close

Вход

Забыли?

вход по аккаунту

?

Патент USA US2500757

код для вставки
March 14.. 1950
w. KlERsTED, JR
REMOVAL 0F ASPHALTIC CONSTITUENTS
FROM HYDRÜCARBON OIL
Filed Maren 12, 1947
2,500,757
0,1/9,
'2,500,757
Patented Mar. 14, 1950
UNITED STATES „PATE/N
2,500,757
REMOVAL '0F ASI’HALTICl CONSTITUENTS.
FROM`~HYDROCARBON OIL
WynkoolnKiersted;> Jr., Scarsdale,~N; Y., assigner ' ' f
to
N. Texaco
.Y.,ya corporationcf
Development‘Corporation,
Delaware '
New-York;~ y
Application'v March l2, 1947, Serial No. 734,[email protected] i ‘
4 Claims.
1 »
(01.119.6--130' '
.
This invention relatesi to a `method ofremov
increasing lthe concentration :o‘fithis-lresinouslma
ing asphaltic and resinous. `constituents-.from
terial in the feed oil in this manner by >as‘much
as 200 to 300%. In this way' it isfoundthat .more
hydrocarbon oil and .morefpartìcularly¿to„,the
removal of such constituents from mineral lubri
cating oil stocks.
The invention broadly contemplatesa:contin-` o
’ uous countercurrent -m'ethod ofv removing as
phaltio and resinous or hard and soft asphaltic
constituents from hydrocarbon oil by extraction
in a series of separate stages .with a solvent liquid 10
adapted to precipitate asphaltic»constituentsffrom ,
eifective . and rapid ‘ precipitation . ioff, rasph'altic
material is secured-withthe.result.ithatßthefch'arge
rate to a given yplant mayfbe :increased:bywasy
-much as 50% for V.thesamequantity of circulat
ing solvent.' In ‘otherJ words vthensolvent''Jdosage
may be decreasedfby from' 2001a-100%". i ‘ `1
Another feature of the invention .involvesnr‘e
cycling of some deasphaltedfloilrto«thezirritial or
preceding stage of 'the series?l The amounttso
Y
recycled is correlated with theïftemperaturesmain
The invention has application to thedeasphalt
tained in the.initialJstageïparticularly’whenusing
ing of mineral lubricating oil stocks with asol
vent comprising liquiiied normally gaseous hydro 15 a Aliquiiied normally gaseous»hyd-rocarbonpzln
order to maintainsuch a solvent liquiiied atïaele
carbons such as propane, .butana'ormixtures
the oil.
vated temperatures, -. substantial!A pressure - :is »re
thereof.
quired which necessitates the employmentvièof
In -accordance ‘with the invention, «the treat
heavy’equipment. t
ment of the feed oil is eñ‘ected during passage
The higher 4the temperatura-¿the moref‘insol
through a series of settling and'separating-'stages 20
uble the resinous >material.-.„,1t ‘.appears,»=x'howarranged in series. The fresh feed oil is intro
ever, that effective ‘resin VseparationScan-abe.se
duced to an intermediate vstage of: the' series
cured at somewhat lower"temperaturesabyk the
wherein it is subjected to contact with the solvent
addition cf. some deasphalted f'oil=:f:to:~.the=: resin
in suitable proportions and at a suitable tempera
ture level so as to effect separation into a lpri 25 separating stage.` The fadditionfiofnthis:oil'has
the eñîect of v'displacing¿more io'f lthe relatively
mary asphalt phase and a-primary oilfsolution
phase. The resultingprimary Iasphaltçphase‘gis n insoluble material, :i. e;„resinousfmaterialf¿from
the oil solution. Theamountloffrecycle oil-may
removed and conducted'tovonezor more succeed
. _ range from about ,10i to l25% ¿ofithe'primaryfphase
ing stages in the series wherein- itzis subjected
to contact with additional 's_olventfliquid at some 30 oilentering the 'resinl separatingtstage. > Iniorder
lto describe the vmethod. of.` ñowrintmoreydetail,
what lower temperatures yso` as to effec-t «separa
reference will now bewmad'e @tot-àtheffiaccompany
tion of retained oil from thefasphalticv and ,res
ing drawing.
