ll

i
7

124
750

 

TH _

LIQUID EXTRACTION IN A PACKED
PULSE COLUMN

Yhosis f0: 9910 Degree of M. S.

M!CH£GAN STATE COLLEGE

DOMINIK MARTIN SCHULER
i953

V '\
1E5
T:

'I

 

 

 

 

 

 

195".“

If f - -f '1 .‘u../.7.‘~ f ’Q'IOI I,“ - 1 1C a r); 'v'y‘pﬁu *1)... (q, . h f5? 7?; {\f
.mk-AJIJ It ‘ Ii"‘=UA ".u A I : Mpg 1». an”: Luau-J: w

by

30min1k Eartin Schuler

$ubm1ttal to the Graduate School of Richigan
State College of Agriculture auﬁ Aggliﬂd
Science in partial fulfillment of the

rcguirencnta for the de;rce of

~~n (inf-*9“ ‘gcc (H \T?“,f"§‘
:wi-‘JL .:. A-r ;,-\,;nr..x-...'.

Canartment of Chemical gagineering

1953

A i"f .7271} IA‘EI OE?

Vie writer wishes to eXprcas his aggreciation to

:r. u. u. COOper for $13 helpful tugbeations anﬁ

counsel during the course of tits inventigation.

T5; ”113". 0.?" C '1 1'37 i7?"IS

a
Intra‘action .1?
Tbﬂoretical Part 8
”igerimental ?Mrt 10
Fe suits 15.
ﬁiscvsniau of renults 23
Summary 5

bibliograghy 27

V‘,H‘:¢f .\-'.H‘x:“i VT
1. ‘l'ia.<*.Q./-!(3¢Irl'£.‘

Continuous liqnid-liquid extraction is usoi imlustriallg to a
grout extent where separation or purification oy distillation or ad-
oorption is ianractical. Extra tion is often performed in vertical
towers. containing a.rayo. eiovo ylatoo. or saffloo. or they moy coon
tain a packing such an Fasckig rings. In any case. one of the main
problems 1o to obtain aioqnato mano transfer in a roaoonaolo height of
towor. To do thio it in ﬁeairablo to have among other things a high
interfaoiol area between the two liquid streams.

Baffle-type columno may be considoroa as vortiCal mixer-settlers
in which the Contact of the two liquid otreamo is atago-wiso. h ffor-
oat types of baffles are in use, but the efficiency. 1.6. tic number
of the theoretical etagea, is nauolly far less than a column of the
same height and decign would $1ve in dietillation. In extraction th
ef‘foctivonooo of an actual stage is usually a small fraction of one
tioorotical plate.

In ograj columns one of the two liquids is dish road in fine
drogleto in the second to obtain a high interfacial area. The height
raglirod for oao theoretical stage in tbooe towera also it usually high.
A packed column Lgnerally gives a better efficiency than one without
packing. and this may be due to an increase in turJulonoe and inter-
facial area. Powevor. even in thene columns the efficiency 18 usuAlly
poor Locauao the only forco available for mixing of the streams is the

difference in ionsity of the two liquido.

ﬁechanical cont3ctora other than towers hnvo also been used to
some extent. Vitractiou in a set of miiero and aottlera is common
practice. Another ﬁovico extensively used in acme in us “1913 the
ﬁo&.ialnia :. L30.. co trifusal can Motor. which uses a big 33 epoed
rotor wi‘h a ariral ribbon for contacting the two liquid ttreamm.
Bartela and 371331213531 (1) report that one of '33-.er unite ma «333.31%-
1ent to about four theoretical stgges. ‘ho acmpany claims that some
reﬂui3eo contain as «many on 15 theoretical ota as

The mechanical difficulties involvod in devices of this tort and
the generally poor 53orfornance of ez;raction colunos which are not
aﬁitatei hag stimulatoﬁ efforts to design vertical extraction columnn
in which M 3itionalm 2. icel oner3y is mgpliod to tho qystam. 3} cc
ways of ﬁning thin have been investigatoi:

a) A toroato mi3= in and oettlio5 zones. with mechanicallg opera-
ted stirrora (usually with a rotating shaft to Operate tho stirroro):

b) Vi.ration of tie whole baffle auaomqu in the tower:

0) ml: 3tion of the liqail phaoov vzhile plates or p3ckin3 are in
a 5 30d pomition.

& vortical tower with a motorbdriven. rotating shaft in tho coon

tor.o 3Lich a number of stivrora havo bcca mounted. was mi mi and
to~ro31L 3 .vontigatol oy mibol (3, 3). “Lo original colvon coo-
tainei wire monk packed calmih “ no nos and mixing zones enur3izei my

stirrera att,chod to a ehaft roaching from tho top of the column to
the bottom, with a bear 33 in tho liquid at the uottom
In this column. ona stage. consistin; of a mixing and a aottling

zone. can have an efficiem y which exceeds the effect of one theoreti-

cal 8:333 because of the aiiitional contactin3 of the two liquid streams
in the settling zone. 039 actual 93339 is usually nearly equivalent to
one thearatical stage.

