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Патент USA US2123821

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Patented July l2', 1938
' 2,123,821
UNITED sfl'iiriasl ~PATENT OFFICE
2,123,821
PROCESS FOR FRACTIONALLY DISTILLING l
HYDROCARBON LIQUIDS
Malcolm P. Youker, Bartlesville, Okla., assigner
to~ Phillips Petroleum Company, Bartlesville,
Okla., a corporation of Delaware
Application November 2s, 1,932, serial No. 644,721
8 Claims.
(Cl. 196-73)
Y' My new improvement pertains particularly to
o, the separating into fractions a mixture formed
by mixing lubricating oil with light petroleum
will vcollect in the accumulator II will, through
manipulation of valve I2, be permitted to flow
in regulated quantity through the pipe I3 intoA
the top of fractionating column 'I and thence
distillate, the process being at least partially car
ried out under sub-atmospheric pressure to thus
downward o-ver bubble trays 8. The liquid which l1
maintain
will then be caused to flow downward over bub
low distillation
temperatures.
l The
process may be ‘advantageously used to separate
ble trays 8 will contact the vapor rising through
other hydrocarbon liquids into desired fractions. . these bubble trays and will condense thereon a
An object of my new process is the obtainment - portion of such vapors. The quantity of liquid
of sharp fractionation between the fractions pro
duced. Another object of my new process is to
separate petroleum liquids into fractions at mini
mum temperatures, thus avoiding the detrimen
tal~ effect of cracking lin _the manufacture of
caused to ñow through pipe I3 into the top of
fractionating column 'I will be so regulated as to
condense within fractionating column l Vall of
the vapors of lubricating oil which will rise there
through and the condensate so produced will
lubricating oils. Other objects of my new proc
flow downward through fraction-ating column 1
Yess will be made apparent in the following speci
over bubble trays 8. A pipe I4 in which is mounted a valve I5 is connected intoA fractionating
fication.
v
The improvements which are set forth here
' in are largely a particular combination of im
provements which were originally disclosed in
column 'I immediately over an intermediatemn’e
of bubble trays 8 and if it is so desired a fraction
of the material flowing downward over bubble 20
applications for United States patent made by the trays 8 may be withdrawn from the fractionating
present applicant under the following dates and` column ‘i therethrough and through a cooling de
United States Patent Office Serial Numbers:
i 431,291, ñled February 25, 1930 and 592,614, ñled
25
February 12, 1932, now U. S. Patent 2,035,209.
vice which is not shown. Liquid which will
flow downward through fractionating column 'l
will be withdrawn from the lowest of bubble trays
8 through a pipe I6 into a pump I'I. The ma
terial which will‘be thus delivered to pump I1
the attached drawing on which a form of ap ' will be forced thereby through the tube I8 which
paratus by which my new process may be carried passes through the furnace 4 and delivers into
My new process will be understood from the
following description taken in connection with
80 out is illustrated in side elevation.
u
the lower portion of fractionating column 1 under
A mixture of hydrocarbon liquids which has
been formed by mixing lubricating oil with light
petroleum distillate for the purpose of facilitat
ing the dewaxing or other treatment of such
bubble- trays 8. The material thus passed through
lubricating oil will be delivered through pipe I
delivered through tube I8 will collect in the bot
tom of fractionating column 1. Liquid delivered
through tube 3 into separator 5 will flow thence
through pipe I9 to a pump 20 and will be forced
thereby through a tube 2| which passes through
furnace 4 and delivers into the lower portion of 40
to pump 2 and thence by means of pump 2
through
furnace
5. The
40 furnace
the tube 3 which passes through the
4 and enters the vapor liquid separator
material »so passed through tube 3 and
4 is heated in passage through the fur
nace 4 to a temperature such that practically all
of said light hydrocarbon distillate and -a por--l
tion of the said lubricating oil will be vaporized
therein and said material will be then delivered '
the tube I8 will be heated therein and partially
vaporized andthe vapors thus formed will flow
upward through fractionating column 1. Liquid
a fractionating column 22 at a point below bub
ble trays 23 which are disposed in fractionating
column 22. The liquid which is passed through
the tube 2| will be heated and partially vaporized
45 into separator 5 in the form of a mixture of , therein and will be delivered therefrom in a par
vapor and liquid. Vapor which enters separator tially vaporized’state into the lower portion of
fractionating column 22, and _vapors thus de
5 will flow thence through pipe 6 into fraction
livered into _fractionating column 22 will ñow
ating column 'I and thence upward through frac
tionating column 'l and bubble trays8 which are upward therethrough Aand through the bubble
disposed within .fractionating column 'l`v and `trays 23 `and thence through a pipe 24 and 50
thence through pipe 9 and a condenser IIl into
accumulator tank II. Vapor which passes
through the pipe 9 and the condenser l0 will be
condensed therein and will flow in the liquid
55 vstate into the accumulator II. Liquid which
through condenser 25 into accumulator tank 26.
