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Патент USA US2411809

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Patented Nov. 26', 1946 i '
Walter H. Rupp, Mountainside, and Richard ‘0.
_ -
Wright, Elizabeth, N. J., assignors to Standard’
Oil Development Company, a corporation of
Original application .July 14,v 1943, Serial No.
494;654. Divided and this application March 23,
1944, Serial No. 527,728
5 Claims.
(Cl. 202-4153) I
_This invention relates to apparatus for sep
arating one substance in vapor form from two
immiscible liquid substances, and more particu
larly it relates to an apparatus for fractionating
ping~ section added onto the lower part of the
main scrubbing and fractionating tower.
It has now been found that any isobutylene
dissolved in the alcohol portion or the fractionat- '
and stripping isobutylene out of the mixed prod 5 ing tower bottoms can be substantially completely
rejected from the alcohol phase by diluting the
not obtained when regenerating isobutylene from
alcohol phase with water to about 2—12% alco
an- acid solution thereof.
hols. The polymer phase‘ dissolves isobutylene,
isobutylene has many important uses‘ ‘as ‘a raw
however and is inherently immiscible with water
material in the manufacture of important com
or the dilute aqueous solution of the alcohols, and
mercial products, such as in the manufacture of 10 therefore
it is one object of the present invention
2,2,4-trimethyl pentane by polymerizing isobu
to separate and remove the alcohol-water solu
tylene to (ii-isobutylene and then hydrogenating
tion from the bottoms before stripping the latter
with steam to recover dissolved isobutylene. _An
tylene with a small proportion of a diole?n such 15 other object is to provide means especially adapt
ed for ‘effecting this separation and stripping iso
as butadiene or isoprene, as well as in the manu
from the polymer in the most ‘efficient
' facture of-many other chemical products. How
the latter, in the manufacture of synthetic rubber
of the butyl rubber type by copolymerizing isobu
ever, for these various uses, the isobutylene should.
One advantage of this invention is that it per- in most cases be relatively pure for best results“
the stripping of the polymer bottoms sep
and a suitable process for obtaining it in desired
arately from the much‘larger quantity of alco
purity has been to contact mixed ?uids (gase
hol-water solution, and thereby effects the strip- '
ous or liquid phase) containing isobutylenewith
ping with'a much smaller quantity of steam than
a dilute sulfuric acidof, for instance, about 65%
be necessary to strip the, entire fractionat
concentration at ordinary temperature and then 25 ing tower
bottoms. Another advantage which re
to strip the resulting acid extract to liberate the
the one just mentioned is thatvif the
isobutylene. In/this mannerlthe stream which
stripping is effected in‘ a section added on to the
is stripped from the extract consistsof isobutyl
bottom of the fractionating tower, this stripping
ene, in admixture, with minor amounts, e. g.,
section may be constructed with a much smaller
about 2% to 6% of isobutylene polymers, such 30 size than if the alcohol-water solution were also
as di-isobutylene polymers with traces offtri-iso
being stripped. A still further advantage is that
'butylene or higher polymers, about 30% or 40%
the use of the smaller amount of steam for this
of alcohols, chie?ysecondary and tertiary butyl
stripping permits a 'relativelyhigher emciency
alcohols, and water. One possible method for
in the fractionation and scrubbing taking place
separating thelisobutylene from these polymer .; 35. in the fractionating tower.
and alcohol impurities is wtO fractionate the mix‘
The present invention comprises injection of
ture in a tower used as a combination scrubbing
the maximum volume of dilution water into, the
and fractionating tower in which the vapors rich‘
in isobutylene are fed in at the bottom bf the
. top of the scrubbing tower folowed by separat
ing the dilute alcohol-polymer mixture into two
. tower and water is fed in at the top of the tower 40 separate liquid phases, one the upper lighter
for scrubbing the alcohols (which are Water-solu
ble) out from the rising vapors, with the result
‘that substantially pure isobutylene gas, having
phase consisting essentially of oily polymer con
taining isobutylene gas dissolved therein, and the
lower phase of dilute alcohol containing substan
a purity of abouty90% or 95%,fis removed from
tially no isobutylene or polymer. These phases
the top of the tower while the bottoms from the 45 may be separated-by gravity "either by settling
' tower consist of a mixture of the scrubbing wa
or by centrifuging or by other suitable means,
and this separation may be e?ected either in a
ter, the alcohols, and the polymers which have
accumulated during the fractionation process.
settling. drum entirely extraneous from'the frac- '
tionating tower or may be carried out in aset
These bottoms also contain a small but substan
~"~“e-tiai ‘amount of isobutylene in solution and here 50 tling section added to the bottom of the fraction-.
ating tower. This separation is preferably car
tofore, where any .attempt has been made ,to re
ried out continuously and in conjunction with a
cover this dissolved isobutylene, the entire bot
continuously ‘operated scrubbing and fractionat
toms stream has been subjected to stripping by
a suitable material, such as steam, this being done I ing tower. ' The polymer layer ‘only is sent to a
either in a separate tower or in a‘. separate strip oil/stripping section for removal of isobutylene.
