Grease

Patented Aug.
14, 1951
2,564,561
UNITED STATES PATENT OFFICE

2,564,561
GREASE COMPOSITION
Emmett S. Carmichael and Eldon L. Armstrong,

Jackson Heights, N. Y., assignors to Socony
Vacuum Oil Company, Incorporated, a corpo
ration of New York
'No Drawing. Application May 20, 1944,

Serial No. 536,604
10 Claims. ( Cl. 25240.5)
This invention is directed to improvements in

barium base greases, that is, to grease composi
tions consisting basically of mineral oils in ad
mixture with barium soaps of fatty acids or with
a su?icient proportion of such barium soaps
present to give to the greases the characteristics

usually recognized as attributable to barium base
greases. Such barium base greases are, in gen
eral, excellent greases and may be used suc
cessfully for a number of applications, such as
for example, for chassis, water pumps, motor

bearing and wheel bearing applications under
both high and low temperature conditions and
at high or low rates of shear.
These greases, however, like many other
greases, are not too stable in their ordinary
form at temperatures near or above the normal
boiling point of water.

This invention has for its object the provision
of novel and improved barium base greases char
acterized by high stabilities at temperatures well
above those temperatures at which the normal
types of barium base greases become highly un
stable.
Various tests exist for measuring the stability
of greases under high temperature conditions.
2
friction Bearing Manufacturers Association.
This machine has been developed to study the
structural stability of greases when agitated
in a working ball bearing under speci?ed condi
, tions at known temperatures. Essentially, it is
a ball bearing assembly operated at 3450 R. P. M.
by a vertical motor and suspended in an oil bath,
the temperature of which can be conveniently

maintained at any level up to 300 F. The inner
race of the bearing is mounted on the extension
spindle of the motor,'and the outer race can
be rigidly set in a grease cup. This cup is free
to turn with the bearing to allow torque measure
ments. A known amount of grease is packed
into the bearing and around the shaft. The
bearing is shielded by a plate on the bottom
side with a small circular clearance between the
shield and the outer race. Any leakage of oil

or molten grease through this clearance is col
lected on the bottom of the grease cup and can
be quantitatively determined. The initial test

is conducted at 80-85 F., and subsequent tests
are maderat 150 F., 180 F. and 220 F. as
required, the duration of each being 20 minutes.

During all of these tests, separation of oil, change
of structure, channelling, and aeration are noted,
Those most generally used are the tests known
in addition to the torque readings. The B. E. C.
as A. S. T. M. dropping point test D566-42

and the B. E. C. test.
The ?rst test is a method of test for dropping
point of lubricating greases, described on pages
113-115, of the September, 1943 issue of the
A. S. T. M. Standards of Petroleum Products
and Lubricants, Prepared by Committee D-2.
This dropping point test consists essentially of ,
tester is valuable for predicting the suitability

of greases for ball bearing lubrication at elevated
placing the grease within a grease cup which

has an open ori?ce of speci?ed diameter at the
bottom and is surrounded by a heating jacket.
Upon raising the temperature gradually, the

temperature is observed at which the ?rst drop
of grease passes through the ori?ce.
This test gives information as to when the
grease is softened, by heating, to a point of
leakage and dropping through an ori?ce of
speci?ed diameter. Although the test is made 45
temperatures.
This invention has for its principal object
the provision of barium base greases of improved
stability, as measured by these two methods of
test and is based upon the discovery that a
very considerably enhanced stability may be
conferred upon such greases by the incorporation
therein of a salt of an aliphatic acid of low
molecular weight. To describe both the con
ventional barium base greases and certain modi
?cations made therein within the scope of this
invention, the following formulae are presented:
TABLE I
Grease Grease Grease

N o. 1
No. 2
18. 0
14.0
N o. 3
on a grease sample in a perfectly quiescent state
and, therefore, may not represent the actual

service conditions, it gives valuable indication
as to the consistency which may be expected'in
grease feeding devices at elevated temperatures
stearic Acid, Per Cent __________________ ..