The Avapors which flow through the pipe 24 and
condenser 25 will be condensed therein and will
flow into accumulator 26 in a liquid state.
A
portion of the liquid which thus flows into ac
55
2
2,123,821»
.
cumulator 26 will, by regulation of valve 2'Il
be permitted to flow in regulated quantity through
pipe 28 into the top of the fractionating column
conventional practice as to permit the with
drawal of a naphtha fraction from` the accumu
lator I I, a distillate fraction through the pipe I4,
22 and will flow thence downward through the
fractionating column 22 and bubble trays 23,
a light neutral lubricating oil fraction from the
accumulator 26, a heavy neutral lubricating oil
fraction through the 'pipe 30, and a bright stock
contacting vapors which ñow upward through
fraction-ating column 23, and will condense a por
tion of such vapors on the bubble trays 23. The'
quantity of liquid permitted to flow through the
pipe 28 into the top of fractionating column 23
will be so regulated as to condense within the
fractionating column 22 any desired part of the
vapors which rise through fractionating column
22. The liquid condensate produced by such con
densation of vapors within the fraction-ating ,
column 22 will ñow downward over bubble trays
23. A portion of the condensate which will flow
downward over bubble trays 23 may be with
drawn from the fractionating column 22 by
20 means of a pump 29 through a pipe 30 which is
connected into fractionating column 22 immedi
ately over an intermediate one of bubble trays
23. That portion of the liquid which will flow
downward in fractionating column 22 which is
25 not withdrawn through the pipe 30 will flow to
the bottom of fractionating column 22. Liquid
which will collect at the bottom of fractionat
ing column 1 will be caused to flow by means of
a pump 3| through a pipe 32 into the fractionat
30 ing column 22 and onto one of bubble trays 23
which is intermediate between the bubble tray
from which liquid may be drawn through pipe
30 and the lowestof bubble trays 23. A pipe 33
in which is mounted a pump 34 leads from the
35 bottom of the fractionatíng column 22 through
coolers, which are not shown, and will be utilized
to withdraw from the bottom of fractionating
column 22 liquids which collect therein. A vac
uum pump 35, preferably of the steam jet type,
which is mounted in pipe 36 which leads from
the top of accumulator 26 will be utilized lto
maintain a high vacuum in the accumulator 26,
the fractionating column 22, and interconnecting
pipes. Valve 31 is mounted in a pipe 38 which
leads from the top of accumulator tank II. Al
though it is not necessary to the successful oper
ation of the process, an absolute pressure of pref
erably from one to four atmospheres will be
maintained in the' accumulator I I, the fractionat
ing column l, and interconnecting pipes. A sup
ply of hydrocarbon gas will> be made available for
delivery through the pipe- 38 into the accumu
lator II for the purpose of maintaining pressure
in the accumulator I I if such supply of gas should
in any particular case be found necessary for the
purpose outlined..
