Recent Advances in Petrochemical Science ISSN: 2575-8578
Review Article Recent Adv Petrochem Sci Volume 6 Issue 5 -November 2019 Copyright © All rights are reserved by Basma Mohammed Kadhim DOI: 10.19080/RAPSCI.2019.06.555699 Prediction of The Behavior for Polymer Blends Using Thermodynamic Model
Khalid Farhod Chasib1 and Basma Mohammed Kadhim2* 1Petroleum & Gas Engineering Department, University of Thi Qar, Iraq 2Industrial Water Department, Thi Qar, Iraq Submission: October 14, 2019; Published: November 05, 2019 *Corresponding author: Basma Mohammed Kadhim, Industrial Water Department, Thi Qar, Iraq
Abstract
Two polymer blends were prepared. The first one was Poly methyl methacrylate (PMMA) and Poly vinyl acetate (PVAc), and the second was Poly vinyl chloride (PVC) and Polystyrene (PS). The first blend prepared by mixing two polymers (PMMA, PVAc) with co-solvent (Chloroform) at different weight percentages (0/100, 20/80, 40/60, 50/50, 60/40,80/20,100/0). The second blend prepared by mixing two polymers (PVC, PS) with co-solvent N, N dimethylacetamide (DMAC) at different weight percentages (0/100,20/80,40/60,50/50,60/40,80/20,100/0). Two processes were used for preparation; dissolution process was used at a room temperature (25oC) and (1atm.) pressure using co-solvent. Viscosity test was performed for stock solutions (1%wt/v=1g/dL) and other concentrations (0.75, 0.6, 0.5, 0.4, 0.3 g/dL (, these concentrations are obtained by dilution of stock solution. The obtained data were collected and substituted accordance to equations (Huggins Equation) and certain criteria ( Interaction parameters ΔB , μ ) to identify the miscibility (or compatibility).To get polymer blends in solid state, The same DSCprocedure and FTIR. to prepare the stock solution of diluted solutions followed but the stock solutions of polymer blends were at concentration (10%wt/v) for all different compositions and then followed solvent casting ( evaporation then drying) . the solid-state samples were taken to hold tests of
The aim of the present work was to study the thermodynamic behavior of polymer blend via determination of miscibility. Miscibility (or immiscibility) tests are performed in three techniques: viscometry method, DSC analyzer and FTIR to test polymer blend in solid state. It was found from the viscosity method that for first blend (PMMA/PVAc), the interaction parameters (ΔB, μ) are positive for all compositions therefore the system is miscible whilst the second system (PVC/PS) is immiscible where the interaction parameters (ΔB, μ) are negative. Differential scanning colarimetry (DSC) analyzer gave thermogram curves revealing one glass transition temperature for PMMA/PVAc blends except at (20/80) composition, this indicates that the system is miscible except at (20/80) composition. But, PVC/PS blends showed two glass transition temperature, so the system is immiscible. FTIR analysis for PMMA/ PVAc blends depicted a weak interaction between the two polymers and solvent due to the miscibility establishment, whilst for PVC/PS blends, there was no interaction between two polymers to establish the miscibility, this indicates immiscible system. Calculations of Flory –Huggins interaction parameter for two systems was performed and the results pointed to miscible blend for PMMA/PVAc blends and immiscible blend for PVC/PS blends. So, there is a good agreement between the experimental results andKeywords: calculations of interaction parameter based on Flory – Huggins theory.
