Experiment 4

Pulsed Column Liquid Liquid Extraction Unit.

1. Objective: The students should be able to: o Operate a Liquid Liquid Extraction Experiment using a Pulsed Column Liquid Liquid Extraction Unit. o To determine the tie lines connecting the bimodal curves in the toluene !ater acetone s"stem. o To determine the height equivalent theoretical plates #$ETP% &or column b" using equilateral triangular diagram. o To investigate the e&&ect o& the pulsation stro'e on the $ETP. 2. Introduction. Extraction is a unit operation used to separate components based on their Chemical (i&&erences instead o& di&&erences in Ph"sical Properties. )hen separation o& components o& a Liquid *ixture becomes ine&&ective or ver" di&&icult b" means o& (istillation+ and then Liquid Extraction is one o& the main alternatives to consider. , !idel" used terminolog" describes the s"stem in terms o& : o F : Feed. o S : Solvent. o R : Raffinate. o E : Extract. The &ollo!ing diagram indicates the Flow of Streams nd !om"onents In Liquid # Liquid Extraction S$stem.

Each stream consists o& t!o components. The Feed Stream consists o& the required component # Solute % and Solvent # Diluent or Feed Solvent or Raffinate Solvent %. The Raffinate Stream

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has the same components as the Feed+ though the proportions are di&&erent. On the other hand+ the Extract Stream consists o& the required component # Solute or Exracted Component % and Solvent # Extracting Solvent or Extractant %. The di&&erence bet!een the Extracted !om"onent # Solute % and the Extractin% Solvent or Extractant should be made clear at all times. .ince the Feed is a t!o component s"stem+ b" convention+ the material to be Extracted is commonl" re&erred to as the Solute !hile the other component is generall" re&erred to as the &iluent. The Raffinate has the same components as the Feed+ though hope&ull" it is much less concentrated in Solute i.e.+ it is said to be leaner. ,n ideal unit !ith per&ect Extraction gives a Raffinate !hich has one component onl"+ that being 'ure &iluent.

The liquid used to strip the Solute &rom the Feed is re&erred to as the Solvent. $o!ever+ Solvent is a general term and can sometimes be con&using as &or example b" describing the &iluent as the Feed Solvent. The term Feed Solvent should then be avoided. The Solvent a&ter becoming enriched in solute leaves the s"stem as the Extract. The 'ulsed !olumn Liquid # Liquid Extraction (nit #*odel: P!"% has been designed to demonstrate the )asic 'rinci"les of a Liquid # Liquid Extraction 'rocess. The /ormal *ode o& Operation is that the Light Phase and $eav" Phase Liquids are pumped Counter Currentl" into the Pac'ed Extraction Column. The $eav" Phase !ill enter the top o& the column and &lo! do!n!ards+ !hile the Light Phase !ill enter the bottom o& the column and &lo! up!ards due to (ensit" (i&&erences. Counter Current 0lo! among the pac'ings in the column and pulsation o& the t!o phases !ill cause the trans&er o& .olute Component &rom one phase # Raffinate % to the other # Extract %. The 1a&&inate !ill emerge at the bottom !hile the Extract !ill emerge at the top o& the Extraction Column. This Liquid # Liquid Extraction 'rocess is carried out among the Column Pac'ings to give a higher degree o& separation. .ample Points are provided at 'e" positions around the unit to allo! collection o& both Light and $eav" Phase Liquids. 2n this !a"+ e&&ects o& pulsation stro'e and &eed &lo! rates o& both phases on the extraction e&&icienc" can be evaluated b" means o& .ample ,nal"sis. Components o& Pulsed Column Liquid Liquid Extraction Unit are as &ollo!s : o Feed Vessels #3- * )2% 4raduated C"lindrical 5essels !ith 67 L capacit". o Column #8-% a (/ 9: Pac'ed Column !ith -: mm Ceramic .addles. E&&ective $eight o& column is 6.7 m. o Dosing Pumps #P- * '2% :.67 ') Piston Pumps !ith up to ;6 L<h capacit". o Pulsator #P=% :.67 ') Pulsator Pump !ith a 6: mm stro'e and 7: $> &requenc". o Receiving Vessels #3= * )+% 4raduated C"lindrical 5essles !ith 67 L capacit". o Pulsation Dampers #37 * ),%.