In a can-inch column. hei3hts equivalent to a thearetical stage
of 2.2 in. have be~n obtainad by Neheihsl. In a geni—comnercial multi-
ﬁta;6 extraction column. 1? in. in diameter. ﬁenigned 3y “chcibml,
the hei3hts quivalant to a theoretical Etaga variei from 9 to 15

30133 (3).

For a deoiun of an extraction tower with a vertically Viératoi
plata 33933313, Van Eijck (S) was 3rﬁntci a patent in 1935. In that
gatant to deﬁcrioca also a nystam with the platos in fixed pasition.
but with a pulmcd liquii phase.

For the ayotem with a vi ratei 313t3 ovoeaolj no fartLor informa-
tion was found in the litargture. But the other modification with
fixed plaioo uni pulacd liguid pL3ao has been atuiici during recent
years. Several atOQic anew“: inatallations of this kinl havo'been
built and Operatod, but few 3etaila have been publiahci (ﬂ).

“taco. 3.1;? 5.302331; and. 326-3316? (7) 3mm? dosigzzad a 33:39.11 pails-:38 Mama‘-
tioa column with :erforatad plates. and invaniJEtoi its perfornanco.

To 3;;1J a vibr3ting motion to the liquii ,haso the iaveatigatora usod

‘

.. 2'
I

.,?",.*'1.3. an low on 10 in.

“a
M:

a cam—drivan hollows yulsatcr. Values 0
have been obtained w tn the eyetom wateruiznamyl alcohol. The ﬂiameter
of the column was 1 in.

k packei extraction column with pulaod liquii phase was invaoti-
gated by ?cick And Anderaon (8). They extracted bonzoic acia and

acetic acid from toluene with water. and operated a column with a

I ' w ' r': -1 1
niameter a: 1 7/1. 13.. £11133 with j/o in. n"Ii r1133 3r 3 in.
ﬁciahou 3333163. “or nenzoic 3013 the rapartuﬁ haigkta cf a transfer
unit vnry from 1}.5 to 3.07 feet far the unpulsei column, and for the

Hui ca lung iron 0. 7}? ta 0.535 ft. 13 tha c293 of acati

O

aciﬂ the
b3153t of a transfer unit was 1.1 33d 0.“ ft. f3? the ungulrad $31 333
pulsed colu3a reagectively. It is inzereatin; to note tLat 1:3 graat-
eat increase in peri ormnnce due to p3 ;aation we wrel 13 the caqa 3f
the be3soic 3313 where the efficiency withoxt 331331103 was very poor.
A similar iHVBetigatia3 was publiaha -i b3 ”3:: fer; and ”iaéqndt
(9). ihcy give the inz'3rr3tio:1 t3 -ﬁt in a packet colut.3 o. 1; 13. dia-

meter. filléd with } in. ?&3ch15 rings, the heibﬁt of a tkearatical

“

stage was ?.8 in. without zyvzlﬁ ation and 1.13. with yulaation.

In .033 of tzeso refer '.ces only a few invariant dstsil3 are

given about the aziractOt per ?3rnance.

:33 -

.Le present investigation was ”3 ert3ke. as the firnL nt:3 in 3

horou111 study of the pcrfarma: ca of ”-1321 303.1m33 far 11 xii-

liquid extraction.

II.'77§?3".‘“T CAI. FIG-3"}?
CJ-lculra $.19; .91: tLe fl’icie‘e'tcj of tits-3 '71" wri’Er.

“he data for the per1ormanca of a column may as 6?;3 re 98} in
T. .E.W. (height equivalent to a theoretical stage). or as 1.7.0.
(twin..t ofa t*axcfor u it). whila F.T.ﬁ. yosceasea some thaoretical
advantaﬂea ever H.F.T.S.. its ccrrect use raquirea knowleﬁga of the
fluid film resistances. H.?.T.S. has seen need here 313cc 1% may as
com uted frOm tPQ coagotitioza of the streams a: frog e"u111brium
data. In case tha equili'rium line and the oyeratinﬁ line have the
name slope. aha numerical values of H.V.ﬁ.?. a.d ‘ “T U. are 113.1tical.
Co minimiza the uncertainty of data Scheibel (15) progosed to mdke

he Operating line nearly parallel to the equilibrium line. there

the slopes of the tun lines differ greatly the number of transfer units
would Ci1fur greatly. depatnding upon which of $16 films has been as umcd
to Le con trolling.

1% all tie rur .3 made in t1 1% lnvesti uvtion. tb 6 oz ractant (water)
had a zero cancanuration of the aalute (acetone) at the etart. Further—
more. the distribution coefficient was relatively constant.

In sue h ce.9es he number of theoretical stages may be calculated
accnrding to the furrula:

,: f 1) Y
. 1 ,t (:11) ~33-
H
whicl.18 developed. for 1? stance, in De" "V's F niuook (16). In this

formula 3 rapresenns the number of iﬁeal stages; and x awd 33 are the

0

concentrations of the naluta in aha naivent (caroon tetrachlarids)
far tha incoming Raﬁ leavinj rtrnmmc revactively. 5 may be callad
”the thractiOQ fictgr". It is ﬁ‘v ratio ﬁf tEe @1033 of £33 equili-

brium curvn to tke alaya of the operatiaw line.

a
V v \ q ‘7 1 '0 ‘
1t in ayernfare also éivan by age ratio kg; Whore x in the dis-

triuution caefficieat of th solute (acetone ; I 13 tye flow of the
calvegz (carbaa twtrachloride), and E is tEe flow of the extractant
(WRth). ihe'units URud 1n thia report are alwayﬂ gram mcls for

acetonn and liters per hour for solves: aad uxtractaat.

