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Патент USA US2132441

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Oct. 11, 1938.
H_ ROSEN-[HAL
'l
2,13%441.
EXTRACTION OF PETROLEUM FROM SOLID MATERIALS
Filed Aug.Á 4,> 1934
l 4
ToPPlÑG UNIT
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l
2,132,441
Patented Oct. 11, 1938
~ UNITED STATES kPAT1.=;1\1'1‘ OFFICE
2,132,441
PETROLEUM FROM SOLID
EXTRACTION OFMATERIALS
'
Henry Rosenthal, New York, N. Y.
yApplication August 4, 1934, Serial No. '738,405
8 Claims.
(Cl. 19E-14) ,
gasoline as it is produced in the vapor recovery
processpior portion of the petroleum refining process.
My invention relates to ofa novel
oilfrom oil shale
the extractor proper, the solvent mixes with
and .methods of extractionboiling hydrocarbons, theInoil
shale, and during the operation the shale
utilizing as solvent lo w
are normally gaseous
'particularly those which
peratures. It
es
and
¿QS at atmospheric pressur the tem
of pe
extraction
to
is particularly related ,
troleum oil from oil shale in a continuous man
ner and in a process
where solvent is removed
from the extract as a part of
the petroleum re
ered as a
' ¿1,0 `ñrlíng, and where the solvent is recov
portion of the petroleum reñningy process.
f recovering
My invention provides means ,o
and in
petroleum oil from oil shale in a simple
oil is substantially removed, but some of the sol
vent will remain within the pores of the shale.
Where ra solventvhaving a low boiling point is
used, separation of the solvent from the shale
can easily be accomplished by applying heat to
the shale after the oil has been removed. With U10
such low boiling solvent, substantially complete ` '
-recovery of the solvent from the shale may be
eiiected. This separation of the solvent from
`the spent shale is accomplished by converting
expensive manner. Where oil shale is used as a the solvent into the vapor state. By my present 1
liquid product obtained invention, these vapors are recovered along with '
¿1,5 source oi petroleum, the
lfractionated
into a number lcondensable vapors produced in the petroleum
must be refined , and
oil can refinery, in the vapor recovery section of the
of separate products before the shale method
refinery. v
be used commercially. Thus, the usual empera
20
The objects of my invention, thus, are:
is to subject the petroleum oil to
high
`t
oil
are
vaporized
1. To provide novel apparatus for and meth
of
the
¿20 tures whereby portions
and the vapors are recovered af ter fractionation ods of separating a solvent from the extract in
the process of extracting oil from shale.
as gasoline, kerosene, gas oil and similar prod
ude ma
ucts. -The temperatures to which the cr
be either below the point
terial is subjected may
25 or above the point at which pyrolytic reactions
separation of the mate
take place prior to the
YAs a by-product of
rials into commercial cuts.
there
is produced a gas
the refining operation,
2l. To provide novel means for recovering the
solvent vapors removed from the spent shale 25
after extraction.
3. To utilize the lighter fractions of petroleum
such as
containing hydrocarbon compounds
d analogous mate
reñning as an extraction medium in the re
moval of shale oil and to circulate these frac
tiòns substantially continuously between the ex- 30
tractor and the petroleum reñnery. Other ob-`
jects of my invention are apparent from these
30 propane, butane, pentane, an
be condensed
rials of other series which lmay
a number of ways;
specifications.
into a liquid under pressure in
these hy
My invention may best be described by refer
the usual method being to ñrst absorb
th
which
they
ence to the accompanying drawing which is a 35
xed
gas
wi
drocarbons from the n s of a high boiling pe
part of this specification. In this drawing
35 are associated, by mean unds are then usually
Figure l is a diagrammatic layout of one em
troleum oil. These compo struum by means of
bodiment
of my invention.
removed from the oil men
separately from the fixed
Figure 2 is an elevation of a preferred form
»heat and are recovered
been associated. of extractor for use in connection with my in- 4o
gases with which theyof_ have
“natural gasoline” and vention.
