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Патент USA US2406681

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2,406,581
Patented Aug. 27, 1946
UNITED STATES PATENT» OFFICE
2,406,681
OATALYTIO CONVERSION oF
HYDROCARBONS
Nelson B. Haskell, Port Arthur, Tex., assignor to
-
The Texas Company, New York, N. Y., a cor
poration of Delaware>>
Application June 25, 1943, Serial No. 492,210
6 Claims. (Cl. 26o-683.5)
1
This invention relates to a continuous process
for effecting catalytic conversions of hydrocar
bons such as isomerization of saturated hydro
carbons.
'
v
The invention has to do with the catalytic con
version of hydrocarbons by the action of a con
version catalyst comprising metallic halide-hy
2
sisting essentially of aluminum chloride-hydro
, carbon complex liquid characterized by having
a heat of hydrolysis of about 350 calories or more
per gram of complex liquid or having a heat of
hydrolysis substantially above about 320 to 330
calories per gram of complex liquid. Such com
plex liquid will contain free aluminum chloride
which may be present as a solution in the com
plex liquid or may be suspended therein as un
10 dissolved solid aluminum chloride. It may be
present in both dissolved and suspended form.
rate reaction zones, each zone containing com- o
The catalystV may consist of molecularly dispersed
plex catalyst liquid containing a different con
" drocarbon complex. It involves effecting the re
action during passage of the hydrocarbons un
dergoing treatment through a plurality of sepa
cen‘tration of metallic halide..
In accordance with the invention a stream of
aluminum _chloride in a complex formed by the
reaction of aluminum chloride with an aliphatic
feed hydrocarbons is subjected to contact under
conversion conditions with a liquid catalyst which
hydrocarbon;
comprises metallic halide-hydrocarbon complex
from this main reaction zone will' contain a sub
The stream of hydrocarbon_products issuing
stantial amount of dissolved aluminum chloride.
having a relatively high content of metallic hal
This stream is then passed through another re.
ide. Thereafter the hydrocarbon products con
action zone 'wherein itis subjected to contact
taining some metallic halide in solution are sub
with complex liquid which is relatively lean in
jected to contact with complex liquid having a
free aluminum chloride, ~being characterized, for
relatively low content of metallic halide and
example, by having a heat of hydrolysis of not
capable of removing the dissolved metallic halide
more'than about 260 calories per gram of com
from the hydrocarbon products so that the hy
drocarbon products are discharged from the ñnal 25 plex liquid or substantially below about 320 to
330. As a result of this contact the lean complexV
reaction zone of the process substantially free
becomes enriched with aluminum chloride which
from metallic halide. The complex liquid used for
it has removed from the hydrocarbons undergo
making this final contact with hydrocarbon prod
ing treatment andthe treated hydrocarbons may
ucts of reaction becomes enriched in metallic
halide and is used in a separate zone for treat 30 be discharged free or substantially free from alu
minum chloride.
.
ing a separate stream of fresh feed hydrocar
Contact between the hydrocarbon products and
bons under conditions such that at least partial
complex liquid of relatively low aluminum chlo
conversion is effected. The hydrocarbon prod
ride content is continued until the complex liquid
ucts of reaction from this separate reaction zone
are passed to the first-mentioned reaction zone 35 has become enriched and is characterized by hav
ing a heat of hydrolysis in the range about 300 to
containing catalyst of relatively high metallic
320 calories per gram. Thereafter the enriched
halide content.
complex is removed from further contact with
In this separate reaction zone the metallic hal
hydrocarbon products of reaction and is used for
ide content of the complex liquid is reduced there
by forming a relatively lean complex which may 40 treating another and separate stream of feed hy
drocarbons. This separate stream is subjected
be used for effecting removal of dissolved metal
to contact with the enriched complex under isom
lic halide from the hydrocarbon products in the
erizing conditions so that at least partial isomer
ñnal reaction zone.
ization of the hydrocarbons is effected and is
’Also in accordance with the invention a sepa
rate stream of feed hydrocarbons may be passed 45 accompanied by a progressive decrease in the alu
minum chloride concentration of the complex.
directly to the main reaction `zone containing the
When the aluminum chloride content has been
complex catalyst of relatively high metallic halide
Vdecreased so that the complex liquid is charac
content and make-up metallic halide may be dis
terized by having a heat of hydrolysis of not more
solved in this separate stream of feed hydrocar
bons so as to compensate at least in part for me- - than about 260 calories per gram of complex it is
removed from further contact with fresh feed
tallic halide disappearance from the system and
hydrocarbons and is then used all or in part for
particularly from the main reaction zone where
contact with hydrocarbon products in the final
in it is desired to maintain a relatively high con
reaction zone.
centration of metallic halide.