10

1. 7'.i@ﬁcri;;?*.i?“. Of the Abuarpttﬁ.

 

Fhe apparatua deﬁigncd to 56% same i1formation abnut the perfor-
mance of a packed pulse column is reproduced in detail in Fi;uro 1.

It cancisted mainly of a column of gyrcx glass with a diameter of
5.2 cm and a length of 199 cm. There was only one kinl of packing in
use. which connictcd oi ﬁaschi; rings made of pyrex 513cc with inside
and outniie diameterc of 0.55 and 0.?8 cm respectively'and a length
of 0.?8 cm. The packing had a height of 81 cm. It was supported cy
a flat spiral mada of monel metal. On this spiral ware place} two
layers of Faschig ringa with a diameter of 1.15 cm, in order to allow
a wider egacinl in the winding of the spiral. "he spiral itself vac
sup orted from the cotton of thc column by means of two eup,ortind
stripa made of monel.

3 the: 231 of the column was closed with a rubber ntopgcr through
which tie ilacs tubing for tha different liquii streans extenﬁeﬂ. Che
ctegyer at the lower and of the 0015mm vac covered with a layer of
aercury, adout 0.? cm in height. to keep it protected from the influence
of the malvunt. The upper 930396: was in direct cantact viii the air
space a.ova the liquid.

The g.c..‘..s1-a3«.t‘.-'>r concistod of a brass bellows with an inner ﬁlameter
of_5.5 cm and anon: 10 corrugations. T33 pulsative motion was produced

\

by an adjustable motor-lriven eccentric. Fbc ballows was co prenscl

hv a ﬂaring

~ I «J

and ﬂraun back by tFe prencure of the liquid Mien the 90,133

Overflow

, Polyethylene
Packed Column

 

 

Restrictions

.
| ‘. Ia. _
I}?! .1 A
.lIIllllIl.’ ll" I'll‘-
‘5'“..‘1 I’ll...

_
.
“ ll NV. ...
a
l

_

II lll'l- -‘liu |I

 

 

 

 

 

 

 

\N'lllllll... “VIII! ...|.
Mr. .lnlu I t .l . I II -
IHIN up“ Ill- .D. I I III
- ... Fur { llll il.--..-.

 

- 4
u .
t‘ll‘i .III' M a”

 

 

 

 

 

 

 

 

~ v. 5....
m so aa 80 Hm So on
k) 1..I 4: t 3!}! In J \ III. t
1' {llllfw .“rlll I. r {I
l V.
c“ A 5 8H
J
.m
x
; ,

Damping Flask

1

FIGURE

 

Extractiyn Colunn

with Pulsars?

Pulsator

 

11

was comgrssssd hy the eccentric. Vhe bellows was closed with a rubber
stepper which lasted three or four weeks. i glass tube wit} an inner
diameter of 1.15 am co.iected the bellows with the bottom of the
column.

To get a relatively steed? overflow of the liquiﬂs during pulse-
tion, care was taken to have a free air space of 7 to 10 cm height
setween the run er stooper and the liluii level at the too of the col-
umn. For adiiticnal damping the air space was connected t3 a small
glass tu,e to a bottle haviog a volume of about two liters.

TLe two solvents to Operate the column were stored overhead in
two S-gsllon bottles. ate height of the shelf for the two settles.
measured frcm the bottom of tie column, was 2?0 cm.

For most of the experiments the flow of the two solvents was con-
trolled by fixed restrictions in the form of little glass nozzles in~

side tte tubing. the connections of the glass tubin; were sods with

;.>o.1;;6 the" 16 as mild ng.

 

ch system scetcne-water-cerbon tetrachloride was sslecteﬁ because
of convenience in hasiling, sci because the ﬁistrizution coefficient
is relatively constant. in contraiistinction to most dissociatisg com-
pennis. Furthermore. the quantitative analysis of acetone is not too
cosplicated.

The experiments were always started with a mixture of oeracn tet-
rachloride (Dow, technical Grade) and acetone (ﬁerce G.?. reagent grade).
The acetone was extracted with untreated tap water. The extact, after

8 splinh. was discarded to the sewer. and after addition of more acetone

the carbon tetrachloride was used in tho next run. “J moans 9f thi”
procedure no ci'itional uork for regeneration of tie solvents was re-

(glared.

I"

montcnt.

0‘

). ﬁnalfric of écctnnc
for the quantitative analysis of acetone several methods have

been describol in t} a lit crot"ro: and .;hio and ‘~chulz (10);;wva an

abstract for different matholo 25 years £59.

The reation of acetone with Lyﬂroxylamine k:;.:3rocL13riﬁe. in which
tte amount of acetone 13 determinod my titration of the Lyirochloric
acid formed. was considered tLe most convenient mothoc. It is in
frequent nae for the jetcrmination of certain Letoncc. and rye first
fro,occl for acetone by Locpnor (11). In tLio azaalgzis certain conJi-
tionc. mar' oi wLich re invcctigatod :y Marts o (12}. havc to no
consilcrcd in order to obtain ruliablc and regroduciolc results.

