Note : Les descriptions sont présentées dans la langue officielle dans laquelle elles ont été soumises.
~7'7~7
LUBRICANT ADDITIVE
The present invention relates generally to lubricant
additive compositions, and more particularly relates to
friction-reducing and extreme pressure lubricant additives.
In the production of lubricants numerous substances,
for example, oleic acid, tricresyl phosphate, sulphur bearing
compounds, tricresyl phosphate, sperm oil and sulfurized sperm
oil, may be added to the base lubricant to contribute various
properties or characteristics to the finished lubricant.
Included among these are additives to improve extreme pressure
and film strength properties of the lubricant; oxidation
inhibitors; rust inhibitors, detergents; viscosity index
improvers; pour point depressants; and oilinessr antiwear and/or
antiweld agents.
The terms "extreme pressure", "film strength
properties", and also "oiliness" and "lubricity" refer to the
ability of lubricants to reduce friction and prevent wear and
welding between working surfaces of bearings and gear teeth
when, as a result of extreme pressure, low speed, high
temperatures or reduced viscosity, the film which normally
completely separates moving parts becomes thin enough to permit
partial metal-to-metal contact. When moving machiné parts are
subjected to more severe conditions of load, speed and temperature,
as for example, the high tooth pressures and high rubbing
velocities often encountered in hypoid and spur~type gearing,
base lubricating oils themselves do not have the necessary
qualities to provide adequate lubrication; metal-to-metal contact
would occur which results in scoring, galling and local seizure
7~7~
-- 2 --
of the gear teeth; therefore it is necessary to employ lubricants
which contain extreme pressure additives. Conventionally employed
additives of this type, and also additives for imparting antiwear
properties to the lubricants, are generally phosphorus, chlorine
and/or sulfur compounds which react with metal surfaces to reduce
friction and prevent welding.
Numerous lubricant compositions which contain anti-
wear agents and or extreme pressure additives are known, and
have been described in various patents and other literature.
For instance, Johnson describes in U.S. Patent 2,220,843 an
extreme pressure lubricant which comprises a major proportion
of a refined lubricating oil and as additives, a sulfurized
ester of an unsaturated acid and a heavy metal naphthenate.
In U.S. Patent 2,276,341 (Prutton) an extreme
pressure lubricant is described, which comprises a hydrocarbon
lubricating oil, from about 1~ to about 5~ of a metal
naphthenate or naphthenic acid ester, and any one of a wide
variety of halogenated organic compounds.
Kaufman et al disclose in Canadian Patent 427,435,
granted May 8, 1945, lubricants for use under high pressure
conditions; these are prepared by first preparing a sulfurized
lubricating oil by heating the oil and sulfur at temperatures
of 320 - 375F., and then incorporating a small amount of
lead naphthehate in the sulfurized oil.
An objective of the present invention is to provide
a lubricant additive composition which functions both as a
friction reducing agent and as an extreme pressure additive.
Another objective of the invention is to provide a
lubricant additive which, when incorporated in a lubricant,
7~ L7
-- 3
substantially improves the low temperature viscosity
characteristics of the lubricant.
A further objective of the invention is to provide
a friction-reducing and extreme-pressure lubricant additive of
a relatively high degree of uniformity, but which is relatively
easy to manufacture, requiring a minimum of quality control.
A yet further objective of this invention is to
provide an effective friction-reducing and extreme-pressure
lubricant additive which does not require the presence of
corrosive phosphorus -, nitrogen - or halogen-containing
compounds and/or sulfurized compounds to impart the desired
degree of extreme-pressure properties thereto.
The present invention provides an improved lubricant
additive composition which imparts friction reducing, lubricity
and extreme pressure properties to lubricants, and which does
not require the use of complex phosphorus-, chlorine-, nitrogen-
and/or sulfur- containing organic compounds such as characterize
most known lubricant additives of this type.