In each of the foregoing operations contact
The invention has particular application in the
>between hydrocarbons~ and complex of different
isomerization of saturated hydrocarbons with an
aluminum chloride concentration is advanta
aluminum halide catalyst such as aluminum chlo
geously effected in the presence of a promoter
ride. Thus in carrying out the process as applied
such as hydrogen chloride and under tempera
to the isomerization of hydrocarbons with an alu
minum chloride catalyst it is contemplated em- f .ture conditions such Ythat isomerization consti
tutes the principal reaction.
ploying in the main reaction zone a catalyst con
2,406,681
3
4
An important.- advantage of ¿the process has-.to
do Withtheemployment in at leastbne stageiof
the process of a complex liquid catalyst which
contains free metallic halide in substantial"
amount and beyond that required for forming
the complex compounds.
'-»areisubjected to contact with aluminum chloride
It has been found that a complex liquidcatalyst'
» hydrocarbon complex liquid having a heat of hy
--iamount of. dissolved v.aluminum chloride, for ex
;„am'ple about 0.01 to _01.20% by Weight. The dis
charged hydrocarbons are conducted through a
-branch pipe 6 to the lower portion of a ñnal re
actor '1. In this iinal reactor the hydrocarbons
containing free metallic halide Aiseiltective inpro > ...d-rolysis not in excess of about 300 to 320 calories
ducing a high rate of conversion. _Atythefsame
Per-gram ofxcomplex and preferably having a heat
time, however, there is an appreciable amount of
.fof_xhydrolysis- substantially below this, as, for ex
metallic halide migration from the reaction Zone,
ample, about. 260 calories, or in the range or“ about
-"200 `to ‘300 calories per gram. The contact is also
effected-in the presence of promoter at a tempera
the metallic halide being dissolved in> the'eñiuent
hydrocarbon stream and thus being carriedout of
the reaction zone. The disappearance of metallic
ture corresponding approximately to that prevail
.halide from the reaction zone _is undesirablefrom lo.. .ingin the reactor 4.
the. standpoint. of ,maintaining a.. uniformly `high
'ÍTheisomerization reactionV being slightly exo
level _of conversion. . The. presence _ofthe dissolved
.'thermic. the .hydrocarbon stream leaving .the re
«_aluminum. halide. inv .the _. eñluent. hydrocarbon
actor 4 will be at an elevated temperature` which
_ >stream resultsfin accumulation orprecipitation. of
maybe> suiiicient- to. maintain .thedesired tem
lthe metallicfhalide. in subsequent.. stages „ofT _the " perature inthe reactor l. .,However, it is contem
.process _unless provisionis ,made for >effecting-its
plated that .a _differenttemperature may be main
removal.
Y _tained in. thereactor 'I_.eithcr below or above-that
'_Therefore, in__accordance with the;present_.in_preyaílinggin vthe-reactor ê.
vention `the _.eñiuent hydrocarbon streamissub
jected to intimatecontactwith- complex/liquid
„LA stream .of .hydrocarbons _ .comprising isomer
ized hydrocarbonsand .substantially vfree from
aluminum.. halide .is...c_ontinuously drawn oiï from
which is. _ relatively. lean. Vin l„free _.metallic.' halide.
It' _hasybeen .found that_`this’_lean. complex .liquid
yexerts preferential solvent. action' forthe. .metallic
halide and thereby effects its removal§from~îthe
hydrocarbon products .in `whichthe_metallic _Whal
ide may .bepresentas a. solute. ,lnthis-way. the
lean complexliquid is. .enriched .and _the Yresulting
_enriched _complex may.. .then be v.utilized _in effect
the upper portion. 0f.V the. reactor -{.through a pipe
8 communicatingwitha discharge pipeä which
advantageously communicates with suitable frac
30» tionating `equipment .wherein isomerized _hydro
‘ carbons may be'fractionated from .unreacted hy
;drocarbonstopermit segregation-.of _the unreacted
hydrocarbons for recycling throughrthe'system
Vif desired.