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EXP 4/Jan 14

-. !.emicals and ncillar$ Equi"ments Required: a.% Chemicals 1equired. o ,cetone #.olute%. o (iioni>ed )ater# (iluent% o Toluene #.olvent%. b.% ,ncillar" Equipments 1equired: T!o 6:::ml ?ug and t!o 67ml bea'ers. .eparating &unnels#0or settling and separating the mixtures% Conical &las's *easuring C"linder and standard laborator" apparatus 1e&ractometer . +. O"eratin% Instructions. +.1 /eneral Start0u" 'rocedures. -. Prepare the &ollo!ing chemicals : a% 0eed #$eav" '.ase%: *ixture o& #cetone $ %ater &olution. Prepare 6: litres o& 7:!t @ mixture o& #cetone in )ater b" mixing appropriate quantities o& the #cetone in (istilled )ater. b% Prepare 6: litres o& Solvent #Light '.ase%: Pure 'oluene. 6. Ensure that all valves are closed. =. 0ill 0eed 5essel 3- !ith the #cetone $ %ater &olution and 0eed 5essel 36 !ith the Pure 'oluene Solvent( (etermine the composition o& the &eed #heav" phase% using re&ractometer. ;. Turn on the po!er suppl" 7. Turn on the main po!er control s!itch. A. Open valves 5= and 5;. .!itch on 0eed Pump P-. B. ,llo! the #cetone $ %ater Solution #$eav" Phase% to enter the column and &ill to a level o& about -: cm above the solvent inlet. .!itch o&& Pump P-. 9. Open valve 5;. .!itch on .olvent Pump P6. C. ,s the .olvent #Light Phase% enters the column+ care&ull" !atch the 2nter&ace Level !hich &orms bet!een the Light and $eav" Phases. *aintain the inter&ace level at 6 = cm above the solvent inlet.

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-:. Once the liquid starts to over&lo! at the top o& the column+ stop Pump P6. --. The unit is no! read" &or experiment. +.2 /eneral S.ut # &own 'rocedures. -. .!itch o&& pumps P-+ P6 and P=. 6. Close valves 5= and 5;. =. Open valves 57+ 5A and 5C to drain all liquid &rom the experiment. ;. Open valves 5-= and 5-; to drain all liquid &rom the 1eceiving 5essels 3= and 3;. 7. Turn o&& the po!er &or the control panel. ' R1 2 +.- &etermination of Equilibrium Solute &istribution 31ie lines4 'RO!E&(RES2 -. Prepare A heterogeneous mixtures o& !ater+ acetone and toluene in A di&&erent conical &las's according to the compositions recommended in the table in appendix 0. 6. ,gitate the mixtures prepared in step - &or about ;: minutes. 5ote2 To prevent emulsi&ication+ do not agitate the mixture too vigorousl". =. .top the agitator. Pour each o& the mixtures into a separating &unnel. Let the mixture settle into t!o distinct clear la"ers !ith a sharp inter&ace. ;. )ithdra! a sample o& each phase and measure the re&ractive index o& each phase. ,gain+ ta'e an average o& three readings &or each phase. The !ater rich phase #ra&&inate% !ould be the heav" phase and toluene rich phase !ould be the light phase #extract%. 7. 1epeat the experiment #step 6 to =% &or all mixtures. A. Using calibration curve prepared in ,ppendix 3- and 36+ determine the composition o& acetone in each phase. B. 1ecord the results in the table in ,ppendix 0.

' R1 )2 +.+ Ex"eriment2 Extraction of cetone from 6ater (sin% 1oluene. 2n this experiment+ there are t!o &eeds to the *ixer and t!o outlet &lo!s &rom the .ettler. 0eed 0lo!s: .olvent: Toluene #Light Phase%. 0eed: ,cetone )ater *ixture #$eav" Phase%. Outlet 0lo!s: Extract : Toluene 1ich Phase. 1a&&inate: )ater 1ich Phase.

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'RO!E&(RES2 -. Per&orm the general start up procedures #.ection ;.-% 6. Turn on the both pumps P- and P6 and set the desired 0eed and .olvent &lo! rates b" adDusting the pumpsE &requencies and displacements. =. 8eep the pulsator pump P= turned o&&. ;. ,llo! both liquids to &lo! into the collection vessels 3= and 3; respectivel". The bottom product contains the )ater 1ich Phase #1a&&inate % !hile the top product contains the Toluene 1ich Phase # Extract %. 7. *onitor the 2nter&ace Level. *aintain it at about 6 = cm above the .olvent inlet b" adDusting the height o& the Over&lo! Tube. A. Turn on the Pulsator Pump P= and set the Pulsation .tro'e Length. B. Let the experiment run &or a !hile to attain stead" state. 9. Open valve 5-: to !ithdra! a -: ml sample o& 1a&&inate and open valve 5-6 to collect a -: ml sample o& Extract . 5ote2 Ta'e samples at suitable time intervals and measure their 1e&ractive 2ndices. )hen the readings are consistent over time+ stead" state has been reached. C. 1ecord the 1e&ractive 2ndex o& both samples and use the given Calibration Curves #,ppendix 3% to determine the ,cetone #.olute% composition in each phase. -:. 1ecord all data in the given .ample Table in appendix ,. --. 1epeat the experiment #steps = to -:% b" turning on the pulsator pump P= and changing the pulsation stro'e length. 0ix the same &lo! rate and &eed composition throughout the !hole experiment. 5 L7SIS 8 &IS!(SSIO52 Discuss all your results. The uestions !elo" only serve as a guideline. #our discussion &)ould not only limit to these uestions. 'art 2 $se the samples ta!les in %ppendix % for data collection. 'art )2 $se the samples ta!les in %ppendix & for data collection. -% (etermine !eight percent acetone o& the ra&&inate and extract b" re&er to calibration curve given in appendix C- and C6.