Candelilla Wax, Per Cent...
Glacial Acetic Acid, Per Gen
____ ______ __
4. 0
____ ______________ -.
Glycerine, Per Cent ____________________ ._
14. 0
4. 0
4.0
l. 0
2. 5
6.5
Cent ________________________________ __
11. 2
9. O
19. 0
and which, in turn, has a bearing on the con

sumption of the grease.
The second test is conducted in the so-called
Solar Red Oil, Per Cent _____________ _;___
69.8
70. 5
52. 5
B. E. C. grease testing machine, developed by
ventional barium base grease formulated of
Barium Hydroxide, Ba(OH)2.8HzO, Per
Of the above greases, grease No. 1 is a con
the Bearing Engineers Committee of the Anti 55 stearic acid, glycerine, barium hydroxide and oil
2,564,561
from the use of wax such that the grease con_

taining both barium acetate and wax is a better
grease from many standpoints than the grease

containing only the barium acetate.
ent but-"with the major difference being that

candelilla wax has been added. This wax aifects
With respect to this wax candelilla or montan
certain changes in the texture and consistency
wax or other similar waxes may be used.
of the grease and such wax additions may be

made in various amounts for this purpose,
Grease No. 3 is a grease embodying the teaching
of 10% of the total ingredient, the preferred

amount being from about 1% to about 5%
With; respect to the barium acetate, while that
salt is one, which it is preferred to use to secure
this desired temperature stability, there may be

used in its place any of the salts of the lower
molecular weight mono-basic aliphatic acids,

the upper limit of molecular weight being de?ned
by~>a mono-basic fatty acid not having over six
carbon atoms.
'
TABLE II'
Grease Grease- Grease
No.1 No.2. No.3.
4., S. T. M. Dropping Point, -F_____,.__._
240
343 30
235.
This barium acetate or its equiv
20 alent will normally be used in amounts of not
jected to the A. S. T. M. drop-ping point test in

the manner described above, the following results
were observed:
In
general, such wax should not be used in excess
of this disclosure in that its formula also con-L

tains glacial acetic acid and su?icient: barium hy
droxide to neutralize that acid, giving rise to:
an admixture of oil, barium stearate soap, barium
acetate, glycerine and candelilla wax. The
above greases may be prepared in accordance
with any of the usual compounding procedures
such as those described vby Klemgard on page
682 of Lubricating Greases: Their Manufacture
and Use, Reinhold Publishing Corp. (193.7) .
When samples of these three greases were sub
not confer heat stability. However, other im

provements in other characteristics do follow
and constitutes a mixture of oil, barium stearate

soap, and a small amount of glycerine. Grease
No. 2 is essentially the same composition with a
slight increase in the amount of glycerine pres
From the above it will be observed that the

conventional grease indicated a substantial loss
of stability, as indicated by the dropping point

test, at 240 F., while grease No. 2- containing
candelilla wax was of practically the same sta
bility. However, grease No. 3 exhibits. a drop
ping point 100- higher than does the conven
tional grease, thus indicating a major and sig
ni?cant. increase in temperature stability.
Similar results were found when the. three
greases were submitted to the B. E. C. test, in
which the following results were found:
over about 10% of the ?nal composition, the

minimum amount to be used. being about 0.5%
and the preferred amount. being from 1% to 7%.
Also in such greases the barium soap of the
fatty acid will, in general, be not more than
about 30% of the ?nal composition, the pre
ferred range being from 5%. to 20% of such cons
stituent.
We claim:
1. Improved, barium base greases character

ized by stability at temperatures in excess; of
200 F. formed by compounding together from
5 to 20% of high molecular Weight fatty acid
soap forming materials, from 0.5 to. 5% ofmonm
basic fatty acids of not over6 carbon atoms, from
1 to 10% of a wax selected from the group con
sisting-v of candelilla and montan wax and sur?
cie-nt barium hydroxide, to react with the above

acidic constituents, the remainder being lubri
eating oil.
2,. An, improved barium grease composition
characterized by stability at temperatures in
TABLE III
B. E. c. tests
Grease.No. 1
Temp.
a F. '
Timeot
Test
Total Leakage
GreaseNo. 2
Temp.,
O F
Min.
Time 01'
Test
Grease No. 3
TotaLLeakage-
Temp.
- F;
Min.
Time of
'Test
Total
Leakage
Min.
80
150
20
20'
80
150
20
20
80'
150
180
20.
180
2o
10%._--. - -
20
20
- - --
180
20
220
20
220
20
Full Cup l_._,.
220
20
None.
Trace.
'0
5%.
1 Gorrcsponds-to approximately 30%" of total quantity of grease used.
excess of 200 F. produced by compounding to

