A general procedure to systematize the search of several alternatives enabling the separation of non-ideal binary mixtures such as pressure-swing distillation, azeotropic and extractive distillation is presented. The use of heterogeneous entrainers is specially highlighted

Baudouin, Olivier

Gerbaud, Vincent

Joulia, Xavier

Rodríguez-Donis, Ivonne

English

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10.90.80.70.60.50.40.30.20.10 10.90.80.70.60.50.40.30.20.101 0.9 0.8 0.7 0.6 0.5 0.4 0.3 0.2 0.1 0Acrylonitrile [S] Water [SN]Acetonitrile [SN]LLVEHeteroazeotrope [UN]E + BVapour lineA + BxDxOYTopexE10.90.80.70.60.50.40.30.20.10 10.90.80.70.60.50.40.30.20.101 0.9 0.8 0.7 0.6 0.5 0.4 0.3 0.2 0.1 0Entrainer TB (°C)  Process Rejection Acetic acid  118 1.87 BED 1, 3 Allyl alcohol 97 1.23 BED 1, 2, 3 Aliphatic Alcohols 96 - 118 1.50 BED 3 Water 100 398 HBED - n-Butyl acetate 126 .5 0.11 BED 3 Furfural 161. 4 0.42 BED 1, 2, 3 Pyridine 115.2 0.52 BED 1, 2, 3 Nitrobenzene 210.6 0.05 BED 1, 2, 3 4-methyl-2-pentanone 116.7 0.18 BED 2, 3 Methyl cyclohexane  101 0.02 HBED 2, 3  Chloroform (A) 61.1°C + Methanol (B) 64.5°C + Water (E) 100°CREGSOLexpert : Entrainer Selection Tool for Waste Solvent Recovery by Batch Distillation ProcessesRODRIGUEZ DONIS Ivonne, GERBAUD Vincent, BAUDOUIN Olivier, JOULIA Xavierivonne.rdguez@infomed.sld.cu; Vincent.Gerbaud@ensiacet.frObjective: General procedure to systematize the search of several alternatives enabling the separation of non-ideal binary mixtures such as pressure-swing distillation, azeotropic and extractive distillation. j tiv : eneral procedure to syste atize the search of several alternatives enabling the separation of non-ideal binary ixtures such as pressure-s ing distillation, azeotropic and extractive distillation.REGSOLexpert A wizard computer tool including 224 feasibility rules, and 326 batch azeotropic and extractive distillation processes. Systematic checking for each entrainer candidate for determining its feasibility to be used in rectifying or stripping batch column.  A list of potential homogeneous and heterogeneous entrainers E in an optimal time for separating A and B as any industrial mixture.Strategy for solvent recovery by distillation3 – Column configurationREGSOLexpert software algorithm Extractive Distillation (HEBD)tr ti  i till ti  ( )excellent agreement20 mol/hr150 WN= 45yTOPFE DExtractive SectionA + B20 moles25°C(1 toxic, 2 pollution, 3 cost)A B1 - Selecting Entrainer with RegSolExpert®-0.99140.9690WaterChloroformMethanolpurity recovery98.0%89.6%-0.99880.99060.995791.6%95.1%-A B = 0.1910.90.80.70.60.50.40.30.20.10 10.90.80.70.60.50.40.30.20.101 0.9 0.8 0.7 0.6 0.5 0.4 0.3 0.2 0.1 0xDDecanter Tie LineAB=1xPTop Destination Region:XTOPMethanol (B) 64.5°C [S]Water (E)100.0°C [SN] azeoAE56.3°C [S]azeoAB 53.3°C [S]Chloroform (A) 61.1°C [ SN ] azeoABE53.1 °C [UN]LLVELLE  (25°C)VapourLine2 - Residue Curve MapUSE:  Extraction of bioactive substances from biological sourcesTMIN Azeotrope: T = 53.5 °C, XA= 0.654 – Simulation vs Experiments: heat up 12 min: R  FE = 0 120 min: R  FE = 20 100 min: R = 1.4 (-D)  FE = 20      60 minR = 10 (-D)  FE = 20 20 min: E-B separation FE = 0  R = 1.5   250 min10.90.80.70.60.50.40.30.20.10 10.90.80.70.60.50.40.30.20.101 0.9 0.8 0.7 0.6 0.5 0.4 0.3 0.2 0.1 0Methanol (B) [S]azeoAE[S]azeoAB [S]xS2Water (E) [SN] Chloroform (A)[SN]R = 1.4xS2expx’S3Expxx’s2xs3xs4x’s3XD=XIIR xS2ExpazeoABE [UN]YTOPColumn x profilextopInitial chargexS1R = 10S4ExpIndustrial ApplicationsBrabant Industry case: Cyclopentanone (130.6°C) – Propylene