U.S. patent application number 10/699510 was filed with the patent office on 2005-05-05 for high throughput preparation of lubricating oil compositions for combinatorial libraries.
Invention is credited to Balk, Thomas J., Wollenberg, Robert H..
Application Number | 20050095714 10/699510 |
Document ID | / |
Family ID | 34550985 |
Filed Date | 2005-05-05 |
United States Patent
Application |
20050095714 |
Kind Code |
A1 |
Wollenberg, Robert H. ; et
al. |
May 5, 2005 |
High throughput preparation of lubricating oil compositions for
combinatorial libraries
Abstract
A high throughput preparation of a plurality of different
lubricating oil compositions for combinatorial libraries and
subsequent high throughput screening for lubricant performance is
provided. The methods can advantageously be optimized using
combinatorial chemistry, in which a database of combinations of
lubricating oil compositions are generated. As market conditions
vary and/or product requirements or customer specifications change,
conditions suitable for forming desired products can be identified
with little or no downtime.
Inventors: |
Wollenberg, Robert H.;
(Orinda, CA) ; Balk, Thomas J.; (San Francisco,
CA) |
Correspondence
Address: |
Michael E. Carmen, Esq.
DILWORTH & BARRESE, LLP
333 Earle Ovington Blvd.
Uniondale
NY
11553
US
|
Family ID: |
34550985 |
Appl. No.: |
10/699510 |
Filed: |
October 31, 2003 |
Current U.S.
Class: |
436/55 ;
422/62 |
Current CPC
Class: |
B01J 19/0046 20130101;
B01J 2219/00486 20130101; Y10T 436/25 20150115; B01J 2219/00756
20130101; B01J 2219/00698 20130101; B01J 2219/00704 20130101; B01J
2219/0036 20130101; G01N 33/30 20130101; B01J 2219/00689 20130101;
B01J 2219/00695 20130101; B01J 2219/00481 20130101; B01J 2219/00495
20130101; B01J 2219/00585 20130101; B01J 2219/00691 20130101; Y10T
436/12 20150115; B01J 2219/00364 20130101; B01J 2219/00599
20130101 |
Class at
Publication: |
436/055 ;
422/062 |
International
Class: |
G01N 033/03 |
Claims
What is claimed is:
1. A method for preparing a plurality of different lubricant oil
formulations comprising: a) providing a major amount of at least
one base oil of lubricating viscosity and a minor amount of at
least one lubricating oil additive for combination to formulate a
lubricating oil composition; b) providing a plurality of test
reservoirs; c) combining, under program control, the major amount
base oil of lubricating viscosity and lubricating oil additive in
varying percentage compositions to provide a plurality of different
lubricating oil composition samples; and, d) containing each of the
different lubricating oil composition samples in the plurality of
test reservoirs.
2. The method of claim 1, wherein the test reservoirs comprise
recesses in a unitary body.
3. The method of claim 1, wherein the test reservoirs comprise
individual receptacles.
4. The method of claim 1, wherein the combining step (c) is
performed within each respective test reservoir.
5. The method of claim 1, wherein the combining step (c) is
performed outside of the test reservoirs.
6. The method of claim 1, wherein the combining step (c) comprises
metering predetermined respective amounts of the base oil of
lubricating viscosity and the lubricating oil additive, the
metering being automatically controlled by a computer
controller.
7. The method of claim 1, wherein the combining step (c) includes
mixing of the base oil of lubricating viscosity and the lubricating
oil additive.
8. The method of claim 7, wherein the mixing is accomplished by
static mixing.
9. The method of claim 7, wherein the mixing is accomplished by
agitation.
10. The method of claim 9, wherein the agitation comprises
mechanical stirring.
11. The method of claim 10, wherein the agitation comprises
ultrasonic agitation.
12. The method of claim 1, further comprising the step of heating
the base oil of lubricating viscosity or lubricating oil additive
or both.
13. The method of claim 1, wherein the base oil of lubricating
viscosity is a natural or synthetic oil.
14. The method of claim 1, wherein the lubricating oil additive is
selected from the group consisting of antioxidants, anti-wear
agents, detergents, rust inhibitors, dehazing agents, demulsifying
agents, metal deactivating agents, friction modifiers, pour point
depressants, antifoaming agents, co-solvents, package
compatibilisers, corrosion-inhibitors, ashless dispersants, dyes,
extreme pressure agents and mixtures thereof.
15. The method of claim 1, wherein the plurality of lubricating oil
compositions includes at least five samples.
16. The method of claim 1, wherein the plurality lubricating oil
compositions includes at least 100 samples.
17. The method of claim 1, wherein each of the lubricating oil
composition samples has a volume of no more than about 20 ml.
18. The method of claim 1, wherein each of the lubricating oil
composition samples has a volume of no more than about 15 ml.
19. The method of claim 1, wherein each of the lubricating oil
composition samples has a volume of no more than about 10 ml.
20. The method of claim 1, wherein each of the lubricating oil
composition samples has a volume of no more than about 5 ml.
21. The method of claim 1, further comprising analyzing the
plurality of lubricating oil compositions.