This test it will be observed, con?rms by par
allel. results. the ?nding of the A. S. T. M. test 60 gather
in that at 220 F. both the conventional grease
Per cent
No. 1 and grease No. 2, which is the conventional
Stearic acid __________________________ __ 14.0
grease plus a wax had both leaked su?iciently
Candelilla wax ____ ..__ ________ ______, _____ __
4.0
to give a full cup, while at the same temperature
Glacial acetic acid _______________ -1"--- 4.0
only 5% of grease No. 3 had leaked into the cup. 65 Glycerine _______________ -g ____________ __ 6.5
These results indicate a very substantial and
Barium hydroxide, Ba(OH)2.8H2O ___,_____,_' 179.0
useful increase in the temperature stability of

barium base greases and'very considerably widen
Lubricating oil ____________ _e___,_,__ _____ __ 52.5
the ?eld to which they may be applied, render--v

3. An improved barium base grease composi=
ing them capable of use in a great number. of 70 tion characterized by stability at temperatures-in
applications at temperatures above the boiling
excess of 200 F., comprising lubricatingoil and a
point of water wherein they have formerly not
sui?cient proportion of the barium soaps of fatty
been capable of use with a particularly good
acids tocharacterize the grease as one having a
degree of e?iciency.
barium base and, in addition thereto, a small pro
It, is also apparent that the wax ingredient does. 75. pqrtion. sui?cient to. stabilize the crease of the
2,564,561
barium salt of a mono basic fatty acid having

not more than 6 carbon atoms.
grease as one having a barium base to which have
4. An improved barium base grease composition

characterized by stability at temperatures in ex
cess of 200 F., comprising lubricating oil and a
sunicient proportion of the barium soaps of fatty
lize the grease but not over about 10 per cent

barium acetate and not over about 10 per cent of
a wax selected from the group consisting of mon
tan and candelilla waxes.
acids to characterize the grease as one having a
9.~=*An improved barium base grease composition

been added a small proportion suf?cient to stabi
barium base and, in addition thereto, a small

proportion suf?cient to stabilize the grease of
barium acetate.
5. An improved barium base grease composi
tion characterized by stability at temperatures
in excess of 200 F., comprising lubricating oil,
a suf?cient proportion of the barium soaps of
fatty acids to characterize the grease as one hav
ing a barium base, and a small proportion sufii
cient to stabilize the grease of barium salts of
mono basic fatty acidshaving not more than 6
carbon atoms and, in addition thereto, a small
proportion of a wax selected from the group con
sisting of montan and candelilla waxes.

cessgiof 200 F., comprising mineral oil, between

H]
about 5 and about 30 per cent by weight of the

barium soaps of fatty acids, and between about
0.5 and about 10 per cent by weight of the barium
salt of a mono basic fatty acid having not more
than 6 carbon atoms.

characterized by stability at temperatures in ex?

cess of 200 F., comprising mineral oil, between
about 5 and about 30 per cent by weight of the
barium soaps of fatty acids, and between about
20 0.5 and about 10 per cent by weight of barium
acetate.
EMMETT S. CARMICHAEL.
ELDON L. ARMSTRONG.
cess of 200 F., comprising lubricating oil and

a su?icient proportion of the barium soaps of
REFERENCES CITED
high molecular weight fatty acids to characterize
The following references are of record in the
the grease as one having a barium base and a
?le of this patent:
small proportion su?'icient to stabilize the grease
but not over about 10 per cent of the barium salt

