Note: Descriptions are shown in the official language in which they were submitted.
CA 02268286 1999-04-09
WO 98!17748 PCTIEP97/0591~4
JREA GREASE COMPOSITION
The present invention relates to urea grease
compositions and to gears containing such compositions.
Petroleum cost has increased sharply since so-called Oil
Shock, and resourcing saving and energy saving ideas
have been constantly intended in every industrial field,
reflecting its influence.
In the motor vehicle industry, compact and light
general motor vehicles have been developed, and the
number of vehicles employing constant velocity joints
(hereinafter, abbreviated as CVJ) have increased.
Further, CVJ is also employed in 4 wheel drive vehicles
and vehicles of four wheel independent suspension type,
and the demand is growing. CVJ, which is also called
constant velocity universal joint, is a joint which
transmits rotation keeping constant angular speed and
torque, and has different types depending on various
uses. The lubricating agents used for the CVJ are
exposed to severer condition as a motor vehicle achieves
higher power and higher speed and CVJ itself becomes
compact, and therefore, a grease is demanded which
reduces friction and wear on sliding portions. Further,
a seal boot member is required to be mounted on CVJ to
prevent leaking of a grease and to prevent invasion of
foreign materials and water from outside. As for this
material, chloroprene rubber is generally used and
polyester resins are also commonly used.
A grease which is excellent in low friction and wear
resistance suppresses vibration and noise of a vehicle
' body at a time of starting and accelerating and during
driving. Moreover, due to its temperature suppressing
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WO 98/17748 PCTIEP97/05914
effect, durability of a seal boot member can be
improved. However, excessive increase of temperature
promotes ageing of the seal boot member and degradation
of a lubricating agent and extremely shortens the life
of CVJ.
On the other hand, in the steel industry, continuous
operation of mechanical equipment has been further
developed. With the technical revolution, there have
been a strong demand in high quality of a product,
improvement in production process capacity, ensuring of
reliability of an apparatus, and the like. Lubrication
conditions are very severe, since greases used in these
mechanical apparatus are in a tough environment, that
is, high temperature, contact with water, high
possibility of invasion of foreign materials such as
scale, and the like, and are continuously exposed to
severe conditions day and night. A grease is required
which has excellent seal resistance and reduces friction
and wear to lengthen the life of mechanical parts and to
prevent sudden failure to the utmost. Further, the
parts to be lubricated of industrial machinery, machine
tools, and the like suffer from considerable friction,
and excessive wear causes reduction in accuracy of the
machine, so that the mechanical parts have to be
replaced. As described above, to reduce friction and
save wear is an important object of the present
invention.
Therefore, in the parts to be lubricated as
described above, lithium-based greases have been
conveniently used using sulfur-based compounds such as
sulfurized fat and oil, sulfurized olefin and the like,
lead naphthenate, metal dithiophosphate, metal
dithiocarbamate-based additive and the like. Recently,
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Ii
CA 02268286 2005-O1-31
- 3-
a lithium complex grease and a urea grease which are
superior in heat resistance to lithium-based greases
have been increasingly used.
Under this situation, as one of typical prior art,
S U.S. Patent No. 4,519,312 discloses a grease using
aromatic amine phosphate as an organic additive
containing no sulfur in a urea grease. Further,
U.S. Patent No. 4,890,790 discloses a grease comprising
a urea grease, an organic molybdenum compound, and zinc
dithiophosphate. Japanese Patent Publication (JP-B) No.
09-39590(1992) discloses a urea grease comprising as an
essential component a sulfur-phosphorus-based extreme
pressure additive comprising
1) molybdenum dialkyldithiocarbamate sulfide and
2) one or a combination of two or more selected from
the group consisting of sulfurized fat and oil,
sulfurized olefin, tricresyl phosphate, trialkyl
thiophosphate and zinc dialkyl dithiophosphate.
Although some of the greases in the prior art are
recognized to have reducing effects in friction and
wear, full satisfaction has not been attained. Further,
there are disadvantages that sealants deteriorate under
high temperature. For example, an aromatic amine
phosphate and lead naphthenate degrade polyester resins
and a sulfurized fat and oil degrades chloroprene
rubber, respectively, and a sulfurized olefin extremely
degrades both chloroprene rubber and polyester resins.