22. The method of claim 1, further comprising storing information
regarding the identity of the lubricating oil compositions in the
plurality of combinations of lubricating oil compositions in a
database.
23. A system for preparing a plurality of lubricant oil
formulations, under program control, which comprises: a) a supply
of at least one base oil of lubricating viscosity; b) a supply of
at least one lubricating oil additive; c) a plurality of test
reservoirs; d) means for combining selected quantities of the at
least one base oil of lubricating viscosity with selected
quantities of the at least one lubricating oil additive to form a
plurality of lubricating oil composition samples; and, e) means for
dispensing each lubricating oil composition sample in a respective
test reservoir.
24. The system of claim 23, wherein the base oil of lubricating
viscosity is a natural or synthetic oil.
25. The system of claim 23, wherein the lubricating oil additive is
selected from the group consisting of antioxidants, anti-wear
agents, detergents, rust inhibitors, dehazing agents, demulsifying
agents, metal deactivating agents, friction modifiers, pour point
depressants, antifoaming agents, co-solvents, package
compatibilisers, corrosion-inhibitors, ashless dispersants, dyes,
extreme pressure agents and mixtures thereof.
26. The system of claim 23, wherein the test reservoirs comprise
recesses in a unitary body.
27. The system of claim 23, wherein the test reservoirs comprise a
plurality of individual receptacles.
28. The system of claim 23, further comprising a computer
controller for automatically controlling said means for combining
and means for dispensing.
29. The system of claim 23, wherein said means for dispensing and
said plurality of test reservoirs are movable relative to each
other.
30. The system of claim 23, further comprising a computer
controlled metering apparatus for metering selected quantities of
the base oil and additive for mixing to provide the lubricant oil
samples.
31. The system of claim 23, wherein the means for combining
comprises a mixer.
32. The system of claim 31, wherein the mixer is a
baffle-containing static mixer.
33. The system of claim 31, wherein the mixer is a mechanical
stirrer.
34. The system of claim 31, wherein the mixer is an ultrasonic
mixer.
35. The system of claim 23, further comprising a heater.
36. The system of claim 23, wherein the means for dispensing
includes a mixing chamber and a nozzle extending from the mixing
chamber, the nozzle terminating in an outlet opening through which
the lubricant oil composition samples are rejected.
37. The system of claim 36, further including means to pressurize
the mixing chamber to eject the lubricating oil composition
samples.
Description
BACKGROUND OF THE INVENTION
[0001] 1. Technical Field
[0002] The present invention relates generally to high throughput
preparation of a plurality of different lubricating oil
compositions for combinatorial libraries and subsequent high
throughput screening for lubricant performance.
[0003] 2. Description of the Related Art
[0004] The use of a combinatorial approach for materials synthesis
is a relatively new area of research aimed at using rapid synthesis
and screening methods to build libraries of polymeric, inorganic or
solid state materials. For example, advances in reactor technology
have empowered chemists and engineers to rapidly produce large
libraries of discrete organic molecules in the pursuit of new drug
discovery, which have led to the development of a growing branch of
research called combinatorial chemistry. Combinatorial chemistry
generally refers to methods and materials for creating collections
of diverse materials or compounds--commonly known as libraries--and
to techniques and instruments for evaluating or screening libraries
for desirable properties.
[0005] Presently, research in the lubricant industry involves
individually forming candidate lubricating oil compositions and
then performing a macro-scale analysis of the candidate
compositions by employing a large amount of the candidate to be
tested. Additionally, the methods employed for testing each
candidate composition require manual operation. This, in turn,
significantly reduces the number of compositions that can be tested
and identified as leading lubricating oil compositions.
[0006] Drawbacks associated with conventional screening procedures
can be seen as follows. For example, governmental and automotive
industry pressure towards reducing the phosphorous and sulfur
content of lubricating oil compositions used as, for example,
passenger car and heavy duty diesel engine oils, is leading to new
research to identify oil compositions which can satisfy certain
tests such as, for example, oxidation, wear and compatibility
tests, while containing low levels of phosphorous and sulfur. In
this context, United States Military Standards MIL-L-46152E and the
ILSAC Standards defined by the Japanese and United States
Automobile Industry Association at present require the phosphorous
content of engine oils to be at or below 0.10 wt. % with future
phosphorous content being proposed to even lower levels, e.g., 0.08
wt. % by January, 2004 and below 0.05 wt. % by January, 2006. Also,
at present, there is no industry standard requirement for sulfur
content in engine oils, but it has been proposed that the sulfur
content be below 0.2 wt. % by January, 2006. Thus, it would be
desirable to decrease the amount of phosphorous and sulfur in
lubricating oils still further, thereby meeting future industry
standard proposed phosphorous and sulfur contents in the engine oil
while still retaining the oxidation or corrosion inhibiting
properties and antiwear properties of the higher phosphorous and
sulfur content engine oils. In order to accomplish this, a large
number of proposed lubricating oil compositions must be tested to
determine which compositions may be useful.
[0007] Additionally, similar changes in specifications and changing
customer needs also drive reformulation efforts in other lubricant
applications such as, for example, transmission fluids, hydraulic
fluids, gear oils, marine cylinder oils, compressor oils,
refrigeration lubricants and the like.