ing catalytic; _conversion_..of, at'. least _ abortion Aof
.thefresh.feedhydrocarbons _
" Theïñovv of converte-:i> hydrocarbon lproducts
. It has. _been _found thatan.aluminumbhloride
‘ through the reactor 1 _is continued until the. com
hydrocarbon complex liquid _characterized by. hav
:plex rcatalyst liquid thereinhasbecome enriched
ing a heat _of hydrolysis inthe range about 200 to
With.'aluminum. chloride to theextent. that it is
260, calories poly-gram of .complex liquid iscapable
characterized by havingaheat of 4hydrolysis of
__ of effecting removal of _aluminum halide'. from-.so
ab'out'300‘ toi 320,.calories_ per gram. of4 complex.
Thereafter thehydrocarbon product stream yfrom
.the reactor v«Lisdiverted .from .the reactor l and
lution in hydrocarbons _and will. continue to. exert
this. effect _until_it_is. characterizedbyhaving. a
heat of. hydrolysis inthe range .about 3_00..to _320
4.insteadpassedthrough abranclrpipe. l5 leading
calories per._ gram. _’ As.. soon as v»the_'._.heat _ off _hy
j_to a reactor i6. `_In_other .words the direction of
drolysis reaches a substantially higher _valuealu- " iflow is _reversed before .the .complex inthe reactor
. mînllm . halide is given. up.. and is ,extractedthere
1' becomes saturated with aluminum chloride so
'from bythe .hydrocarbons with .which the. „com
.that-itßfails to -_remove-it entirely from the hydro
.plex isbrought _intoßohtact
' carbons passingj therethrough.
" In order todescribelthe processor 'the .inyentìon
'In thereactor. i0. _the..,hydrocarhofi stream is
in .more detail referencewillnow be. made tothe 50 _.broughtinto contactwith complex liquid of .low
ç accompanying .drawing comprising a.. diagram _of
l dov/'illustrating ,one method _of practicing-«them
`'aluminum chloride content such as initially' used
_.in. the reactor.` 1. ...The eii‘luent stream ofnhydro
' vention as applied tothe isomerization _of normal
carbonsl. from thereactor. lli free fromaluminum
halideisfdl'awn _oiï througha pipe iï> which'com
-_.rnunicates_ with.. the previously mentioned pipe- 9.
‘_'When__the,_product.stream «has been diverted
butane with an aluminumchloride catalyst. pro- l
moted'wíth hydrogen chloride.
Referring to the drawing normal butane is _con
ductedgfrom asource notshown througha pipe I
' from the reactor 1 a separatestream. of heated
_and passed through a heater 2 wherein it is heated
butane. feed, .is conducted. from the heater 2
to a temperatureof about`200° F. _or to a tempera
_ through apipef lilleading to thelower portion
`ture‘within the range 160 to 240". F. A portion .of 60 'of the. reactor. l. ._ Sincethecomplex retained in
' theheated stream is diverted through a _branch
¿the reactor 'l _has been enriched withalurninum
pipe3' and. introduced to thelower portion _of a
chloride it is relatively active as ,an »isomerization
main reactionl tower. 4. In the reactor` 4. itsub-r
catalystso .that butane feed. passing therethrough
jected to contact'with aluminumlchloride-hydro
in the .presence of. promotenundergoes .isomeri
‘ carbon-complex liquid `catalyst characterized by
`zation to a‘substantial extent. ‘.'During .this opera
*having-a heat of‘hydrolysis'inv the range about
i330“ to j350 calories-»pergram of_ catalyst" liquid.
tion'thejstream of hydrocarbons .leavingthe tcp
of the, reactor .l comprising. isobutane,..normal
f Contact between the heated hydrocarbons andthe
butane and any aluminum _chloride thatmay be
catalyst liquid is effected in the -presencehiîghy
dissolved thereinds ,continuously ._drawn- off
`-drogen chloride under conditions VV:such >_that 70 through'aj..pipe 20 communicating. with a.. pipe
- isomerization` constitutes the principal" reaction.
2 I. -through which it is returned `to thelowerpor
I 'The »converted and» unconverted Ahydrocarbons are
tion' of the reactori'll wherein _it is _subjected to
continuously» discharged from» the _upper portion
furthertreatment in the presenceoîthe. fresh
v of the `reactor 4 through a4 pipe-'Sïand' the'dis
« charged
hydrocarbons -will -)contain - a
vsmall
feed butane entering .through’the'pipe 3.
