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Патент USA US2411808

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Nov. 26, 1946.
'W_H,RUPP
"
ET
AL
'
2,411,808 \
SEPARATION OF ‘HYDROCARBONS FROM WATER MISCIBLE
LIQUIDS BY DISTILLATION AND WASHING
‘
Filed July 14, 1943
2,411,808
’ Patented Nov. 26, 1946
UNITED STATES PATENT orrlcs
-_
2,411,808 '
ROCARBONS FROM
OF HYD
SEPARATION
WATER MISCIBLE LIQUIDS BY DISTILLA
TION AND WASHING
Richard 0.
Walter H. Rupp, Mountainside, and Standard
to
Wright, Elizabeth, N. J., assignors'
a corporation
of
Oil Development Company,
Delaware
Application July 14, 1943, Serial No. 494,654
8 Claims.
1
(Cl. 202-395)
added on to the-lower part of the main scrubbing
and fractionating tower.
process of separating '
This invention relates to a
one substance in vapor form from two immiscible
It has now been found that any isobutylene dis
solved in the alcohol portion of the fractionating
tower bottoms can be substantially completely
rejected from the alcohol phase'by diluting the
alcohol phase with water to about 242% alcohols.
The polymer phase dissolves isobutylene, however
liquid substances, and more particularly it re
and apparatus for iractionating
and stripping isobutylene out of-the mixed prod
' not obtained when regenerating isobutylene from
an acid solution thereof.
and is inherently immiscible with water or the
Isobutylene has many important uses as a raw
material in the manufacture of important com
mercial products, such as in the manufacture of
. dilute aqueous solution of the
alcohols, and there
fore it is one object of the present invention to
separate and remove the alcohol-water solution
from the bottoms before stripping the latter with
butylene to di-isobutylene and then hydrogenat
steam to recover dissolved isobutylene. Another
ing the latter, in the manufacture of synthetic
rubber of the butyl rubber type by copolymerizing '15 object is to provide means especially adapted for
effecting this separation and stripping isobutyl
isobutylene with a small proportion of a diole?n
ene from the polymer in the most efficient man
such as butadiene or isoprene, as well as in the‘
products.
’manufacture of many other chemical
ner.
One advantage of this invention is that it per
However, for these various uses, the isobutylene
should in most cases be relatively pure for best 20 mits the stripping oi the polymer bottoms separa
rately from the much larger quantity of alcohol
results, and a suitable process for obtaining it in
water solution, and thereby e?ects the stripping
desired purity has been to contact mixed fluids
with a much smaller quantity of eam than would
(gaseous or liquid phase) containing isobutylene
be necessary to strip the entire fractionating
with a dilute sulfuric, acid of, for instance, about
ordinary’ temperature and
tower bottoms. Another advantage which re
25 sults from the one just mentioned is that if the
. 65% concentration‘ at
then to strip the resulting acid extract to 'lib
stripping is effected in a section added on to the
erate the isobutylene. In this manner the stream
bottom of the fractionating tower, this stripping
which is stripped from the extract consists of iso
section may be constructed with a much smaller
butylene, in admixture with minor amounts, e. g.,
about 2% to 6% or isobutylene polymers, such as 30 size. than if the alcohol-water solution were also
being stripped. A still further advantage is that
(ll-isobutylene polymers with traces of tri-iso
the use or the smaller amount of steam for this
butylene or higher polymers, about 30% or 40%
stripping permits a-relatively higher e?iciency in
of alcohols, chie?y secondary and tertiary butyl
alcohols, and water. One possible method for
separating the isobutylene from these polymer
and alcohol impurities is to fractionate the mixd
the fractionation and scrubbing taking place in
fractionating tower.
.
35 the.The
present invention comprises injection of
ture in a tower used as a combination scrubbing
and iractionating tower in which the vapors rich
in isobutylene are fed in at the bottom of the
the maximum volume of dilution water into the
top of the‘scrubbing tower followed byseparating .
the dilute alcohol-polymer mixture into two sep
tower and water is fed in at thetop of the tower 40 arate liquid phases, one the upper lighter phase
consisting essentially of oily polymer containing
for scrubbing the alcohols (which are water-solu
isobutylene gas dissolved therein, and the lower
ble) out from the rising vapors, with the result
phase of dilute alcohol containing substantially
that substantially pure isobutylene gas, having a
no isobutylene or polymer. These phases may be
purity of about 90% or 95%, is removed from the
separated by gravity either by settling or by cenv
top of the tower while the bottoms from the tower 45 trifuglng or by other suitable means, and this
consists of a mixture of the‘ scrubbing water, the
separation may be effected either in a settling
alcohols, and the polymers which have accumu
drum entirely extraneous from the fractionating
lated during the fractionation process. These
be carried out in a settling section
bottoms also contain a ' small but substantial
added
to
the
bottom
of the iractionating tower.
