Solid anti-friction devices – materials therefor – lubricant or se – Lubricants or separants for moving solid surfaces and... – Organic compound containing boron
Reexamination Certificate
1996-12-24
2003-11-04
McAvoy, Ellen M. (Department: 1764)
Solid anti-friction devices, materials therefor, lubricant or se
Lubricants or separants for moving solid surfaces and...
Organic compound containing boron
C508S324000, C508S371000, C508S391000, C508S419000, C508S420000, C508S433000, C508S440000, C508S442000, C508S460000
Reexamination Certificate
active
06642187
ABSTRACT:
TECHNICAL FIELD OF THE INVENTION
This invention relates to lubricating compositions, concentrates and greases containing the combination of an organic polysulfide and an overbased composition or a phosphorus or boron compound.
BACKGROUND OF THE INVENTION
Polysulfides have been used to provide extreme pressure protection to lubricating compositions. However, polysulfides may lead to copper corrosion, seal compatibility, oxidation stability, and thermal stability problems. It is desirable to find a polysulfide which when used in combination with other additives provides good extreme pressure properties to lubricants without the above adverse effects.
SUMMARY OF THE INVENTION
This invention relates to a lubricating composition comprising a major amount of an oil of lubricating viscosity, (A) at least one organic polysulfide comprising at least about 90% dihydrocarbyl trisulfide, from about 0.1% up to about 8% dihydrocarbyl disulfide, and less than about 5% dihydrocarbyl higher polysulfides, and (B) at least one overbased metal composition, at least one phosphorus or boron compound, or mixtures of two or more thereof. The invention also relates to concentrates and greases containing the above combination. The invention also relates to methods of making the organic polysulfide.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The term “hydrocarbyl” includes hydrocarbon as well as substantially hydrocarbon groups. Substantially hydrocarbon describes groups which contain heteroatom substituents that do not alter the predominantly hydrocarbon nature of the substituent. Examples of hydrocarbyl groups include the following:
(1) hydrocarbon substituents, i.e., aliphatic (e.g., alkyl or alkenyl) and alicyclic (e.g., cycloalkyl, cycloalkenyl) substituents, aromatic-, aliphatic- and alicyclic-substituted aromatic substituents and the like as well as cyclic substituents wherein the ring is completed through another portion of the molecule (that is, for example, any two indicated substituents may together form an alicyclic radical);
(2) substituted hydrocarbon substituents, i.e., those substituents containing non-hydrocarbon groups which, in the context of this invention, do not alter the predominantly hydrocarbon nature of the substituent; those skilled in the art will be aware of such groups (e.g., halo (especially chloro and fluoro), hydroxy, mercapto, nitro, nitroso, sulfoxy, etc.);
(3) heteroatom substituents, i.e., substituents which will, while having a predominantly hydrocarbon character within the context of this invention, contain an atom other than carbon present in a ring or chain otherwise composed of carbon atoms (e.g., alkoxy or alkylthio). Suitable heteroatoms will be apparent to those of ordinary skill in the art and include, for example, sulfur, oxygen, nitrogen and such substituents as, e.g. pyridyl, furyl, thienyl, imidazolyl, etc.
In general, no more than about 2, preferably no more than one heteroatom substituent will be present for every ten carbon atoms in the hydrocarbyl group. Typically, there will be no such heteroatom substituents in the hydrocarbyl group. Therefore, the hydrocarbyl group is hydrocarbon.
The term reflux ratio refers to the ratio of the amount of material returned to the distillation apparatus to the amount of material removed from the distillation. For instance, a reflux ratio of 5:1 means that five parts of distillate are returned to the distillation apparatus for every one part removed from the apparatus.