[0008] However, as stated above, present research in the lubricant
industry does not allow for reformulation to occur in an
expeditious manner. As such, there exists a need in the art for a
more efficient, economical and systematic approach for the
preparation of lubricating oil compositions and screening of such
compositions for information correlating to the actual useful
properties of the compositions.
[0009] Accordingly, it would be desirable to rapidly prepare a
plurality of sample candidate lubricating oil compositions
utilizing small amounts of each sample. In this manner, a high
throughput preparation and subsequent screening of a vast number of
diverse compositions can be achieved to identify leading
lubricating oil compositions.
SUMMARY OF THE INVENTION
[0010] A method for preparing a vast number of diverse lubricating
oil compositions and system therefor is provided herein.
Accordingly, in one embodiment of the present invention a method
for preparing a plurality of different lubricant oil formulations
is provided comprising the steps of (a) providing a major amount of
(i) at least one base oil of lubricating viscosity and (ii) a minor
amount of at least one lubricating oil additive for combination to
formulate a lubricating oil composition; (b) providing a plurality
of test reservoirs; (c) combining, under program control, the major
amount of the at least one base oil of lubricating viscosity and
the at least one lubricating oil additive in varying percentage
compositions to provide a plurality of different lubricating oil
composition samples; and, (d) containing each of the different
lubricating oil composition samples in the plurality of test
reservoirs.
[0011] In a second embodiment of the present invention, a system
for preparing a plurality of lubricant oil compositions, under
program control, is provided comprising (a) a supply of at least
one base oil of lubricating viscosity; (b) a supply of at least one
lubricating oil additive; (c) a plurality of test reservoirs; (d)
means for combining selected quantities of the at least one base
oil of lubricating viscosity with selected quantities of the at
least one lubricating oil additive to form a plurality of different
lubricating oil composition samples; and, (e) means for dispensing
each lubricating oil composition sample in a respective test
reservoir.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] Various embodiments are described below with reference to
the drawings wherein:
[0013] FIG. 1 is a schematic diagram of a system for preparing a
plurality of different lubricating oil compositions; and,
[0014] FIG. 2 is a schematic illustration of a dispensing system of
the invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT(S)
[0015] The invention is directed to the high throughput preparation
of a plurality of different lubricating oil composition samples for
subsequent testing for lubricant performance properties. The
expression "high throughput" as used herein shall be understood to
mean that a relatively large number of different lubricating oil
compositions can be rapidly prepared and analyzed. In general,
varying quantities of at least one base oil of lubricating
viscosity and at least one lubricating oil additive are introduced
in respective test reservoirs so that each reservoir contains a
different lubricating oil composition. The procedure is
advantageously accomplished under program control and is
automatically controlled by, for example, a microprocessor or other
computer control device. The expression "program control" as used
herein shall be understood to mean the equipment used herein in
providing the plurality of lubricating oil compositions is
automated and controlled by a microprocessor or other computer
control device.
[0016] The lubricating oil compositions for use in the high
throughput preparation method of this invention include as a first
component a major amount of base oil of lubricating viscosity,
e.g., an amount of greater than 50 wt. %, preferably greater than
about 70 wt. %, more preferably from about 80 to about 99.5 wt. %
and most preferably from about 85 to about 98 wt. %, based on the
total weight of the composition. The expression "base oil" as used
herein shall be understood to mean a base stock or blend of base
stocks which is a lubricant component that is produced by a single
manufacturer to the same specifications (independent of feed source
or manufacturer's location); that meets the same manufacturer's
specification; and that is identified by a unique formula, product
identification number, or both. The base oil for use herein can be
any presently known or later-discovered base oil of lubricating
viscosity used in formulating lubricating oil compositions for any
and all such applications, e.g., engine oils, marine cylinder oils,
functional fluids such as hydraulic oils, gear oils, transmission
fluids, etc. Additonally, the base oils for use herein can
optionally contain viscosity index improvers, e.g., polymeric
alkylmethacrylates; olefinic copolymers, e.g., an
ethylene-propylene copolymer or a styrene-butadiene copolymer; and
the like and mixtures thereof. As one skilled in the art would
readily appreciate, the viscosity of the base oil is dependent upon
the application. Accordingly, the viscosity of a base oil for use
herein will ordinarily range from about 2 to about 2000 centistokes
(cSt) at 100.degree. Centigrade (C). Generally, individually the
base oils used as engine oils will have a kinematic viscosity range
at 100.degree. C. of about 2 cSt to about 30 cSt, preferably about
3 cSt to about 16 cSt, and most preferably about 4 cSt to about 12
cSt and will be selected or blended depending on the desired end
use and the additives in the finished oil to give the desired grade
of engine oil, e.g., a lubricating oil composition having an SAE
Viscosity Grade of 0W, 0W-20, 0W-30, 0W-40, 0W-50, 0W-60, 5W,
5W-20, 5W-30, 5W-40, 5W-50, 5W-60, 10W, 10W-20, 10W-30, 10W-40,
10W-50, 15W, 15W-20, 15W-30 or 15W-40. Oils used as gear oils can
have viscosities ranging from about 2 cSt to about 2000 cSt at
100.degree. C.
