Title of Invention

AN ASPHALT PAVING COMPOSITION AND METHOD OF PREPARATION THEREOF

Abstract An asphalt paving composition and method of preparation thereof are disclosed. The asphalt paving composition comprises an asphalt binder, aggregate, and an alkaline anti-stripping additive, wherein the asphalt binder comprises asphalt and polyphosphoric acid. The method for improving the resistance to stripping of an asphalt pavement prepared using an asphalt paving composition that comprises asphalt and aggregate involves modifying the asphalt paving composition by adding polyphosphoric acid and an alkaline anti-stripping additive to the asphalt paving composition.
Full Text BACKGROUND OF THE INVENTION
1. FIELD OF THE INVENTION
The present invention relates to asphalt pavement anti-stripping additives, and more
particularly to the use of polyphosphoric acid in conjunction with an alkaline additive to improve
the adhesion between an asphalt binder and aggregate.
2. DESCRIPTION OF THE RELATED TECHNOLOGY
As is well known, asphalt is commonly used as a paving material. Typically, the asphalt,
often referred to as "asphalt cement" or "asphalt binder," Is mixed with an aggregate to form an
asphalt concrete suitable for paving. Thus, the asphalt concrete comprises aggregate held
within a continuous phase of the asphalt binder by adherence of the asphalt binder to the
aggregate. Unfortunately, however, asphalt binder has a tendency to lose its adhesive bond
with the aggregate, particularly in the presence of moisture, in a process known as "stripping."
Specifically, the adhesion between polar molecules within the asphalt and polar molecules on
the aggregate surface is disrupted by water (a polar molecule) from rain or underground
sources. The stripping of asphalt binder from aggregate surfaces reduces the life of the
pavement and is a serious problem throughout the many millions of miles of highways
throughout the world. In addition to stripping, water acts like a solvent in asphalt thereby
decreasing asphalt viscosity, reducing strength, and increasing rutting.
In view of the foregoing, numerous efforts have been made over the years to reduce
asphalt stripping. Many such efforts have been directed to including various additives to the
asphalt binder compositions or even to the aggregate to increase the binder-aggregate
adhesion. A typical type of anti-stripping additive comprises surface-active agents such as
amines, preferably liquids, that have polar head-groups that exhibit an affinity for polar surfaces
like that of the aggregate. The amines also typically contain long, non-polar fatty chains that
exhibit a high affinity for asphalt binder. The molecular structure of a surface-active amine also
tends to lower the interfacial tension between the asphalt binder and the aggregate, thereby
increasing the strength of the adhesive bond between the two. Examples of such polyamines
include AD-HERE HP PLUS (a trade designation of Arr-Maz Custom Chemicals, Inc. of Winter
Haven, Florida, USA) and PAVE-BOND LITE (a trade designation of Rohm and Haas). Such
anti-strips are usually mixed with the asphalt binder prior to pumping the modified binder to the
mixing plant.


Alternatively, the modification of asphalt binders with polyphosphoric acid has been
known for quite some time (see, e.g., U.S. Pat. No. 3,751,278), although its benefits as an anti-
stripping additive may not have been recognized until more recently. Polyphosphoric acids
may be reacted with asphalt to increase the asphaltene fraction or asphaltene dispersion of the
binder. This change is the believed to be the primary reason for a change in the temperature-
viscosity relationships of the asphalt binder. Specifically, at elevated temperatures, a binder
comprising polyphosphoric acid tends to have a higher viscosity than the same binder without
polyphosphoric acid. Conversely, at lower temperatures, a binder comprising polyphosphoric
acid tends to have a low viscosity that the same binder without polyphosphoric acid. A
secondary reason for the increase of the high temperature viscosity is believed to be hydrogen
bonding between un-reacted acid (free acid sites) and the asphalt. Some studies indicate that
the hydrogen bonding may be at least partially neutralized or reversed by the presence of
conventional amine anti-strips, and as a result, there is a belief by some of those skilled in the
art that polyphosphoric acid and amine anti-strips should not be used together.
A further alternative for improving adhesion is the use of hydrated lime (often simply
referred to as "lime") in paving compositions. Typically, lime is added to the paving composition
by treating the aggregate. The use of lime in asphalt paving has been known for at least 80
years, but its benefits as an anti-stripping additive was not known until more recently.
Specifically, it is believed by those of skill in the art that lime reacts with highly polar molecules
to form insoluble salts that tend not to attract water. This prevents said polar molecules from
reacting with other molecules in the paving composition to form water-soluble soaps that
promote stripping (see, e.g., Petersen, J.C., H. Plancher, and P.M. Harnsbergen, "Lime
Treatment of Asphalt to Reduce Age Hardening and Improve Flow Properties," Proceedings,
MPT, Vol. 56, 1987).
An additional method of improving adhesion by treating the aggregate includes applying
polymer coatings to the particles (see, e.g., U.S. Pat. Nos. 5,219,901 and 6,093,494).
Specifically, U.S. Pat. No. 5,219,901 discloses a technique for reducing stripping tendencies
.that involves coating the aggregate with a thin, continuous film of a water-insoluble high
molecular weight organic polymer, such as an acrylic polymer or a styrene-acrylic polymer.
Although many of the foregoing methods of improving stripping resistance have been
effective to various degrees depending on numerous factors such as the type of asphalt, type of
aggregate, amount of additive, etc., a need continues to exist for an asphalt concrete or paving
composition having increased adherence or anti-stripping behavior in addition to other qualities
that make it a desirable paving material (e.g., cost, ease of use, resistance to rutting, cracking,
fatigue, oxidation and aging, etc.).


