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Патент USA US2132108

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Patented Oct. 4, 1938
2,132,108
UNITED STATES
PATENT OFFICE
2,132,108
D'EWAXING PETROLEUM OILS
Eugene C. Herthel, Flossmoor, IlL, assignor'to
Sinclair Re?ning Company, New York, N. Y., a
corporation of Maine
No Drawing. Application July 5, 1934,
Serial No. 733,857
9 Claims.
This invention relates to improvements in the
dewaxing of hydrocarbon oils, more particularly
to the dewaxing of petroleum stocks in the manu
facture of lubricating oils. The invention relates
particularly to improvements in the diluents de
scribed in an application of Edward J. Martin ?led
February 21, 1934, Serial Number 712,412. The
(Cl. 196—18)
without necessarily involving prejudice to the
ei?ciency of the dewaxing operation and without
necessarily involving sacri?ce of the advantages
of the high boiling ester diluents.
The following examples of operations embody
ing the use of composite diluents of this invention
will further illustrate the invention:
invention is also useful in connection with the
Example 1.—A Mid-Continent overhead long
diluents described in my application ?led July
10 5, 1934, Serial Number 733,858 now Patent
residuum having a viscosity of 120 seconds at
2,056,723.
The diluents described in application Serial
Number 712,412 comprise the ethyl esters and
mixtures of ethyl esters higher boiling than acetic
15 ethyl ester including the valeric ethyl esters, pro
pionic ethyl esters and butyric ethyl esters, and
ethyl esters and mixtures of ethyl esters boiling
within the range 185°-315° F.
In accordance with this invention, these high
20 boiling ethyl ester diluents are used in conjunc
tion with hydrocarbon diluents, of boiling range
lower than that of the oil to be dewaxed, such as
benzol, mixtures of benzol and toluol, mixtures
of benzol and petroleum naphtha and mixtures of
25 toluol and petroleum naphtha for example. If, in
the absence of propionic ethyl ester, the propor
tion of ethyl esters higher boiling than propionic
ethyl ester is limited to about 25% of the com
posite diluent as a minimum, or if the proportion
30 of ethyl esters higher boiling than propionic ethyl
ester is limited to about 7.5% of the composite
diluent as a minimum, propionic ethyl ester being
present in proportion limited to about 17.5% of
the composite diluent as a minimum, a given
35 volume of the composite diluent is usually about
as effective as the same volume of the high boil
ing ethyl esters.
210° F. is diluted with 300% of its own Volume
of a composite diluent consisting of 1 part (by
volume) of a mixture of ethyl esters boiling within
the range 185°—315° F. and including about 70%
(by volume) of propionic ethyl ester, the bal- ‘
ance being principally iso valeric ethyl ester, and ' 15.
3 parts of benzol, the mixture is chilled to —14° F.,
about 16.4% of precipitated wax having a melting
point of about 126° F. is separated from the ?uid
stock mixture by ?ltration, and the composite
diluent is steam distilled from the ?uid stock 20
mixture to produce a dewaxed oil having a pour
test of 4° F.
Example 2._A Mid-Continent overhead long
residuum having a viscosity of 120 seconds at
210° F. is diluted with 300% of its own volume of
a composite diluent consisting of 1 part (by
volume) of a mixture of ethyl esters boiling
within the range 185°~315° F. and including about _
70% (by volume) of propionic ethyl ester, the
balance being principally iso valeric ethyl ester, 30
and 3 parts of a blend of 20% toluol and 80% ben
zol, the mixture is chilled to —10° F., about 8.0%
of precipitated wax having a melting point of
about 137° F. is separated from the ?uid stock
mixture by ?ltration, and the composite diluent
is steam distilled from the ?uid stock mixture
to produce a dewaxed oil having a pour test of
The invention is similarly useful in conjunc
16° F.
,
.
tion with the high boiling alkyl ester diluents,
Example 3.—A Mid-Continent overhead long
40 other than the high boiling ethyl ester diluents, ‘ residuum having a viscosity of 120 seconds at
including normal butyl valerate, isopropyl Valer
210° F. is diluted with 300% of its own volume of
ate, normal propyl valerate, and secondary butyl a composite diluent consisting of 1 part (by
valerate, normal butyl butyrate, normal butyl volume) of a mixture of ethyl esters boiling
caproate, normal butyl propionate, iso butyl Within the range 185°—315° F. and including about
45 butyrate, iso butyl iso butyrate, iso butyl pro
70% (by volume) of propionic ethyl ester, the
pionate, iso butyl valerate, propyl butyrate, propyl balance being principally iso valeric ethyl ester,
iso butyrate, propyl propionate and propyl iso and 3 parts of a blend of 50% toluol and 50%
valerate, described in application Serial Number petroleum naphtha, the mixture is chilled to
733,858.
_14° F., about 5.6% of precipitated wax having‘
50
Since these high boiling esters are more costly a melting point of about 143° F. is separated from
than the hydrocarbon diluent component of the the ?uid stock mixture by ?ltration, and the com
composite diluent of this invention, this invention posite diluent is steam distilled from the ?uid
makes possible important economies with respect stock mixture to produce a dewaxed oil having a
to the cost of the total volume of diluent required pour test of 16° F.