2,41 1,809
I vThe alcohol-water solution separated in the
' "settling'drum may, if desired, be recycled to the _
extract stripping zone for dehydration to isobu~
'tylene, or'maybe subjected to further puri?ca
> suitable liquid level indicator controls. ~ A balance
tion or processing steps to re?ne and concentrate
the alcohols for sales uses as such.
- phases from the settling drum ‘I and removal of
the polymer from the stripping section it! may be\
made automatic as well as continuous by use of ‘
line I: may be provided in order to maintain pres
‘ sure balance between the overlying vapor space
Similarly after the ‘dissolved isobutylene has
been stripped from the polymer. the latter may,
likewise be subjected to, puri?cation or other’
processing steps, either for use as such or for con
in the settling'drum ‘I and the vapor in frac
tionating tower 2. The entire equipment may be
operated at any desired pressur , such as atmos
10 pheric pressure or super? or sub-atmospheric
version ‘into other products of equal or higher ,
’ butylene into 2.2,4-trlmethyl pentane by hydroge
nation, etc., or for regeneration into isobutylene
by heat or catalytic cracking.
pressure. Also, if desired, the settling drum may
vbe placed at a lower level, in which case it would,
of ‘course, be necessary to‘ pump the polymer solu
tion from line 9 into the stripping section 10;
01’ the invention will be better understood from
the following description read in combination
with the accompanying drawing, in which Fig. I
- or in conjunction with,-_the settling drum v‘I, as,
_ for instance, using the settling drum 1 for set
molecular weight as by converting the di-iso
alternative previously suggested in a‘
_'I'he objects, advantages, and further details.15 vAnother
general way is the use or a centrifuge in place of,
tlingout the major proportion of the alcohol
represents a vertical section of a scrubbing and 20 water
solution from the oily polymer phase and ‘
fractionating tower with a reduced steam strip- '
then'passing the latter through a centrifuge to
ping section beneath it and an extraneous set
remove a minor residual, proportion of alcohol- _
tling drum, whereas Fig.‘ II represents the lower
water phase. '
portion of a. fractionating tower and the upper‘,
Referring to Fig. II of the drawing, the bottoms
portion of a' lower steam stripping section with 25
which'collect in the bottom tray 5 of the frac
a ksettling section integrally interposed there
. tionating tower 2 are
between. In these several ?gures, like reference
numerals indicate like‘ parts.
Referring to Fig. I, a mixed vapor rich in iso
permitted to ?ow by gravity
through line It into the middle portion- of the
settling section II constructed. immediately be
and communicating with the fractionating
butylene and containing alcohols and small 30 “' neath
tower 2. In this settlingsection I5, the alcohol
amounts of polymer are fed from an isobutylene
water phase settles substantially free of polymer
regenerating apparatus‘ not shown, through line
and isobutylene, and is removed 'continuously
I into scrubbing. and-fractionatin'g tower 2 near
through line It while the polymer solution'con
the bott om thereof, while water is fed through
line 3 into the top of the tower 2 to scrub the 35 taining dissolved isobutylene rises to form ‘a sub
stantially clear upper liquid layer ‘and ‘over?ows
rising vapors and thereby remove the alcohols
down throughthe hollow central portion ll of
therefrom which are‘wat'er-soluble, and to dilute
the settling section IS on to the toptray of the
steam stripping section III constructed imme
throughout the tower by suitable heating and/or 40 diately beneath and communicating with the set
cooling coils, not shown. It is preferable, when "tling section It. This embodiment of the inven- '
‘the alcohol so that a polymer layer will separate.
desired ‘ temperatures
tion provides added 'silrnplicity'and e'?iciency in '
scrubbing and fractionating isobutylene‘ to re
that it requires a minimum of apparatus and con- .
