exp_4_pulsed column liquid - liquid extraction

8/18/2019 Exp_4_Pulsed Column Liquid - Liquid Extraction

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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!ie t&e &ei#&t equi'a$et t&eoretica$ p$ate" ()ETP* +or co$u! , u"i#

equi$atera$ tria#u$ar dia#ra!%

• To i'e"ti#ate t&e e++ect o+ t&e pu$"atio "tro.e o t&e )ETP%

2. 0 INTRODUCTION

Extraction i" a uit operatio u"ed to "eparate co!poet" ,a"ed o t&eir C&e!ica$ Di++erece"

i"tead o+ di++erece" i P&"ica$ Propertie"% /&e "eparatio o+ co!poet" o+ a Liquid

Mixture ,eco!e" ie++ecti'e or 'er di++icu$t , !ea" o+ Di"ti$$atio0 ad t&e Liqi!

Extraction i" oe o+ t&e !ai a$terati'e" to co"ider%


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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 1ater-

ric& 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 Feed Vessels (63 % B2* – 7raduated C$idrica$ 8e""e$" 1it& 9: L capacit%

o Column (;3* – a DN


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+.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

• T1o 9===!$ Bu# ad t1o 9:!$ ,ea.er"%

• Re+racto!eter idex %

+.2 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 &a)e*2 Pure Toluene%

9 E"ure t&at a$$ 'a$'e" are c$o"ed


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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 *%

% Ope 'a$'e 83= to 1it&dra1 a 3= !$ "a!p$e o+ Ra++iate ad ope 'a$'e 839 to co$$ect a

3= $ $ + E


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+.+ 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 equi'a$et t&eoretica$ p$ate" ()ETP* o+ t&e extractio co$u! +or

di++eret pu$"atio "tro.e% No o+ t&eoretica$ p$ate" are o,taied +ro! Que"tio @%


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$&&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 * Extract(To$uee ric& p&a"e*

Re+racti'e

Idex

So$ute

(Acetoe*

Co!po"itio

(1t *

Re+racti'e

Idex

So$ute

(Acetoe*

Co!po"itio

(1t *


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$&&ENDI, B

Data Ca/i=ration Cr;e 3or To/ene Ric &a)e

No 8o$u!e (!L* A'era#e /ei#&t (#* A'e% /ei#&t Re+racti'e

Idex

(A'e*To$uee /ater Acetoe To$uee /ater Acetoe Acetoe To$uee

3 3=>%3 9%: 39% >F

@ >% >%3 :>%= ::% 9%= >9%> >9%> ::% 3%>@=>

> :=%= :%> %> >@%3 >%= :9%F :9%F >@%3 3%>3>

: @%: %@ %> @9%@ %= =% =% @9%@ 3%>==

3%@ 9@%= %= 99%= >%= >%= 3>%= 3%@%= >%= 3>%= 3%@%= :3%= :3%= @%= 3%@3<

: 3% :F% :=%> 3%= :F%: @F% @F% 3%= 3%@::

3%> >F


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$&&ENDI, C

Eqi/i=rim !ata Bino!a/% #o/=i/it( Data 3or $cetoneTo/eneater #()tem

To/ene Ric pa)e ater Ric pa)e

$cetone >6t

?@ ater>6t?@ To/ene>6t?@

$cetone >6t

?@ ater>6t?@ To/ene>6t?@

F%F 9%>9 %@F

3F%>< 9%F9 %= @%3> 9>%3%3 @%F :>%>9 :%9 %:F

:9%@= :%9 >9%>@ :3%99 >:%< @%3=

=% %9= @9%3> @F%: : 3@% mL@ 9ea;( &a)e >ater

Ric@

Li5t &a)e >To/ene

Ric@

To/ene ater $cetone Re3racti;e

In!ex

? ei5t

>$cetone@

Re3racti;e

In!ex

? ei5t

>$cetone@

3 9@%9 9=%= %: 3%@93 :3% 3%@@: F%<


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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

NA/Exp4/SEPT 143=


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>% Locate t&e poit GR01&ere a$$ operati# $ie" "&ou$d !eet%

NA/Exp4/SEPT 1433


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:% 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"%

NA/Exp4/SEPT 1439


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$&&ENDI, E

NA/Exp4/SEPT 143@


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NA/Exp4/SEPT 143>

exp_4_pulsed column liquid - liquid extraction

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