Experiment 1 Solid Liquid Extraction

Solid-Liquid extraction unit (Model: BP 40)

The SOLTEQ solid-liquid extraction unit (Model: BP 40) is desined to o!erate as a "ixed-#ed extractor either in a #atch or continuous $ode o" o!eration% Pure sol&ent &a!our enerated in the re#oiler (B') rises throuh a !aced colu$n (') and is condensed in a &ertical *ater-cooled condenser (+,) #e"ore #ein cooled do*n in a !roduct cooler (+4)% The liquid sol&ent is then directed *ither to the collectin &essel (B) or throuh the extraction &essel (B,)% . !re-heater  (+) is !ro&ided to allo* "or extraction !rocesses at di""erent sol&ent te$!erature%

Solid to #e extracted is contained inside a lass container *ith !orous #ed su!!ort% The container  is then !laced in the extraction &essel (B,) the sol&ent and extracted solute (no* in solution) "ro$ the extraction &essel $a/ #e returned to the re#oiler *here the sol&ent is reenerated "or  "urther extraction% General Operating Procedures

The !rocedures outlined #elo* *ill ser&e as a eneral uideline "or o!eratin the equi!$ent and runnin the ex!eri$ent%

11 11

!ali !ali"r "rat atio ion n o# o# Sol Solut utee !o$ !o$po posi siti tion on

he$icals needed: Peanut oil (solute) n-1exane (sol&ent) '% Pre!are $ixtures o" !eanut oil and n-hexane in di""erent co$!ositions2 &ar/ "ro$ 0%0 to '%0  oil 3  sol&ent% ,% se the reco$$ended cali#ration &olu$es in the sa$!le ta#le in .!!endix 5% se a #asis o"  '00  sol&ent% % 6or exa$!le (0%'  oil 3  sol&ent): a) +eih +eih '00  o" n-hexane sol&ent in a #eaer%  #) Then2 *eih '0  o" !eanut oil (PO) in another #eaer% c) .dd the oil into the sol&ent to "or$ a ho$oenous solution%

%ote: 5o this ste! quicl/ to a&oid sol&ent e&a!oration since n-hexane is &olatile%

4% Measure the densit/ o" the cali#rated solution% 7% Plot a cali#ration cur&e o" densit/ &s% solute co$!osition% 8% se that cali#ration cur&e "or "urther ex!eri$ents%

1&

Sa$pling Procedures

.ll sa$!les should #e collected in sa$!lin &ials *ith ca!s to a&oid excessi&e e&a!oration o" the sol&ent% The sa$!les *ill #e used "or densit/ $easure$ents later%

'% E""luent sa$!lin a) Place a sa$!lin &ial #elo* &al&e 9%  #) O!en &al&e 9 and collect a!!roxi$atel/ 70 $l o" e""luent in the sa$!lin &ial% c) lose &al&e 9% ,% e#oiler sa$!lin %ote: Sa$!le taen "ro$ the re#oiler *ill #e at the #oilin !oint o" the sol&ent and $ust #e

handled *ith extra care% a) Place a sa$!lin &ial #elo* &al&e 9'%  #) O!en &al&e 9' and collect a!!roxi$atel/ 70 $l o" re#oiler content in the sa$!lin &ial% Quicl/ close &al&e 9'% c) ool the sa$!le #/ i$$ersin the &ial in cold *ater%

% 5istillate sa$!lin a) Place a sa$!lin &ial #elo* &al&e 9''%  #) O!en &al&e 9'' and collect a!!roxi$atel/ 70 $l o" distillate in the sa$!lin &ial% c) lose &al&e 9''%

1'

!arging o# res Solid

6ill the extraction &essel B, *ith "resh solid *hene&er it is required in the ex!eri$ent%

'% Screen so$e crushed !eanuts to o#tain solids o" si;es #et*een , $$ and 4 $$% +eih a!!rox% '000  o" the !eanuts% ,% hare the extraction &essel B,: a) Ensure that the extraction &essel is drained o" sol&ent%  #) are"ull/ re$o&e the &essel co&er and the solids container% c) 5iscard an/ used solid in the container% d) 6ill the container *ith the screened !eanuts% e) are"ull/ !lace the container #ac into the extraction &essel% ") e!lace the extraction &essel co&er% % hec that the sol&ent "eed line is !ro!erl/ connected to the extraction &essel%

14

Sol*ent +e#ill in te +e"oiler

+hen the sol&ent le&el in the re#oiler is lo*2 re"ill as necessar/% '% S*itch o"" the heater +' !o*er% ,% .llo* the sol&ent te$!erature in the re#oiler to dro! #elo* #oilin !oint and o#ser&e until the  #oilin has sto!!ed% % O!en re#oiler ca! quicl/ re"ill the re#oiler to $ini$i;e esca!e o" sol&ent &a!or% <$$ediatel/ close &al&e re#oiler ca!% 4% S*itch on the heater +' !o*er%