In one aspect, the present invention resides in a
lubricant additive composition which comprises:
(1) 35~ by weight of a 24% ~by weight) solution of
lead naphthenate in an organic solvent therefor;
(2) 40% by weight of "Tellus 32 Oil" (trademark)
which is a blend of HVI 100 Neutral Oil with HVI 250 Neutral Oil;
and
(3) 25~ by weight of desulfurized diesel oil.
Desirably this composition includes about 1% by weight (in the
lead naphthenate solution) of a non-aromatic odorant material.
In another aspect, this invention provides a
,
.
_ 4 _ ~ ~77~7
"heavy-duty" lubricant additive composition which, in its
essentials, comprises: 11) a lead soap of an organic acid,
preferably lead naphthenate; (2) an oil of a minimum viscosity
of 45 SUS at 100F.; (3) desulfurized diesel oil or an
equivalent thereof; (4) a zirconium soap; and (5) a calcium soap.
More particularly, this aspect of the invention resides in a heavy
duty lubricant additive composition comprising:
(1) about 5% to about 45% by weight of a lead soap of an
organic acid, said lead soap being in the form of a solution
in a liquid solvent therefor, said solution containing from
; about 10% to about 32% by weight lead;
(2) 20%-50% by weight of an oil having a viscosity in the range
of from about 45 SUS at 100F. to about 3000 SUS at 100F.;
(3) 5% - 40% by weight of desulfurized diesel oil, or of a
hydrocarbon oil having physical characteristics comparable
to said diesel oil;
(4) 0.10% - 5.00% by weight of an oil-soluble zirconium-
containing soap selected from the group consisting of
zirconium naphthenate, zirconium 2-ethylhexanoate,
zirconium 3,5-dimethyl hexanoate, and zirconium neo-
decanoate, or mixtures thereof; and
(5) 0.10% ~ 5.00% by weight of calcium in an oil-soluble
form, as calcium naphthenate or calcium 2-ethylhexanoate.
Desirably the composition contains also from about 0.1~
to about 3% by weight of a non-aroma~ic odorant material
for assisting in product identification.
Desirably also this "heavy duty" composition contains in addition
an antioxidant in an amount of from about 0.01% to about 1.00%
by weight of said composition.
An odorant is desirably included as a means of easy
~7~7
-- 5 --
product identification. This may be incorporated in the lead
soap ~olution in an amount ranging from 0.1% to about 3.0~ by
weight based on said lead soap solution. The odorant may be
any of a wide variety of odorant substances, with the proviso
that it is non-polluting and non-toxic; thus nitrobenzene is
not suitable as an odorant ~or purposes of the present invention,
and is excluded.
The lead soap employed may be of the basic neutral
or acid positive type, preferably it is lead naphthenate, the
lead content of which may vary from about 10~ to about 32%
by weight. However, basic, neutral or acid positive lead
compounds produced from other organic acid radicals than naphthenic
acid may be utilized as partial or total substitutes for lead
naphthenate, in the formulation of the present invention. The
organic acids may be, if desired, of animal or vegetable origin
as well as hydrocarbon-derived.
The oil component is preferably a hydrocarbon oil,
which may range in viscosity from about 45 SUS at 100F. to about
1200 SUS at 100F.; and may be predominantly paraffinic,
predominantly naphthenic, or a mixture of paraffinic and
naphthenic. Oils of vegetable or animal origin may, however,
be usefully employed in the formulations of the present
invention, as may synthetic lubricants such as organic diesters,
polyglycols (polyethylene oxide or polypropylene oxide),
; silicone oils, phosphate esters (eg. tricresyl phosphate),
and polyphenyl ethers; and polyolefins, eg. of the polybutene/
polyisobutylene types.
The upper limit of viscosity for the oil used as
component (2) of our additive compositions is that at which
.,
.
~L'77i~l7
-- 6 --
the oil can no longer readily penetrate into moving machinery
parts under service conditions of temperature and pressure.
Thus, there may be used, as component ~2) of our composition,
any oil of the above classes which has a viscosity ranging
from a minimum of about ~5 SUS at 100F up to any viscosity
level that would not seriously inhibit the flow of additive to
the moving parts, under operating conditions. As a practical
matter, the upper limit of viscosity of the oil which may be
used is believed to be about 3000 SUS at 100F.