Further, in other prior art, Japanese Patent
Application Laid-Open (JP-A) No. 08-157859 (1996)
discloses the use of as additives a molybdenum
dialkyldithiocarbamate sulfide and triphenylphosphoro-
thionate, and Japanese Patent Application Laid-Open (JP-
A) No. 62-2275197 (1987) discloses the use of as
m
CA 02268286 1999-04-09
WO 98!17748 PCT/EP97/059I4
- 4-
thickening agents a lithium soap of 12-hydroxy fatty
acid, lithium phosphate formed from a phosphate such as
trimethyl phosphate or triphenyl phosphate. Further,
Japanese Patent Application Laid-Open (JP-A) No.
03-231993 (1991) discloses a grease composition using a
phosphate oil in a urea compound.
The present invention relates to a urea grease which
is excellent in frictional properties and wear
resistance and also has good fitting property to
sealants such as chloroprene rubber and polyester resin.
More particularly, the present invention relates to a
urea grease composition suitable for application to such
parts to be grease-lubricated as constant velocity
joints, ball joints, and ball bearings in motor vehicles
and bearings and gears of various industrial equipments
such as the steel and industrial machines and machine
tools.
The present invention relates to a urea grease
composition comprising a urea grease and as additives
(A) a molybdenum dialkyldithiocarbamate sulfide
represented by the formula:
R1
-C-S OzOmS~
RZ S
wherein R1 and RZ each independently represents a group
selected from the group consisting of alkyl groups
having from 1 to 29 carbon atoms; m is 0 or an integer
of from 1 to 3; and n is an integer of from 1 to 4;
provided that the sum of m and n is 4, and (B) a
triphenyl phosphate represented by the formula:
SUBSTITUTE SHEET (Ril~l.E 26)
,~ _._ _t . .. . . _.
CA 02268286 1999-04-09
WO 98/17748 PCT/EP97/059I4
- 5-
O = P O
3
The compounds corresponding to the above-mentioned
component (A) have a high melting point. Examples of
those compounds include diethyl sulfide-molybdenum
dithiocarbamate, dibutyl-molybdenum dithiocarbamate,
diisobutyl sulfide-molybdenum dithiocarbamate, di(2-
ethylhexyl)sulfide-molybdenum dithiocarbamate, diamyl
sulfide-molybdenum dithiocarbamate, diisoamyl sulfide-
molybdenum dithiocarbamate, dilauryl sulfide-molybdenum
dithiocarbamate, distearyl sulfide-molybdenum
dithiocarbamate. They are preferably mixed in the form
of powder, and the amount added is from 0.5 to 10% by
weight, preferably from 0.5 to 5% by weight based on the
total weight. When the amount added is less than 0.5%
by weight, effect of improvement in friction resistance
and wear resistance is generally insufficient, and when
over 10% by weight, no further improvement will
generally occur.
As triphenyl phosphate has a melting point of 50°C
and is solid at ambient temperature, it is preferred
that the powder is blended with the base grease at a
temperature of not less than 50°C. The amount of
component (B) preferably is from 0.1 to 10% by weight,
more preferably from 0.1 to 5% by weight based on the
total weight. When the amount used is less than 0.1% by
weight, improvement in friction resistance and wear
resistance properties generally cannot be achieved, and
when over 10% by weight, further lubricating ability
generally cannot be obtained.
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CA 02268286 1999-04-09
WO 98117748 PCTIEP97l059I4
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As to the urea compound, any of known thickening
agents of urea type can be used. For example, diurea,
triurea and tetraurea may be used.
As the base oil, a mineral oil and/or a synthetic
oil can be used. If the urea compound is used as a
thickening agent it is preferably applied in an amount
from 2 to 35% by weight based on the total weight of the
base oil and the urea compound.
Also, various additives such as an antioxidant,
anticorrosion agent, extreme pressure agent, polymer and
the like can further be added to the composition of the
present invention.
The urea grease composition according to the
invention are especially suitable for use in gears, more
specifically constant velocity joints. Therefore, the
present invention further relates to gears, more
specifically constant velocity joints, containing such
grease.
Example and Comparative Example
2U The present invention will be specifically described
by Examples and Comparative Examples hereinafter,
however it is not construed to be limited to them.
Additives were added to base greases in blending ratios
as shown in Tables 1 to 5 (all of them are shown in o by
weight), the mixtures were treated by three-roll mill to
obtain greases of Examples and Comparative Examples.