“:o urocedurc Hrc1erred for the dctcrmination of acetaac in the
two solvents. water and/carbon tetrachloride. followed in 5oncral the
inventi: 5ction ofi Bonnet t and yonovan (13).

ﬂ valxmo of 20 ml of the col: tion wlocc acetone content was to be
deter; 11M ran first neutralized with 331. us in3 notW l cran5o as as
ioﬁicator. ahero wan thou aﬁdeﬂ a volume of 10 m1 of hgiroxylwmine
*Jirockloriie solution of 1.ﬁ0 normalitf, ani finally a valune of 10 m1
of o+asmizm L ‘roxilo of 0.?9 normality. For comylction of the re-
uction this mixture was than expaecd fort two hours at room tcm19rat1rc.
Aftﬂr this time th mixture was titrated with hydrochloric acid. using
methyl cran5c no an iniicator. To prcvont losses due to vaporization

& 1’ -m1rlonnave« {139% with a 51389 Stoﬁyer was used. the

13

procedure with carbon tetmchmrme was swath; the same as with the
aqueous. 9011131022. out baczusc of 't}.;a fact. thzat we reaction grahasly
gnaw-ins only in the aqueous 33 page. the use of £21:'J‘.1"r3,:1;z was lament-ad.
'10 convict they two 111111115 well without causing 105mm, the stagger-ad
{12-13}: wan mf‘ecz';a.szically rota-steal arouai its axis in an 12-m112csd 91mm.
A 1.2 cm Macks; ring 13 the flag}: was intended t;- 1zxa'sum 15.33% the.
mixiag would be turbulent.

1

-Le hyiroxylamina method 18 reparted by K0?cman (18) as not
givin; satisfactory results in cam vu-ry wall amounts: of acetnne
have to be determined. Therefore, Roma tests were undertaken to
pram: tirie m that}.
your 10 m1 aasrzglea of an 0.}‘L3 normal timeout; solution of ace-
tom were analyzed; two 111 the pres-sauce of 39:0 :31 a: carbon totmcblar-

6

1:18 23:3. ti-e other two alone. I'}'*,e gamma with carbon teztrachlm'izlu

were Shawn thoromgily bafom ﬁg readonta (Eigydrorwlsmine lgnirrscnlaria‘.

V

3otz'sai‘sm Eviclraxitie) were sci-“ed. '1'1 tration with 1‘}.‘3‘;u. narml

‘1:
a31& required 8.75 ané 8.57 ml of tydrachloric acid for the sinwle
flu-o stage-011:3 mlthimm.‘ For this autism in which carbon tetraci'xlor-
1-.’.e ma grave-m. £23.32 anti {3.633 ml. ware r- quiz-(zed.

Ira-:1: “$32036 analyses the calculate; acetone content. 11‘! 3.3:) milli-
mols for a 13 m1 gaggle.

Tince tie aggraegxﬂgt was better than e:~‘__;;aected and fa: better £222.21
necessary, this analytical method a peers satisfactory.
1%. «Stem afﬁéic '*‘:§+;:‘.ri'r:-fr-1’T-=*al Imrmtij'tirm.
.

’ﬂ'ze eye; tum tin-3631' consideration. a pa :ze-Ji puma (-3me 110:: colmm.

ma 9. (great. mmbsr of process varialxlee uh ch determine its performance.

1!;

the praceas variables which might be taken into consiieration are:

1. ”1nd of packing:

2. Uiametar 3f packiﬂﬁﬁ

3. Fcight of packing:

“. “agraa of settling of packing:
3. Tiamater of the emfracting column;
’. ‘mplituia of pultatioxg
. $rugucacy of pulsatian;

E. Vtapa of paladtian curva;

9. ?low rateﬁ of solvent;
10. T%a particular calvents and solute;
1. Choice of cautinuoua phase in the column;
1?. ”ivection of tranefer of rnluta.

.-.>
:5

investigation incluﬂing all the process variables vault re-
quire an crtremnlg lﬂrge number of test runs. The exhcrimﬁatal waﬂz.
iferefore. cnubi include only a very limiteﬂ selnction of this grest
sun ﬁt of ﬁOSuibilitiaﬁ.

Fur thin investigation these variables hxva been cut Soun to only
ona kind of packing (0.?6 ”aschi; r1359). one height of packing
(31 cm), one iiamctar cf the column (5.2 cm}, and aster always as the
cantiauouc phiﬁn and as the extractant. 1L6 pulse frecuency was kﬁgt
cacttaat aaﬁ the motion of the pulses wan plwayn a nroximntelg a pin
wave.