75
vThe flow of feed butano through îthe. reactor l
'2,406,681
5
. is continued until the aluminum chlorldecontent
of the complex therein has become diminished so
that the heat 'of hydrolysis of the'complex is re
duced to about 260 calories per gram or lower.
Thereupon the ñow of hydrocarbons through the
reactors 1 and
I6 is reversed. f Y
K
Y
'
_
ADuring the time that the reactor Tis being
used as a final stage reaction zone theV separatev
stream of feed butane flowing through the pipe
I8 is conducted through a branch pipe 22 lead
ing to the lower portion ofthe .reactork I6. Dur
ing passage of the heated feed Vbutane through
the reactor I6 the enriched complex now present
therein undergoes a decrease in its aluminum
chloride content. The outlet stream of hydro
carbons from the vessel IS during this period is
drawn off through a pipe 23 which communi
cates with the pipe 2l previously mentioned.
Another separate stream of normal butane
6
4,'-that is; whenfadding the hydrogen'chloride and
aluminum halide in solution in feed hydrocar
bons it is contemplated employing separate
streams of feed hydrocarbon for this purpose and
separately injecting them into vthe reaction ves
In the preferred mode of operation the reac
tion‘vessels comprise unpacked vertical towers
containing a stationary column of complex liquid
catalyst,y the height of the liquid column ranging
from about 10 to 60 feet and Ypreferably being
about 25 to 40 feet in height. The feed hydro
carbons are introduced to the lower portion of the
liquid columnv in dispersed liquid phase and
caused to rise in dispersed phase through the
stationary column of complex by difference in
gravity and without subjecting the catalyst liquid
to mechanical stirring. _
~
While the use of non-stirred and non-packed
feed is passed through a pipe 30 to a heater or 20 towers is mentioned, nevertheless the method of
operation is applicable withA packed reaction
heat exchanger 3l and from there passed to a
towers,
or with mechanically agitated reactors.
solution vessel 32. The solution vessel 32 is filled
Complex liquid catalyst may be initially pre
with granular or lump aluminum chloride which
pared by reacting aluminum chloride with an
may be introduced to the vessel> from a hopper
25 aliphatic hydrocarbon in the presence of hydro
gen chloride at temperatures in the range 100 to
During passage of the butane stream through
300° F. for example. An effective preformed
the vessel 32 solution of aluminum chloride in
complex may beprepared by reacting aluminum.
the butane occurs. The resulting solution is con
chloride with straight run kerosene which is sub
ducted through a pipe 34 to the lower portion
30 stantially free from oleñnic and aromatic con
of the reactor 4.
I
~
'
stituents,ithe reaction being effected in the pres
The proportion of butane feed diverted through
ence of hydrogen chloride at a temperature of
the vessel 32 andthe temperature to which it is
33.
~
-
`
heated prior to passage therethroughwill depend
upon the amount of aluminum chloride which it'
is desired to introduce to the reactor 4. As previ- -
ously intimated it is contemplated maintaining
the liquid catalyst within the reactor 4 at arela
tively high level of activity. Since there is> some
about'200 to 250° F.
’
n
‘
-
VIt Vis contemplated that some complex is
formed in situ during the course of the conversion
reaction which accounts for some of the catalyst
disappearance and accordingly the active catalyst
employed in the process may actually comprise
catalyst formed in situ, or a mixture of such cata
disappearance or migration of aluminum halide
with preformed catalyst.
'
from the reactor- 4, it is necessary, therefore, to 40 lyst
While aluminum chloride has been mentionedy
add make-up 'aluminum halide to compensate for
in preparing the complex catalyst it is contem
this catalyst disappearance.
y ï
plated that other metallic halides including alu
Advantageously sufficient aluminum halide is
_minum bromide may be employed. ^ Likewise the
added so that the. body of liquid catalyst Within
promoter used in preparing the complexl or in
the reactor 4 will have a heat ofl hydrolysis rang
effecting the conversion reaction may comprise
ing from 330 to' 350 caloriesper gram of -catalyst
other hydrogen halides besides hydrogen chloride.
liquid.
f
'
' ‘
" j
f‘
~ TheY conversion reaction may be `carried out in
The amount of normal butane‘diverted-thróugh
the presence of other agents such ashydrogen
the-vessel 32 may amount toïabout 10 to ~15%
and normally gaseous saturated hydrocarbons.