0 This material is a form
in
Referring to Figure 1, solvent is contained
is usually further fractionated to remove small
2, through
ell as of a fraction in tank l, and is delivered to extractor
portions of ñxed gas as W minating compound.
valve
which propane is the predo
is also theThe
oil 3.shale is delivered to the4 Crusher 4, 45
Frequently in this operation
a fraction
is
the
predominating
where it is reduced to proper size, which I prefer'v
.45 obtained, in. which butane product of this “sta
shall be such that the crushed material will fall
,
"
compound. The principa
“stabilized natural gaso
through a one inch screen and will
lform
of
bilizíng” is a
bon liquid when main
line” which is a hydrocar
pressure, but
on a half inch
the oil shale passes to the screenl
tained underA superatmospheric
ospheric pressure. These properly graded and delivered to the conveyor
it is transferred to the feed hopper 1
thatv is, thebutane
thewhich
extractor 2. From the hopper, the crushed
“stabilized” natural fB,of by
cut, the propane cut, ‘orsolvent
the for removing the
cut, I use as
which it is asso
shale oil from the rock with`
natural
‘_ 55 elated, r~or I may
use` the unstabilized
oil shale is delivered through rotary valve 8 to
the sealed inlet compartment 9 of the extractor,ì55
2
'2,132,441
from which it passes through rotary valve I0
to the extraction cylinder II.
The operations within the extraction cylinder
can best be explained by referring to Figure 2.
The oil shaleV entering the cylinder from rotary
valve I0 is passed into the rotating cylindrical
compartment, I2a, by means ofthe deñector vane
rotating cylindrical compartment
meets a strong'solution about to be
discharged from the extraction cylinder il. The
rotation of the compartment I 2a carries the shale
forward and upward and discharges it into rotat
ing compartment i221, where the solution strength
is somewhat weaker than that in compartment
I2a. In a similar manner the shale is carried
reaches compartment 12d, into
solvent is delivered through the
valve 3. The shale, leaving compartment I2dv
and delivered to the compartment I2e by defiector
20
vane I3e, is substantially free from shale oil, butA
including propane, butane etc. are separated from
the liquid components. These gases with their
condensable vapors are shown as leaving the
cracking unit through the valve 35.
The solution passing through Valve 26 is de
livered to the tube-still 36 by the pump 31.
In the tube-still 36 the solution is heated and
delivered to the fractionating column 38 from
which as shown a number of side cuts are re
moved. As shown, a gasoline cut is removed
from the top of the column, passed through the
condenser 39 and delivered to the separator 40,
the gasoline being withdrawn from the bottom of
the separator through valve 4I and the vapors
and non-condensable gases including propane and
butane are Withdrawn from the separator through
valve 42.
'
The vapors and gases removed from the crack
ing unit through the valve 35 and/or removed
4from
the topping unit through the valve 42, are
will be wet with solvent besides carrying amounts
delivered to- theA vapor recovery unit 43. This 20
of solvent by absorption and similar means.
therotary cylinder I2e the spent shale is drained may be of any well known type and therefore
of its solvent and is passed by means of deflecto-r
vane I3f to the compartment I 4. The spent shale
with its absorbed solvent is passed4 from the com
partment I4 to the conveyor I5. The conveyor I5
is provided withY a heating jacket I6, into which
30
suitable heating medium is admitted through the
valve I1, and discharged through
While in the conveyor I5 the spent shale is heated
to the rotary valve I9, which discharges the spent
35 shale into the sealedV outlet compartment 20
45 to the stabilizer or column 46. The fixed gases',
dissolved in the liquid which is delivered through 30
pipe 45, are removed through pipe 41. The stabi
lized gasoline is removed from the bottom of
the column and delivered to the tank 48. Pro
butane vapors through valve 50, and delivered to 35
the condenser 5I, in which they are liquefied and
fromrwhich the liquid is delivered to tank 52.