50
amount of isobutylene in solution, and heretofore,
where any attempt has been made to recover this
dissolved isobutylene,
the entire bottoms stream '
has been subjected to stripping by a suitable ma
terial, such a steam, this being done either in a
separate tower or in a separate stripping‘ section
This separation is preferably carried out continu
ously and in conjunction with a continuously
operated scrubbing and fractionating tower. The
polymer layer only is sent to a. stripping section
for removal of isobutylene.
-
_
2,411,808
4
The alcohol-water solution separated in the
settling drum may, if desired, be recycled to the
operation, and even th
phases from the settli e removal 01' the two liquid
extract stripping zone for dehydration to iso
trate the alcohols for sales uses as such.
ng drum 1 and removal of
th
butylene, or may be subjected to further puri_
?cation or processing steps to re?ne and concen
'
Similarly after the dissolved isobutylene has
10
mospheric pressure or super,
> molecular weight as by converting the dl-isobu
or sub-atmospheric
pressure. Also, if desired, the settling drum may
be placed at a lower level, in w
hich-case it would,
tylene into 2,2,4-trimethyl pentane by hydrogena
tion, etc., or for regeneration into isobutylene by
heat or catalytic cracking.
The objects, advantages, and further details
of the invention will be better understood from
the following description read in combination
with the accompanying drawing, in which Fig. I
represents a vertical section of a scrubbing and
fractionatlng tower with a reduced steam strip
'
'
20
xtraneous set
remove a minor residual
tling section integrally interpos
In these several ?gures, like ed therebetween.
reference numerals
indicate like parts.
water phase.
Referring to Fig. II of the drawing,
25
the bot
toms which coll ect in the bottom
tray
5 of the
fractionating to wer
flow by
30 beneath and communicating with the fractionat
35
mer' and isobutylene, and is removed continu
ously through line I6 while
the polymer solution
ing vapors and thereby remove the alcohols
therefrom which are water-soluble, and to dilute
the alcohol so that a polymer layer will sep
arate. The desired temperatures are maintained‘
40
isobutylene to re
move polymers and alcohols therefrom,'to main
; tain a temperature of about
100° to 150° F. in the
bottom of the tower, about 100° to 130° F, in the 45 automatic with the provision of a liquid level in
dicator control for regulating the flow of alcohol
middle portion and about 90° to 110° F. at the top
water solution removed through line “if
of the tower. Substantially pure isobutylene is
If desired, instead, of using . open stripping
steam, one may use a reboiler, which, of course,
50 would be located in the same position as the strip
ping section II).
A conventional design of an isobutylene scrub
ber tower would require a stripping section about
6 times the cross sectional area and about 10
shown, while the upper liquid phase consisting
essentially of oily polymer-containing isobutylene 55 times the amount of stripping steam as for the
system described above. This illustrates numeri
‘dissolved therein is removed from the settling
cally the advantages of the invention in respect
drum 1 through line 9 and returned to the upper
to the savings in steam consumption and in re
portion of the stripping section Ill constructed
gard to the reduction in size of the stripping‘ sec
below and communicating with the fractionating 60 tion
required.
tower 2. Steam is fed through line I I into the
Although the in vention has been described
lower portion of said strippingsection ID in order
above as specifically applied to the recovery of
to strip the dissolved isobutylene from the de
isobutylene from t he fractionating tower bot
scending polymer solution. The isobutylene
able isobutylene-regenerating
apparatus
not
toms containing polymers, alcohols and water,
ution rises out of '
the stripping section up through the bottom tray 65 in its. broader as pect, the invention may be ap~
plied to any fractionating tower where the vbot
5 of the fractionating tower 2 and mixes with the
other vapors rising therethrough. Polymer liquid
toms consist of two or more immiscible liquids,
and where the dissolved vapor occurs primarily
now substantially free from dissolved isobutylene
in solution in one of these liquids. Other ex
is removed from the stripping section III through
‘ stripped from said polymer 501
line II. The desired temperature may be main
tained in this stripping section III by suitable
heating and/or cooling coils, not shown.
'
The equipment just described and illustrated in
Fig. I is advantageously adapted to continuous
70 amples of applications of this invention are as
follows:
‘
v
1. In a solvent extraction, for stripping ex
tract from the liquid solvent.v
2. In manufacturing butadiene, for removing
75 butenes and butadiene from pol ymer lay-products.
liquid and a higher b0 ng hydrocarbon liquid
.
i1‘
,
,
.