Polymer blends; Flory –Huggins interaction parameter; Miscibility; DSC; Gas constant; Hydrogen bonding; Critical solution Abbreviations:temperatures; Dipole-dipole interaction; Ionic interaction; Resembling crystallization Scanning Calorimetry PVC: Poly Vinyl Chloride; PS: Polystyrene; PMMA: Poly Methyl Methacrylate; DMAC: Dimethylacetamide; DSC: Differential
Introduction and Theoretical Framework
the manufacturer by offering improved processability, product Polymeric materials find growing applications in various productivity. Polymer blends have received much attention since uniformity, quick formulation changes, plant flexibility and high fields of everyday life because they offer a wide range of applica- tion relevant properties. Blending of polymers is a technological blending is a simple, effective approach to develop new materials way for providing materials with full set of desired specific prop- individual polymers. Miscibility between two components is gov exhibiting combinations of properties that cannot be obtained by erties at the lowest price, e.g. a combination of strength and tough- - ness, strength and solvent resistance, etc. Blending also benefits erned by the thermodynamics represented by the Gibbs free en-
Recent Adv Petrochem Sci 6(5): RAPSCI.MS.ID.555699 (2019) 00141 Recent Advances in Petrochemical Science
Consider two polymers having glass transition temperatures
mix mix mix T and T . The mo ergy of mixing (G = H - TS ). The mixtures are miscible when g 1 g 2 1 2 S the value of Gmix is negative, i.e., low value of Hmix and high value of and respective molar enthalpies H and H - andmix the S mix . Immiscibility is a rule in polymer blends because both the H lar enthalpy of a mixtureHmix = of xH11 the two + xH 2polymers 2 +∆H is:m mix are unfavorable. The Smix is unfavorable because there (4) are few molecules of large molecular weight per unit volume. The Hmix is also unfavorable because the van der Waals dispersion Where xi m represents the mole fraction of polymer i in the force is always positive. However, when the specific interactions blend and ⧍H is the excess enthalpy of mixing. teraction are established, the miscibility between two polymer such as hydrogen bonding, dipole-dipole interaction, or ionic in- mixtures can be achieved [1]. (5)
If two polymers are mixed, the most frequent result is a sys- tem that exhibits a complete phase separation due to the repulsive 1 2 The thermodynamic cycle for the mixing process is represent- interaction between the components (i.e. the chemical incompat- mix T l to T 2 at constant ed by Eq 5, where H , H , and H are the changesg g of enthalpies ibility between the polymers). Complete miscibility in a mixture when the temperature is increased from of two polymers requires∆G that =∆ the H following −∆ TS condition <0 is fulfilled: Tg T T mm m pressure for polymerg 1, polymer 2, and their blend, respectively.g and yields l Tg 2 Where m, m, and m Hm( 1) and Hm( 2) are the excess enthalpies of mixing at mix ∆. SolvingH = xHxHEq ∆ 5 for + H ∆ +∆ HT21 −∆ HT ΔG ΔH ΔS are the Gibb’s free energy, the en- mix 11 2 2 m ( gg) m ( ) thalpy and entropy of mixing at temperature T, respectively. The The enthalpy changes corresponding to heating the individual (6) Tg T most important characteristic of a polymer blend of two (or more) 1 to g 2 polymers is the phase behavior. Polymer blends (like low molec- Tg 2 components and the mixture∆=H from c1 dT are [3]: ular weight solvents) can exhibit miscibility or phase separation 11∫ p Tg1 and various levels of mixing in between the extremes (e.g., partial T ∆=g 2 g miscibility). H22∫ cp dT (7) Tg1 For a stable one-phase system, criteria for phase stability of 2 Tgs binary mixtures of composition∂∆ ∮ atG fixedm temperature T and pres- ∆
How to cite this article: Khalid Farhod Chasib, Basma Mohammed Kadhim. Prediction of The Behavior for Polymer Blends Using Thermodynamic Model. Recent 00142 Adv Petrochem Sci. 2018; 6(5): 555699. DOI: 10.19080 RAPSCI.2018.06.555699 Recent Advances in Petrochemical Science
TTgg12 z −1 φφ12 2 ln =−β 1 γspe ln lnφ1++ ln φφ 22 ln T er r T mers, and β =∆∆zR/( M11u C pp) ., RM u and Cpp are the gas constant, gg1 12 1 dipole-dipole interaction, or ionic interaction between two poly- where Tg1 and Tg12 are the Tgs (9) are of the pure polymer1 1 and2 of the molecular [4]. weight of the repeat unit, and the isobaric spe- the blend of polymer 1 and polymer 2, respectively. ∮ and ∮ cific heat of polymer 1, respectively [4]. lattice coordination number. spe is a proportionality constant the volume fractions of components 1 and 2, respectively. z is the A schematic phase diagram is shown in (Figure 1). There are Ὑ three regions of different degree of miscibility: representing the specific interaction such as hydrogen bonding,
Figure 1: Phase Diagram for Liquid Mixtures with The Upper and The Lower Critical Solution Temperature, UCST and LCST, Respectively.