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6% (etermine the required theoretical extraction stage &rom the pulsed column liquid liquid extraction experiment results. 1e&er to calculation guide. =% Calculate the height equivalent theoretical plates #$ETP% o& the extraction column &or di&&erent pulsation stro'e. 9E1' : Effective column .ei%.t * 5o of t.eoretical "lates
;% 0rom the available data+ do a mass balance calculation around the extraction column and obtain the extract and ra&&inate &lo! rates.

""endix ! &or a step b" step

7% (iscuss the various &actors that !ould help to increase the rate o& trans&er o& solute to solvent phase.
A% Explain ho! pulsation &requenc" increases the trans&er rate in pulsed columns. ;.< REFERE5!ES -. *cCabe and .mith+ #6::7%+ $nit 'perations of Chemical Engineering+ Bth Edition+ *c4ra! $ill. 6. 1obert E.Tre"bal.+ #-C9-%+ (ass Transfer 'perations+ =rd Edition+ *c4ra! $ill.

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''E5&I= ' R1 2 +.+ &etermination of Equilibrium Solute &istribution 31ie lines4

mount in mixture 3mL4 5o cetone 6 = ; 7 A 6: ;: A: 9: -:: -6: 6ater C: 9: B: A: 7: ;: 1oluene C: 9: B: A: 7: ;:

6ater ric. ".ase Refractive Index cetone !om"osition 3wt>4

1oluene Ric. '.ase Refractive Index cetone !om"osition 3wt>4

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''E5&I= ) ' R1 )2 +.+ Ex"eriment2 Extraction of cetone from 6ater (sin% 1oluene. Results2 0eed 12 0eed Composition

0eed &lo!rat e #L<hr %

.olvent &lo!rat e #L<hr

.olvent to 0eed ratio

Pulsatio n stro'e #mm%

1a&&inate Extract #!ater rich phase % #,cetone rich phase% Time 1e&ractive .olute 1e&ractive .olute #min% 2ndex #,cetone% 2ndex #,cetone% Composition Composition #!t @% #!t @%

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''E5&I= !1

-:

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''E5&I= !2

--

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-6

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""endix & S1E' )7 S1E' ! L!(L 1IO5 /(I&E -. Obtain the equilibrium data &rom ,ppendix E or &rom literature. Plot the binodal<solubilit" curve on a triangular plot #,ppendix 0%. 6. Plot the corresponding tie lines on a triangular plot #,ppendix ,%. =. Locate the points &or: 0eed+0 .olvent +. 1a&&inate+1 Extract +E 0eed and solvent mixture+*

-=

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""endix & ;. Locate the point F1+!here all operating lines should meet.

7. (ra! a tie line &rom point E to its equilibrium point on the bimodal plot. Connect an operating line &rom that equilibrium end o& the tie line to point F1. Extend that operating line so that it intersects !ith the bimodal plot at the other end. (ra! another tie line &rom that ne! intersection and continue until a tie line has passed the operating line connecting 1 and ..

A. Count the number o& tie lines contained inside the E 0 1 . quadrilateral#it ma" not be a rounded number%.That !ill be the number o& required theoretical stage to achieve &inal ra&&inate and extract compositions.

-;

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""endix E Equilibrium data )inodal* Solubilit$ &ata for cetone01oluene06ater S$stem

cetone 3wt >4 C.BC -C.;9 ;-.A76.=: A:.AB A=.79

1oluene Ric. ".ase 1oluene3wt 6ater3wt>4 >4 6.;6 9B.B9 6.C6 BB.A: =.CB 7.6B B.6: 66.7; 7;.;6 ;6.;= =6.-; -=.9C

6ater Ric. ".ase cetone 3wt >4 A=.C= A=.-; 79.9; 7-.66 =C.A7 -C.C; 6ater3wt>4 6-.A9 6;.99 =;.6B ;7.A9 79.CB B9.9A 1oluene3wt>4 -;.=C --.C9 A.7C =.-: -.=9 -.6:

-7

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''E5&I= F

-A

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