‘move polymers and alcohols therefrom, to main-'
necting- parts and may be made completely auto
tain a temperature of about 100° to 150° F; in the
bottom of the tower, about 100° to ‘130° the 45 matic with the provision of a liquid level indicator
control for regulating the flow of alcohol-water
'7 middle portion and about 90° to 110° E. at the top
, 'solution'removed' through line’ I6.
of the tower. Substantially pure isobutylene
If desired, instead of vusing open stripping
removed from the top of the tower through line
steam, one may use a reboiler, which, of course,
4 and the bottoms which collect in the bottom
tray 5 ‘are removed through'1ine\6 into settling 50 would be located in the same position as the strip
ping section It). I
drum 1 from which the lower alcohol-‘water phase
A conventional design of an isobutylene scrub-,
. is withdrawn through line 8 and pumped to suit- _
’ able
‘ ber tower would require a stripping section about
shown, while the upper liquid phaserconsisting
essentially of. oily polymer-containing isobutylene
dissolved ‘therein is removed from the settling
_ drum 1 through line .9 and returned to the upper
portion of the stripping section I ll constructed
below and communicating with the fractionating » '
tower 2. Steam is fed through line ll into the 60
6 times ‘the cross sectional area and about. 10
times the amount of stripping steam as for the _ I
system described above. This illustrates numer
ically the advantages of the invention in respect
to the savings in steam'consumption and in re
gard to the reduction in size of the stripping, sec-,
tion required.
Although the invention has been described
above as speci?cally applied to the recovery of
lower portion of said stripping section III in order
to strip the dissolved isobutylene from the de
isobutylene from they :fractionating tower bot-'
scendlng polymer solution. The isobutylene
toms containing polymers, alcohols and water, in
stripped from said polymer solution rises out of
the stripping section up through the bottom tray 65 its broader aspect, the invention may be applied
5 of the fractionating tower 2 and mixes with the _ to any fractionating» tower where the bottoms
other vapors rising therethrough. Polymer liq
consist of two or more immisicble' liquids, and '
uid now substantially free from dissolved iso
where "the dissolved vapor occurs primarily .in
butylene is removed from the stripping section 7
solution in one of these liquids. Other examples
l0 through .line I2. .The desired temperature may 70 of applications of this invention are as follows:
be maintained in this stripping section III by suit
1. In solvent extraction, for stripping extract
able heating and/or cooling coils, not shown.
from the liquid solvent.
The equipment just described and illustrated
2. In manufacturing butadiene, for removing
in/ Fig. I is advantageously adapted to ‘continuous
butenes and butadiene from polymer by-products.
operation, and even the removal of the two liquid 75 3. In isopropyl alcohol manufacture, for re
moving isopropyl alcohol from'polymer by-prod
.This is a division of Your copending application
entitled “Separating ?uids and apparatus there
for,” Serial No. 49%,654, ?led July 14, 1943.
It is not intended that this invention be lim
ited to the specific examples and embodiments
which have been given‘ merely for the sake of ii
1 -
’ '
We claim:
1. Apparatus for separating one substance in
vapor form from two immiscible liquid sub
stances, comprising an elongated tower contain
means for feeding the supplementary ?uid in '
liquid form into the upper part of the fractionat
ing zone.
3. Apparatus according to claim 1 having
means for feeding the supplementary ?uid in
vapor form into the lower section of the strip
ping zone.
4. Apparatus according to claim 1 having
means for feeding the supplementary ?uid in liq
10 uid form into the upper part of ‘the fractionating
zone, and also'hav'lng means for feeding the'same
supplementary ?uid in vapor form into the lower
section of the stripping zone.
5. 'Apparatus according to claim 1 in which the
mg a fractionating zone, an intermediate liquid- .
15 said stripping zone has a substantially lesser ca
liquid separating zone,'and astripping zone for
bottoms from said fractionating zone, means for
feeding into said ,fractionating zone near the
pacity' than would normally ‘be required for the
stripping of the entire bottoms from the frac
tionating zone, but su?icient capacity for strip
bottom thereof a mixture of ?uids to be sepa
ping one liquid separated from the mixed liquid
rated, means for removing vapor from the top
fractionating bottoms, there being direct vertical
of said fractionating zone, means for, conducting
vapor connection between the bottom, middle,
liquidgbottoms from the fractionating zone into
the separation zone, means for removing two
separate liquids from the separation zone, means
for conducting one of the liquids from said sep
aration zone into the stripping zone, means for
removing.v vapor and vapor-free liquid bottoms
and upper sections of said tower, there being also
means .for conducting the mixed liquid bottoms.
from the upperor fractionating section of the
tower directly into the middle portion of the mid
dleior separating section of the tower and means
for permitting liquid to over?ow from the upper
from said stripping zone, said apparatus also hav
portion of the separating zone directly and with
ing means for supplying thereto supplementary
in the interior of the tower into the upper por
?uid immiscible in the liquid state, with one of
tion of the bottom or striprpingv section of the
said two immiscible liquid substances, and with
condensate of the substance to_be removed in
vapor form.
2. Apparatus according to claim 1 having
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