As described above, the present invention relates to compositions containing (A) at least one polysulfide having specific proportions of sulfides in combination with (B) at least one overbased composition, at least one phosphorus or boron compound, or mixtures thereof. In one embodiment, the organic polysulfide (A) is present at concentrations in the range of about 0.1% to about 10% by weight, or from about 0.2% up to about 8%, or from about 0.3% up to about 7%, or from about 0.5% to about 5% by weight. Here, as well as elsewhere in the specification and claims, the range and ratio limits may be combined. In one embodiment, the overbased composition, the phosphorus or boron compound, or mixture thereof (B) is present in an amount from about 0.05% up to about 10%, or from about 0.08% up to about 8%, or from about 0.1% up to about 5% by weight.
Organic Polysulfide
The organic polysulfide is a mixture comprising at least about 90% dihydrocarbyl trisulfide, from about 0.1%, or from about 0.5% up to about 8% dihydrocarbyl disulfide, and less than about 5% dihydrocarbyl higher polysulfides. Higher polysulfides are defined as containing four or more sulfide linkages. In one embodiment, the amount of trisulfide is at least about 92%, or preferably at least about 93%. In another embodiment, the amount of dihydrocarbyl higher polysulfides is less than 4%, or preferably less than about 3%. In one embodiment, the dihydrocarbyl disulfide is present in an amount from about 0.1%, or from about 0.5% up to about 5%, or preferably from about 0.6% up to about 3%.
The sulfide analysis is performed on a Varian 6000 Gas Chromatograph and FID detector SP-4100 computing integrator. The Column is a 25 m. Megabore SGE BP-1. The temperature profile is 75° C., hold 2 min., to 250° C. at 6° C./min. The helium flow is 6.0 ml/min plus make-up. The injection temperature is 200° C. and the detector temperature is 260° C. The injection size is 0.6, ul. References are the monosulfide, disulfide and trisulfide analogues to the sulfur composition for analysis. The references may be obtainied by fractionating the product to form sulfide fractions (S1, S2 and S3) to be used for analysis. The procedure for analysis is as follows. (1) An area % determination is run on each of the reference samples to determine its purity. (2) An area % determination is run on the sample to be tested to get a general idea of its composition. (3) A calibration blend is accurately weighed based on the area % results of the sample to be tested: then the internal standard toluene, is added to the blend in an amount equal to approximately one-half of the weight of the largest component. (This should give an area approximately the same as that of the largest component.) (4) The weights of each component (i.e., S-1, S-2 and S-3) are corrected by the % purity from step 1. (5) The calibration blend is run in triplicate using the corrected weights and then calculated, using the following formula, to reflect the multiple peaks in S-1 and S-2:
RF
=
(
concentration
of
components
*
)
(
total
area
of
peaks
)
(
area
of
internal
standard
)
(
concentration
of
internal
standard
)
*
Adjusted for purity of the standard i.e.: component weight times
percent purity equals concentration of component.
(6) These response factors, plus the response factor for the single S-3 peak are used for determining weight percent results for the samples to be tested. (7) Results for S-1 and S-2 are adjusted to include all the peaks attributed to them. (8) Higher polysulfides are determined by difference using the following formula:
S
-4=100%−(
S
-1
+S
-2
+S
-3+light ends)
Light ends are defined as any peaks eluded prior to the internal standard.
The organic polysulfide generally has hydrocarbyl groups each independently having from about 2 to about 30, preferably from about two to about 20, or from about 2 to about 12 carbon atoms. The hydrocarbyl groups may be aromatic or aliphatic, preferably aliphatic. In one embodiment, the hydrocarbyl groups are alkyl groups.
The organic polysulfides may be derived from an olefin or a mercaptan. The olefins, which may be sulfurized, contain at least one olefinic double bond, which is defined as a non-aromatic double bond. Olefins having from 2 up to about 30, or from about 3 up to about 16 (most often less than about 9) carbon atoms are pa
Beebe Ross L.
Schwind James J.
Esposito Michael F.
Gilbert Teresan W.
McAvoy Ellen M.
The Lubrizol Corporation
Tritt William C.
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