Suitable oils for use as the oil component of
the compositions of this invention are those sold by Shell
Oil Company under the trademark "Tellus", which oils are,
among other things, used for hydraulic purposes. The "Tellus"
oils will have been compounded with a number of additives to
lower pour point, improve oxidation resistance, etc. Examples
of oils which are suitable for use in the present invention
are set forth in Tables I and II.
Also included herein for reference purposes
(see Table III) are the characteristics of a number of Shell
base stocks. It is our belief that to produce an oil
corresponding to "Tellus 32", a blend of HVI 100 Neutral/
HVI 250 Neutral Oils would be used, to which blend various
additives will have been incorporated.
; Other oils comparable in physical properties to the
"Tellus" oils referred to above may be used in the compositions
of this invention, such as, for example, the "Harmony" M
oils produced by Gulf Oil Company.
HVI Brightstock oils may also be used as the oil
component of the compositions of this invention. Such Brightstock
~177~L7
-- 7 --
oils as are commonly processed and used on the North American
continent have a viscosity @ 210F. in the range of 120-170
S~S and more particularly in the range of 150 - 165 SUS. Such
oils will have viscosities @ 100F. in the range of 2000-3000
SVS. The enclosed Tables IV and V show representative examples
of HVI Brightstock oils.
The lubricant additive compositions of this invention
also include from about 5~ to about 40% by weight of desulfuriæed
diesel oil, or of hydrocarbon oil of comparable physical
characteristics having other applications than for diesel purposes.
Such oils may optionally contain additives to control icing, rust
and corrosion buildup, etc., as is well known to those skilled
in the art. Suitable desulfurized diesel oils are those sold by
Gulf Canada Limited under the trademarks "Gulf Diesel Fuel 20X",
"Gulf Diesel Fuel 25", and "Gulf Diesel Fuel 40". The
characteristics of these oils are set forth in Tables VI, VII and
VIII.
The compositions of this invention also include
from about 0.10% to about 5.00~ by weight of an oil-soluble
zirconium-containing soap which is selected from the following:
æirconium naphthenate, zirconium 2-ethylhexanoate, zirconium
3,5-dimethyl hexanoate, or zirconium neo~decanoate, or mixtures
thereof.
Finally, there is included in the composition of
this invention from about 0.10~ to about 5.00% by weight of
calcium in an oil-soluble form as calcium naphthenate or
calcium 2-ethylhexanoate.
No special preparation techniques or mixing
equipment are necessary to prepare the lubricant additive of
,.,
7~1~7
-- 8 --
the present invention. This is an advantage in terms of its
production and production-related costs, and also serves to
ensure that due to ease of manufacture, product uniformity can
be more readily guaranteed.
It is not uncommon in the preparation of extreme
pressure oils and greases for the manufacturer of such products
to sulphurize one or more of the oils used in the preparation
thereof. This is not only time-consuming but can also be a
variable operation, and requires that extreme environmental
care be taken. In the lubricant additive of the present
invention it is not necessary that a sulfurized oil be used as
an ingredient; and the additive of this invention is a simply
and easily produced composition of high uniformity requiring no
involved processing techniques and a minimum of quality control.
Desirably the compositions of the present invention
also contain a small amount of an oil-soluble dye or comparable
colorant material, to assist in product identification.
In preferred compositions according to this invention
there is included between about 10~ and about 15% by weight of
a liquid organic solvent for the lead soap. Such solvent may
be for example mineral spirits ("Shellsol"*, "Varsol 3139"**,
etc.~ which imparts a high degree of penetration to the
composition. Effective penetration is very important, if
the composition is to perform satisfactorily. While the lead
compound present in the formulation is the active ingredient,
it is only effective as a friction reducer/lubricating agent/
extreme pressure additive if it can penetrate to the working
* Trademark
** Trademark
9L~77B~7
g
parts in which it is to function. The required penetration
properties are supplied by the organic solvent (eg. mineral
spirits) present in the lead soap solution and also, to a
lesser extent, by the desulfurized diesel oil in the
formulation. This aspect of the formulation is believed to
be critical.
