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 GROUP 14

CHEM ENG 3023:

Chem Eng Unit Ops Lab
Preliminary KIN1: Continuous Stirred Tank
Reactor (CSTR e!"erimental desi#n$

Grou" leader: %i##in&ot'am )att'e*

(a11+,-1.
Grou" mem&ers: /iu %ui N$ (a110+-
Go' C'in %o* (a12100
3ue date: 1 Se"tme&er 211
5!"eriment to &e conducted: 2 Se"tem&er 211
3emonstrator: 5ric /i67en %su
5!"erimental Code KIN Grou" No$ 14
1
)arks , 4 -  1
Grou" Re"ort: s"eci8c o&9ecties; releant
leader t'eory; correct o"eration "rocedure;
correct ta&les <or collectin# data; risk
Matthe assessment
w Interie*: understand t'e "ro9ect; &e
Higginb <amiliar *it' o"eration "rocedure;
otham address key issues or c'allen#es <or t'e
1195318 "ro9ect; assess "otential risks; "ro6
actie attitude <or e!"erimental
"re"aration
O"eration: correct o"erational
"rocedure; concentration on t'e
e!"erimental *ork; collect ra* data and
note do*n t'e o&serations; o"erate
inde"endently; no accidents
H!i N Interie*: understand t'e "ro9ect; &e
Li! <amiliar *it' o"eration "rocedure;
1179322 "artici"ate in t'e e!"erimental
"re"aration; &e a*are o< "otential risks
O"eration: concentration on t'e
e!"erimental *ork; collect ra* data and
note do*n t'e o&serations; "artici"ate
in t'e o"eration$
Chin Interie*: understand t'e "ro9ect; &e
How <amiliar *it' o"eration "rocedure;
Goh "artici"ate in t'e e!"erimental
1201772 "re"aration; &e a*are o< "otential risks
O"eration: concentration on t'e
e!"erimental *ork; collect ra* data and
note do*n t'e o&serations; "artici"ate
in t'e o"eration$
"im:

 T'e KIN1 continuous stirred tank reactor (CSTR e!"eriment aims to

determine t'e reaction order and rate constant <or t'e &ase 'ydrolysis o<
et'yl acetate &y sodium 'ydro!ide in a continuous stirred tank reactor$

#a$%g&o!n' an' (igni)$an$e:

C'emical reactors are a u&i=uitous "iece o< tec'nolo#y *it'in t'e c'emical
"rocessin# industry em"loyed *'ereer a c'emical trans<ormation is
re=uired to #enerate a desired "roduct$ )any arieties o< reactor 'ae &een
deelo"ed to co"e *it' s"eci8c a""lications; CSTRs suc' as t'e one used in
t'is e!"eriment are ty"ically em"loyed in continuous li=uid "rocessin#
o"erations and are alued <or t'eir relatiely sim"le construction o"eration
and scala&ility (Kirk6Ot'mer 22$

Sa<e and e>ectie o"eration o< any reactor re=uires a t'orou#'

understandin# o< reaction kinetics and &e'aiour$ T'e KIN1 CSTR e!"eriment
uses t'e 'ydrolysis o< et'yl acetate ia sodium 'ydro!ide as a e'icle *it'
*'ic' to e!"lore and deelo" an understandin# o< reaction kinetics$

 *e+e,ant -heo&.:

?ase 'ydrolysis o< et'yl acetate

 T'e &ase 'ydrolysis o< et'yl acetate may &e *ritten as

−¿
−¿ → EtOH + Ac ¿
¿
 EtAc + OH 

Under &asic conditions t'e reaction is considered irreersi&le and may &e 8rst
or second order$ @or <eed in stoic'iometric "ro"ortions t'e rate may &e
e!"ressed as

−¿ ¿
OH 
¿
r = k  ¿
1

−¿ ¿
OH 
¿
−¿
¿
OH 
¿
¿
r = k  ¿
2

A steady state mass &alance on t'e 'ydro!ide ion #ies

 −¿¿
OH 
¿
−¿
¿
OH 
¿
¿
v¿

Be also 'ae t'e s"ace time ( <or a CSTR #ien 'as

V 
τ =
v

%ence

−¿¿
OH 
¿
−¿
¿
OH 
¿
¿
¿

Com&inin# (3) *it' e=uations (1) and (2) #ies

−¿
¿
OH 
¿
−¿
¿
OH 
¿
−¿
¿
OH 
¿
¿
¿
¿
¿

And
 −¿¿
OH 
¿
−¿
¿
OH 
¿
−¿
¿
OH 
¿
2
¿
¿
¿
¿
¿
¿

It <ollo*s t'at i< a "lot o< t'e #rou" on t'e le<t o< e=uation (4 a#ainst s"ace
time is a strai#'t line t'rou#' t'e ori#in t'e reaction <ollo*s 8rst order
kinetics; like*ise i< t'e same is true <or e=uation (, t'e reaction <ollo*s
second order kinetics$ In &ot' cases t'e slo"e o< t'e line is e=ual to t'e rate
constant k$