Glycol Monomethyl ether (146°C) Heterogeneous Azeotropic  Distillation (HABD)t r  z tr i   i till ti  ( )Acetonitrile (A) 81°C + Water (B) 100°C + Heterogeneous (E)USE:  Liquid chromatography separation in pharmaceutical IndustryTMIN Azeotrope: T = 77 °C, XA= 0.671 - Selecting Heterogeneous Entrainer with RegSolExpert®Initial List: 55 candidates from several chemical families (DIPPR database)Heterogeneous E: Acrylonitrile and Chloroform form unstable heteroazeotrope with H202 - Residue Curve Map     and 3 – Column configuration Chloroform [S]Acetonitrile [SN]Heteroazeotrope [UN]Water [SN]A + BE + BLLVEVapour linexExD YTopexO D, xDT = 25°CV = 70 mL12.2 mol, xON. = 50150 W4 – Simulation vs Experiments0.920.930.940.950.960.970.980.9911.010 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1Total Pressure (atm)xA020406080100120140T (°C)2– (xA(azeot), Tazeot) vs PA + BxA=0.996T=93.1°CX (mass)A 130.5 0.6B 146 0.3287isopropanol 82.3 0.0353Water 100 0.02volatil impurityn-methyl pyrrolidone 204.3 0.016 heavyimpurityTB (°C)ComponentsA [sn]B [sn]isopropanol [s]Water [sn]Homogeneous [UN][S]Heterogeneous [S]Heterogeneous[S]volatil impurityA, xAD10 mol, xA mass=0.6N. = 501500 WP= 0.3 atm00.10.20.30.40.50.60.70.80.910.00 0.20 0.40 0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.000.980.9810.9820.9830.9840.9850.9860.9870.9880.9890.990.9910.9920.9930.9940.9950.9960.9970.9980.9993- Column Configuration4- Simulation ProSim Batch1- Mixture analysisXAD distillateXAS stillXAD(average) =0.9951Recovery yield (A)= 92.5%XAS Time (h)xA molarChloroform Acrylonitrile (* experimental values)Aqueous PhasexWater=0.9996Recovery=97.8%xWater=0.947Recovery=92.6%*xWater =0.946*Recovery =89 %Entrainer Phase xE=0.9990Recovery=81%xE=0.712Recovery=72%*xE=0.6916*Recovery =69%Final Stillxacetonitrile= 0.9945Recovery= 99.2 %xacetonitrile= 0.992Recovery= 95.6%*xacetonitrile = 0.995*Recovery= 91.8%BAb acdef fedAB<1.5cf ePressure Swing Distillationr r  i  i till tiMixture AB:  Determination AB azeotrope or AB ideal aheterogeneousbhomogeneous AB<1.5Pressure swing distillation cxazeot  constant, Tboiling<30°C1- Chose entrainer candidates Ei for d e fComputation azeotropes: AEi, BEi, ABEi2- Residue curve map of ABEiTopological stability: A, B, Ei, AB, AEi, BEi, ABEi3- Feasibility rule chekingNot matchmatch4 - Batch distillation sequences 5- Simulation + Economic evaluationCONCLUSIONSHeterogeneous entrainers have a more privileged position than homogeneous. Higher number of ternary diagram match with feasible rulesPressure swing distillation is a privileged option. It doesn’t involve additional entrainer. Simple performance in one or two batch distillation column operating at different pressures.Heterogeneous entrainers in HABD: little amount of entrainer, separatrix can be crossed by the still path, simplest batch distillation sequence, more flexible reflux policy (entrainer-rich phase or both decanted phases)Heterogeneous entrainers in HEBD: Complex ternary residue curves are feasibles, withdrawal of saddle binary heterazeotrope at the column top by feeding E at the top of the column , more flexible reflux policy as HABDWater seems a promising candidate for treatment organic wastes by HEBD and HABD. cheap, non toxic, non pollutant

REGSOLexpert: Entrainer Selection Tool for waste solvent recovery by batch distillation processes

http://oatao.univ-toulouse.fr/2943/1/Gerbaud_Poster_2943.pdf

REGSOLexpert: Entrainer Selection Tool for waste solvent recovery by batch distillation processes

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