BRIEF SUMMARY OF THE INVENTION
Briefly, therefore, the present invention is directed to a novel paving composition
comprising an asphalt paving composition comprising an asphalt binder, aggregate, and an
alkaline anti-stripping additive, wherein the asphalt binder comprises asphalt and
polyphosphoric acid.
The present invention is also directed to an asphalt paving composition consisting
essentially of asphalt, aggregate, polyphosphoric acid, and an alkaline anti-stripping additive.
Additionally, the present invention is directed to an asphalt pavement comprising a
compacted asphalt paving composition that comprises an asphalt binder, aggregate, and an
alkaline anti-stripping additive, wherein the asphalt binder comprises asphalt and
polyphosphoric acid.
Further, the present invention is directed to a method for improving the resistance to
stripping of an asphalt pavement prepared using an asphalt paving composition that comprises
asphalt and aggregate, the method comprising modifying the asphalt paving composition by
adding polyphosphoric acid and an alkaline anti-stripping additive to the asphalt paving
composition.
The present invention is also directed to a method for preparing an asphalt paving
composition, the method comprising mixing a modified asphalt binder that comprises an asphalt
and polyphosphoric acid with aggregate and an alkaline anti-stripping additive to produce the
asphalt paving composition.
Additionally, the present invention is directed to a method of paving a surface with an
asphalt paving composition, the method comprising depositing the asphalt paving composition
onto the surface and compacting the deposited asphalt paving composition, wherein the
asphalt paving composition comprises asphalt, aggregate, polyphosphoric acid, and an alkaline
anti-stripping additive.
DETAILED DESCRIPTION OF THE INVENTION
In accordance with the present invention, it has been discovered that, surprisingly, the
addition of polyphosphoric acid and an alkaline anti-stripping agent (e.g., lime) in an asphalt
paving composition substantially increases the resistance to stripping of the paving
composition. Thus, in one embodiment, the present invention is directed to an asphalt paving
composition that comprises an asphalt, aggregate, polyphosphoric acid, and an alkaline anti-
stripping agent. Typically, the asphalt paving composition of the present invention may be
formed by mixing a modified asphalt binder and an aggregate mixture, wherein the asphalt
binder comprises asphalt modified with polyphosphoric acid and the aggregate mixture
comprises aggregate treated with an alkaline anti-stripping agent (e.g., lime). It is possible,

however, to add the lime to the paving composition after the mixing of the aggregate and
asphalt binder have begun (e.g., by injecting hydrated lime into a drum mixer just after the
asphalt binder is injected).
A,_ Asphalt
Asphalt is defined by the ASTM as a dark brown to black cementitious material in which
the predominant constituents are bitumens that occur in nature or are obtained in petroleum
processing. Asphalts characteristically contain very high molecular weight hydrocarbons called
asphaltenes. These are essentially soluble in carbon disulfide, and aromatic and chlorinated
hydrocarbons. Bitumen is a generic term defined by the ASTM as a class of black or dark-
colored cementitious substances, natural or manufactured, composed principally of high
molecular weight hydrocarbons, of which asphalts, tars, pitches and asphaltenes are typical.
The ASTM further classifies asphalts or bituminous materials as solids, semi-solids, or liquids
using a penetration test for consistency or viscosity. In this classification, solid materials are
those having a penetration of not more than 1 millimeter when a load of 100 grams is applied
for 5 seconds while at 25 °C and semi-solids are those having a penetration of more than 1
millimeter when a load of 50 grams is applied for 5 seconds while at 25 °C. Semi-solid and
liquid asphalts predominate in commercial practice today.
Asphalt has viscous properties, which allow it to flow, and elastic properties, which resist
flow. At elevated temperatures, the viscous properties dominate and the asphalt tends to flow
or deform. At lower temperatures, the elastic properties dominate and the asphalt tends to
resist flow. All types of asphalt, both naturally occurring and synthetically manufactured, are
suitable for use in his invention. Naturally occurring asphalt is inclusive of native rock asphalt,
lake asphalt, etc. Synthetically manufacture asphalt is often a by-product of petroleum refining
operations and includes air-blown asphalt, blended asphalt, cracked or residual asphalt,
petroleum asphalt, propane asphalt, straight-run asphalt, thermal asphalt, etc. Examples of
asphalt, which are often referred to by their extraction location, include Wyoming Sour, Saudi
Heavy, West Texas intermediate, California Valley, Venezuelan, and Canadian.
Asphalt chemistry can be described on the molecular level as well as on the
intermolecular (microstructural) level. On the molecular level, asphalt is a mixture of complex
organic molecules that range in molecular weight from several hundred to several thousand.
Although these molecules affect behavioral characteristics of the asphalt, the behavior of
asphalt Is largely determined by the microstructure of the asphalt, which is that of a dispersed
polar fluid. Specifically, a continuous three-dimensional association of polar molecules
(asphaltenes) dispersed in a fluid of non-polar or relatively low-polarity molecules (maltenes).
All these molecules are capable of forming dipolar intermolecular bonds of varying strength.


