longo, Cibl C. Silva, Kila K.. Aracava, Bruna R. Garavazo Sparation Enginring Laboratory (LES), Dpartmnt of Food Enginring (ZEA / FZEA), Univrsity of Sao Paulo (USP) PO Box: 3, Zip Cod: Pirassununga SP Brazil. Th main goal of this ork as to valuat th thanol prformanc on th xtraction procss of soyban oil. Th influnc of procss variabls, solvnt hydration and tmpratur as valuatd using th rspons surfac mthodology. In addition, th kintics of xtractabl substancs from soyban flaks ith thanol as solvnt as studid and th rsults r modld considring th modl of So and Macdonald. It can b notd that oil solubility in thanol as highly affctd by th atr contnt hil incrasing tmpratur only promots th incrasd lvl of solubl solids xtraction for conditions hr solvnts ith lo contnts of moistur ar usd. Th fr fatty acids xtraction is improvd by incrasing th moistur contnt in th solvnt hil th rtntion indx is only dpndnt on solvnt moistur contnt. Th valus for this dpndnt variabl incras as th solvnt hydration lvls incrass. It as also obsrvd that th moistur transfr procss, from th soyban flaks to th xtractd phas, is not tmpratur dpndnt. In gnral, th non-linar multipl rgrssion allod us to obtain modls ith good prdictiv capability. In th kintic study, th rsults producd by th modl of So and Macdonald r found to b in good agrmnt ith th xprimntal data (0.89 < R < 0.99). 1. Introduction Th sarch for altrnativ solvnts to xtract dibl oil from oilsds has rgaind attntion mainly du to groing nvironmntal concrns rlatd to th us of hxan, th most common solvnt usd around th orld. This fossil solvnt is chosn du its high stability and high capability of dissolving oil. Furthrmor, this solvnt allos on to obtain a dfattd mal of good quality that can b usd in food formulations for human consumption. A varity of solvnts hav bn proposd to rplac hxan as xtractant of vgtabl oils: atr ith or ithout nzyms, aldhyds, ktons, shortchain alcohols, among othrs (Johnson and Lusas, 1983). Rplacing hxan ith a biornabl solvnt may b intrsting, spcially if th substitut is largly availabl, it prsnts lo cost and similar xtracting fficincy for nutral lipids and nutracutical compounds (Rodrigus and Olivira, 010). In Brazil, th high volum of thanol production allos on to purchas this matrial at lo prics, ncouraging rsarch on

2 th substitution of hxan by thanol (Rittnr, 199). Th main goal of this ork as to valuat th thanol prformanc on th xtraction procss of soyban oil.. Matrials and Mthods.1 Matrials Th solvnts usd in this ork r absolut thanol, from Mrck (Grmany), ith purity gratr than 99.5 %, and aquous solvnts ith varying moistur contnts, in th rang of.97 to 0.01 %, on mass basis, prpard by diluting dionizd atr into absolut thanol. Soybans, prviously crackd, dhulld and flakd, r kindly supplid by Cargill (Brazil) and r usd as rcivd, ithout furthr prtratmnt. Soyban flaks r charactrizd in trms of oil contnt, protin contnt, and moistur contnt according to official mthods (AOCS, 1998). All masurmnts r prformd in quintuplicats. Th ra matrial as also charactrizd in trms of fr fatty acids (FFA) by titration (IUPAC 1979).. Mthods: quilibria and kintic studis Batch xtractions r carrid out in 50 ml isothrmal cylindrical clls built in pyrx glass, according to procdur dvlopd by Rodrigus and Olivira (010). Th clls r sald to avoid solvnt losss and th systm tmpratur as controlld in a prst valu (40 to 60) ± 0.1 C using a thrmostatic bath (Tcnal, Brazil). Th solid-liquid systms r obtaind by adding knon masss of soyban flaks and solvnt in th mass ratio of 1:4.5 (solid: solvnt). Th pr-st quantitis of flaks and solvnt r ighd in analytical balanc ith radability of g (Adam, UK). For xprimnts rlatd to th phas quilibria study, a magntic stirrr as usd (Ika, Grmany) to agitat th mixtur for at last 4 hours. In th cas of kintic study, sampls of raffinat and xtractd phass r obtaind vry 5, 10, 15, 0, 30, 50, 60, 180, 300 and 1440 minuts. Th stirring vlocity as kpt constant at 800 rpm for all th xtraction xprimnts. For both kinds of xprimnts, th raffinat phas mass as ighd on an analytical balanc and th xtractd phas composition as masurd according to th folloing mthods: FFA concntration as dtrmind by titration (IUPAC, 1979). Th total solvnt concntration as dtrmind by vaporation at 60 C. Th atr concntration as dtrmind by Karl Fischr titration (AOCS, 1998). Th solubl substancs composition as dtrmind by diffrnc. In this ork, all masurmnts r prformd, at last, fiv tims..3 Rspons surfac mthodology Th rspons surfac mthodology (RSM) as usd to invstigat th ffct of som procss variabls (tmpratur and atr contnt in th solvnt) on th solubl substancs, and FFA transfrs, during an quilibrium stag of th solid liquid xtraction procss. Th fatty compounds and atr transfrs r calculatd by q 1 (Rodrigus and Olivira, 010). EP EP i solid solid i m Ti (%) = 100 (1) m hr m is th mass, is th mass fraction, EP is xtractd phas, solid rfrs to soyban flaks at th bginning of th xtraction procss, i is solubl substancs or FFA. In this cas, th xtractd phas mass as dtrmind by mass balanc (Rodrigus