How to cite this article: Khalid Farhod Chasib, Basma Mohammed Kadhim. Prediction of The Behavior for Polymer Blends Using Thermodynamic Model. Recent 00143 Adv Petrochem Sci. 2018; 6(5): 555699. DOI: 10.19080 RAPSCI.2018.06.555699 Recent Advances in Petrochemical Science
∂∆2 G binodals, m = 0 a) The single-phase miscible region between the two Spinodal: ∂φ 2 pT, (11) als and spinodals, and ∂∆3 G b) The four fragmented metastable regions between binod- m = 0 Critical point: ∂φ 3 pT, dered by the spinodals. (12) c) The two-phase separated regions of immiscibility, bor- The diagram also shows two critical solution temperatures, The experimental phase diagrams are often not symmetrical, unless the molecular weights of the components are similar, and in the case of large differences in molecular weights, they can be the lower, LCST (at higher temperature), and the upper, UCST (at highly non-symmetric. With phase separation, the binodal defines lower temperature). The phase diagram with two critical points is between the composition of the component 1 rich phase and component2 2 a rule for mixtures of low molar mass components, whereas the the binodal points can be employed to determine the relative rich phase (Figure 2). The tie line noting temperature T polymer blends usually show either LCST (most) or UCST [5]. , and component The binodals (Figure 1). separate miscible (one-phase) and amounts of each phase. The tie line is illustrated1r in (Figure 3). The metastable region, the spinodals separate metastable and two- volume fraction2r of component 1 rich phase, ∮ phase region. The thermodynamic conditions for phase separa- 2 rich phase, ∮ , can be determined from the expression, with ∮ ∂∆ tions are given by: Gm representing the overall φcompositionφφ− of the component noted in = 0 1r b ∂φ (Figure 3). = Binodal: pT, (10) φ2r φφ− a (13)
Figure 2: Free Energy of Mixing Versus Volume Fraction Generalized Behavior for Various Positions on The Phase Diagram.
Figure 3: Tie-line Calculation of Phase Compositions.
How to cite this article: Khalid Farhod Chasib, Basma Mohammed Kadhim. Prediction of The Behavior for Polymer Blends Using Thermodynamic Model. Recent 00144 Adv Petrochem Sci. 2018; 6(5): 555699. DOI: 10.19080 RAPSCI.2018.06.555699 Recent Advances in Petrochemical Science
∆=Hm RT χφ12 φ Highly miscible polymers exhibit single phase behavior over the entire temperature-volume fraction space available for ex- (15) determined. At low temperatures, the ucst cannot be determined perimental verification. If ucst or lcst behavior exists, it cannot be For binary systems the Flory-Huggins equation can be ex-
pressed in the following form:φφ due to the glassy state restricting molecular motion (phase sepa- 12 ∆=−Gm RT lnφ1 + ln φ2 + χφ 12 φ ration); and at higher temperatures, polymer degradation occurs rr12 before phase separation can be observed. With highly immisci- phase region with the binodal curves virtually overlapping the y where χ (16) ble polymer blends, the phase diagram is virtually all in the two- parameter. R is the universal gas constant, and T is the absolute is the so-called Flory-Huggins binary interaction axis at 0 and 1.0 volume fraction. temperature. The first two terms of the right-hand side in Equa- The phase separation takes place when a single-phase system tion 16 are related to the entropy of mixing and the third term is suffers a change of either composition, temperature or pressure originally assigned to the enthalpy of mixing. i that forces it to enter either the metastable or the spinodal re- metastable region, the phase separation occurs by the mechanism entropic contribution is very small, and the miscibility or immis gion. When the system enters from single-phase region into the For polymers having infinite molar mass (i.e. r is infinite) the - cibility of the system mainly depends on the value of the enthalpy resembling crystallization – slow nucleation followed by growth χ is negative. of the phase separated domains. By contrast, when the system of mixing (Equation 15). Miscibility can only be achieved when immiscibility the phases separate spontaneously by a mechanism is forced to jump from a single-phase into the spinodal region of χ but it is The term ‘parameter’ is widely used to describe depends on such quantities as temperature, concentration, pres called spinodal decomposition [6]. definitively better characterized by the term ‘function’, because χ sure, molar mass, molar mass distribution and even on model pa Starting point for most of the theoretical interpretations of - polymer solutions and blends is the Flory-Huggins lattice theo- - on polymer solutions. Thus the model restrictions are no change length. ry. It is basically an extension of the concept of regular solutions rameters as the coordination number of the lattice and segment For polymers, the miscibility can only be achieved when χ < . The parameter at the critical point can be obtained of volume during mixing (incompressible model), the entropy of χcr χ χcr mixing is entirely given by the number of rearrangements during mixing (combinatorial entropy) and the enthalpy of mixing is 2 from the definition of the critical11 point 1 (Figure 1) and Equation caused by interactions of different segments after the dissolution χcr = + 16 as follows: 2 rr of interactions of the same type of segments. It is a mean-field 12 where r model, i.e. only average interactions are taken into consideration. i (17) The main problem was to find an expression for the entropy of is the number of polymer segments (which is propor- mixing because it was found experimentally that polymer solu- solutions. Assuming a rigid cubic lattice model, this problem was tional to the degree of polymerization). tions show significant deviations from values expected for ideal based on the assumption that χ It should be mentioned that the Equations 16 and 17 are χcr independently solved for polymer solutions by Huggins & Flory is not a function of composition, [3]. Statement is only a of function The ofProblem the molar masses [7].
