U.S. patent number 3,622,512 [Application Number 04/822,309] was granted by the patent office on 1971-11-23 for grease compositions of polyol aliphatic esters.
Invention is credited to John B. Christian.
United States Patent |
3,622,512 |
Christian |
November 23, 1971 |
GREASE COMPOSITIONS OF POLYOL ALIPHATIC ESTERS
Abstract
Grease compositions comprising (1) as a base fluid a polyol
aliphatic ester and (2) as a thickener finely divided sodium
montmorillonite clay. The clay may be used as the sole thickener or
it may be used in combination with a finely divided fluorinated
ethylenepropylene copolymer. Also, molybdenum disulfide or antimony
dialkyldithiocarbamate may be added to the compositions. The
compositions have both good wear characteristics and good extreme
pressure characteristics at temperatures in the -65.degree. F. to
350.degree. F. range. The grease compositions are useful in heavily
loaded airframe bearings, screw jack actuators, journal bearings,
and in other applications where there is sliding, rolling,
oscillating, or other forms of motion where wear and extreme
pressure are factors.
Inventors: |
Christian; John B. (Yellow
Springs, OH) |
Assignee: |
|
Family
ID: |
25235698 |
Appl.
No.: |
04/822,309 |
Filed: |
May 6, 1969 |
Current U.S.
Class: |
508/141; 508/136;
508/138 |
Current CPC
Class: |
C10M
7/00 (20130101); C10M 2201/066 (20130101); C10N
2040/02 (20130101); C10M 2201/103 (20130101); C10M
2211/06 (20130101); C10N 2050/10 (20130101); C10M
2213/02 (20130101); C10M 2213/062 (20130101); C10N
2050/08 (20130101); C10N 2010/10 (20130101); C10M
2219/068 (20130101) |
Current International
Class: |
C10m 007/36 ();
C10m 007/24 () |
Field of
Search: |
;252/28,33.6,25,21,565 |
References Cited
[Referenced By]
U.S. Patent Documents
Primary Examiner: Wyman; Daniel E.
Assistant Examiner: Vaughn; I.
Claims
I claim:
1. A grease composition comprising (1) a base fluid, (2) a
thickener, and (3) a solid lubricant; said base fluid being a
polyol aliphatic ester having a viscosity at 100.degree. F. of from
about 25 to 35 centistokes, a viscosity at 210.degree. F. of from
about 4 to 6 centistokes, a pour point of about -70.degree. F., a
flash point of from about 450.degree. to 525.degree. F. and having
the general structural formula:
wherein R is a substituted alkane containing from 1 to 3 carbon
atoms, R' is an alkyl group having from three to 12 carbon atoms,
and n is an integer having a value of from three to four; said
thickener being selected from the group consisting of sodium
montmorillonite clay and a mixture of sodium montmorillonite clay
and fluorinated ethylenepropylene copolymer characterized by the
structure:
wherein n is an integer of sufficient value to give the copolymer
an average molecular weight of about 150,000 with said thickener
comprising about 15 to 20 weight percent of said composition; and
said solid lubricant being selected from the group consisting
of
wherein R is selected from the group consisting of n-butyl, amyl,
hexyl, 2-ethylhexyl, and decyl and wherein said solid lubricant
comprises about 4 to 6 weight percent of said composition.
2. The composition of claim 1 wherein said thickener is sodium
montmorillonite clay.
3. The composition according to claim 1 wherein said thickener is a
mixture of sodium montmorillonite clay and fluorinated
ethylenepropylene copolymer and where said mixture comprises about
8- 9 weight percent of the clay and about 8- 9 weight percent of
the copolymer.
4. The composition according to claim 3 wherein the solid lubricant
is
5. The composition according to claim 3 wherein the solid lubricant
is MoS.sub.2.
Description
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention is in the field of grease lubricating materials.
2. Description of the Prior Art
With the advent of high-speed aircraft and aerospace vehicles and
the increase in their scope of operations under heavy load
conditions, serious demands have been made on greases. To meet
these demands, the prior art has achieved substantial advancement
in the synthesis of a variety of lubricating oils. There are many
oils which have desirable lubricating properties and are capable of
functioning under moderately heavy loads. Attempts have been made
to incorporate these oils into grease formulations capable of
preserving their lubricity at the points where originally desired.
The prior art has had little success in these attempts. Grease
systems which have been used with reasonable degrees of success
have involved the complicated, costly, and time consuming addition
of many different materials to the basic lubricating oil. Also,
while the various additives have provided improvements in one or
more areas, they have not provided all the improvements desired and
have often subtracted from the potential of the grease system in
some areas while they were improving it in others. For example,
where a prior art grease formulation might be made capable of
withstanding exposure to oxidation or evaporation conditions by an
additive, the same additive might also lower the lubricity of the
system or make the system unable to prevent excessive wear under
heavy load conditions.
Montmorillonite clays are well known as thickeners in the prior
art. For example, silicone polymer oils have been thickened with
clay to form a grease with the consistency of vaseline. However,
despite the contributions of the prior art, the need continues for
grease compositions with both good wear properties and good extreme
pressure properties over a wide range of temperatures.
SUMMARY OF THE INVENTION
The practice of this invention allows one to formulate a grease
composition which has both good wear properties and good extreme
pressure properties at temperatures in excess of 350.degree. F.