3 and Olivira, 010). A factorial dsign as plannd to obtain quadratic modls for th rsponss of intrst. Th complt st comprisd trials plus a star configuration (or axial points) ith thr rplicats in th cntral point (11 trials) (Box t al., 1978). Contour curvs r thn sktchd using th quadratic modl for th statistically significant variabls. Th Statistica softar (Statsoft, v. 9.0) as usd to analyz th rsults folloing th cntral composit dsign. To tst th prdictiv capacity of th statistical modls obtaind in this invstigation, th avrag rlativ dviations (ARD) r calculatd according to q. n x calc x 100 ARD(%) = y i y i y i () i = 1 n hr y i is th rspons transfr, n is th numbr of trials, x and calc ar rlatd to th xprimntal data and thos stimatd using th RSM modls, rspctivly..4 Kintic modl Th mathmatical modl proposd by So and Macdonald (Mzian and Kadi, 008) as usd to corrlat th kintic data. This modl considrs that this xtraction occurs according to to simultanous procsss: (a) oil occurring on th sd surfac is quickly rmovd by simpl ashing ith th solvnt; and (b) th xtraction of any rmaining oil in th brokn or unbrokn clls is govrnd by a diffusion procss in to stps occurring insid th sd: slo (diffusion 1), and a vry slo (diffusion ). Th concntration (C) at any tim (t) of oil in th solvnt is givn by th folloing quation: C = C d ( 1 xp( k t) ) + C ( 1 xp( k t) ) + C ( 1 xp( k t) ) C = C + C + C d d hr C is th oil concntration at quilibrium; C is th ashing stp; C and C ar th diffusion constants rlatd to stps 1 and ; k, k and k rprsnt th mass d transfr cofficints of th ashing and diffusion stps (min -1 ), and th numbrs 1 and rprsnt th rlativ indxs to th first and th scond diffusion. Valus of th mass transfr cofficints k, k and d k as ll as th oil yilds at quilibrium 1 d C, C and d C hav bn calculatd numrically ith a non-linar last squars fitting mthod using th program Origin 8.0. d (3) 3. Rsults and Discussion Dnsity of th soyban flaks usd in this ork as 335 ± 18 kg m -3, basd on tn rplicats. Th rsults obtaind for th diffrnt charactrizations of th solid matrial r: moistur, (6.63 ± 0.09) %; Oil (dry basis) (1.83 ± 0.13) %; Fr fatty acids (dry basis) (0.4 ± 0.01) %; Protin (dry basis) (38.83 ± 0.55) %. To vrify th ffct of th procss variabls, tmpratur (T) and atr contnt in th solvnt (W), on th xtraction procss, a factorial dsign as implmntd. Tabl 1 prsnts all combinations of th studid variabls in th statistical analysis and th corrsponding rsponss for th factorial dsign. Th statistical analysis yildd th folloing modls, qs 4 to 7, rprsnting th rsponss, as a function of statistically significant variabls, hr W*, and T* ar codd variabls.