40
" The solvent entering through the valve 3 into I
through
with the necessary absorbers, compressors, stills, 25
tanks, condensers, etc.V The liquid product com
prising propane, butane and pentane is With
drawn from the absorption unit through the pipe
pane vapors may be removed through valve 49 or
where it is subjected to a vacuum applied through
pipe 2l. This vacuum acts to eliminate the sol
the rotary compartment I2d, passes in contact
with the shale about to be discharged from the
extraction cylinder. It is then delivered consecu
45 tively to rotating cylinders I2C, I2b, and I 2a in
counterñow to the movement of the shale, and
is then discharged from the extraction cylinder
by outlet pipe 23.
Again referring to Figure 1, the spent shale is
50 ' discharged from rotary
valve 22, to conveyor 24,
whichV delivers it to any convenient location.
The solution discharged from the extractor
only sufficient detail is shown to explain the op-eration in connection with this invention. The
rectangle 44 represents the usual-absorption unit
The propane or butane may be delivered to the
solvent storage tank I by opening valve 53, or the
natural gasoline may be delivered to tank I by 40
opening valve 54.
»
The exhauster 55 is connected on its suction
side to the sealed inlet compartment 9 and re
moves therefrom solvent vapors Which enter the
compartment 9 through the rotary valve I0 and 45
the air which enters the compartment 9 through
the rotary valve 8. I prefer that exhauster 55
be so adjusted that the pressure maintained
withinY the sealed inlet compartment 9 be slight
ly above the pressure of the atmosphere. The 50
'exhauster 55 compresses the gases and vapors
55
recovery unit 43.
Exhauster 51 is connected on its suction side 55
with the sealed'outlet compartment 20. I prefer
`the ñgure, only sufficient detail being shown to
60 fully explain my invention.
The solution passing through valve 25 enters
the pump 29 which delivers it to the cracking
still 30 where it is subjected to conditions favor
able to cause pyrolytic reaction. After passing
exhauster 51 be so adjusted that it main
tains Within the outlet compartment a pressure
of less than half a' normal atmosphere.
gases and vapors removed by exhauster 51 from
the sealed outlet compartment 20 are compressed
through the cracking still, the solution is delivered
to the reaction chamber 3l and the dephlegmator
32, where a portion is condensed and is recircu
lated through the cracking still 30 by the pump
34. The vapors from the dephlegmator 32 pass
70 into the rectification portion of the cracking unit
as represented by the rectangle 33. This rectangle
here represents the various fractionating col
umns, condensers, storage tanks
paratus making up the balance of the cracking
‘is unit,
including the separator in which the gases
the cracking unit and/or the topping unit.
65
Many changes may be made in the details of
my invention Without departing from thespirit
of my invention, and I do not limit myself to the
particular forms shown.
Having described my'invention so that it may 70
be readily understood by one skilled in the art,
I claim:
'
1. The method of extracting oil-shale which
comprises dissolving'shale-oil in a hydrocarbonî‘n;
3
2,132,441
liquid that is gaseous at normal temperatures
and pressure by contacting the oil-shale with
said hydrocarbon delivered and applied
to» said
is in the liquid
' oil shale while said hydrocarbon
phase, maintaining said hydrocarbon in the liq
uid phase while in contact with said oil-shale;
withdrawing the solution; subjecting the solu
tion,while said solution still contains- substantial
amounts of the solvent, to the action of heat at
such temperature that pyrolytic reactions take
while said hydrocarbon is in the liquid phase,
maintaining said hydrocarbon in the liquid phase
while in contact with said petroleum bearing solid
material; withdrawing the solution; subjecting
the solution, while said solution still contains
substantial amounts of the solvent, to the action
of heat at such temperature that pyrolytic re
actions takey place; then separating the solution
into fractions, including one fraction of the char
acter of the solvent used; and returning a por
tion of said fraction to the dissolving step.
