Experiment 4 PULSED COLUMN LIQUID-LIQUID EXTRACTION UNIT
1.0
OBJECTIVE •
Operate a Liquid – Liquid Extractio Experi!et u"i# a Pu$"ed Co$u! Liquid – Liquid Extractio Uit%
•
To deter!i deter!ie e t&e t&e &ei#&t &ei#&t equi'a equi'a$e $ett t&eore t&eoretic tica$ a$ p$ate" p$ate" ()ETP* ()ETP* +or co$u! co$u! , u"i# u"i# equi$atera$ tria#u$ar dia#ra!%
•
2. 0
To i'e"ti#ate t&e e++ect o+ t&e pu$"atio "tro.e o t&e )ETP%
INTRODUCTION INTRODUCTION
Extraction i" a uit operatio u"ed to "eparate co!poet" ,a"ed o t&eir C&e!ica$ Di++erece"
i"tead i"tead o+ di++erece" di++erece" i P&"ica$ P&"ica$ Propertie"% Propertie"%
/&e "eparatio "eparatio o+ co!poet co!poet"" o+ a Liquid
Mixtur Mixturee ,eco! ,eco!e" e" ie++ ie++ect ecti'e i'e or 'er 'er di++ic di++icu$ u$tt , !ea" !ea" o+ Di"ti$ Di"ti$$at $atio io00 ad t&e Liqi! Extraction i" oe o+ t&e !ai a$terati'e" to co"ider%
T&e equi$atera$-tria#$e dia#ra! de'e$oped , )uter ad Na"& i" co!!o$ u"ed +or !u$ti"ta#e extractio ca$cu$atio" i'o$'i# terar ""te!"% I practice0 to$uee i" u"ed a" "o$'et to re!o'e t&e "o$ute0 acetoe0 +ro! 1ater4 t&e to$uee-ric& p&a"e i" ca$$ed t&e extract0 ad t&e 1aterric& p&a"e t&e ra++iate%
T&e +o$$o1i# dia#ra! idicate" t&e 5$o1 o+ Strea!" Ad Co!poet" I a Liqi! ' Liqi! Extraction #()tem.
Co!poet" o+ Pu$"ed Co$u! Liquid – Liquid Extractio Uit are a" +o$$o1" 2 o
o
Feed Vessels (63 % B2* – 7raduated C$idrica$ 8e""e$" 1it& 9: L capacit% Column (;3* – a DN <= Pac.ed Co$u! 1it& 3= !! Cera!ic Sadd$e"% E++ecti'e )ei#&t
+.0
E,&ERI-ENT$L &ROCEDURE#
+.1
Cemica/) an! $nci//ar( Eqipment) Reqire!2
C&e!ica$" Required% •
Acetoe (So$ute*%
•
Diioied-/ater( Di$uet*
•
To$uee (So$'et*%
Aci$$ar Equip!et" Required2
+.2
•
T1o 9===!$ Bu# ad t1o 9:!$ ,ea.er"%
•
Re+racto!eter idex %
enera/ #tartp &roce!re).
3% Prepare t&e +o$$o1i# c&e!ica$" 2 a* 5eed ()ea' &a)e*2 Mixture o+ Acetone – Water solution% Prepare 9= $itre" o+ :=1t !ixture o+ Acetone i /ater , !ixi# appropriate quatitie" o+ t&e Acetone i Di"ti$$ed /ater%
,* Prepare 9= $itre" o+ Solvent (Li#&t
*2
luene
3=% T&e uit i" o1 read +or experi!et% Experiment Extraction o3 $cetone 3rom ater U)in5 To/ene.
I t&i" experi!et0 t&ere are t1o +eed" to t&e Mixer ad t1o out$et +$o1" +ro! t&e Sett$er%
5eed 5$o1"2 So$'et2 To$uee (Li#&t P&a"e*% 5eed2 Acetoe – /ater Mixture ()ea' P&a"e*%
Out$et 5$o1"2 Extract
2 To$uee Ric& P&a"e%
Ra++iate2 /ater Ric& P&a"e% &ROCEDURE#
3% C&ec. to e"ure t&e $iquid "tart" to o'er+$o1 at t&e top o+ t&e co$u!0 "top Pu!p P9% 9% Tur o t&e ,ot& pu!p" &1 ad &2 % @% Tur o t&e Pu$"ator &mp &+ ad "et t&e Pu$"atio Stro.e Le#t&% >% Let t&e experi!et ru +or a 1&i$e to attai "tead "tate% :% A$$o1 ,ot& $iquid" to +$o1 ito t&e co$$ectio 'e""e$" 6@ ad 6> re"pecti'e$%
T&e
,otto! product cotai" t&e /ater Ric& P&a"e (Ra++iate * 1&i$e t&e top product cotai" t&e To$uee Ric& P&a"e ( Extract *%
+.+ enera/ #t ' Do6n &roce!re).
3% S1itc& o++ pu!p" P30 P9 ad P@% 9% C$o"e 'a$'e" 8@ ad 8>% @% Ope 'a$'e" 8:0 8 ad 8F to drai a$$ $iquid +ro! t&e experi!et% >% Ope 'a$'e" 83@ ad 83> to drai a$$ $iquid +ro! t&e Recei'i# 8e""e$" 6@ ad 6>% :% Tur o++ t&e po1er +or t&e cotro$ pae
%$4.0
$N$L7#I# 8 DI#CU##ION.
Discuss all your results. The uestions !elo" only serve as a guideline. #our discussion should not only limit to these uestions.