4 T = + (4) T sol (%) W * W * 10.70T * T * (%) = W * W * T * T * 3.43T * -.96W*T* (5) FFA + RI(kg/kg) = W* (6) Watr EP (%) + Tabl 1: Factorial dsign: + star configuration + cntral points Codd Variabls Actual Variabls Rsponss W* T* W a T b T sol b T FFA RI c d Watr EP (mass %) ( C) (%) (%) (kg/kg) (%) a Contnt of atr in th solvnt (% in mass); b Transfr (%); c Rtntion indx (mass of adhrd solution mass of inrt solid); d Watr contnt in xtractd phas (% in mass). = W*-0.35T* 0.47T* (7) Tabl shos th analysis of varianc (ANOVA) for ths rsponss at 95.0% confidnc. As it can b sn in Tabl, th vast majority of rsponss prsntd high corrlation cofficints and accptabl ARD valus. Tabl : Analysis of Varianc (ANOVA) Sourc of variation T sol (%) T FFA (%) RI Watr EP SS a SS a SS a SS a Rgrssion Rsidual Total F valu (F list) (4.53) 6.13 (3.69) 3.80 (5.1) (4.35) CC b ARD (%) c a Sum of Squars; b Corrlation cofficint; c Avrag rlativ dviation (q ). With ths statistical modls, qs 4 7, it is possibl to sktch contour curvs that rprsnt th influnc of tmpratur and atr contnt in th solvnt on th rsponss (Fig 1). In Fig. 1(a) it can b obsrvd that th solubl substancs transfr (T Sol ) is strongly influncd by th atr contnt in th solvnt. In fact, th incras of atr contnt in thanol strongly supprsss th solubl substancs xtraction hil incrasing tmpratur only promots th incrasd lvl of solubl solids xtraction for conditions hr solvnts ith lo contnts of moistur ar usd. Figur 1(b) shos

5 that th FFA xtraction incrass ith incrasing tmpratur. This ffct is mor significant hn th moistur contnt in th solvnt is lo. In Fig. 1(c) can obsrv that th rtntion indx is only dpndnt on solvnt moistur contnt. Th valus for this dpndnt variabl incras as th solvnt hydration lvls incrass. In Fig. 1(d), it can b sn that th moistur transfr procss, from th soyban flak to th xtractd phas, is not tmpratur dpndnt. Figur 1: Contour curvs of rsponss xprssd as a function of atr contnt in th solvnt (mass %) and tmpratur ( C). (a) T Sol ; (b) T FFA ; (c) RI; (d) Watr EP. Exprimntal data of kintic of xtraction, givn in Fig., r fittd ith th mathmatical modl of So and Macdonald. Vry good fits ar obsrvd as shon by th high valus of th cofficints of dtrmination (0.89 < R < 0.99). As xpctd, th incras in tmpratur rsults in an incras in oil yild in th xtract phas. Th chang in yild can b xplaind by th fact that th ris in tmpratur incrass th solubility and th facility of diffusion of th oil hil dcrasing viscosity. 4. Conclusions Th xprimntal dsign allod us to obtain statistical modls using th RSM. Th statistical analysis nabld us to slct th procss conditions, tmpratur and solvnt moistur lvls, to maximiz T Sol and to minimiz RI. In gnral, th rsults sho that th oil xtraction procss from soyban using thanol is possibl. In addition, this study shod that th modl of So and Macdonald gav xcllnt fits of th xprimntal data of oil xtraction using thanol ith diffrnt hydration lvls as solvnt.

6 Figur : Extraction yild vrsus contact tim shoing th ffct of tmpratur ( C) and diffrnt atr contnts in th solvnt. (a) (0.06±0.01) mass %; (b) (5.98±0.01) mass %; (c) (15.01±0.07) mass %.( ) So and MacDonald modl. Acknoldgmnts Th authors ish to acknoldg FAPESP (Fundação d Amparo à Psquisa do Estado d São Paulo - 009/ and 008/5658-8) and CNPq (Conslho Nacional d Dsnvolvimnto Cintífico Tcnológico). Rfrncs AOCS, 1998, Official Mthods and Rcommndd Practics of th Amrican Oil Chmists Socity. AOCS Prss, Champaign. Box G.E.P., Huntr, W.G. and Huntr J.S., 1978, Statistic for Exprimntrs an Introduction to Dsign, Data Analysis and Modl Building. John Wily & Sons, N York. IUPAC, 1979, Standard Mthods for th Analysis of Oils, Fats and Drivativs. Prgamon Prss, N York. Johnson L.A. and Lusas E.W., 1983, Comparison of altrnativ solvnts for oils xtraction. Journal of th Amrican Oil Chmists Socity, 60, 9 4. Mzian S. and Kadi H., 008, Kintics and Thrmodynamics of Oil Extraction from Oliv Cak. Journal of th Amrican Oil Chmists Socity, 85, Rodrigus C.E.C. and Olivira R., 010, Rspons surfac mthodology applid to th analysis of ric bran oil xtraction procss ith thanol. Intrnational Journal of Food Scinc and Tchnology, 45,

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