The lattice theory for the enthalpy of mixing in polymer solu- tions, developed by Flory and Huggins, can be formally applied The factors affecting the miscibility of polymer blends will be to polymer mixtures, which provides a rough estimation of the examined experimentally and predicted thermodynamically. The mers and m miscibility of the polymers. Assuming random mixing of two poly- miscibility and dynamics of phase separation will be investigat- m determine both the binodal and the spinodal curves. The relation ΔV = 0 yields the well-known expression for the combi- ed experimentally for different polymer blends concentrations to ship between the binodal curve and the phase transition, such as natorial entropy of mixing ΔSφφ of the Flory-Huggins theory: - ∆=−SR12lnφφ + ln melting and glass transitions, will be studied to discuss the com m 12 rr12 (14) - is i patibility of blend system including solid component. The glass predicted thermodynamically to establish polymer miscibility. Where i is the volume fraction of the component i and r transition temperature will be experimentally determined and the number of polymer segments, R is the gas constant. It can be Purpose of The Study seen thati the entropy of mixing decreases with increasing molar mass (r is proportional to the degree of polymerization) and van- perature Tg analysis by DSC will be evaluated. Tg will be cor ishes for infinite molar masses. Applying the concept of regular The miscibility of the blends through glass transition tem- solutions and assuming all pair interactions in the frameworkm of a - mean-field theory yields for the enthalpy of mixing ΔH : related with a measure of the intermolecular interactions, such as How to cite this article: Khalid Farhod Chasib, Basma Mohammed Kadhim. Prediction of The Behavior for Polymer Blends Using Thermodynamic Model. Recent 00145 Adv Petrochem Sci. 2018; 6(5): 555699. DOI: 10.19080 RAPSCI.2018.06.555699 Recent Advances in Petrochemical Science
χ Method and Procedures the Flory-Huggins interaction parameter, . The effect of blend ratios on the mechanical properties and the probability [8]. to The binary blends will be made by mixing solutions (approx- creating compatible system for the polymer blend will be studied. imately 3% w/w) of each polymer in 98% formic acid. The solu- DSC and FTIR measurements will be prepared by casting the poly Methods of polymer blends preparation, and the best methods tions will be stirred for 2h at ambient temperature. The films for for detecting miscibility will be studied. The thermodynamic re- - oC and lationships will be applied to determine the free energy of mixing, mer solutions into shallow soda-glasso dishes and allowing the sol- heat of mixing, the binodal and spinodal curves, the critical points vent to evaporate slowly. The thin films will be dried at 60 weight. Blend compositions will be 80/20, 60/40, 50/50, 40/60 and thus the phase behavior [9]. Phase behavior and phase sep- placed under vacuum at 70-80 C for at least 3 days to constant and 20/80 by weight. aration kinetics of polymer solutions will be investigated exper- imentally. The miscibility and dynamics of phase separation will to determine both the binodal and the spinodal Sampling be investigated in solutions of different polymer concentrations Differential scanning calorimetry (DSC) Review of The Literature
DSC measurements will be performed on a DuPont 910 DSC The kinetics of phase separation in “polymer + solvent” sys- solutions can be induced by changes in the temperature, the sol Differential Scanning Calorimeter equipped with a Thermal Anal- tems is of continuing interest. The phase separation in polymer o ysis Data System (TA-2000). The samples will be first heated - and then the samples will be quenched cooled to 0oC to prevent from room temperature to 250 C and maintained for 2 minutes, vent (concentration or composition) or the pressure. Binder et al [8,9] studied the kinetics of spinodal decomposition of polysty- rate was 10o the unstable region. Phase separation process was monitored by crystallization before thermograms will be taken. The scanning rene solutions in cyclohexane induced by a temperature jump into C /min. In the isothermal crystallization experiments at room temperature, the