I< a linear re#ression "roides a "oor 8t to &ot' e=uations 'i#'er or non6

inte#er orders may &e inesti#ated$

)easurin# ion concentration

%ydro!ide ion concentration *it'in t'e CSTR cannot &e measured directly; a
conductiity meter is instead used to measure t'e conductiity o< t'e reactor
eDuent$ So lon# as t'e assum"tion t'at t'e reactor is "er<ectly mi!ed 'olds
true t'is is *ill #ie an accurate readin# o< ion concentration$

 T'e reactor eDuent contains t'ree electrically conductie s"ecies: NaE O%F
and AcF$ T'e conductiity ( is #ien &y

+¿
¿
 Na
¿
−¿
¿
OH 
¿
−¿
¿
 Ac
¿
κ =¿

A mole &alance #ies:

 +¿¿
 Na
¿
−¿
¿
OH 
¿
¿
¿

−¿¿
 Ac
¿
−¿
¿
OH 
¿
−¿
¿
OH 
¿
¿
¿

Com&inin# e=uations  0 and . yields

−¿ ¿
OH 
¿
−¿
¿
OH 
¿
¿ ( i +i )
0  Na  Ac

¿
κ  ¿
¿

Or

−¿¿
OH 
¿
¿

B'ere A is a constant t'at can &e determined ia cali&ration$

"ppa&at!s an' Mate&ia+s:

E/!ipment !n$tion "''itiona+ Ino&mation

Name
Continuous Contains and Com"osed o< a $/ Pers"e! tank
Stirred Tank mi!es reactants containin# t*in a#itators and an
Reactor (CSTR$ allo*in# reaction im"eller reactant inlets "roduct
 to reac' sam"le stream and drain stream$
e=uili&rium$
 ! A?? )easure and )easurement taken as a "ercenta#e
S"'erical &all mani"ulate o< t'e <ull scale reactant Ho* o<
Ho*meters$ reactant Ho* 1$/min(STP
rates$ Scale accuracy o< J1 o< ma! Ho*$
 Tem"erature )easures reactor
6
Pro&e$ tem"erature$
Conductiity )easures stream )easurements taken in milli6
meter and Ho* conductiity Siemens "er centimetre (mScm$ A
cell$ allo*in# reactant cali&ration cure must &e deelo"ed
concentrations to to inter"ret t'e readin#s taken &y
&e determined$ t'e conductiity meter$
 ! Reactant Store 2$2,) 5t'yl Pressurised &y com"ressed air
stora#e essels Acetate and su""ly "rior to e!"eriment to su""ly
Sodium %ydro!ide reactants to t'e a""aratus$
solution$
Com"ressed Air Pressurises )a!imum "ressure o< 22k"a
su""ly reaction stora#e
tanks "rior to
reaction$
As"irator and 3ra* reactor
*ater acuum eDuentstandard
"um"$ solutions t'rou#'
conductiity meter 6
to ena&le
measurement o<
conductiity$
Assorted Used to measure
Glass*are and "re"are
cali&rations
solutions$
-ab+e 1  5!"erimental a""aratus descri"tion$

Mate&ia+
Sodium %ydro!ide (NaO%
solution$
5t'yl Acetate (5t Ac Solution
Sodium AcetateSodium
%ydro!ide Solution (NaO%Ac
Solution
3istilled *ater (%O
-ab+e 2: )aterials
(pe$i)$ations
2$1) Stock solution$
2$2,) Reactor <eed solution$
2$1) Stock Solution
2$2,) Reactor <eed solution$
2$2,62$1) Cali&ration solution$
Used in t'e dilution o< Stock solutions to
"roduce cali&ration solutions$
&o$e'!&e:

Start6u" "rocedure

1$ C'eck t'at t'ere is com"ressed air su""lied to t'e a""aratus and t'at t'e
air su""ly ale on t'e *estern *all o< t'e la&oratory is o"en$
$ Close t'e reactant tank air &leed ale$ Slo*ly o"en t'e reactant tank air
su""ly ale allo*in# t'e reactant <eed tanks to "ressurise$
-$ Turn t'e conductiity meter on at t'e *all$

Cali&ration "rocedure

1$ Produce 2$2, 2$2,2 2$20, and 2$122 )olar NaO% cali&ration solutions
<rom t'e 2$122 )olar stock solution and distilled *ater$ Cali&ration
solutions o< NaO%NaAc mi!ture *it' similar concentrations s'ould already
&e "roided$
$ 3ra* t'e 2$2, )olar standard NaO% solution into t'e conductiity Ho*
cell ia t'e as"irator ale until t'e Ho* cell is <ull$ Tra" t'e solution in t'e
cell &y closin# t'e - *ay ale to t'e o> "osition$ Record stand solution
conductiity$
-$ @lus' t'e cell *it' "ure *ater and re"eat <or eac' standard solution
measurin# conductiity eac' time$