In case excessive pressure
should develop in accumulator II gas may be
vented therefrom through pipe 38. As a result
of the maintenance of comparatively high pres
sure in the fractionating column l and compara
tively low pressure in the iractionating column
22 the liquid which will be delivered from the
bottom of f-ractionating column l through the
pipe 32 into fractionating column 22 will in sub
stantial amount vaporize upon entry into frac
tionating column 22. The extent to which liquids
which will be passed through the furnace 4 will
be heated and the introduction of refluxed liquid
into the tops of fractionating columns ‘I and 22
70 will all be so regulated that desirable fractions
of the material delivered by the pump 2 to the
process may be separated into desirable fractions.
For instance, when charging a mixture of lubri
eating oil and naphtha, to the apparatus, the
75 apparatus may be so regulated in accordance with
fraction through the pipe 33. A pipe ,38 in which
is mounted a-valve 4,0 is connected ,into the lower
portion of accumulator II and will serve to with
draw from the accumulator II liquid which will
collect. therein. A pump 4I which is mounted
in a pipe 42 which- is connected into accumulator
26A will serve'to withdraw liquid which will col
lect in accumulator 26.
Steam may if desirable
be admitted into Atubes I8, -2l, and 3 through
pipes 43, 44, and 45‘, respectively. Valves 50, 5I,
and 52 are'mounted in pipes 43, 44, and 45, re
spectively.
In case steam is admitted into any
part of the apparatus it will ultimately be con
densed and delivered in the liquid phase into'ac
20
cumulators II or 26, as the case may be, and pipes
46 and 48 in which are mounted valve 44 and
pump 49, respectively, arerprovided for withdraw*
ing water from these accumulators.
While I have described in detail‘the use of one
form of apparatus with which my new process
may be carried out, it should be understood thaty
I do'not propose to limit myself to these details
but intend to claim lbroadly all the inherent ad
vantages of my new improvements.
For in
30
stance, both of the fractionating columns shown
may be operated at atmospheric pressure or at
any other pressure and any mixture of liquids
may be charged to the apparatus and separated
into any desirable fractions. While the heat
ing tubes 3, I8, and 2I are shown mounted in a
single furnace, it may be found advantageous to
mount these heating „tubes in separately fired
furnaces and I may do so.
I claim:
_
40
1. The process for fractionally distilling hydro
carbon oils comprising passing a mixture con
sisting of lubricating oil stock adrnixed with a
lighter diluent oil, such as naphtha, in a restricted
stream through a heating zone and thereby heat 45
ing the mixture to a distilling temperature, sepa
rating the heated mixture under the inñuence
of the heat impounded therein into a first liquid
fraction and a first vapor fraction, rectifying said
first vapor fraction under super-atmospheric 50
pressure, thereby separating a second vapor frac
tion from a second liquid fraction, additionally
heating said first liquid fraction and then'simul
taneously rectifying said first and second liquid
fractions in a single rectifyíng zone under sub
atmospheric pressure.
55
’
2. The process for fractionally distilling lubri~
eating oils comprising passing a mixture consist
ing of lubricating oil stock admixed with a lighter
diluent oil, such as naphtha, in a restricted stream 00
through a heating zone and thereby heating the'
mixture to a distilling temperature, then dis
charging the heated mixture into a separating
zone, dividing said mixture in the separating
zone into a ñrst vaporous fraction and a first
liquid fraction under the influence of the heat
impounded therein, introducing said vaporous
fraction into the medial portion‘ of a first recti
fication zone and therein separating the same into
a second liquid fraction and a second vaporous 70
fraction, withdrawing a portion of the second
liquid fraction and introducing it into the medial
portion of a second rectification zone maintained
under sub-atmospheric pressure and at a pres
sure below that existing in the first rectification
3
2,123,821
zone, passing the first liquid fraction from said
separating zone, reheating it and introducing it
into the lower portion of the second rectification
zone, subjecting the oil in each of said rectifica
tion zones to refiux condensation and thereby
separating distillates from the oil, withdrawing a
light distillate from the first rectification zone,
and withdrawing heavier distillates from the
second rectification zone.