UNITED STATES PATENTS
of a mono basic fatty acid having not more than 30 Number
Name
Date
6 carbon atoms.
v2,038,148
I.
Ott et a1 _________ __ Mar. 10, 1936

2,070,781
2,154,383
:2,197,263
su?icient proportion of the barium soaps of high 35 2,332,247
Morway et al _______ __ Oct. 19, 1943
r 2,332,825
Zimmer et al _______ __ Oct. 26, 1943
molecular weight fatty acids to characterize the
grease as one having a barium base and a small
proportion su?icient to stabilize the grease but

not over about 10 per cent of the barium salt of
acetic acid.
40
8. An improved barium grease composition

Ott et al. ________ __ Apr. 11, 1939
Carmichael et a1. ____ Apr. 16, 1940
2,355,099
Morway et al ______ __ Aug. 1, 1944
2,417,428
2,417,433
McLennan ________ __ Mar. 18, 1947

McLennan ________ __ Mar. 18, 1947
OTHER REFERENCES
-McLennan, Methods of Compounding Barium

Greases, Article in National Petroleum News,
Apr. 5, 1944, pp. R234, R236, R238, R239.
sufficient proportion of the barium soaps of high
molecular weight fatty acids to characterize the
Brunstrum et a1. ____ Feb. 16, 1937
45

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Patented Aug.

UNITED STATES PATENT OFFICE

Emmett S. Carmichael and Eldon L. Armstrong,

'No Drawing. Application May 20, 1944,

10 Claims. ( Cl. 25240.5)

This invention is directed to improvements in

present to give to the greases the characteristics

for example, for chassis, water pumps, motor

boiling point of water.

the temperature of which can be conveniently

shield and the outer race. Any leakage of oil

be quantitatively determined. The initial test

required, the duration of each being 20 minutes.

Those most generally used are the tests known

in addition to the torque readings. The B. E. C.

as A. S. T. M. dropping point test D566-42

tester is valuable for predicting the suitability

placing the grease within a grease cup which

bottom and is surrounded by a heating jacket.

Upon raising the temperature gradually, the

Grease Grease Grease

on a grease sample in a perfectly quiescent state

and, therefore, may not represent the actual

stearic Acid, Per Cent __________________ ..

Glycerine, Per Cent ____________________ ._

and which, in turn, has a bearing on the con

Solar Red Oil, Per Cent _____________ _;___

B. E. C. grease testing machine, developed by

ventional barium base grease formulated of

Barium Hydroxide, Ba(OH)2.8HzO, Per

Of the above greases, grease No. 1 is a con

from the use of wax such that the grease con_

grease from many standpoints than the grease

ent but-"with the major difference being that

With respect to this wax candelilla or montan

certain changes in the texture and consistency

wax or other similar waxes may be used.

of the grease and such wax additions may be

of 10% of the total ingredient, the preferred

this desired temperature stability, there may be

molecular weight mono-basic aliphatic acids,

4., S. T. M. Dropping Point, -F_____,.__._

This barium acetate or its equiv

20 alent will normally be used in amounts of not

jected to the A. S. T. M. drop-ping point test in

general, such wax should not be used in excess

of this disclosure in that its formula also con-L

not confer heat stability. However, other im

and constitutes a mixture of oil, barium stearate

From the above it will be observed that the

of stability, as indicated by the dropping point

over about 10% of the ?nal composition, the

1. Improved, barium base greases character

sisting-v of candelilla and montan wax and sur?

cie-nt barium hydroxide, to react with the above

Full Cup l_._,.

1 Gorrcsponds-to approximately 30%" of total quantity of grease used.

excess of 200 F. produced by compounding to

4., S. T. M. Dropping Point, -F___,.._

Lubricating oil ____________ _e___,_, _ 52.5

Ott et a1 _______ Mar. 10, 1936

Morway et al _____ Oct. 19, 1943

Zimmer et al _____ Oct. 26, 1943

Ott et al. ______ Apr. 11, 1939

Morway et al ____ Aug. 1, 1944

McLennan ______ Mar. 18, 1947