3% P$ot t&e ca$i,ratio cur'e +or to$uee ric& p&a"e ad 1ater ric& p&a"e (Re+racti'e idex '" acetoe 1ei#&t percet* , re+er data #i'e i $ppen!ix B% 9% Deter!ie 1ei#&t percet acetoe o+ t&e ra++iate ad extract i $ppen!ix $ , re+er to ca$i,ratio cur'e prepare i que"tio 3% @% Deter!ie t&e required t&eoretica$ extractio "ta#e +ro! t&e pu$"ed co$u! $iquid-$iquid extractio experi!et re"u$t" , co"truct t&e #rap& u"i# equi$atera$ dia#ra! #i'e i Appedix E% Re+er to $ppen!ix D +or a "tep , "tep ca$cu$atio #uide% >% Ca$cu$ate t&e &ei#&t
i'a$et t&e
tica$ p$ate ()ETP* o+ t&e extractio co$u! +or
$&&ENDI, $ Experiment Extraction o3 $cetone 3rom ater U)in5 To/ene. Re)/t)
5eed RI 5eed Co!po"itio
5eed +$o1rat e (L?&r *
So$'et +$o1rat e (L?&r
So$'et to 5eed ratio
Pu$"atio "tro.e (!!*
Ti!e (!i*
Ra++iate (1ater ric& p&a"e * Re+racti'e So$ute Idex (Acetoe* Co!po"itio (1t *
Extract (To$uee ric& p&a"e* Re+racti'e So$ute Idex (Acetoe* Co!po"itio (1t *
$&&ENDI, B
Data Ca/i=ration Cr;e 3or To/ene Ric &a)e
No
3 9 @ > :
8o$u!e (!L* To$uee /ater Acetoe 3=>%3 F3%< >% :=%= @%: 3%@
9%: @%= >%3 :%> %@ 9@%=
39% 9:%9 :>%= %> %> <3%
A'era#e /ei#&t (#* To$uee /ater Acetoe @%3 @9%@ 3>%=
=%@ 3%3 9%= >%= %= 99%=
3=%= 3F%< >9%> :9%F =% >%=
A'e% /ei#&t Acetoe To$uee 3=%= 3F%< >9%> :9%F =% >%=
@%3 @9%@ 3>%=
Re+racti'e Idex (A'e* 3%>:@ 3%>>F 3%>@=> 3%>3> 3%>== 3%@<
Data Ca/i=ration Cr;e 3or ater Ric &a)e
No
3 9 @ > :
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99%= 9:%3 @>% >%3 :F
<3% <=%3 >% :%= := >
A'era#e /ei#&t (#* To$uee /ater Acetoe 3>%= 39%9 %F @%= 3=
99%= 9:%= @>%: >%= :F :
>%= 9%< :<% :3%= @F
A'e% /ei#&t Acetoe To$uee >%= 9%< :<% :3%= @F
3>%= 39%9 %F @%= 3=
Re+racti'e Idex (A'e* 3%@<3 3%@<9 3%@3 3%@3< 3 @::
$&&ENDI, C
Eqi/i=rim !ata Bino!a/% #o/=i/it( Data 3or $cetoneTo/eneater #()tem To/ene Ric pa)e $cetone >6t ?@ F%F
ater Ric pa)e
ater>6t?@
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Data 3or #o/te Di)tri=tion >Tie /ine)@
No
Vo/me >mL@ To/ene
ater
9ea;( &a)e >ater Ric@ $cetone
Re3racti;e In!ex
? ei5t >$cetone@
Li5t &a)e >To/ene Ric@ Re3racti;e In!ex
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$&&ENDI, D
#TE& B7 #TE& C$LCUL$TION UIDE
3% O,tai t&e equi$i,riu! data +ro! Appedix C% Dra1 t&e equi$i,riu! data ,ioda$?"o$u,i$it cur'e +or to$uee ric& p&a"e ad 1ater ric& p&a"e (Acetoe +ractio '" To$uee +ractio* o a tria#u$ar p$ot (Appedix E*% 9% P$ot t&e corre"podi# tie $ie" o+ acetoe +or to$uee ric& p&a"e ad 1ater ric& p&a"e o a tria#u$ar p$ot (re+er to Appedix C*% @% Locate t&e eac& poit" +or o a tria#u$ar p$ot ,a"ed o2 5eed05 So$'et 0S Ra++iate0R(re+er to Ta,$e appedix A* Extract 0E(re+er to Ta,$e appedix A* 5eed ad "o$'et !ixture0M
3=
NA/Exp4/SEPT 14
>% Locate t&e poit GR01&ere a$$ operati# $ie" "&ou$d !eet%
33
NA/Exp4/SEPT 14
:% Dra1 a tie $ie +ro! poit E to it" equi$i,riu! poit o t&e ,i!oda$ p$ot% Coect a operati# $ie +ro! t&at equi$i,riu! ed o+ t&e tie $ie to poit GR% Exted t&at operati# $ie "o t&at it iter"ect" 1it& t&e ,i!oda$ p$ot at t&e ot&er ed% Dra1 aot&er tie $ie +ro! t&at e1 iter"ectio ad cotiue uti$ a tie $ie &a" pa""ed t&e operati# $ie coecti# R ad S%
% Cout t&e u!,er o+ tie $ie" cotaied i"ide t&e E-5-R-S quadri$atera$(it !a ot ,e a rouded u!,er*%T&at 1i$$ ,e t&e u!,er o+ required t&eoretica$ "ta#e to ac&ie'e +ia$ ra++iate ad extract co!po"itio"%
39
NA/Exp4/SEPT 14
$&&ENDI, E
3@
NA/Exp4/SEPT 14
3>
NA/Exp4/SEPT 14