V.e test runs include} the following investigation:

&) ?loeiiab rates w thaut pulnation and with diffnrcat pales
axplituﬁa: in a well scttlat packing;

a) Tfficiencg of the column at constant flow rmtea ani different
pulse an litudes in a well settled packing;

c) ”friciancy cf tﬂe calumn at one giva: pulse amplitude an.
éifferent flow rates of the solventa in a well settled packing;

d) Cow9°r1rna of the c.ficianc; of tie column at given flaw raten

and palsa an litudea far a well aattlad packing in 020 case and loose

15

filloﬂuin.fack1ng in the other case.
5. Q--.‘-I"-'4t_171-; ‘I‘roi‘o’t‘ro
$39 of tho two fooﬂ oottloo ovorhooﬂ woo filloa V th tap water aud
the othor With carbon tetractlorido contﬁinin; angroximotoly 1 percent
acetone by wmight. Io moot runs tho flow to the column wag fixod by
nozzles in tho lines. the pulse soglitudo of the lixuid was dotoroioed
by moanuriog tho total di-plocomaat of t?e liquiﬂ ourfooo at the top
of the column. «he flow rates were determined by measuring the over-
flow from tie column in a given timo by moono of graduated cyliooors
of one and two litero volume. The interface of tho two liquids was
naintoinod at a constant lovol by adjuotind the height of the flexi-
ble overflow for the carbon tetrachloride. Samples were collected
from each stream 35 or #0 minutes after getting the oyorotio; caoﬁiu
tiono (flow owl lovol) constant. Since the total ho1&Up in the column
was only 2.5 liters. this flow rate wax oufficiont to roglooo the liquiﬁ

in tho column several tiaoa ﬂaring each run.

3...:
UK

17 ’.‘." {‘1 3"? £51"
. . H. L.’.‘Ja.,‘-I

 

the adta for the distributian of neetogn in water and carbon tetra-
chlariiasereréaterminei by ahnkin; thnrsnghlf nearly aquml part3 of the
123.0 malvents tafgﬁth’i‘. with an amount of acetone in a acgé-.rator;y' funnel.
Cnmtlaa were takgn fram tbs twn layorm anﬁ anaxyzeﬁ. The temperature

was 31.2” C. t—dti‘éin 0.5”-

£2153 reﬁllts £3.73; .lfﬁvﬁﬁ 13 232318 I.

 

unncentratlan of acetanc. millimols/liter

 

.. . t- .1. . .. ' - .. .
p30 )Hare . -tvlu,eua~e Histrzuution
W -—— . A“
a f 'f
rnctf‘c*Ar+ J,

   

c.-

uxbmem

173 83.0 1
233x5 1}“) 1
153.8 . ?1.0 “.1.
' 1

1

05.13.)
0

{a - ~* ‘ w 3
{3.1. ".4 (an. i
33. 17.” 3o 7
1;.52 5.u7 2.@9

1%: shown in the graph. tigurg g. the ratio of tin can.entraticn
of acetjno in the two solvsnta is an an ially canetant in the range
unier cansideration. The average value for the éiatribution cceffin

'7’: .
\

clent W 13 2.135 an a valumetric haste for tie salutiona. .J; comgaric
son, wcidall (l7) ragortad iistribution coefficients of 3.295 and

3.235 at a tanpcrature sf ?5° 3. far the rangn covarad.

1?

'J- u h ’- '? ,. .
2. 3mm in“; vat-.022. my 2212111294 203135251.

The 5123011112; rates hava been aietermtnaﬁ. for tit): 2;.-:222.ls'ez‘. coltzsm
unarier norm]. camiutione with well set; 43:1 pad-£1513. ‘37}:e *‘zata have no
111511 (1.2.;1-99 of regrmlunibility. 301292123": 12609.net:- of a. twat-martin which
m_;: ":39 invnlvnd.

TﬂjLﬁ 2.

.7- . n.- 1 .1 I" '2
2'2‘2- 1:1. .- “3314.5.“2; -.t.:.:.*.2,r~:*1.

 

1'“! ., 4- A 14A ..
. s; 7*?22 .22 2.... m"? 3...? 3:323;

V m

Yaﬂ “h?"ﬁ Cﬂlk ”haﬁa
i .. A- ’ »_..

 

33,) 1;.83

,
1*.n “v.2
\‘£&.l 1?.U
394.2 . 21.2
1%.“ 31.6

The; data. are 13.111552?th in 2’1_;ure 3.

«mar-ﬂing; to literature reported. by “fa-03M}. (13). the m2; of they
sqmre 2::th of tie line-2.12 a‘zgpczrﬂcial liquid velocitias (based of the
empty tower aroma section) at £1,109.11; mould. give a. stra.i.5E'-.t line
for each system of liq-21169.. It was furthermore shown that tm m of
them tun 82:13.36 rants 1:5 nearly a cone-taut for each watem.

In the {$223.22. I‘t‘ihgtre '3, the. 52.2.2.2: of the square roots of titzets.
yclmitiea 1:3 also Nicki-r1. It aggxeam nearly a Egarizontal 111123. at!
expéctad.

3. Ilhﬁﬂing_f“t§_fﬁr {Fe ﬂﬁlﬁﬁl Tﬁlvmn.
:29. ﬂats. ft)? 1:112.» {10051213,- ratea for the pulsed 091mm with mall

settle-.3. 3}“..01-"1121; are given in. Table 3. ‘='«"3.th 1.2;113at103 tire r23¢.:ort mi

18

instabilities were ovex graater than in the unpulsai column. the re-
sults are corresnoeiingly lens reproﬁncible. “be puleu frequency was

always 125 étrokes par minute.