!autions: ,O %O open re"oiler cap .ile te te$perature in te re"oiler is still "oiling 1/

General Sut-,o.n Procedures

'% O!en all &ent &al&es 982 9= and 9>% ,% Place a container under &al&e 9'0% O!en &al&es 942 972 9? and 9'0 to drain all liquid "ro$ the equi!$ent% % Shut-do*n the re#oiler as "ollo*s:

a) Let the coolin *ater run% S*itch o"" the heater +'%  #) lose &al&e 9', "or total re"lux% c) .llo* the sol&ent in the re#oiler to cool do*n to roo$ te$!erature% d) E$!t/ the re#oiler B' #/ drainin all liquid throuh &al&e 9'% 4% Shut-do*n the coolin *ater "lo*s as "ollo*s: a) Let the coolin *ater run until the sol&ent in the re#oiler has cooled do*n to roo$ te$!erature%  #) lose &al&e 9'% 7% lean the extraction &essel B, as "ollo*s: a) Ensure that the &essel is drained o" sol&ent%  #) are"ull/ re$o&e the &essel co&er and the solids container% c) 5iscard the used solid and clean the container% d) are"ull/ !lace the container #ac into the extraction &essel% e) e!lace the extraction &essel co&er%

%ote: .l*a/s clean the solids container thorouhl/2 es!eciall/ the !orous su!!ort2 to !re&ent

$olds "ro$ ro*in a$on the !ores%

xperi$ent 1: !ontinuous ,o.n.ard xtraction o# Peanut Oil (PO) ro$ Peanuts sing n-2exane

OB3!5:

To in&estiate the e""ect o" sol&ent "lo* rate on the extraction o" Peanut oil (PO) "ro$ crushed Peanuts #/ continuous do*n*ard extraction throuh a "ixed solid #ed%

P+O!,+S:

'% Per"or$ the eneral start-u! !rocedures (section '%')% hec that all &al&es are initiall/ closed exce!t the &ent &al&es 982 9= and 9>% Ensure that the extraction &essel B, is e$!t/ o" solids% ,% O!en &al&es 9,2 97 and 9',% Mae sure &al&e 9', is "ull/ o!en to o#tain the $axi$u$ sol&ent "lo* rate% % .llo* the sol&ent to !ass throuh the !roduct cooler +42 "lo* indicator 6<-0'2 !re-heater  +2 extraction &essel B, and #ac into re#oiler B'% 4% Monitor the sol&ent "lo* rate at the "lo* indicator 6<-0'% Once it is relati&el/ constant2 record the &alue% 7% lose &al&e 9', to !re&ent an/ $ore sol&ent "ro$ enterin the extraction &essel B,% lose &al&es 9, and 97% 8% hare "resh solid in the extraction &essel (section '%)% ecord the solid@s *eiht% =% ecord the initial re#oiler te$!erature% Then tae a sa$!le "ro$ the re#oiler and $easure its densit/% ?% To start the extraction2 o!en &al&es 9, A 97 and o!en &al&e 9',% O#ser&e the "lo* o" sol&ent throuh the solids in the extraction &essel B,% >% Once the e""luent has started "lo*in into the re#oiler B' throuh &al&e 9,2 start the ti$er and collect the "irst sa$!le o" the e""luent at ti$e t  0% 5eter$ine the densit/% '0% ontinue sa$!lin the re#oiler contents and e""luent e&er/ 7 $inutes% 5eter$ine each sa$!le@s densit/% .lso record the re#oiler te$!erature at the s!eci"ied ti$e inter&als%

''% Sto! the ex!eri$ent *hen the e""luent densit/ deter$ined in ste! '' sho*s no sini"icant solute co$!osition (nearl/ !ure sol&ent)% ',% S*itch o"" the heater +' !o*er and drain the re#oiler% e"ill the re#oiler *ith "resh sol&ent (section '%4)%

6%6L7SS 6%, ,S!SSO%S:

'% 5ata collection% 6or di""erent sol&ent "lo* rates2 use a ne* ta#le% a) Enter the $ass o" solids and sol&ent "lo* rate "or e&er/ set o" ex!eri$ent%  #) .t the s!eci"ic ti$e inter&als2 record the re#oiler te$!erature and each sa$!le@s densit/% c) O#tain the solute co$!osition "ro$ the cali#ration cur&e (section '% ')% ,% 6or e&er/ set o" ex!eri$ent (di""erent sol&ent "lo* rate): a) Plot a ra!h o" re#oiler content co$!osition &s% ti$e%  #) Plot a ra!h o" e""luent co$!osition &s% ti$e% c) Esti$ate the total a$ount o" extracted solute%

%ote: To "ind the total a$ount o" extracted solute2 calculate the area #elo* the ra!h o" e""luent

co$!osition &s% ti$e2 then $ulti!l/ the area *ith the sol&ent "lo* rate%