samples will be rapidly heated to melt blends samples of 9-11 mg will be used KF Chasib [21]. Starting time- and angle-resolved light scattering at ambient pressures ing temperature to remove any previous crystallinity. The samples - Berghmans et al, [10] recently carried out a numerical study of temperature-induced phase separation kinetics of polymer solu- 50, 100 and 150o o sults showed that anisotropic structures and morphologies can be will be held for 6h at a certain crystallization temperature (TC = tions subjected to a linear spatial temperature gradient. Their re- 10oC /min under dry nitrogen atmosphere. C), and then will be heated to 250 C at a rate of Fourier transform infrared spectroscopy (FTIR) induced by a gradient temperature jump. In addition to tempera- ture quench, phase separation can also be induced by exposing the solution to a nonsolvent vapor as antisolvent. Binder K [11] The FTIR spectra will be collected on dry thin film polymer reported the kinetics of phase separation in a polymer solution blend samples using a UNICAM (Mattson 5000) spectrophotom- (poly sulfone in N-methyl-2-pyrrolidinone) film induced by a non- eter by sandwiching the film samples between two KBr disks. All solvent vapor, water. The data were analyzed based on Cahn-Hil- of the films will be sufficiently thin to be within a range where the liard linear theory in the initial stages of phase separation. and 150o Beer-Lambert law is obeyed. Films will be annealed at 50, 100, 1. Much attention has been paid to the phase behavior of poly- C for 6h, then 32 scans will be made for each TC at a res- mers in compressed fluids at high pressures Guenet JM [12-14]. Instrumentationolution of 8 cm However, these have mostly focused on the liquid-liquid (L-L) The most common method to establish polymer miscibility phase boundary, with limited data on the solid-fluid (S-F) bound- ary. For crystallizable polymer-solvents systems, it is possible T to observe the S-F boundary as well as L-L phase boundary in a is Differential Scanning Calorimetry (DSC), withg which determi- Questionphase diagram and/ Farhod or Hypotheses [14-17]. nation of the glass transition temperature ( ) IR spectroscopy has proved to be an excellent tool to study the hydrogen-bonding behavior in polymer blends. If the blend is immiscible, the absorp- It is reasonable to believe that the changes of thermal enthalpy tion spectrum of the blend will be the sum of those for the compo- are caused by the occurrence of phase separation during anneal- nents. If the blend is miscible because of the specific interactions, ing. Therefore, the phenomenon is indicative of the occurrence of then differences will be noted in the spectrum of the blend relative phase separation Khalid FC [18-20]. The changes of thermal prop- to the sum of those for the components. The FTIR investigation of erties of blends composed of polymer can provide information a miscible blend will not only reveal the presence of such an inter- about the occurrence of phase separation, and thermal analysis Dataaction, Collection but will provide and information Analysis on which groups are involved can be used to determine the phase boundary of such blends. The teraction, or ionic interaction between two polymers reduce the specific interactions such as hydrogen bonding, dipole-dipole in- overall entropy Several approaches based on kinetic or thermodynamic fea- tures of the glass transition phenomenon will be proposed to
How to cite this article: Khalid Farhod Chasib, Basma Mohammed Kadhim. Prediction of The Behavior for Polymer Blends Using Thermodynamic Model. Recent 00146 Adv Petrochem Sci. 2018; 6(5): 555699. DOI: 10.19080 RAPSCI.2018.06.555699 Recent Advances in Petrochemical Science