10
3. The process for fractionally distilling lubri
cating oils comprising passing a mixture consist
ing of lubricating oil stock admixed with a lighter
diluent cil, such as naphtha, in a restricted
stream through a heating zone and thereby heat
'15 ing the mixture to a distilling temperature, then
discharging the heated mixture into a separating
zone, dividing said mixture ' in the separating
zone into a first vaporous fraction and a ñrst
20
liquid fraction under the infiuence of the heat
impounded therein, introducing said vaporous
fraction into the medial portion of a first recti
fication zone and therein separating the same into
a second liquid fraction and a. second vaporous
fraction, withdrawing a portion of the vsecond
25
liquid `fraction from the lower portion of. the
first rectification zone, reheating it and returning
it to the bottom portion of the ñrst rectification
zone for supplying heat to the bottom portion of
the first rectification zone, withdrawing another
30 portion of the second liquid fraction and intro
ducing it into the medial portion of a second
rectification zone maintained under sub-atmos
pheric pressure and at a pressure below that
existing in the first rectification zone, passing the
35 ñrst liquid fraction from said separating zone,
reheating it and introducing it into the lower
portion of the second rectification zone, subject-‘
ing the oil in each of' said rectification ~zones to
reflux condensation and thereby separating dis
40 tillates from the oil, withdrawing a light dis
tillate from the first rectification Zone, and with
drawing heavier distillates from the second recti
fication zone.
4. The process for fractionally distilling lubri
45 cating oils comprising passing a mixture consist
ing of lubricating oil stock admixed with a lighter
diluent oil, such as naphtha, in a restricted
stream through a heating zone and thereby heat
ing the mixture to a distilling temperature, then
rectification zone below the upper ends of said
rectification
zones.
-
I
5. The process for fractionally distilling lubri
cating oils comprising passing lubricating oil
stock admixed with‘a lighter diluent oil, such as
naphtha, in a restricted stream through a heat
ing zone and thereby heating the mixture to a
distilling temperature, then discharging the heat
ed mixture into a separating zone, dividing said
mixture in the separating zone into a first vapor
ous fraction and a first liquid fraction, introduc
ing said vaporous fraction into the medial por
tion of a first rectification zone and therein sepa
rating the same into a second liquid fraction and
a second vaporous fraction, withdrawing a por
tion of the second liquid fraction from the lower
portion of the first rectification zone, reheatingit
and returning it to the bottom portion of the first
rectification zone for supplying heat to the bot
tom portion of the first rectification zone, with
20
drawing another portion of the second liquid
fraction and introducing it into the medial por
tion of a second rectification zone maintained
undersub-atmospheric pressure and at a pres
sure below that existing in the ñrst rectification 25
zone, passing the first liquid fraction from said
separating zone, reheating it and introducing it
into the lower portion of the second rectification
zone, subjecting the oil in each of, said rectifica
tion zones to refiux condensation and thereby 30
separating distillates from the oil, withdrawing
a light distillate from the first rectification zone,
withdrawing heavier distillates from the second
rectification zone, and admixing steam with the
first liquid fraction before introducing that frac 35
tion into the second rectiñcation zone.