This invention also allows one to incorporate solid lubricants and
additives into grease compositions in such manner that the wear and
extreme pressure properties of the compositions will be improved.
The grease compositions of this invention are useful in heavily
loaded airframe bearings, screwjack actuators, journal bearings,
and other places where sliding, rolling, oscillating, or other
forms of motion take place and wear and extreme pressure are
factors.
The invention may be briefly summarized by stating that the grease
compositions comprise a polyol aliphatic ester base fluid and a
finely divided montmorillonite clay thickener. Finely divided
fluorinated ethylenepropylene copolymer and molybdenum disulfide or
antimony dialkyldithiocarbamate are also used as additives.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The polyol aliphatic ester, which is the base fluid of the grease
compositions of this invention, may be characterized by the general
formula:
wherein R is a substituted alkane containing one to three carbon
atoms, R' is an alkyl group containing three to 12 carbon atoms,
and n is an integer having a value of three to four; and wherein
the polyol aliphatic ester is further characterized by the
following properties.
Viscosity at 100.degree. F. about 25 to 35 centistokes Viscosity at
210.degree. F. about 4 to 6 centistokes Pour point about
-70.degree. F. Flashpoint about 450.degree.-525.degree. F.
additives such as molybdenum disulfide and antimony
dialkyldithiocarbamate may be used, with advantage, in the
compositions of this invention. The antimony dialkyldithiocarbamate
may be characterized by the formula:
wherein R is an alkyl selected from the n-butyl, amyl, hexyl,
2-ethylhexyl, and decyl groups with amyl being preferred.
The fluorinated ethylene propylene copolymer is a copolymer of
perfluoropropylene and tetrafluoroethylene, preferably of equimolar
amounts and characterized by the structure:
wherein n is an integer of sufficient value to give the copolymer
an average molecular weight of about 150,000.
The physical characteristics of the thickeners are important.
Montmorillonite clay should be finely divided having a surface area
of about 15.9 m..sup.2 /gram, a particle size of about 0.75 to 1.0
micron, and a density of about 3.09 grams/cc. If fluorinated
ethylenepropylene copolymer is used with the clay, the copolymer
should have a surface area of about 1.0 m..sup.2 /gram, a particle
size of about 0.15 micron, a density of about 2.18 grams/cc., and
an average molecular weight of about 150,000.
The following examples give compositions which were formulated in
the percentages indicated. The percentages are by weight unless
otherwise specified. Where a percentage range is given a number of
compositions were made up in the range specified and the physical
characteristics were in the range specified. The ingredients were
mixed thoroughly and blended to a grease consistency by passing
five times through a three-roll paint mill with the roller opening
set at 0.002 inch at room temperature. Other standard grease
homogenizing apparatus, however, may be used with equal results.
The compositions resulting from the following examples were
thermally stable to at least 350.degree. F. and exhibited both good
wear and good extreme pressure properties at that temperature.
Where molybdenum disulfide or antimony dialkyldithiocarbamate was
added, it was added to the oil prior to blending on the three-roll
mill. Worked penetration, dropping point, mean Hertz load, and
four-ball wear test (steel on steel) mean determined in accordance
with Methods 313.2, 1421.1, 6403, and 6514, respectively, of
Federal Test Method Standard No. 791a. The oscillating bearing test
was conducted in accordance with Military Specification
MIL-G-27549.
EXAMPLE I
Composition
78-80% polyol aliphatic ester
7.5-8.5% fluorinated ethylenepropylene
7.5-8.5% sodium montmillonite clay
4.0-6.0% antimony dialkyldithiocarbamate
Test-results
worked penetration 315-320 dropping point 475-490.degree. F.
four-ball wear scar (60 kg. load, 1,200 r.p.m. 167.degree. F., 2
hours) 0.9-0.95 mm. oscillating bearing test 300,000 cycles mean
Hertz load 90-95
EXAMPLE II
Composition
77-80% polyol aliphatic ester
8-9 % fluorinated ethylenepropylene
8-9 % sodium montmorillonite clay
4-5 % molybdenum disulfide
Test-results
worked penetration 335-345 dropping point 500-515.degree. F.
four-ball wear scar (60 kg. load, 1,200 r.p.m. 167.degree. F., 2
hours) 0.95-1.00 mm. oscillating bearing test 250,000-270,000
cycles mean Hertz load 84-89
EXAMPLE III
Composition
84% polyol aliphatic ester 16% sodium montmorillonite clay
TEST-RESULTS worked penetration 336 dropping point 562.degree. F.
four-ball wear scar (60 kg. load, 1,200 r.p.m., 167.degree. F., 2
hours) 1.10 mm. mean Hertz load 21
The foregoing are three specific examples which serve to indicate
to those skilled in the art how the grease compositions were made
up. When sodium montmorillonite clay, is used alone as the
thickener, it may be present in the amount of about 15-20 weight
percent of the composition. When fluorinated ethylenepropylene
copolymer is used in conjunction with the clay the two (clay and
copolymer) added together should comprise about 15 to 20 weight
percent of the composition. If a solid lubricant is used it should
comprise about 4 to 5 weight percent of the composition. The base
fluid comprises that weight percent of the composition over and
above the total of thickener and solid lubricant to make the total
weight percent of the composition 100.
* * * * *