Reactor "rocedure

1$ Close t'e CSTR drain ale and sli#'tly o"en t'e reactor eDuent control
ale$
$ Turn t'e - *ay ale to direct reactor eDuent t'rou#' t'e conductiity
Ho* cell$
-$ Turn t'e mi!er on and <ully o"en &ot' Ho* meters to 8ll t'e CSTR$
4$ Reduce &ot' reactant Ho* rates to 12 mani"ulate t'e eDuent "ur#e
ale to maintain steady Ho* t'rou#' t'e conductiity cell$
,$ A<ter e=uili&rium 'as &een reac'ed allo* t'e reactor to o"erate <or one
residence time &e<ore measurin# conductiity$
$ Re"eat ste"s 46, increasin# Ho* &y 12 eac' time$

S'ut do*n "rocedure

1$ Turn t'e as"irator o> 

$ Turn t'e conductiity meter o> at t'e *all
-$ Close t'e reactant tank air su""ly ale
4$ Gently close reactant control ales to reduce reactant Ho* to Lero
,$ Slo*ly o"en t'e reactant tank air &leed ale
$ O"en t'e reactor drain ale and drain t'e reactor
0$ Turn t'e -6*ay ale to t'e conductiity sam"le line turn t'e as"irator on
and clean *ater t'rou#' t'e Ho* cell$ /eae t'e cell <ull o< clean *ater &y
turnin# t'e -6*ay ale to t'e o> "osition$
(aet. an' *is% "ssessment:

 T'e c'emicals used in t'is e!"eriment "ose a num&er o< risks care s'ould &e
e!ercised *'en 'andlin# all solutions$ C'emical s"illa#es "ose &ot' a c'emical
and sli" 'aLard and s'ould &e re"orted to t'e e!"eriment su"erisor
immediately$

Sa<ety #lasses closed toe s'oes and <ull len#t' clot'in# must &e *orn at all
times to miti#ate t'e risk "osed &y t'is and surroundin# e!"eriments$

Epe$te' *es!+ts:

Cali&ration o< t'e conductiity cell *ill yield a relations'i" &et*een 'ydro!ide ion
concentration and conductiity o<:

−¿ ¿
OH 
¿
−¿
¿
OH 
¿
¿ ( i +i )
0  Na  Ac
¿
κ  ¿
¿

As detailed in t'e releant t'eory section it is e!"ected t'at results *ill 8t eit'er
8rst or second order kinetics$ T'is *ill "resent as a linear relations'i" &et*een

−¿
−¿¿ ¿
OH 
OH 
¿
¿ −¿
−¿ ¿
¿ OH 
OH 
¿
¿ −¿
−¿  or ¿  and s"ace time "assin# t'rou#' t'e ori#in <or 8rst and
¿ OH 
OH 
¿
¿ ¿
¿ ¿
¿ ¿
¿ ¿
¿ ¿

second order kinetics res"ectiely$

Nomen$+at!&e:

i molar conductiities M1 cm61/mol61

k1 rate constant s 61
k rate constant /mol 61s61
r reaction rate mol/61s61
 reactor olume /
v
 reactor <eed rate /s61
 τ 
 reactor residence time s
 conductiity M 1 cm61

*ee&en$es:

)ann U$ (22 Reactor Technology, Kirk6Ot'mer 5ncyclo"edia o< C'emical

 Tec'nolo#y 7o'n Biley and Sons

'an# % (211 Chemical Engineering Unit Oeration! "a#oratory $ro%ect!

&an'al, 3e"artment o< C'emical 5n#ineerin# Uniersity o< Adelaide
un"u&lis'ed$
5ata ent&. sheets:

Cali&ration

One

NaO% conc$ () Conductiity (mScm Tem"erature (QC

2$2,
2$2,2
2$20,
2$122

NaO%NaAc conc$ () Conductiity (mScm Tem"erature (QC

2$2,
2$2,2
2$20,
2$122

-wo

NaO% conc$ () Conductiity (mScm Tem"erature (QC

2$2,
2$2,2
2$20,
2$122

NaO%NaAc conc$ () Conductiity (mScm Tem"erature (QC

2$2,
2$2,2
2$20,
2$122

Reaction data

Reactant @lo* rate Residence time (s Conductiity  Tem"erature

( (mScm (QC
12 ,2$2
2 -,
-2 1$0
42 1$,
,2 1-2
2 12.$-
02 +$+
.2 .1$-
+2 0$
122 ,