In a preferred aspect of the invention the
composition contains ~.4% by weight of lead in the form of
basic lead naphthenate.
The oil present in the formulation (Component (2))
acts as a general lubricant, and also as a dispersant for the
lead soap.
The addition of an oil soluble zirconium soap in
a basic, acid positive or neutral form, it is believed, serves
to synergize the effect of the lead soap present in the
formulation while the calcium in an oil-soluble form can act
as a dispersant for the lead soap and as a synergist; and
also has the ability to improve the alkali resistance of the
formulation.
One preferred composition of the present invention
comprises:
35% by weight 24% lead naphthenate solution
(containing 1% by weight of an odorant matarial);
40% by weight "Tellus 32 Oil"; and
25% by weight of desulfurized diesel oil.
A unique characteristic of the lubricant additive
composition of the present invention is that it fuctions both
as a friction reducing agent and as an extreme pressure additive.
Of the two characteristics the ~riction reducing properties of
",
,.,
~L~77~
-- 10 --
the composition will perhaps be more evident to the user. It is
very effective in lubricating the moving parts of gear boxes,
automobile engines, transmissions, general bearings, journals,
etc.
The effectiveness of the compositions of this
invention as a friction reducing agent and extreme pressure
additive has been demonstrated by actual testing, for which
purpose a test piece was especially built. Also demonstrated
was the effectiveness of the additive of this invention when
lubricating oil containing the additive was removed from the
bearing. The traces of oil/additive remaining on the bearing
gave sufficient lubricity to allow the shaft to be rotated at
high speed for an extended period of time. The same test
has been performed in selected test engines, i.e. where the treated
oil is drained from the crankcase, under which circumstances the
engine continues to perform for an extended period of time
without seizure occurring.
A further important feature of the composition
of the present invention is that, when said composition is
incorporated in a lubricant, it substantially improves the
low temperature viscosity characteristics of the lubricant.
Attached hereto as Table IX is viscosity information generated
by the Ontario Research Foundation which demonstrates in a very
clear manner that the incorporation of our friction-reducing,
extreme pressure additive composition in multi-grade and
straight-grade engine oils beneficially affects the low
temperature viscosity of such oils, which in turn would have a
profound effect on the "cold start-up" of car and truck engines
lL~77~
and machinery operating in low-temperature external locations.
Straight grade and multi-grade motor oils containing our
lubricant additive will have lubricity characteristics at low
temperatures which are superior to those of many of the multi-
grade en~ine oils now on the market.
While the present invention has been described
herein in terms of certain preferred embodiments, it is to
be understood that this invention is not to be llmited thereto,
as certain modifications and variationSin the ingredients
and proportions thereof may be made, as will be apparent to
those skilled in the art. It is desired, therefore, that the
invention be limited only by the claims which follow.
, .
~778~
-12-
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~7'7~7
Table IV
SHELLFLEX* 810
BRIGHTSTOCK OIL
TYPICAL VALUES
Specific Gravity/60F 0.892
Viscosity SSU @ 100F 2819
Viscosity SSU @ 210F 161
Aniline Point F 260
Pour Point F 0
Viscosity Gravity Constant 0.801
Colour ASTM D1500 3.0
Flash Point F (C.O.C.) 620
Average Molecular Weight 750
C.C.R. % 0.05
I.B.P. F 812
50% F 1028
Molecular Analysis (Clay Gel)
Polar Compounds 2.3
.
Aromatics 20.5
Saturates' 77.2
',:
~ * Registered Trade Mark - Shell Canada Limited
~. : - -~ . . .. . . .. . . . .