[0017] Base stocks may be manufactured using a variety of different
processes including, but not limited to, distillation, solvent
refining, hydrogen processing, oligomerization, esterification, and
rerefining. Rerefined stock shall be substantially free from
materials introduced through manufacturing, contamination, or
previous use. The base oil of the lubricating oil compositions of
this invention may be any natural or synthetic lubricating base
oil. Suitable hydrocarbon synthetic oils include, but are not
limited to, oils prepared from the polymerization of ethylene or
from the polymerization of 1-olefins to provide polymers such as
polyalphaolefin or PAO oils, or from hydrocarbon synthesis
procedures using carbon monoxide and hydrogen gases such as in a
Fisher-Tropsch process. For example, a suitable base oil is one
that comprises little, if any, heavy fraction; e.g., little, if
any, lube oil fraction of viscosity 20 cSt or higher at 100.degree.
C.
[0018] The base oil may be derived from natural lubricating oils,
synthetic lubricating oils or mixtures thereof. Suitable base oil
includes base stocks obtained by isomerization of synthetic wax and
slack wax, as well as hydrocracked base stocks produced by
hydrocracking (rather than solvent extracting) the aromatic and
polar components of the crude. Suitable base oils include those in
all API categories I, II, III, IV and V as defined in API
Publication 1509, 14th Edition, Addendum I, December 1998. Group IV
base oils are polyalphaolefins (PAO). Group V base oils include all
other base oils not included in Group I, II, III, or IV. Although
Group II, III and IV base oils are preferred for use in this
invention, these preferred base oils may be prepared by combining
one or more of Group I, II, III, IV and V base stocks or base
oils.
[0019] Useful natural oils include mineral lubricating oils such
as, for example, liquid petroleum oils, solvent-treated or
acid-treated mineral lubricating oils of the paraffinic, naphthenic
or mixed paraffinic-naphthenic types, oils derived from coal or
shale, animal oils, vegetable oils (e.g., rapeseed oils, castor
oils and lard oil), and the like.
[0020] Useful synthetic lubricating oils include, but are not
limited to, hydrocarbon oils and halo-substituted hydrocarbon oils
such as polymerized and interpolymerized olefins, e.g.,
polybutylenes, polypropylenes, propylene-isobutylene copolymers,
chlorinated polybutylenes, poly(1-hexenes), poly(1-octenes),
poly(1-decenes), and the like and mixtures thereof; alkylbenzenes
such as dodecylbenzenes, tetradecylbenzenes, dinonylbenzenes,
di(2-ethylhexyl)-benzenes, and the like; polyphenyls such as
biphenyls, terphenyls, alkylated polyphenyls, and the like;
alkylated diphenyl ethers and alkylated diphenyl sulfides and the
derivative, analogs and homologs thereof and the like.
[0021] Other useful synthetic lubricating oils include, but are not
limited to, oils made by polymerizing olefins of less than 5 carbon
atoms such as ethylene, propylene, butylenes, isobutene, pentene,
and mixtures thereof. Methods of preparing such polymer oils are
well known to those skilled in the art.
[0022] Additional useful synthetic hydrocarbon oils include liquid
polymers of alpha olefins having the proper viscosity. Especially
useful synthetic hydrocarbon oils are the hydrogenated liquid
oligomers of C.sub.6 to C.sub.12 alpha olefins such as, for
example, 1-decene trimer.
[0023] Another class of useful synthetic lubricating oils include,
but are not limited to, alkylene oxide polymers, i.e.,
homopolymers, interpolymers, and derivatives thereof where the
terminal hydroxyl groups have been modified by, for example,
esterification or etherification. These oils are exemplified by the
oils prepared through polymerization of ethylene oxide or propylene
oxide, the alkyl and phenyl ethers of these polyoxyalkylene
polymers (e.g., methyl poly propylene glycol ether having an
average molecular weight of 1,000, diphenyl ether of polyethylene
glycol having a molecular weight of 500-1000, diethyl ether of
polypropylene glycol having a molecular weight of 1,000-1,500,
etc.) or mono- and polycarboxylic esters thereof such as, for
example, the acetic esters, mixed C.sub.3-C.sub.8 fatty acid
esters, or the C.sub.13oxo acid diester of tetraethylene
glycol.
[0024] Yet another class of useful synthetic lubricating oils
include, but are not limited to, the esters of dicarboxylic acids
e.g., phthalic acid, succinic acid, alkyl succinic acids, alkenyl
succinic acids, maleic acid, azelaic acid, suberic acid, sebacic
acid, fumaric acid, adipic acid, linoleic acid dimer, malonic
acids, alkyl malonic acids, alkenyl malonic acids, etc., with a
variety of alcohols, e.g., butyl alcohol, hexyl alcohol, dodecyl
alcohol, 2-ethylhexyl alcohol, ethylene glycol, diethylene glycol
monoether, propylene glycol, etc. Specific examples of these esters
include dibutyl adipate, di(2-ethylhexyl)sebacate, di-n-hexyl
fumarate, dioctyl sebacate, diisooctyl azelate, diisodecyl azelate,
dioctyl phthalate, didecyl phthalate, dieicosyl sebacate, the
2-ethylhexyl diester of linoleic acid dimer, the complex ester
formed by reacting one mole of sebacic acid with two moles of
tetraethylene glycol and two moles of 2-ethylhexanoic acid and the
like.