produce novel materials with combined characteristics in T provide a theoretic foundation for the equations currentlyg used to predict the compositional dependence of the of blends of having both improved application properties and low-cost miscible polymers Information on the experimental details and advantages in material performance. any special procedures used for preparation of the mixtures (tem- b) Polymer blend represents very important field in perature of mixing, type of solvent, drying processes, etc) can be processing of new materials, which has better properties in found in the original references [1-7]. The experimental data ana- comparison with the net polymers. They are significant also Limitationlyzed will be obtained and Delimitation using conventional DSC and FTIR. from ecological and economical viewpoint. phase transitions, such as melting and glass transitions, c) The relationship between the binodal curve and the in low molecular weight materials is the combinatorial a) The most important factor leading to miscibility entropy contribution which is very large compared to high blend system including solid component. become important to discuss the compatibility of binary molecular weight polymers. This contribution is the reason
d) Considerable interest in the study of polymer blends that solvent-solvent mixtures offer a much broader range of aspects. Particularly, much attention has been paid to because of their importance in academic and technical miscibility than polymer-solvent combinations. The range of miscibility and phase behavior in polymer blends. is even much smaller. miscible combinations involving polymer-polymer mixtures
Tg predicting lcst behavior unless a temperature dependent 12 b) The Flory-Huggins approach is not directly capable of e) Glass transition temperature values are useful indeedT for a variety of purposes. Particularly needed are increasing temperature is employed. g value exhibiting increasing values (negative to positive) with blends; they tell us whether the blends are miscible, values as a function of composition for binary polymer
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g) Many polymer pairs are not only immiscible but also Binder K, Fratzl P (2001) Phase transformations in materials. interaction between the blend constituents, which is a 12. Weinheim Wiley-VCH. incompatible, Compatibility arises from thermodynamic Guenet J M (2007) Polymer-solvent molecular compounds. Amsterdam Elsevier. Significancefunction of theirof the physical Study and chemical structure 13. Henderson I C, Clarke N (2004) Two-Step Phase Separation in Polymer 14. Blends. Macromolecules 37(5): 1952. synthetic polymers has proven to be a suitable tool to a) Blending of friendly environmental polymers with Kirby C F, Mchugh M A (1999) Phase behavior of polymers in supercritical fluid solvents. Chem Rev 99: 565.
How to cite this article: Khalid Farhod Chasib, Basma Mohammed Kadhim. Prediction of The Behavior for Polymer Blends Using Thermodynamic Model. Recent 00147 Adv Petrochem Sci. 2018; 6(5): 555699. DOI: 10.19080 RAPSCI.2018.06.555699 Recent Advances in Petrochemical Science
15. 19.
Farhod Chasib K (2013) Extraction of phenolic pollutants (phenol and Khalid F C (2018) Study the Vapor-Liquid Equilibrium and Excess p-chlorophenol) from industrial wastewater. Journal of Chemical & Volume for the Binary Mixtures of Aqueous Solutions of Two Industrial 16. Engineering Data 58(6): 1549-1564. Petroleum Solvents and Aromatic Hydrocarbon. Recent Adv Petrochem 20. Sci 5(4). Al Jiboury, K F C (2013) Adsorption of phenol from industrial Simulating the Distillation Curves and ASTM Distillation Temperature, wastewater using commercial powdered activated carbon. Journal of Khalid F C, Srikanth K P (2017) An Investigation on the Feasibility of Selcuk University Natural and Applied Science 114-123. 21. International Journal of Oil, Gas and Coal Engineering 5(5): 80-89. 17. Chasib K F (2017) Extraction of Kerogen from Oil Shale using Mixed Reversible Ionic Liquids. The Eighth Jordan International Chemical K F Chasib (2013) Study on the effect of adding co-solvent 18. Engineering Conference, p. 1,2. 1911.(n-alkoxyethanol) to sulfolane on the toluene extraction, Scientia Iranica. Transaction C, Chemistry and Chemical Engineering 20: 1899- Khalid F C (2018) Experimental Measurement and Thermodynamic Modelling of Vapor-Liquid Equilibria Correlations for Prediction Azeotropic Behavior and Fitting Multicomponent Mixtures Data. Progress Petrochem Sci 1(2).
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How to cite this article: Khalid Farhod Chasib, Basma Mohammed Kadhim. Prediction of The Behavior for Polymer Blends Using Thermodynamic Model. Recent 00148 Adv Petrochem Sci. 2018; 6(5): 555699. DOI: 10.19080 RAPSCI.2018.06.555699