‘,94 3.: \«~

“imaging; 2:: 1:1 3“.s..“f3*:23'3 301mm.

Pulse Flow rate
Amplitude liters per hour
2'3 1315‘.

 

O 20.? 1?.0
0. 50 18-. 1908
0. '35 10. 22 1‘. 5
0.88 16.3 13,?
1.15 13.2 13.9

”he (ata are plotted in ii are a. TLe plot 3f tbn quare roots
of tra valacities in this case apwnars to me a elizhtly CRTVEi line.
4'4. fifriﬁ ti 2!} cf 3':- rf’grrﬁnce 1-2.1 4.132 7" .1922. .12.. mwll $35.61.

The inventigaticn was performéd at conntﬁnt flow rates anﬁ V&ri-
able pulse amplituia. The frequancy of the pulsatinn wag 12ﬁ strokes
per miante. tre well settleﬁ packing cansietai of 0.?3 cm Ranchig
rings. the heiqht of tha packing wax 31 ca. tte continuuus phasa was
wqtar. which waa also the extractant. The flow rate of the caraon

tetrachloride wag 18.9 liters. aha thr valocity of the water 13.2

liters per hour. The temyaraturo was 50° 6.. camstaut Within 2° C.

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Ijat 30°

2 I'If ; I 1300" mfIIImoI$ ac e;one {I1FI' I . ‘f“**
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“um Pulse .Acn .nne1,m 11 8319/" ﬁumber
EEO. ‘15-" 11312.6 :4. ' g“ .I: :1; 0f it‘leﬁl 1.130.110 0
.__. ._£1L_. 12. 221. .11 on ._121_._.

 

- 1 0.00 0 21h.5 218.8 70.0 1.13 60.8
’ 2 0.?8 0 2&1 23C.5 53.3 1.77 45.7 -
£- 3 c o 23‘ 213 75.9 1.337 61.0
»"* 0.23 o _ 6 215.5 A7.1 2.13 38.0 -«
5 0 o 2%} 212 77.3 1.3» 63.4
6 0.28 o 239 217 12.9 2.25 36.0
7 0 O 19' ' “‘4'”. 5 (J30). 1. 31 {1'8
L;,/3 0.40 o 252 228 31.5 2.51 32.2 —»
9 O 0 1?? 183. 61.0 1.31 *1.8
"’ 1-0 5.82 o 2. 185 16.93 3.62 22.1; .._
11 c o 122 105.8 52.5 1.32 60.8
2. 0.23 o 2'371'.) :72 9 .93 11.53% 1-137
13 o 0 252.5 203.5 (7. a 1.31 11.3
(14: 1.15 o 313 211.5 11.15 5.01 15.1
1_5 o 0 203.5 222.2 6’. 1 1.34 50.1
; ~41.) 1.10 0 1.17.5 2214-.5 11. 37 11.23 1:11» _._
17 3.20 o 311 217 20.1 2.21 13.9
13 0.20 o 222 :2. 1.57 2.10 19.7

t?u column started at the pﬁlnation of about 1.1 GM.

1'15”.

-' ;-u

data are reprasented 1n the Mr

11211810 the {£467,213}; QB a, “10:3 atalvrted to

the nambar

a
LI .

UHH Wit?

at C.?O Cm.

.4
.- -' if.
.f1::t 9

In this test the

flow

2. For theaa

$73.31: .

r51 be. 1-2111 111ve:1t.1g;.a

£11 0

Tea 80.719
of 11021 stages.

W3°41‘

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Lﬂq-‘y— ‘

variatio»

atlljd.

5'" 011’ I-‘gﬂ
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The

get 115

9.3111, figure 5.

Flaoding of

at the same-am-

ted up by the

31111 sad

there is a break 11 the curve regresentina

of the pcrfarneaca of the pu13£é col-
pmlso amplitude was fixed

the: conditions were as LiVBJ oefcre in Table 4.

 

 

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Tulncﬁ gg.utn wit} Enriaslp low12.tqg.

Run flaw rate Evaber

   

 

30. _ _ . of ideal 1.1. m .S.
1...... 1111110 11.1.12" 3.3.1. on La 32211. 41122-222 on

303.0 121.2 27.0 3.08 23.3
116 125 $8.1 2.82 28.7
5?? 122 13.29 1.15 ~2.8
323 131 122.3 1.51 -53.6

2.71.1.5 131.3, 111.. 57 11. 1.2 10 . . :5
1?!" PS7 70 55 20 80 2'1’09

25 15-“? “-28 129 25? 6.00 2 .23 26.3
26 12.37 77 121 202 2.53 2.22 33.5
“7 12.1? 5.69 139 #55 2.8 2.66 30.4
3 13.10 5.? 126.5 330 3.1 2.? 29.1
2 11.33 10.23 222 265 10.3 3.02 — 25.

.67.2 232 6 .27 1.36 - 23.2
319 227 20.1 2.28 18.9

3.33 3.20
15.1 13.8

_,.I

The results of this table are rlottad in Eigures 5 and 7- together

0600000000000

ux...‘ 4‘3
H “2

with mere data.
Aﬁiscontinu.1cy at a flow r222 of 5 to 5 liters per haur of 501-
vent may b0 oucervad. 2.32rentL2 at least two influences are involved

in ﬁetermining the performance of the column.