3. In isopropyl alcohol manufacture, for re
moving isopropyl alcohol from polymer by
immiscible in water in a fractionation zone, said
product. intended that this invention be limited
It is not
to the speci?c examples and embodiments which
and the hydrocarbon liquid being obtained in ad
mixture with the water-miscible organic liquid
have been given merely for
tion'.
normally gaseous hydrocarbon being removed
I
ion of said fractionation zone
at a lower portion of said fractionating zone, the
. improvement which comprises adjusting the di
the. sake of illustra
lution of said water-miscible organic liquid with
.
admixture to reject dissolved nor
We claim:
separating isobutylene in 10
1. In a process of
mally gaseous hydrocarbon substances there
of alcohols, water and
from, separating the hydrocarbon liquid from
the diluted water-miscible organic liquid freed of
the normally gaseous hydrocarbon that has been
rejected therefrom, then stripping the separated
hydrocarbon liquid to remove dissolved ‘normally
polymer containing
dissolved‘ isobutylene
by frac
'
the isobutylene
vapor is removed overhead and the other mate
rials in liquid form are
mixed bot
toms, the improvement comprising separating
15
gaseous hydrocarbon therefrom, and recovering
said mixed bottoms into two immiscible liquids,
a heavier one consisting essentially of water ‘con
dissolved therein, su?icient water
‘ dilute the mixture to about
2-12% alcohol strength, whereby isobutylene
is
dthe
hydrocarbon from a
20 uid mixed with 'a higher
rejected from the alcohol-water layer an
lighter one consisting essentially of polymer-con
taining isobutylene dissolved stripping
therein, removing
the poly-.
V the alcohol-water phasethe
anddissolved isobutylene
mer phase to remove
uid in a fractionation zone from which the more
,
hydrocarbon is removed overhead
' mally gaseous
base,
the improvement which coma
introducing scrubbing water into an upper
part of the fractionation zone, diluting the ‘waters
27s miscible organic liquid with said scrubbing water
after the scrubbing water has descended to a
lower part of the fractionation zone to reiect m
therefrom.
2. Process according to claim 1;
bottoms are
'
miscible liquids
30
tionation
place,
and
containingtakes
dissolved
isobutylene
vapor is stripped
in the lower part of the fractionating zone to
major ' propor
3. In a process of, separating a ininor propor
tion of isobutylene vapor from a
tion of alcohols and polymers, by subjecting a‘
mixture of said compounds to fractionation and
recover isobutylene.
'
water scrubbing, and removing ’
countercurrent
isobutylene as vapor, and alcohols, polymers and
as a mixture, the improvement
solved normally gaseous hydrocarbon from ad
water-miscible organic liquid mixed with. the
higher boiling hydrocarbonliquld, separating
said hydrocarbon liquid from the diluted water
immiscible organic liquid, pass
_
"hydrocarbon liquid into a stripping zone wherein
dissolved normally gaseous hydr
stripped therefrom, and passing ~normally gaseous
hydrocarbon in gaseous phase from said stripping
zone up through the fractionation zone counter
currentiy to the scrubbing water for removal
overhead from the fractionation zone.
Process according to claim in which the
6.
admixture is separated by
hydrocarbon liquid
the diluted water-miscible organic
gravity from
zone is in a bottomlporliquid and the stripping
'
tion zone, passing the'.bottoms
tionation zone by gravity into a settling zone 45
of the fractionating zone.
wherein gravity separation takes'placc, removing ' .tion
‘1. Process accord
5 in which the
is separated by gravity from '
an alcohol-water layer from the bottom of said
hydrocarbon liquid _
settling zone, and passing a polymer layer con
the diluted water-miscible organic liquid in-a zone
_
vapor dissolved therein from
thessfractionation
zone.
theupper portion of said settling zone into a 50 outside
8.
accor g to
claim 5 in which the
stripp
dissolved isobutylene is
hydrocarbon liquid is separated by gravity from
removed from the polymer layer, removing iso
the diulted water-miscible organic liquid in a zone ,
butylene-free polymer
bottom ofsaid
stripping zone, and recovering the isobutylene
>
‘
.4. In the process of‘ separating a normally gase 55
irom a water-miscible‘ organic
rreedby stripping.
ous hydrocarbon
superimposed upon the stripping zone.
-
‘
‘
WALTER H. RUPP.
RIOHARD O. WRIGHT.
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