Since these intermolecular bonds are weaker than the bonds that hold the basic organic
hydrocarbon constituents of asphalt together, they will break first and control the behavioral
characteristics of asphalt. Therefore, asphalt's physical characteristics are a direct result of the
forming, breaking, and reforming of these intermolecular bonds or other properties associated
with molecular superstructures. The result is a material that behaves elastically through the
effects of the polar molecule networks and viscously because the various parts of the polar
molecule network can move relative to one another due to the dispersion in the fluid non-polar
molecules.
Asphalt binders are most commonly characterized by the physical properties that
indicate how they perform as a constituent in a paving composition or hot mixed asphalt.
Examples of relevant physical properties include durability and rheotogy, and some tests for
evaluating different aspects of these properties include: thin-film oven test (AASHTO 179 and
ASTM D 1754), rolling thin-film oven test (AASHTO T 240 and ASTM D 2872), pressure aging
vessel test (AASHTO PP1), penetration test (AASHTO T 49 and ASTM D4), softening point
test (AASHTO T 53 and ASTM D 36), absolute viscosity at 60 °C test (AASHTO T 202 and
ASTM D 2171), kinematic viscosity at 135 °Ctest (AASHTO T 201 and ASTM D 2170), ductility
test (AASHTO T 51 and ASTM D113), rotational viscometer test (AASHTO TP48 and ASTM D
4402), dynamic shear rheometer (AASHTO TP 5), bending beam rheometer (AASHTO TP1),
and the direct tension test (AASHTO TP 3).
Rather than refer to an extensive list of physical properties, those in the art typically
categorize asphalt binders by one or more grading systems such as the penetration grading
system, the viscosity grading system, and the Superpave performance grading system.
Penetration grades are listed as a range of penetration units determined according to AASHTO
M 20 and ASTM D 946. The 40-50 grade is the hardest grade, the 60-70, 85-100, and 120-
150 grades are typically used in the U.S., and the 200-300 grade is the softest grade and is
typically used for cold climates such as northern Canada. Viscosity grading is performed on as-
supplied asphalt binder (AC grading) or on aged residue samples (AR grading) according to
AASHTO M 226 and ASTM D 3381. Typical grades for hot mixed asphalt in the U.S. are AC-
10, AC-20, AC-30, AR-4000, and AR 8000. The more recently developed Superpave
performance grade (PG) is generally considered to more accurately and fully characterize
asphalt binders for use in hot mixed asphalt pavements. Superpave performance grading is
based on the idea that an asphalt binder's properties should be related to the conditions under
which it is used. Therefore, the Superpave system uses several tests that are performed
according to AASHTO PP6 at temperatures that depend on the relevant climate conditions.
The Superpave performance grading is reported using two numbers - the first being the
average seven-day maximum pavement temperature (°C) and the second being the minimum