[0025] Esters useful as synthetic oils also include, but are not
limited to, those made from carboxylic acids having from about 5 to
about 12 carbon atoms with alcohols, e.g., methanol, ethanol, etc.,
polyols and polyol ethers such as neopentyl glycol, trimethylol
propane, pentaerythritol, dipentaerythritol, tripentaerythritol,
and the like.
[0026] Silicon-based oils such as, for example, polyalkyl-,
polyaryl-, polyalkoxy- or polyaryloxy-siloxane oils and silicate
oils, comprise another useful class of synthetic lubricating oils.
Specific examples of these include, but are not limited to,
tetraethyl silicate, tetra-isopropyl silicate, tetra-(2-ethylhexyl)
silicate, tetra-(4-methyl-hexyl)silicate,
tetra-(p-tert-butylphenyl)silicate,
hexyl-(4-methyl-2-pentoxy)disiloxane, poly(methyl)siloxanes,
poly(methylphenyl)siloxanes, and the like. Still yet other useful
synthetic lubricating oils include, but are not limited to, liquid
esters of phosphorous containing acids, e.g., tricresyl phosphate,
trioctyl phosphate, diethyl ester of decane phosphionic acid, etc.,
polymeric tetrahydrofurans and the like.
[0027] The lubricating oil may be derived from unrefined, refined
and rerefined oils, either natural, synthetic or mixtures of two or
more of any of these of the type disclosed hereinabove. Unrefined
oils are those obtained directly from a natural or synthetic source
(e.g., coal, shale, or tar sands bitumen) without further
purification or treatment. Examples of unrefined oils include, but
are not limited to, a shale oil obtained directly from retorting
operations, a petroleum oil obtained directly from distillation or
an ester oil obtained directly from an esterification process, each
of which is then used without further treatment. Refined oils are
similar to the unrefined oils except they have been further treated
in one or more purification steps to improve one or more
properties. These purification techniques are known to those of
skill in the art and include, for example, solvent extractions,
secondary distillation, acid or base extraction, filtration,
percolation, hydrotreating, dewaxing, etc. Rerefined oils are
obtained by treating used oils in processes similar to those used
to obtain refined oils. Such rerefined oils are also known as
reclaimed or reprocessed oils and often are additionally processed
by techniques directed to removal of spent additives and oil
breakdown products.
[0028] Lubricating oil base stocks derived from the
hydroisomerization of wax may also be used, either alone or in
combination with the aforesaid natural and/or synthetic base
stocks. Such wax isomerate oil is produced by the
hydroisomerization of natural or synthetic waxes or mixtures
thereof over a hydroisomerization catalyst.
[0029] Natural waxes are typically the slack waxes recovered by the
solvent dewaxing of mineral oils; synthetic waxes are typically the
wax produced by the Fischer-Tropsch process.
[0030] The second component of the lubricating oil compositions for
use herein is at least one lubricating oil additive. Such additives
can be any presently known or later-discovered additive used in
formulating lubricating oil compositions. The lubricating oil
additives for use herein include, but are not limited to,
antioxidants, anti-wear agents, detergents such as metal
detergents, rust inhibitors, dehazing agents, demulsifying agents,
metal deactivating agents, friction modifiers, pour point
depressants, antifoaming agents, co-solvents, package
compatibilisers, corrosion-inhibitors, ashless dispersants, dyes,
extreme pressure agents and the like and mixtures thereof. Greases
will require the addition of appropriate thickeners. A variety of
the additives are known and commercially available. These
additives, or their analogous compounds, can be employed for the
preparation of the various lubricating oil compositions herein.
[0031] Alternatively, the lubricating oil additive(s) can further
contain a diluent oil to form an additive concentrate. These
concentrates usually include at least from about 90 wt. % to about
10 wt. % and preferably from about 90 wt. % to about 50 wt. %, of a
diluent oil and from about 10 wt. % to about 90 wt. %, preferably
from about 10 wt. % to about 50 wt. %, of the foregoing
additive(s). Suitable diluents for the concentrates include any
inert diluent, preferably an oil of lubricating viscosity such as,
for example, a base oil as described hereinbelow, so that the
concentrate may be readily mixed with lubricating oils to prepare
lubricating oil compositions. Suitable lubricating oils that may be
used as diluents can be any oil of lubricating viscosity.
[0032] Examples of antioxidants include, but are not limited to,
aminic types, e.g., diphenylamine, phenyl-alpha-napthyl-amine,
N,N-di(alkylphenyl) amines; and alkylated phenylene-diamines;
phenolics such as, for example, BHT, sterically hindered alkyl
phenols such as 2,6-di-tert-butylphenol, 2,6-di-tert-butyl-p-cresol
and 2,6-di-tert-butyl-4-(2-octyl-3-propanoic) phenol;
sulfur-containing materials, e.g., sulfurized olefins or esters and
the like and mixtures thereof.