inous material. The asphaltand‘resinous mate
As indicated in the., drawing;ir az'series‘fof/.rsepa
rial mixed with some solvent is discharged -from
theiinal stage> of the -series l‘while `oil solution 35 rating .stages designated- byY the‘fnumeralsvzl ,12,
3 and 4, respectively, may .be employedrfxThese
removed from the succeeding-stage orrstages is
stages are merely `,represented-,in îdiagrammatic
recycled to the aforesaid intermediatestage.
form, and _any L suitable design fmaypbe ¿employed
The primary oil-phase removed -from the inter
which rpermits adequate -miXing¿»L.-between: isol
mediate stage retains a vsubstantial amount of
resinous or soft asphaltic material and this phase 40 vent and -oil and separation lof resulting'phases.
Moreover, -additional stages may-abe providedal
is conducted to a preceding or initial stage in the
though at least three stagesar‘e‘essential.
series maintained at a more elevated temperature
An asphalt bearing charge» ioil suchrfas t residual
such that retained resinousmaterialprecipitates
cylinder stock derived -from Mid-Continent'crude
from the solvent solution of oil. The precipitated
material is conducted from the preceding stage 45 is conducted from a source'notfshownfthrough a
pipe 5 and a-pipe-(ìA to theintermediatefstage :2.
A stream of solvent liquid, i. 'ef-propane .or/a
sulting deasphalted oil solution is .separately
propane fractiondrawnffrom astorage l,tank 8
withdrawn from the preceding stage and :passes
through pipes 9 and l0 is conducted v:through a
to a stripping unit for recoveryl of -solvent liquid.
A feature of the invention thus involves con 50 branch pipe l! and thusfinjectedgintothe charge
ducting precipitated resinous-material from the - roil stream flowing throughthe pipe» 6. AInr` this
way eifective mixing between charge oil-andsol
initialstage to the intermediate ~.stage so as to
vent is effected. The ysolvent mayy be injected
increase substantially the concentrationvof this
in the proportion of about .5 to 9fvolumesïoffso1
resinous or soft asphaltic material in the feed
oil undergoing initial treatmentvwith >the solvent 55. vent per volumeof *charge-„oil .,
The mixture of t feedioil Sandi solvent yflows» into
in the intermediate stage. j.It is contemplated»y
to the'aforesaid intermediate stage While the re
2,500,757
3
stage 2 wherein separation into phases occurs,
the temperature being maintained within the
resinous material from the oil.
range of about 135 to 155° F. and usually at
about 145 to 150° F. Under such conditions, a
volumes of resinous material and solvent is drawn
primary asphalt phase is formed comprising as
phalt 'and resins mixed with a minor proportion
of the,` solvent and some oil, and a primary oil
phase comprising oil and resinous material or
- soft asphalt dissolved in the major portion of the
stage I, and thus aid in the precipitation of
The resin precipitate comprising about equal
5
olf through a pipe 4D, exchanger 4l and pipe 42
connecting with the previously mentioned pipe 6
through which it is conducted to stage 2. The
exchanger 4I may be by-passed all or in part if
desired by a pipe 43.
solvent.
The resin precipitate flowing through pipe 40
10
The primary asphalt phase comprising about
is added to the charge oil mixture passing to
equal parts of asphalt and propane is drawn 01T
in a continuous stream through a pipe I2 and
stage 2 so as to aid in obtaining more effective
and rapid precipitation of asphalt and resin from
conducted to the succeedingl stage 3. Additional
the oil.
solvent drawn from the pipe I0 through a branch 15
By way of example, when treating a residual
pipe I3 is injected in the stream flowing through
cylinder stock derived from Mid-Continent crude,
the pipe I2. Solvent equivalent to about 25%
characterized by having an A. P. I. gravity of 2l,
of the total solvent required for the treating
Saybolt Universal viscosity of 220 seconds at 210°
operation is thus added to provide a mixture of
F. and a carbon residue content of 5.2%, a de
- about 10 to 20,or more volumes of solvent for each 20 asphalted and de-resined lubricating oil stock
volume of asphalt.
»
f
.