 

6.mﬁffnc$ of Flow 5ates in Um 31931 Colu'n.
The operating conditions of Table 5 have been reproduceﬁ with

the excegtion tha: there wan no pulaatian and the flow rates were

V 2.391911.

 

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1‘1“

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10.?
5.93
5.8?
5.933
9.15
“.75
“.51

13.1

Humbar
of iﬂeal ﬁ.?.T.S.
2+... , '

fna 2%

67.1 3&300 3301 1.10 7306
“$.5 227.5 23.7 0.95 83.3
3?.8 230 60.“ 1.29 ‘ 52.5
64.4 1?2 26.5 1.06 76.“
203.5 909.“ 66.1 1.33 60.9
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3' I - ‘ 5h.)

       

V

15.2 27 18 .1 $5.8 1.é9 #7.9
18.7 233.5 1“9.3 76.1 1.61 50.3
1800 231 15000 I .8 1055 5202

?02 235. 90.2 1.5 59.1
230 1&8.) no.6 1.30 $3.

2?? as r31.2 1.10 "f8.6
253 250 78.5 1.35 60.0

5.:
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1he renultg of this table are plotted together with the data of

Table 5 on ligurea 5 and 7.

In case of a constant flow of water and a varia 16 rate of carbon

tetrachloride. the efficiency of the un ulsaﬁ column is sli¢ht1y in»

creauei by increasing tha rate of tha carbnn tetrachloride. which 19

the dispersed phase.

varieule

Ia ti

:9 case of a con-tant flow of carban tetrachloriie and a

rate fer the water. wtich is the continuous phana. a maximum

in the a.ficiency of the cclumn oculi be found. at very low apawds

there seems t0 be a vary poor efficiency. probably bacauae of mixing

0f the continuous phase. it hiﬁh agenda there 15 a slight decrease in

a fi.iency up to the point where flooding conditions ara reached.

 

 

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In tha early stages of this investigation it was observed that
some of the runs at low pulaation cauli not be reproﬁuced after high
gulaation runs had been made. This gave the ingreesion that tha dif‘
f9 ence had been caused by settling of the packing auring pulsation of
the liquid phase at high amglitudea.

It was {wand that the volume of the packiag was reduced while
pulsing the column with carbon tetrachlnride. So obtain a progcr
packing the column was firnt filled with liquid ani the ?-ech1g ring
were then poured into the liquid. Because of the densitiea o! pjrex
Elana and carbon tetrachloride being not very different, the ﬁaechig
tinge bnuncei at pulse amplituies of about 1.0 cm, and by this process
the padking as a whole lost in Valume about 13 pcrcont ulthin one hour
of pulsina.

To o;tain a quantitative picture of this influence. Gama test
runs were made. All coalitions were the same as those used to obtain

the data of Table h. oxccgt that the packing was now prepared by ainply

pouring tha leschig r1313 into tha water-fille& column.

TAJIE 7.

 

ﬁun Pulse I 1.. .. Eumber

Ea. Amplitude a F W in CUlg of ideal H.E.T.S.
....1 §EL___.__.-£a 23$. La Pu ..szzzaa. .1431...
a? o 0 G7.“ 117.2 ua.€ 0.92 25.0
48 o.uo 0 108.0 11%.5 39.8 1.19 (8.0
a9 0 o 186.b 200.3 91.5 o.a6 86.1
50 0.55 0 21m 9 7 6-3.7 1.37 5?.1

5 O O “2 910 10}.8 0 OR 82.?
57-3 0.87 0 2&5 Mi! I’~ 3.9 1. [5 145.2
53 1.05 o 342 ”97.7 55.7 2.18 I3?“?
5» 1.10 o 322 ?70 II 5 7.36 53.3

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

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23

The data are shown graphically in F13ura 85 in which the data for
Table a are regresen ted a gain for comparir on. The investigatian could
not be extended tn higher 9ulke 89plituieq bﬁcruae thﬁ packing started

to settla at pulse am li'xdes of aaoat 1. 0 en.

5-. (‘3‘!!! (a «1 ~51 'tv'vv ~ 9 ‘
v. ..‘Ia"..a~.'? In! 0:. . .:‘.S:T."I..;SJ

in ninted out in advance. this investigation could owl” cover a

0‘3

few of the teats requirei to ex lain the behavior of a pulse extrac-

tian column. These few tegta nhnw that pa laation in extraction cclumna

 

miwht have a con?1‘e “ole economic izterest.

‘ 3 5.1.3.)»;-
;

11 th 6 data reportnl. tlﬂ aver of 1ztea1 sta5ae wag lzcreased
by pulaation up to 3.5 times the number obtainei withaut pulsation
under the same c naitione. Treater 1:9 rovementa can be cx9ected after
further luv at 5atioa of 09eratin; conditions gush an pulse frequency.
pulsa anglitude. or typa of packing in the column.