[0033] Examples of antiwear agents include, but are not limited to,
zinc dialkyldithiophosphates and zinc diaryldithiophosphates, e.g.,
those described in an article by Born et al. entitled "Relationship
between Chemical Structure and Effectiveness of Some Metallic
Dialkyl- and Diaryl-dithiophosphates in Different Lubricated
Mechanisms", appearing in Lubrication Science 4-2 January 1992, see
for example pages 97-100; aryl phosphates and phosphites,
sulfur-containing esters, phosphosulfur compounds, metal or
ash-free dithiocarbamates, xanthates, alkyl sulfides and the like
and mixtures thereof.
[0034] Examples of detergents include, but are not limited to,
overbased or neutral detergents such as sulfonate detergents, e.g.,
those made from alkyl benzene and fuming sulfuric acid; phenates
(high overbased or low overbased), high overbased phenate
stearates, phenolates, salicylates, phosphonates, thiophosphonates,
ionic surfactants and the like and mixtures thereof. Low overbased
metal sulfonates typically have a total base number (TBN) of from
about 0 to about 30 and preferably from about 10 to about 25. Low
overbased metal sulfonates and neutral metal sulfonates are well
known in the art.
[0035] Examples of rust inhibitors include, but are not limited to,
nonionic polyoxyalkylene agents, e.g., polyoxyethylene lauryl
ether, polyoxyethylene higher alcohol ether, polyoxyethylene
nonylphenyl ether, polyoxyethylene octylphenyl ether,
polyoxyethylene octyl stearyl ether, polyoxyethylene oleyl ether,
polyoxyethylene sorbitol monostearate, polyoxyethylene sorbitol
monooleate, and polyethylene glycol monooleate; stearic acid and
other fatty acids; dicarboxylic acids; metal soaps; fatty acid
amine salts; metal salts of heavy sulfonic acid; partial carboxylic
acid ester of polyhydric alcohol; phosphoric esters; (short-chain)
alkenyl succinic acids; partial esters thereof and
nitrogen-containing derivatives thereof; synthetic
alkarylsulfonates, e.g., metal dinonylnaphthalene sulfonates; and
the like and mixtures thereof.
[0036] Examples of friction modifiers include, but are not limited
to, alkoxylated fatty amines; borated fatty epoxides; fatty
phosphites, fatty epoxides, fatty amines, borated alkoxylated fatty
amines, metal salts of fatty acids, fatty acid amides, glycerol
esters, borated glycerol esters; and fatty imidazolines as
disclosed in U.S. Pat. No. 6,372,696, the contents of which are
incorporated by reference herein; friction modifiers obtained from
a reaction product of a C.sub.4 to C.sub.75, preferably a C.sub.6
to C.sub.24, and most preferably a C.sub.6 to C.sub.20, fatty acid
ester and a nitrogen-containing compound selected from the group
consisting of ammonia, and an alkanolamine, e.g., those disclosed
in U.S. Ser. No. 10/402,170, filed Mar. 28, 2003, the contents of
which are incorporated by reference herein, and the like and
mixtures thereof.
[0037] Examples of antifoaming agents include, but are not limited
to, polymers of alkyl methacrylate; polymers of dimethylsilicone
and the like and mixtures thereof.
[0038] Examples of ashless dispersants include, but are not limited
to, polyalkylene succinic anhydrides; non-nitrogen containing
derivatives of a polyalkylene succinic anhydride; a basic nitrogen
compound selected from the group consisting of succinimides,
carboxylic acid amides, hydrocarbyl monoamines, hydrocarbyl
polyamines, Mannich bases, phosphonoamides, thiophosphonamides and
phosphoramides; thiazoles, e.g., 2,5-dimercapto-1,3,4-thiadiazoles,
mercaptobenzothiazoles and derivatives thereof; triazoles, e.g.,
alkyltriazoles and benzotriazoles; copolymers which contain a
carboxylate ester with one or more additional polar function,
including amine, amide, imine, imide, hydroxyl, carboxyl, and the
like, e.g., products prepared by copolymerization of long chain
alkyl acrylates or methacrylates with monomers of the above
function; and the like and mixtures thereof. The derivatives of
these dispersants, e.g., borated dispersants such as borated
succinimides, may also be used. Preferably, the dispersants are
polyalkylene succinimides derived from animation of polyalkylene
succinic anhydrides with polyalkylene polyamine.
[0039] If desired, prior to dispensing the at least one base oil
and at least one lubricating oil additive to provide the
compositions herein, as discussed hereinbelow, it can be
advantageous to conduct molecular modeling of proposed compounds
for use in the compositions (i.e., formulations) to determine which
compounds may provide potential leading candidate compositions. For
example, calculations can be carried out involving such factors as,
for example, transition states, bond lengths, bond angles, dipole
moment, hydrophobicity, etc, of the compounds. Accordingly, the
proposed compounds can be screened to determine, for example, which
compounds may perform poorly in an oxidation inhibition process due
to a poor ability to trap intermediate peroxides. This can be
carried out using known software such as, for example, Quantum
Mechanics available from Accelrys (San Diego, Calif.).