-16-
1~l77~
Table V
GULF"PARAFLEX HT 460"
_ _ _ _ . _ _ _
BRIGHTSTOCK OIL
-
TYPICAL VALUES
Density, kg/L @ 15C 0.879
Gravity, API 29.4
Gravity, Specific @ 60F 0.879
Colour ASTM ~0.5
Flash C COC 302
Viscosity:
cSt @ 40C 440
cSt @ 100C 32.33
S.S.U. @ 100F (37.8C) 2343
S.S.U. @ 210F (98.9C) 157.6
Pour Point, C -6
Aniline Point, C 138
Clay Gel Analysis, wt. %
Polar Aromatics 0.5
Aromatics 1.2
Total Aromatics 1.7
Saturates 98.3
Carbon Type Analysis, wt. %
Ca o
Cn
Cp 70
Average Molecular Weight 660
Carbon Number Range 42 - 56
Average Carbon Number 48
Distillation ASTM D 2887
IBP 619F
5% 860 F
10% 948F
30% 1036F
50% 1075-Carbon
No. 50
70% 1112F
90% 1179F
*Trademark
, ~ . . . ... . . .
-17-
~1778:~7
Table VI
GULF CANADA LIMITED
., . . _
PRODUCT TYPICAL ANALYSIS
ULF DIESEL FUEL 20X
A.P.I. Gravity 32-36
Colour 0.5
Sulphur, % 0.5
Cloud Point, F. ~20
Pour Point, F. +10
Flash Point, F. 125 Minimum
Cetane Index 40
Viscosity: Kinematic at 100F. (centistokes) 3.1
SUS at 100F. 36
Distillation:
I.B.P. F. 362
10% 420
50% 528
90% 618
F.B.P. F. 654
-1 R~
~7~3~7
Table VI (Cont'd.)
GULF CANADA LIMITED
~ . . .
SUMMER GRADE
_ _ . . ..
GIJLF DIESEL FUEL 20X
.... _ ._
Typical Chemical Analysis
Calcium 0.030 ppm
Nickel 0.08 ppm
Sodium 0.57 ppm
Lead 0.013 ppm
Potassium 0.10 ppm
Vanadium 0.28 ppm
-19-
~L~77131~
Table VII
GULF CANADA LIMITED
PRODUCT TYPICAL ANALYSIS
GULF DIESEL FUEL 25
A.P.I. Gravity 39.4
Colour 0 5
Sulphur, % 0.5
Cloud Point, F. -10
Pour Point, DF. -25
Flash Point/ F. 145
Cetane Index 46
Viscosity - Kinematic at 100F. (centistokes) 2.0
SUS at 100F. 33
Distillation F:
I.B.P. 344
10% 383
50% 458
90% 565
F'.B.P. 632
Recovery 99
~77~
Table VIII
GULF GANADA LIM_TED
PROD _T TYPICAL ANALYSIS
GULF DIESEL FUEL 40
A.P.I. Gravity 40.4
Specific Gravity 0.323
Colour 10.5
Sulphur, % 0,5
Cloud Point F. -35
Pour Point, F. -40
Flash Point! F. 150
C~tane Number 48
Viscosity: Kinematic at 100F, (centistokes) 1.9
SUS at 100F. 32.0
Distillation F.:
I.B.P. 349
10% 385
50% 440
90% 514
F.B.P. 560
Recovery 99
-21-
1177B17
TABLE IX
Viscositv of"Power Aid"and SAE Oil~ower ~id
¦ V I S C O S I T ~
Sample Speed (rpm) -46C 220C lOOC
SAE 10W30 lO 62,400 112
2066,200 120 30
5063,280 123 25
lOO 14S 1l 33
SAE 20W 5 3BO,000 128
2~296,003 13~ ~0
100 16~ 2~
"Power Aid 20 784 24 1 lO
804 32 1 13
I100 553 42 ~ 16
SAE lOW30/ .
Power Aid 10 1,900 l20
20 2,170 118 14
50 2,400 126 1 28
100 1'l8 1 3
SAE 20W/
Power Aid 10 5,000 120 1
520 5,280 132 25
100 154 30
.. .
.~ .. .. ..
Note: SAE/Power Aid: 1 fl.oz of Power Aid to 1 quart SAE Oil.
Vl~o~ity RVT Model, Spindle #2.
* Power Aid" is the trademark for the friction-reducing,
extreme pressure additive composition of the present
invention.