T;e efii Mi oncy of the column was acea 11y increased ». 3h increas-
in; pulse amplitudes at given pulse frequency 321 given flow rates of
the solvents u9 tn the point at which flon&1n5 occurreﬁ. The height
equivalent of an ideal eta5e wag reﬁuee&. due ta pulsation, from 50
cm ('23.5 in.) ﬂown to 16 cm (6.3 in.) at £19031n3. Th9 flou'rataa of
the nolventa under 1eso conditions were 18.? 11+ era per hour for carbon
tetrachloride and 13.2 liters per hour for water (830 cm or 39.2 ft.
9er hunt vnlncity for the carbcn tetrachloride in the emyty tawar and
4.12 cm or 20.“ ft. per hour for the water which was the cormtinzaul

phase). ﬁecreaning the flow rate of watar at a constant rats far car-

bon tatrachloriﬁe of 13 .9 11+ers per hour also decreased the 91: iciency

of the tcwcr in case of 0.9 on pulse amglituﬂc. 13 cane of no pulgm—
tioa there wag a maximum efficiency of tie column near 8 liters Hater
jer hour.

In case the amount of our on tetrachloride was decreaccl at a
constant speed of 13.2 liters water per hour. there was a decrease in
the number of ideal atagoa in both cases with b.9 Cm pulsation anﬂ also
without pulsation. At a flow rate of 5 to 6 liters carbon tetrachloriﬁe
per hour azﬁ with 0.9 cm yulsation there was a ﬂiﬁcoutinuity in per-

formanca as 2L wn in ? 5uro C, which reminlo that more than one influ-

ecco controls the efficiency of tFe coluin.

 

?eick and Anderson (Q) ragort an improvement due to gulsation up
to a factor of 15, ct where cuch imyrovcmnnte were Observed, the
hei5ht of a transfer unit without pulcation was of the order of 10 ft.
Rowcvor. whero tho initial height of a transfer unit was similar to
the values in this report. the imgrovemnut ﬁne to pulsation was also
nimilar to the improvements of this investigation.

It seems that with gulcation a biguor diameter of packing can be
use& without 109135 too much efficiency.

A comparison of the mata of Tailﬁﬁ h and 7. which are reproduced
in Figure 8. chews clearly the effect of settling of the packing on
efficiency. A lease packing 5iven a conniﬁeracly poorer performance
than a packing which has been settleé well 9y pulsation.

Thin may partly orplain why data reported in the literature about
the performance of packed columns are often 12 such a conniﬁerablo

ﬁinagreemcnt.

The increase of efficiency at the column due to pulsation nigh
be attributeﬁ t3 mare than one grenarcnan. It ran easy to ace differ-
,
excas in thc appearance of the alumn. Vitbnut pulsation big droplets
streamed down the column. but with pa ration. especially at high am-
plitude. these draplets were several times smaller. ani these amallcr
droylets hounccd up and down in the yulecﬂ continuous phase. Hhile
many theories might ue advanced on the basis cf this obcervation. it

is not felt that any of there could be wubatgntiatca withaut further

exyoricentation.

v1. ﬁVkEAFY
As the first Etep, to a more tharough study of the performance
of packed pulsed columnﬁ. an aaparitus was designed, cannisting mainly
of a Calumn ané a pulsator.

The column had a diameter cf 5.? cm (2 in.). and tie langth of

the packing was 81 cm (32 in.). canaisting of Taschig rings with

0-73 0“ diameter. Th8 palattcr cansiated of a cam-driven bellows, which

an 11%& tha pulsating motion to the liquii phase.
In this investigation only to a few of the interesting variables

could ha gich attention, and the reﬁt had ta be left for Saturn

V
I

The results .uOWﬁd that the efficiency of the cclnmn was in-
creaccd with increacing pulse amplitude, up tn the yoint where flood~
n3 occurred. The height equivalant to a theoretical stage was reduced
inc to pulsation from 60 cm (23.5 in.) to 16 cm (6.3 in.) at a pulee

anglitude 0f 1.0 cm and st superficial velociticc of 890 cm (29.2 ft.)

 

26

per hunt for carbon tetrachloride and £22 Cm (23.b it.) per hour for

water.

,rn A

Le 9521 “clenc{ Qf tLg w"10»1 colurq nereaeei 1n evary cage when

‘ha—M' ~— - “"‘-~-

“‘9 . .... I-NW—‘m

he £1ow o1 eifher so1vent was 1“?“61361. Thin was also true for the

‘I an .M ‘__I

. , I." ,u. .... .. ... ~-
"“‘ nah, —.. a. ..Vu- M ..m u"

manulaei column except as high throuéhyut where a 9113ht decrease in

a“

m; 11cienc7 occurrad with increaain 3 watvr rr..e.
Pulsation réduced the capacity of the column a Lig.‘ .13. ﬁt high
tulsn a >11tule t3 :9 flow rates at wfich flao;iz- ozcurrai wars abaut
83 para {vat of those at which £103? in no currel with at pulention.
Tie candition of the packing hai a consiﬁarable influence on per-
formance. The well aettled pack1n3 gave mare theoretical stages for
the same height thaw a laosely filleiain packing. Tia ratio was 1.24 z

1 w thoat pulsation and 2.5 : 1 at high pulse an lituﬂea.

 

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LI 031L711. ° 0

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