[0040] Software for the design of test libraries can be used to
design the original compound test libraries based on input from the
foregoing experimental program(s). This software can be used to
efficiently design test libraries that cover the desired
experimental space and utilize statistical experimental design
methods. Other software can then be used to analyze the data from
the experiments and correlate that data with the structure of the
compounds and/or compound treatment conditions and/or reaction
conditions. Such correlations are often referred to as QSAR
software (Quantitative Structure Activity Relations) available from
Accelrys (San Diego, Calif.). Such QSAR programs can then be used
by the software to design subsequent compound test libraries for
further screening.
[0041] The use of such QSAR programs can add to the efficiency of
screening. As more data is collected, these QSAR programs can
become more efficient at developing compounds libraries with
increased probability for finding desirable compounds. For example,
the compounds analyzed can be formulated into various lubricating
oil compositions, as decribed hereinbelow, and then further
analyzed by way of, for example, regression and analysis
technologies, using known software, e.g., C.sup.2-QSAR available
from Accelrys (San Diego, Calif.). In this manner, validation of
the data obtained from the molecular modeling can be achieved and
then this data can also be stored in a data collector. In this way,
new compounds, conceived by one skilled in the art can be checked
by the QSAR software to predict their activity prior to their
actual synthesis. Additionally, such software tools may be utilized
to prioritize a list of possible compounds being considered for
synthesis in such a way that one skilled in the art will have a
higher probability for success.
[0042] Referring now to FIG. 1, a system 100 is shown for preparing
a plurality of test samples. Vessel 110 contains a supply of the
foregoing base oils of lubricating viscosity B. Vessel 120 contains
a supply of additive A, which can be any of the foregoing additives
useful for modifying the properties of the base oil so as to
provide a lubricating oil composition suitable for the intended use
or application. As one skilled in the art would readily appreciate,
one or more of vessels 110 and vessels 120 can be used when
dispensing more than one base oil and one additive,
respectively.
[0043] Tubular line 111 is a conduit for communicating the base oil
B to nozzle portion 113, from which it can be dispensed into a
selected test reservoir, as described below. The amount of base oil
dispensed is determined by metering pump 112, which can be computer
controlled.
[0044] Tubular line 121 is a conduit for communicating lubricating
oil additive A to nozzle portion 123, from which it can be
dispensed into a selected test reservoir, as described below. The
amount of base oil dispensed is determined by metering pump 122,
which also can be computer controlled. Computer programs and
systems for automatically metering predetermined amounts of
materials in accordance with a preselected program control are
known in the art and can be used herein.
[0045] Nozzles 113 and 123 are preferably in close proximity so
that base oil B and additive A can be simultaneously dispensed in a
test reservoir. Alternatively, base oil B and additive A can be
sequentially added to the test reservoir. The nozzles 113 and 123
can comprise a multichannel pipette or one or more syringe
needles.
[0046] The vessels 110 and 120 can be under pressure. Optionally,
more than two vessels can be employed. Metering pumps suitable for
use in the invention are known and commercially available. In the
event that highly viscous lubricant base stock or additives are
used, the vessels 110 and 120 and/or the tubular lines 111 and 121,
metering pumps 112 and 122, and/or nozzles 113 and 123 can be
heated to facilitate fluid flow therethrough.
[0047] The test frame 130 includes a block 131 of inert material
(e.g., glass, ceramic, metal) having a plurality of recesses 132
for receiving the dispensed base oil and additives. The recesses
provide test reservoirs wherein each reservoir contains a
lubricating oil of a different and predetermined composition, i.e.,
the percentage and/or type of base oil and/or additives in each
composition will vary from one reservoir to another. Optionally,
the reservoirs can be individual receptacles (e.g., test tubes)
mounted upon a rack, instead of being recesses in a block. While
five reservoirs, i.e., recesses 132a, 132b, 132c, 132d, 132e, are
illustrated in FIG. 1, any number of reservoirs can be employed.
For example, a 10.times.10 array of reservoirs would accommodate
100 different lubricating oil formulation samples. It is also
contemplated that liners (not shown), e.g., glass or metal such as
aluminum, can be inserted into recesses 132a, 132b, 132c, 132d,
132e prior to depositing the lubricating oil components.
[0048] The individual reservoirs are adapted to hold relatively
small amounts of lubricating oil samples. The sample size in each
reservoir can be no more than about 20 ml, preferably no more than
about 15 ml, more preferably no more than about 10 ml and yet more
preferably no more than about 5 ml.
[0049] The test frame 130 and dispensing nozzles 113 and 123 are
movable relative to one another. Although manual movement of the
apparatus by an equipment operator is within the purview of the
invention, robotic mechanisms with programmable movement are
preferred. In one embodiment the test frame 130 is mounted upon a
slidable carriage movable in a lateral and/or vertical direction so
as to sequentially position a selected recess under the dispensing
nozzles 113 and 123. In another embodiment, the nozzles 113 and
123, and optionally the vessels 110 and 120, are slidably movable
laterally and/or vertically to accomplish positioning of the
nozzles 113 and 123.