6. The process for fractionally distilling lubri
cating oils comprising passing lubricating oil
stock admixed with a lighter diluent oil, such as
naphtha, in a restricted stream through a heat
ing zone and thereby heating the mixture to a
distilling temperature, then discharging the
heated mixture into a separating zone, dividing
said mixture in the separating zone into a first
vaporous fraction and a first liquid fraction, in
troducing said vaporous fraction into the medial
portion of a first rectification zone and therein
separating the same into a second liquid fraction
and a second vaporous fraction, withdrawing a
portion of the second liquid fraction from the
50 discharging the heated mixture into a separating
' lower portion of the first rectification zone, re
zone, dividing said mixture in the separating zone
under the infiuence of the heat impounded there
in, into a first vaporous fraction containing said
55 lighter diluent oil, and a first liquid fraction,
introducing said vaporous fraction into the me
dial portion of a first rectifying Zone and therein
separating the same into a second liquid fraction
and a second vaporous fraction, supplying heat
60 to the bottom portion of the ñrst rectification
zone, withdrawing a portion of the second liquid
fraction from the lower portion of the first recti
fication zone and introducing it directly into the
medial portion of a second rectification zone
maintained under sub-atmospheric pressure and
at a pressure below that existing in the first
rectification zone, passing the first liquid fraction
from said separating zone, reheating it and intro
ducing it into the lower portion of the second
rectiñcation zone, subjecting the oil in each of
said rectiñcation zones to reflux condensation and
thereby separating distillates from the oil, with
drawing lighter diluent oil from the upper por
tion of the first rectification zone, and withdraw
75 ing heavier distillates from the first and second
heating it and returning it to the bottom portion
of the first rectification zone for supplying heat
to the bottom portion of the first rectification
zone, withdrawing another portion of the second
liquid fraction and introducing it into the medial
portion of a second rectification zone maintained
under sub-atmospheric pressure and at a pressure
below that existing in the first rectification zone,
passing the first liquid fraction from said sepa 60
rating zone, reheating it and introducing it into
the lower portion of the second rectification zone,
subjecting the oil in each of said rectification
zones to reñux condensation and thereby sepa
rating distillates from the oil, withdrawing a
light distillate from the first rectification zone,
withdrawing heavier distillates from the second
rectification zone, and admixing steam with the
charging` stock before passing the charging stock
through the heating zone.
70
7. The process for fractionally distilling lubri
cating oils comprising passing lubricating oil
stock admixed with a lighter-,diluent oil, such as
naphtha, in a restricted stream through a heating
zone and thereby heating the mixture to a dis 75
4
2, 193,891
tilling temperature, then discharging the heated
mixture into 'a separating zone, dividing said
mixture in the separating zone into a first
vaporous fraction and a iirst liquid fraction, in
troducing said vaporous fraction into the medial
portion of a ñrst rectiiication zone and therein
separating the same into a second liquid traction
and a second vaporous fraction, withdrawing -a
portion of the second liquid fraction from the
10 lower portion of the ñrst rectiñcation zone, re
heating it and returning it tothe bottom por
‘tion of the ñrst rectiiication zone for supplying
heat to the bottom portion of the ñrst rectifica
tion zone, withdrawing another portion of the
second liquid fraction and introducing it into the
medial portion of a second rectiiication zone
maintained under sub-atmospheric pressure and
at a pressure below that existing in the first
rectification zone, passing the iirst liquid frac
20 tion from said separating zone, reheating it and
introducing it into the lower portion of the second
rectiñcation zone, subjecting the oil in each of
said rectiiication zones to reñux condensation
and thereby separating distillates from the oil,
withdrawing a light distillate from the ñrst recti
ñcation zone, withdrawing heavier distillates from
the second rectiñcation zone, and adxnixing
steam with the second liquid fraction after it
leaves the first rectification zone and before it
0 enters the second rectiñcation zone.
8. A hydrocarbon oil distilling process which
comprises passing lubricating oil stock admixed
with a lighter diluent oil in a restricted stream
through a heating zone and heating the same
therein, toï a distillation temperature under
super - atmospheric pressure, discharging the
heated mixture into a vapor separating zone and
separating the same therein under super-atmos
pheric pressure into vapors and unvaporized oil,
passing said vapors into a medial portion of a
nrst rectifying zone also maintained under super
10
atmospheric pressure, rectifying said vapors in
said rectifying zone and thereby obtaining a iirst
vapor fraction and a iirst liquid fraction, passing
at least a part of said first liquid fraction directly
from the bottom portion of the first rectiiying
zone into a medial portion oi a second rectifying
zone maintained under sub-atmospheric pressure,
passing unvaporized oil from the vapor separat
ing zone, heating it and introducing it into the
second rectifying zone at a point below that at 20
which said ñrst liquid fraction-is introduced into
`the second rectifying zone, supplying heat to the
bottom portion of the ñrst rectifying zone, subjecting the oil in each of said rectification zones
to reflux condensation and thereby separating 25
distillates from the oil, withdrawing a iight dis
tillate from the first rectiiication zone, and with
drawing heavier distillates at different elevations
from the second rectification zone.
MALCOLM P. Youm.
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