50
by volume of the total butane vcharged to the
It>
may also ber carried out in the presence of in
process and the solution temperature prevailing '
hibiting agents which are useful in »suppressing
inthe vessel 32 may range from room tempera
undesired side reactions such as cracking and
ture to 150° F. or to a temperature approximat
catalyst deterioration. Such inhibitors include
ing that prevailing within the reaction vessel 4.
naphthene hydrocarbons such as cyclohexane.
rI‘he proportion of normal butane`feed passed 55 In some cases a low boiling aromatic hydrocarbon
, directly throughV the pipe 3 to the reactionfvessel
4 may range from about 0 to 50%*by'volume
such asbenzene in smallamount may be useful
in suppressing or inhibiting cracking and catalyst
of the total butane chargedto the process'. '
The hydrogen chloride promoter is drawn fromv l
Isomerization of hydrocarbons other than nor
a source not shownthrough a pipe 40 and in 60
mal butane may be carried out by means of the
deterioration.
part conducted directly to the reactor 4 while
the remainder is conducted through a branch
pipe 4l communicating with the previously men
tioned pipe i8 by which means the promoter is
.
process described.
\
v
'
For example, other hydrocar
bons which maybe isomerized comprise pentane,
hexane, heptane, mixtures thereof and also frac
tions of naphtha which are substantially free
introduced to either or both vessels 1 or I6; 65
froml oleilnic` andV benzenoid or aromatic hydro
While promoter may beused simultaneously in
the three vessels 4. 'l and l5, it is'preferred to
f It. is contemplated also that the procedure de-v
inject it to either of the Vessels 'l and lä'only"
scribe'd'may have application in effecting other
during the period Ythat such vessels are lemployed
for effecting contact between fresh feed butane 70 conversion( reactions besides ' isomeriz'ation,
wherein a metallic halide-hydrocarbon complex
and enriched complex.
I
, `
'
'Y
» type >of catalyst is used at temperatures ranging
It is advantageous whenv employing anv alumià
from normal room temperature to about 300? 1i’.Y
num halide-hydrocarbon complex type of catalyst
Mention has been made of isomerizing normal
to provide for separate injection of promoter and
butane in the liquid phase. However, it is con
make-up aluminum halide to the reaction vessel
carbons.
»
i
.'
'
`
^
2,4065681
7
S
templated 4that 'thev rconversion . reaction may be
of catalyst, effecting said contact in the presence
of hydrogen halide at a predetermined tempera
eiîected 'with hydrocarbons undergoing treatment
in either the gas or liquid phase, or in mixed
ture in the range of about 100 .to 300° F. such
that isomerization constitutes the principal re
from 0.1 to 5% or more by weight of the feed
hydrocarbons and dissolved aluminum halide
from said primary Zonegthrough a, secondary
phase.
`The amountof promoter employed may range
hydrocarbons charged to the process.
action, passing a stream containing isomerized
,
In connection with the method of flow specif
ically illustrated in the drawing it is contem
zone, subjecting the hydrocarbons in the sec
ondary zone to contact in liquid phase with liq
plated `that instead of reversing the hydrocarbon 10 uid aluminum halide-hydrocarbon complex hav
flow through the reaction vessels 'l and Iii, the
ing a heat of hydrolysis of about 260 to 300 cal
vessels may be arranged >for continuous ñow in
ories per gram of catalyst, effecting said sec
one direction therethrough with provision for
ondary contact in the presence of hydrogen hal
transferring the complex liquid from one to the
ide at -a temperature in the aforesaid range such
other. In this way the ñnal contact between hy 15 that extraction of aluminum halide from the en
drocarbon. products and lean complex liquid is
tering hydrocarbon stream occurs, removing
continuously made in the same reaction zone.
from said secondary reaction Zone a stream of
Obviously many modiiications and variations
treated hydrocarbons substantially free from
of the invention, as hereinbefore set forth, may
dissolved aluminum halide and producing as a
be made without departing from the spirit and 20 result of said secondary Contact a complex cata
scope thereof, and,v therefore, only such limita
lyst liquid enriched with aluminum halide, sepa
tions. should be imposedas are indicated in the
rately subjecting »another stream of said feed hy
appended claims.