[0050] In a testing procedure, vessels 110 and 120 are filled with
the selected lubricant base oil and additive(s), respectively. The
apparatus of system 100 is moved such that dispensing nozzles 113
and 123 are positioned above and in alignment with recess 132a. A
metered amount of base oil B and a metered amount of additive A are
simultaneously dispensed into recess 132a. The dispensing nozzles
113 and 123 are thereafter repositioned to be in alignment with the
next recess 132b and the metered amounts of additive A and/or base
oil B are changed in accordance with a predetermined schedule of
variation such that the lubricating oil in recess 132b has a
different percentage composition of additive than that in recess
132a. The pattern is repeated as the nozzles 113 and 123 are
sequentially aligned with the successive recesses 132c, 132d, and
132e so that each recess has a predetermined composition of
lubricating oil.
[0051] The components A and B are preferably combined in the
reservoirs by mixing, for example, by agitation of the frame 131,
static mixing, individual stirring of the contents of the
reservoirs (mechanical or magnetic stirring) or by bubbling the
reservoir with a gas, e.g., nitrogen.
[0052] Optionally, base oil B and additive(s) A can be combined
prior to dispensing into the respective reservoirs. For example, a
single dispensing nozzle having a mixing chamber can be used,
wherein base oil B and additive(s) A are metered into the mixing
chamber and then dispensed through the nozzle into the
reservoir.
[0053] Referring now to FIG. 2, a system 200 for combining and
dispensing a lubricating oil composition is schematically
illustrated which employs a single nozzle assembly 210 having an
elongated injector portion 211 and a mixing chamber 212. The end of
injector portion 211 includes an opening 216 through which the
lubricating oil composition is ejected into the selected test
reservoir.
[0054] A conduit 202 conveys a quantity of base oil B through a
metering apparatus 201 and into mixing chamber 212. Conduit 204
carries a first additive A-1 through metering apparatus 203 and
into mixing chamber 212. Conduit 206 carries a second additive A-2
through metering apparatus 205 and into mixing chamber 212. As one
skilled in the art would readily appreciate, while only two
additive components A-1 and A-2 are shown, it should be understood
that any number of different additives can be individually metered
into the nozzle assembly 210. The metering apparatus 201, 203, and
205 are each automatically controlled by control system 250 which
preferably includes a microprocessor with the appropriate
programming and control connections 251, 252 and 253 for
communicating control signals to the respective metering apparatus.
Control connections 251, 252 and 253 can be, for example,
electrical, optical, pneumatic, or fluidic. The control system 250
determines the composition of the lubricating oil in the mixing
chamber 212 by regulating the amounts of the respective lubrication
oil components (i.e., base oil B, and additives A-1, A-2, etc.)
metered into the nozzle assembly 210.
[0055] Preferably the conduits 202, 204, and 206 are terminated
with one way valves 207, 208, and 209, respectively, to prevent
backflow of the mixing chamber contents in the event that pressure
in the mixing chamber 212 exceeds the pressure in the conduits.
[0056] The lubricating oil components can be mixed together by
various means. For example, mixing unit 213 can be a rotary
impeller, or, more preferably, an ultrasonic probe. Optionally,
baffles 215 can be incorporated into nozzle assembly 210 for static
mixing of the components as they flow through the nozzle
assembly.
[0057] In the event that high viscosity components are being mixed,
a heating unit such as coiled resistance heater 218 can be used to
raise the temperature of the components and thereby lower their
viscosity to improve fluid flow. Heating units can alternatively be
convection units (e.g., hot air blowers), radiant coils, or
conduction heaters, and can be used to heat any part of the system
200 including the component supplies (B, A-1, A-2), the conduits
(202, 204, 206), the metering apparatus (201, 203, 205), the mixing
chamber 212, and/or the injector portion 211 (as shown).
[0058] The contents of the mixing chamber 212 can be moved through
injector portion 211 by, for example, applying pressure from a
pressure source P such as compressed gas. As mentioned above,
one-way valves 207, 208, and 209 prevent backflow of the contents
into the conduits 202, 204, and 206 if the pressure within the
mixing chamber 212 exceeds the pressure within the conduits.
Alternatively, the lubricant base oil and additive sources B, A-1
and A-2 can be pressurized and/or the metering apparatus 201, 203
and 205 can provide pumping pressure to move the materials through
the system.
[0059] The procedure described above provides an array of samples
of varying compositions which can be compiled in a data collector,
e.g., microprocessor, to provide a combinatorial lubricating oil
composition library. The array of samples can then be screened with
respect to selected properties and categorized in the combinatorial
lubricating oil composition library. For example, the plurality of
different lubricating oil compositions can be subjected to further
automated or manual screening tests, e.g., storage stability tests,
oxidation tests, wear tests, etc., for information correlating to
the actual useful properties of the compositions to determine their
efficacy. The results of each of the tests can then be compiled in
the database as stated above to provide the combinatorial
lubricating oil composition library. Alternatively, the system may
be electrically connected to a signal data collector comprising a
computer microprocessor for system operation and control to collect
the data from the various tests over an extended period of time to
compile the combinatorial lubricating oil composition library.
[0060] While the above description contains many specifics, these
specifics should not be construed as limitations of the invention,
but merely as exemplifications of preferred embodiments thereof.
Those skilled in the art will envision many other embodiments
within the scope and spirit of the invention as defined by the
claims appended hereto.
* * * * *