55 to carry out any particular dewaxing operation
Example 4-.—A Mid-Continent overhead long 55
72,132,108
residuum having a viscosity of 120 seconds at
210° F. is diluted with 300% of its own volume
of a composite diluent consisting of 1 part (by
volume) of a mixture of ethyl esters boiling within
Example 9.—A' Mid-Continent paraffin distil
late having a viscosity of 87 seconds at 100° F.
is diluted with 300% of its own volume of a com
posite diluent consisting of 1 part (by volume) of
_ the range 185°-315° F. and including about 70%
a mixture of ethyl esters'boiling within the range
(by volume) of propionic ethyl ester, the balance
being principally iso valeric ethyl ester, and 3
parts of a blend of 50% benzol and 570% petro
185°-3l5° F. and including about 70% (by vol
ume) of propionic ethyl ester, the balance being
principally iso valeric'ethyl ester, and 1 part of a
blend of 35% acetone, 52% benZo-l and 13%
10
10 about 11.0% of precipitated wax having a melt; toluol, the mixture is chilled to —10° F., about‘
ing point of about 126° F. is separated from the" 14.8% of precipitated wax having a melting point
of about 110°VF. is separated from the ?uid stock
?uid stock mixture by ?ltration; and the com
posite diluent is steam distilled from the fluid mixture by ?ltration and the composite diluent is.
stock mixture to produce a dewaxed oil having ‘a steam distilled from the fluid stoclsniixture to
leum naphtha, the mixture is chilled to~-—15° F., .
pour test of 12° F.
15
r
'
Example '5.—A'Mid-Continent paraffin distil- 1
late having a viscosity of 87 secondsat 100° F. is
diluted with 300% or" its own volume of a com
posite diluent consisting of 1 part (by volume) of
20 a mixture of ethyl esters higher boiling than
propionic. ethyl ester and consisting essentially
produce a dewaxed oil having a pour test of 4° F.
Example 10.-A Mid-Continent overhead long
residuum having a viscosity of 120 seconds at 210°
'F. is diluted with 300% of its own volume of a
composite diluent consisting of 1 part (by vol
ume) of a mixture of ethyl esters boiling 'within 20
the range 185°-315° F. and including about 7.0%
(by volume) of propionic ethyl ester, the balance
being principally iso valeric ethyl ester, and 3
parts of a blend of 50% benzol and 50% petrol
of iso ‘Valerie ethyl‘, ester, and 3 parts of a blend
of 50% benzol and 50% petroleum naphtha, the
mixture is clilied to -—15°
about 9.9% of pre
eum naphtha, the mixture is chilled to —20° F., 25
25 cipitated wax having a melting point of about
117.5° F. is separated from the fluid stock mix a about 7.15% of precipitated wax having a melt
ture of ?ltration, and the composite diluent is ing point of about 137° F. is separated from the
steam distilled from the?uid stock mixture to ?uid stock mixture by ?ltration, and the com
produce a dewaxed oil having a pour test of 16° F. posite diluent is steam distilled from the ?uid
stock mixture to produce a dewaxed oil, having a
307 ' Example 6.-—A Mid-Continent paramn distil
late having a viscosity of 87 seconds at 100° F. is pour test of 4° F. This dewaxed oil is treated
with 30 pounds per barrel of 66° Be. sulfuric acid
diluted with 300% of its own volume of a com
and thereafter with 25% (by weight) of fuller’s
posite diluent consisting of 1 part (by volume)
of a mixture ‘of ethyl esters boiling within the earth (Olmstead) at500° F., as in conventional
35? range 185°-°15° F. and including about 70% (by practice, to produce a treated, dewaxed oil having as"
volume) of propionic ethyl ester, the balance be
ing principally iso valeric ethyl ester, and 3 parts
of a blend of 20% acetone and 80% benzol, the
mixture is chilled to' —10° F., about 16.42% of pre
40.: cipitated wax'having a melting point of about
' 106° F. is separated from'the ?uid stock mixture
by ?ltration, and the composite diluent is steam'
distilled from the ?uid stool: mixture to produce
a dewaxed oil having a pour test of 2° F.
a pour test of 0° F.