6. The method of extracting petroleum bear
ing solid material which comprises, dissolvinga
portion of the petroleum in “natural gasoline” 15
by contacting the petroleum bearing solid ma
2. The method of extracting oil-shale which terial with "natural gasoline” delivered and ap
plied to said petroleum bearing solid material
comprises, dissolving shale-oil in “natural gaso
line” by contacting the cil-shale with “natural while maintained in the liquid phase, maintain
gasoline” delivered and applied to said oil shale ing said-“natural gasoline” in the liquid phase, 20
while maintained in liquid phase, maintaining while in contact with said petroleum bearing solid
said “natural gasoline” in the liquidphase while material; withdrawing the solution, then sub
in contact with said oil-shale; withdrawing the jecting the solution, while it still contains a sub
10 place; then separating the solution into fractions,
including one fraction of the character of the
solvent used; and returning a portion of said
fraction to the dissolving step.
stantial amount of said solvent, to the action
of heat at such temperature that pyrolytic re
actions take place; then separating the solution
into' fractions including one fraction analogous
and returning a por-y
to said “natural gasoline”;
tion of said “latter” fraction to the dissolving
step.
'7. The method of extracting petroleum bearing 30
solid material which comprises dissolving a por
30 comprises dissolving Vshale-oil by contacting said tion of the petroleum by contacting said petro
oil-shale with “butane” delivered and applied to leum bearing solid material with “butane” de
said oil shale while maintained in the liquid livered and applied to said petroleum bearing 35
phase, maintaining said “butane” in the liquid solid material while maintained in the liquid
phase, maintaining said “butane” in the liquid
phase while in contact with said oil-shale; with
phase while in contact with said petroleum bear
drawing the solution; then subjecting the solu
tion, while it still contains a substantial amount ing 'solid material; withdrawing the solution;
then subjecting the solution, while it still con
of butane, to the action of heat at such tempera
tains a substantial amount of butane, to the ac 40
ture that pyrolytic reactions take place; then sep
arating the solution into fractions, including one tion of heat at s-uch temperature that pyrolytic
40 fraction of "butane”; and returning a portion
reactions take place; then separating the solu
of said “butane” fraction to the dissolving step. tion into fractions, including one fraction of
4. The method of extracting oil-shale which “butane”; and returning a portion of said “bu
45
comprises dissolving shale-oil by contacting said tane” fraction to the dissolving step.
8.
The
method
of
extracting
petroleum
bearing
oil-shale with “propane” delivered and applied
to said oil shale while maintained in the liquid solid material which comprises dissolving a por
phase, maintaining said “propane” in the liquid tion of the petroleum by contacting said petro
leum bearing solid material with “propane” de
phase while in contact with said oil-shale; with
livered and applied to said petroleum bearing 50
drawing the solution; then subjecting the solu
tion, while it still contains a substantial amount solid material While maintained in the liquid
of said “propane”, to the action of heat at such phase, maintaining said “propane” in the liquid
temperature that pyrolytic reactions take place; phase while in contact with said petroleum bear
ing solid material; withdrawing the solution;
then separating the solution into fractions in
then subjecting the solution, While it still con 55
cluding one fraction of “propane”; and return
ing a portion of said “propane” fraction to the tains a substantial amount of said “propane”, to
the action of heat at such temperature that pyro
dissolving step.
5. The mtehod of extracting petroleum bearing lytic reactions take place; then separating the
solution into fractions including one fraction of
solid material which comprises dissolving a por
tion of the petroleum in a hydrocarbon liquid “propane”; and returning a portion of said “pro 60
that is gaseous at normal temperatures and pres
pane” fraction to the dissolving step.
(Si) sure by contacting the petroleum bearing solid
solution, then subjecting the solution, while it
still contains a substantial amount of said sol
vent, to the action of heat at such temperature
that pyrolytic reactions take place; then sep
arating the solution into fractions including one
fraction analogous to said “natural gasoline”;
and returning a portion of said “latter" fraction
to the dissolving step.
3. The method of extracting oil-shale which
material with said hydrocarbon delivered and
applied to said petroleum bearing solid material
HENRY ROSENTHAL.
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