The stage 3 is maintained at a temperature in
the range of 125 to .135° F., so that further sep
aration between oil and asphalt occurs. The
amounting to at least 90% of the charge oil is
obtained, employing conditions of temperature
and solvent dosage previously indicated.- The
lubricating stock so obtained has an A. P'. I. grav
separated oil Vis continuously withdrawn through 25 ity of about 24.2, a carbon residue content of about
a pipe I6 and recycled to stage 2 as indicated,
1.50, and a color of about 11/8 Tag-Robinson, or
the recycled oil advantageously being commingled
higher.
with the stream of oil and solvent flowing through
By contrast, when treating the same type of
feed oil under similar conditions of temperature
The partially -deoiled asphalt'phase formed in 30 and increased solvent dosage but without re
stage 3 is continuously drawn off through a pipe
cycling the resin precipitate from stage I and
I1 to stage 4„»addition'al solvent equivalent to
resin bearing streams of solvent from stages 3
about 50% kof the total solvent required for the
and 4 to stage 2, only about 83% of de-asphalted
treating operation being added through branch
and de-resined oil of substantially the same qual
the’pipe 6.
M.
,
d
,v
- pipey I 8y so as toprovide a mixture of about 20 35 ity is obtained. In this latter case, the resin
to 40 volumes of solvent for each volume of
precipitate is merely washed with additional sol
.
vent in a separate stage, for example, stage 4,
while the asphalt stream from the preceding
about 120 to 130° F. or suii‘icient to effect sub
stage 3 is passed directly to a solvent recovery
stantially complete removal of retained oil from 40 unit.
the asphalt and resinous material.
While the employment of elevated pressures
As in the case of the preceding stage, retained
has not been referred to specifically in describing
oil separated in stage .4v is continuously with
the process, nevertheless, it is contemplated that
drawn through a 'pipev I9 and then recycled
suiiicient pressure is employed in the system to
through pipe I2 and stage 3 to stage 2.
or. Ul maintain substantially liquid phase conditions
asphalt.`
Stage 4 is maintained ata temperature or
The resulting asphalt and resin mixture froml
throughout the successive stages.
'
which retainedl oil has been removed in stage 14
Also, while mention has been made of using a
is continuously discharged through a pipe 20 to a
liquiñed normally gaseous hydrocarbon as the
solvent, it is contemplated that other de-asphalt
stripper 2| wherein solvent is recovered from
the asphalt and resin material. The recovered
solvent is returned through a pipe 22 to the afore
said storage tank, 8.
The primary oil'phase accumulating ln stage 2
. is continuously removed through a pipe 30 and
conducted to a pipe 3| and a heater or heat .
' exchanger 32, wherein it is raised to a tempera
ture of about 160° F. The resulting heated mix
ture of oil resin and solvent is introduced to stage
Iwhich is maintained at a temperature in the
ing solvents or agents may be employed as for
examp1e,aliphatic alcohols such as propyl, iso
propyl, butyl, or isobutyl alcohols, mixtures
thereof, etc.
"
It is contemplated that the invention has ap
plication to the treatment of other than mineral
type oils for the purpose of effecting separa
tion of resinous or higher molecular weight con
stituents. It may be applied to the treatment
of fatty type oils derived from vegetable and
> rangeof 155 to 165° F., and usually at about 160°
F., so that precipitation of resins from the oil
solution occurs. If desired, some additional sol
animal sources.
- not be required.
pended claims.
l
Obviously many modifications and variations
of the invention, as hereinbefore set forth, may be
vent maybe added from the pipe I0 through a
made without departing from the spirit and scope
branch -pipe 33. However, it is contemplated
thereof,y and therefore only such limitations
that in the usual case,` additional solvent will 65 should be imposed as are indicated in the ap
The resulting deresiniñed oil solution is con
tinuously removed through a pipe 34 and con
I claim:
1. A continuous method of separating as
‘phaltic and resinous constituents from residual
ducted to a stripper 35, wherein the solvent is
recovered from the deasphalted and deresined oil. 70 lubricating oil stock containing both asphalt and
The recovered solvent may be returned through
resin in substantial amounts by treatment with
' pipe 22 to the storage tank 8.