I claim:
drocarbons to contact with said enriched com
v
plex under conditions _such that isomerization
1. In a continuous process for isomerizing nor 25 constitutes the principal reaction and such that
mal butane the steps comprising passing a
said enriched complex becomes denuded of alu
stream of >normal butane in liquid phase through
minum halide, and passing said separately treat
a primary reaction zone, subjecting said butane
ed hydrocarbons to said primary Zone.
in liquid phase to contact therein with a liquid
4, The process according to claim 3 in which a
catalyst consisting essentially of aluminum chlo 30 small amount of make-up aluminum halide is
ride-hydrocarbon complex and aluminum chlo
continuously introduced -to said primary reaction
ride, said catalyst having la heat of hydrolysis
Zone.
of about 330 to 350 calories per gram of catalyst,
5. A continuous isomerization process com
effecting said contact in the presence. of hydro
prising passing a paraffin hydrocarbon feed com
genhalideat a predetermined temperature in 35 prising normal butane in liquid phase through
the range of about 160 to 240° F. such that iso
a primary reaction zone, subjecting said feed in
merization constitutes the principal reaction,
liquid phase to contact therein with a liquid
passing a stream containing isomerized hydro
isomerizatíon catalyst consisting essentially of
carbons and dissolved aluminum chloride from
aluminum chloride-hydrocarbon complex and
said primary zone through a secondary zone, 40 aluminum chloride, said catalyst having a heat
subjecting the hydrocarbons in the secondary
of hydrolysis of .about 330 to 350 calories per
zone to contact in liquid phase with liquid alu
gram of catalyst, eifecting said contact in the
minum chloride-hydrocarbon complex having a
presence of hydrogen halide at a predetermined
heatv of hydrolysis of about 260 to 300 calories
temperature in the range of about 100 to 300° F.
per gram of catalyst, effecting said secondary
such that isomerization constitutes the principal
contact in the presence `of hydrogen halide at a
reaction, passing a stream containing isomerized
temperature in the aforesaid range such that
.hydrocarbons and dissolved aluminum chloride
extraction of aluminum chloride from the en
from said primary zone through a secondary
tering hydrocarbon stream occurs, removing
Zone, subjecting the hydrocarbons inthe sec
from said secondary reaction Zone a stream of
ondary zone to contact in liquid phase with liq
treated hydrocarbons substantially free from
uid aluminum chloride-hydrocarbon complex
dissolved aluminum chloride, and producing as a
having a heat of hydrolysis of about 260 to 300
result of said secondary contact a complex cata- D
calories per gram of catalyst, effecting Said sec
lyst liquid enriched with aluminum chloride,
ondary contact in the presence of hydrogen hal
separately subjecting another stream of normal
. ide at a temperature in the aforesaid range such
butane to contact with said enriched complex
that extraction of aluminum chloride from the
under conditions such that isomerization con
entering hydrocarbon stream occurs, removing
stitutes the principal reaction and such that said
from said secondary reaction zone a stream of
enriched complex becomes denuded of aluminum
treated hydrocarbons substantially free from dis
chloride, and passing said separately -treated hy
drocarbons to said primary zone.
60. solved laluminum chloride, and producing as a
-
2. The process according to claim 1 in which
a small amount of make-up aluminum chloride
is continuously introduced to said primary re
action zone.
3. A continuous isomerization process com
prising passing a parañin hydrocarbon feed com
prisingl normal butane in liquid phase through a
primary reaction zone, subjecting said feed in
liquid phase .to contact therein with a liquid iso
merizationcatalyst consisting essentially of alu
minum halide-hydrocarbon complex and alumi
numhalide, said catalyst having a heat of hy
drolysis in excess of about 320 calories per gram
result «of said secondary contact a complex cata
lyst liquid enriched with aluminum chloride,
separately subjecting another stream of said feed
hydrocarbons to contact with said enriched com
.., plex under conditions such ythat isomerization
constitu-tes the principal reaction and such that
said enriched complex .becomes denuded of alu
minum chloride, and passing said separately
7.0.
treated hydrocarbons to said primary zone.
6. The process according to claim 5 in which
a small amount of make-up aluminum chloride
is continuously introduced to said primary re
action zone.
Y
-
NELSON B. HASKELL.
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