The formulations of the base greases are as
described below. As the base oil, a purified mineral
oil having a viscosity of 15 mmz/sec at 100°C was used.
I. Diurea grease
One mol of diphenylmethane-9,4'-diisocyanate and 2
mol of octylamine were reacted in the base oil, and the
produced urea compound was dispersed uniformly to obtain
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I li i
CA 02268286 2005-O1-31
a grease. The amount of urea compound was 10% by weight
based on the total weight of the base oil and the urea
compound.
II. Tetraurea grease
Two mol of diphenylmethane-4,4'-diisocyanate, 2 mol
of octylamine, and 1 mol of ethylenediamine were reacted
in the base oil, and the produced urea compound was
dispersed uniformly to obtain a grease. The amount of
urea compound was 15o by weight based on the total
weight of the base oil and the urea compound.
III. Lithium complex grease
Hydrogenated caster oil fatty acid was dissolved in
the base oil, to which was added an aqueous lithium
hydroxide solution for neutralization, and the mixture
IS was dehydrated during the reaction. After completion of
the dehydration, azelaic acid was added. The reaction
was carried out with the help of an aqueous lithium
hydroxide solution in the amount necessary for
neutralization. The lithium azelate and lithium 12-
hydroxystearate soap were mixed and dispersed uniformly
to obtain a grease. The amount of lithium 12-hydroxy-
stearate as a thickening agent was 7.5a by weight and
the amount of lithium azelate was 2.5~ by weight,
respectively, based on the total weight of the base oil
and the thickening agent.
The following test were conducted regarding friction
coefficient, wear resistance and fitting property to a
sealant as shown in the tables, and evaluations were
made.
(1) Friction coefficient
Friction coefficient after 15 minutes was measured
under the following conditions using a testing machine
CA 02268286 2005 !O1-31
_ g _
available under the trade-mark ~~Falex" (according
to IP/241/69).
Rotation speed . 290 rpm
Load . 890N (200 lb)
Temperature . room temperature
Time . 15 minutes
Amount of grease . about 1 g of grease was applied
on a test piece
(2) Wear resistance
According to the four ball type wearing test of
ASTM D2226
Rotation speed . 1200 rpm
Load . 392N (40 kgf)
Temperature . 75°C
Time . 60 minutes
(3) Fitting property to sealant
Sealants which were chloroprene rubber of a
polyester resin were immersed in respective grease
compositions and tested under the following conditions
according to the vulcanized rubber physical test of
JIS K6301. The tensile strength and elongation before
and after the test were measured and change (%) was
obtained.
Temperature . 140°C
Immersion Time . 96 hrs
CA 02268286 1999-04-09
WO 98/17748 - 9 _ PCT/EP97/059I4
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SUBSTITU i E SHEET (RULE 2G1
t
CA 02268286 1999-04-09
ff~ 9g~1~~~ PCT/EP97105914
15-
The friction coefficients in Examples 1 to 7 are all
smaller as compared with those of Comparative Examples 1
to 10. Regarding wear resistance, Comparative Examples
5, 6, 7, 9 and 10 provide the same degree of good
results as the examples according to the invention.
However, these Comparative Examples are inferior in
compatability to chloroprene rubber and/or polyester
resin.
For example, Comparative Example 5 gives a large
change in elongation of chloroprene rubber and polyester
resin. Comparative Example 6 gives a large change in
tensile strength and elongation of chloroprene rubber
and polyester resin. Comparative Examples 9 and 10 give
relatively large change in elongation of a polyester
resin. Examples 1 to 7 give an excellent friction
coefficient and wear resistance and also an excellent
fitting property to sealants of chloroprene rubber and
polyester resins.
The grease of the present invention has a low
?0 friction coefficient and is excellent in wear
resistance. As a result, vibration and noise of CVJ of
motor vehicles are suppressed. Further, the grease of
the present invention reduces friction in ball joints
and wheel bearings of motor vehicles and other various
industry machine apparatuses, and can lengthen the life
of machine parts.
The grease of the present invention is excellent in
the fitting property to chloroprene rubber and polyester
resin, and delays the degradation of the sealant of a
sealed apparatus even at high temperature.
SUBSTITUTE SHEET (~'~E 261