Y
‘
Example 11.-—A Mid-Continentoverhead long
residuum having a viscosity of 120 secondsat
210° F. is diluted with 300% of its own volume
of a composite diluent consisting of l-part (by 40E
volume) of a mixture of ethyl esters boiling
within the range 185°—315° F. and including
about 70% (by volume) of propionic ethyl ester,
the balance being principally iso valeric ethyl
Escample 7.—A Mid-Continent'para?ln distil- ' ester, and '3'parts of a blend of 25% toluol and,
45
late having’ a viscosity of 87 seconds at 100° F. is 7.5% benzol, the mixture is chilled to =—20° F.,'
diluted with~300% of its own volume of 'a com-v
posite diluent consisting of 1 part (by volume) of
55:
ume) of prop-ionic ethyl ester, the balance being
?uid stock mixture to produce a dewaxed voil
principally iso valeric ethyl. ester, and 3 parts of '
a blend 7 of 50% benzol and 50% petroleum
having a pour test of 4° F. This dewaxed voil is
treated with 30 pounds per barrel of 66° Be. sul-_ ,
naphtha, the mixture is chilled to —10°' F.,,about
16.2% of precipitated wax having a melting point
of about 109° F.'is separated from the fluid stock
mixture by ?ltration and the composite diluent
is steam distilled from the ?uid stock .mixture
conventional practice, to produce a treated .de
to produce a dewaxed oil having a pour test of
60,
ing point of about 13li.5° F. is separated from
a mixture of ethyl esters boiling within the range r the ?uid stock mixture by ?ltration, and the
composite diluent‘ is steam distilled from the 50"
185°~315° F. and including about 70% (by vol
750
'
about 8.75% of precipitated wax having a melt
4° F.
‘
phuric acid and thereafter with 25% (by weight)
of'iuller’s earth (Olmstead) at 500° F.,Vas in
waxed oil having a pour test of 0° F.
*
As used herein, the term “pour test”'is the
lowest temperature at which the oil will; ?ow,
'when chilled without disturbance, determined,
is diluted with 300% of its own volume of a com
for example, in accordance with method D97-30
of the American Society for Testing Materials.
viscosities herein are viscosities in Saybo1t'Uni-
posite diluent consisting of 1 part (by volume) of
versal.
Example 8.-A Mid-Continent paraffin distil
late having a viscosity of 87 seconds at 100° F.
a mixture of ethyl esters boiling within the range
'185°-315° F. and including about 70% (by vol
. ume) of propionic ethyl ester, the balance being
principally iso valeric ethyl ester, and 3 partsof
a blend of 20% toluol and 80%’ benzol, the mix—
70 .ture is chilled to —l0° F., about 12.2% of precip~
itated wax having a melting point of about 112.5°
F. isseparated from the?uid stock mixture by
?ltration and the composite diluent is steam dis
' tilled from the ?uid stock mixture to produce a
75 dewaxed oil having a pour test of 10° F. .
551 V
‘
.
I claim:
1. In the dewaxing of petroleum oils, the’ im—.
provement which comprises diluting the oil with
a composite diluent comprising 'a high boiling
.alkyl ester boiling within the range 185°-3l5° F.,'
said ester being miscible with the oil to be de 70- '2
waxed, and a major proportion of a volatile hy-.
drocarbon diluent of boiling range lower than
that of the oil to be dewaxed.
.
\
2. In thefdewaxing of petroleum oils, the im
provement which comprises diluting the oil with 7511:
3
2,132,108
a composite diluent comprising an ethyl ester
boiling within the range 185°-3l5° F., said es
ter being miscible with the oil to be dewaXed,
and a major proportion of a volatile hydrocarbon
diluent of boiling range lower than that of the
oil to be dewaxed.
_
3. In the dewaxing of petroleum oils, the im
provement which comprises diluting the oil with
a composite diluent comprising an ethyl ester
10
higher boiling than propionic' ethyl ester, pro
pionic ethyl ester and a major proportion of a
volatile hydrocarbon diluent of boiling range
lower than that of the oil to be dewaxed.
4. In the dewaxing of petroleum oils, the im
15 provement which comprises diluting the oil with
a composite diluent comprising a mixture of
ethyl esters boiling within the range 185°-315° F.,
said ester being miscible with the oil to be de
waxed, and a major proportion of a volatile hy
20 drocarbon diluent of boiling range lower than
that of the oil to be dewaxed.
-
5. In the dewaxing of petroleum oils, the im
provement which comprises diluting the oil with
a composite diluent comprising a mixture of
25 ethyl esters higher boiling than propionic ethyl
ester, propionic ethyl ester and a major propor
tion of a volatile hydrocarbon diluent of boiling
range lower than that of the oil to be dewaxe'd.
6. In the dewaxing of petroleum oils, the im
provement which comprises diluting the oil with
a composite diluent comprising a Valerie alkyl
ester and a major proportion of a volatile hydro
carbon diluent of boiling range lower than that
of the oil to be dewaxed.
7. In the dewaxing of petroleum oils, the im
provement which comprises diluting the oil with
a ‘composite diluent comprising a Valerie ethyl
ester, propionic ethyl ester and a major'pro
portion of a volatile hydrocarbon diluent of boil
ing range lower than that of the oil to be de
waxed.
8. In the dewaxing of petroleum oils, ‘the im
provement which comprises diluting the oil with 15
a composite diluent comprising a butyric alkyl
ester and a major proportion of a hydrocarbon
diluent of boiling range lower than that of the
‘oil to be dewaxed.
9. In the dewaxing of petroleum oils, the im 20 Y
provement which comprises diluting the oil with
a composite diluent comprising a propionic alkyl
ester, said ester being miscible with the oil to
be dewaxed, anda major proportion of a volatile
hydrocarbon diluent of boiling range lower than 25
that of the oil to be dewaxed.
EUGENE C. HERTHEL.
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