a liquefied normally gaseous petroleum C3 and
A small portion of the de-asphalted and de
higher hydrocarbon solvent in a series of stages,
resined ~oil may »be recycled to pipe 3| for com
which comprises passing a stream of feed oil
V'mingling with’the primary oil phase passage to 75 mixed with from about 5 to 9 volumes of said
2,500,757
6
liquefied solvent per volume of feed oil to the
second stage in said series, said stage being
maintained at a temperature of about 135 to 155°
F., effecting separation therein into two primary
liquid phases, one of said phases comprising an
asphalt phase and the other comprising an oil
solvent phase retaining resinous material, sepa
ond stage in said series, said stage being main
tained at a temperature of about 135 to 155° F.,
effecting separation therein into two primary
liquid phases, one of said phases comprising an
asphalt phase and the other comprising an oil
solvent phase retaining resinous material, sepa
rately withdrawing said primary phases, passing
withdrawn primary oil-solvent phase to the pre
rately withdrawing said primary phases, passing
ceding stage, subjecting said primary oil-solvent
withdrawn primary oil-solvent phase to the pre
ceding stage, subjecting said primary oil-solvent 10 phase to settling therein at a temperature of
about 155 to 165° F. such that retained resinous
phase to settling therein at a temperature of
material precipitates therefrom leaving substan
about 155 to 165° F. such that retained resinous
tially deasphalted and deresined oil, discharging
material precipitates therefrom leaving substan
resulting deasphalted and deresined oil from said
tially deasphalted and deresined oil, discharging
resulting deasphalted and deresined oil from said 15 preceding stage, injecting said precipitated res
ins into said stream of feed oil passing to said
preceding stage, injecting said precipitated res
second stage in amount sufficient to increase the
ins into said stream of feed oil passing to said
concentration of resins in said feed stream by
second stage in amount sui‘licient to increase the
about 200 to 300%, passing said primary asphalt
concentration of resins into said feed stream by
phase mixed with solvent in the proportion of
about 200 to 300%, passing said primary asphalt
about 10 to 20 volumes per volume of asphalt to
phase mixed with solvent in the proportion of
the third stage of the series maintained at a
about 10 to 20 volumes per volume of asphalt to
temperature of about 125 to 135° F. such that
the third stage of the series maintained at a
further separation into oil and asphalt phases
temperature of about 125 to 135° F. such that
further separation into oil and asphalt phases 25 occurs, separately withdrawing third stage oil
and asphalt phases respectively, recycling with
occurs, separately withdrawing third stage oil
drawn third stage oil to said second stage, pass
and asphalt phases respectively, recycling with
ing withdrawn third stage asphalt to a final
drawn third stage oil to said second stage, pass
stage, subjecting it to contact in said final stage
ing withdrawn third stage asphalt to a final
with about 20 to 40 volumes of solvent per volume
30
stage, subjecting it to contact in said final stage
of asphalt at a temperature of about 120 to 130°
with about 20 to 40 volumes of solvent per vol
F. thereby effecting substantially complete de
ume of asphalt at a temperature of about 120
oiling of asphaltic and resinous material, dis
to 130° F. thereby effecting substantially com
charging resulting deoiled material, and recy
plete deoiling of asphaltic and resinous material,
cling resulting oil solution from said final stage
discharging resulting deoiled material, and re 35 to
said third stage.
cycling resulting oìl solution from said final
4. The method according to claim 3 in which
stage to said third stage.
a small portion of the deasphalted and deresined
2. The method according to claim 1 in which,
cylinder stock is recycled to said preceding stage.
a small portion of deasphalted and deresined oil
WYNKOOP KIERSTED, JR.
40
is recycled to said preceding stage.
3. A continuous method of separating as
REFERENCES CITED
phaltic and resinous constituents from residual
`
The
following
references are of record in the
cylinder stock derived from Mid-Continent crude
ñle of this patent:
containing both asphalt and resins in substantial
amounts by treatment with a solvent compris 45
UNITED STATES PATENTS
ing essentially liquefied propane in a series of
Number
Name
Date
stages thereby obtaining a lubricating oil stock
2,143,872
Forrest et al. ____ __ Jan. 17, 1939
having a Tag-Robinson color of 11A; and higher
2,143,882
Keith et al. ______ __ Jan. 17, 1939
which comprises passing a stream of said cylin
Lewis ___________ __ May 26, 1942
der stock feed oil with from about 5 to 9 volumes 50 2,284,583
2,367,671
Dickinson et al. -..__ Jan. 23, 1945
of said solvent per volume of feed oil to the sec
w
Документ
Категория
Без категории
Просмотров
0
Размер файла
499 Кб
Теги
1/--страниц
Пожаловаться на содержимое документа