pavement design temperature to be experience (°C). Thus, a PG 58-22 is intended for use
where the average seven-day maximum pavement temperature is 58 °C and the expected
minimum pavement temperature is-22 °C. Asphalt binders that are typically used in the U.S.
have an average seven-day maximum pavement temperature that is within the range of about
50 and about 80 °C and an expected minimum pavement temperature that is within the range
of about 10 and about 40 °C. It is to be noted that as a general rule, PG binders that differ in the
high and low temperature specification by 90 °C or more are typically the result of some sort of
modification in order to improve certain characteristics such as resistance to high temperature
thermal deformation ("creep" or "rutting"), low temperature cracking, or both.
As mentioned above, the paving composition of the present invention is not limited to
any particular asphalt binder or combination of binders. Although any asphalt binder may be
used, it is preferred that the paving composition comprises an asphalt binder or combination of
binders having physical properties suitable for the particular application. The selection of such
an asphalt binder or combination of binders is well known to those of skill in the art. Examples
of commercially available asphalt binders that may be suitable for preparing a paving
composition of the present invention include CONOCO AC-30, DIAMOND SHAMROCK AC-30,
SHELL AR-4000, AMOCO 64-22, CITGO AC-30, CITGO PG 67-22, VALERO PG 64-22, and
HUSKY 85/100.
B. Polyphosphoric acid
A polyphosphoric acid is a series of oxyacids of phosphorous having the general
chemical formula Hn+2(Pn03n+i). More specifically, polyphosphoric acids occur in the P2O5-H2O
system and have a P2O5 content that is above about 74 percent. Polyphosphoric acids are
complex mixtures of ortho- (n=1), pyro- (n=2), tri- (n=3), tetra (n=4), and longer chain polymer
species, the proportions of which are a direct function of the P2O5 content of the acid. Although
polyphosphoric acids may be referred to in terms of P2O5 content, polyphosphoric acids are
typically referred to in terms of an equivalent H3PO4 (phosphoric acid) concentration or
percentage. Preferably, the polyphosphoric acid used in the preparation of the asphalt paving
composition of the present invention has an H3PO4 equivalent concentration of at least about
100%. More preferably, the polyphosphoric acid has an H3PO4 equivalent concentration of at
least about 105%. Still more preferably, the polyphosphoric acid has an H3PO4 equivalent
concentration of at least about 110%. Even more preferably, the polyphosphoric acid has an
H3PO4 equivalent concentration of at least about 115%. Examples of appropriate
polyphosphoric acids include acids having a H3PO4 equivalent content of 105% (P2O5content of
about 76.05%), a H3PO4 equivalent content of 115% (P2O5 content of about 83.29%), or a


H3PO4 equivalent content of 116.4% (P2O5 content of about 84.31%), which are commercially
available from Astaris LLC.
Polyphosphoric acids are not water-based and are less corrosive than a water-based
phosphoric acids, which is advantageous over water-based phosphoric acids. Fror example, the
mixing of phosphoric acid with hot asphalt under typical blending conditions tends to result in
foaming and splattering, whereas polyphosphoric acids are readily incorporated with little or no
foaming and splattering.
Preferably, the amount of polyphosphoric acid added to the paving composition is an
effective amount, that is to say, an amount that increases the adhesion between the asphalt
binder and the aggregate compared to an identical paving composition that contains no
polyphosphoric acid. More preferably, the polyphosphoric acid is added to the paving
composition in an amount that achieves the maximum anti-stripping benefit. Although this
optimum amount depends on several factors including the type of asphalt (i.e., the chemical
composition of the asphalt), the type of aggregate used to make the paving composition, the
moisture content of the asphalt and the aggregate, the inclusion of polymer additives, etc.), it
may be readily determined through routine empirical testing. In general, however, it is believed
that anti-stripping improvements may be observed by including as little as about 0.05% by
weight of polyphosphoric acid in the asphalt binder. Preferably, the concentration of
polyphosphoric acid added to the asphalt is at least about 0.1% by weight of the asphalt binder.
More preferably, the concentration of polyphosphoric acid added to the asphalt is at least about
0.2% by weight of the asphalt binder.
It has also been discovered that the adhesion may be detrimentally affected by
exceeding an upper concentration of polyphosphoric acid. Although this upper concentration
level varies on the particular asphalt, it is preferred that the concentration of polyphosphoric
acid added to the asphalt be no greater than about 2% by weight of the asphalt binder. More
preferably, the concentration of polyphosphoric acid added to the asphalt is no greater than
about 1.5% by weight of the asphalt binder. Still more preferably, the maximum concentration
of polyphosphoric acid is about 1.2% by weight asphalt binder. Even more preferably, the
maximum concentration of polyphosphoric acid is about 1% by weight of the asphalt binder.
Still even more preferably, the concentration of polyphosphoric acid added to the asphalt is
maximum concentration is about 0.7% by weight asphalt binder.
In view of the foregoing, in one embodiment of the present invention the polyphosphoric
acid is at a concentration that is within a range of about 0.05 to about 2.0% by weight of the
asphalt binder. Preferably, the polyphosphoric acid is at a concentration that is within a range
of about 0.1 and about 1.2% by weight of the asphalt binder. More preferably, the


polyphosphoric acid is at a concentration that is within a range of about 0.1 and about 0.7% by
weight of the asphalt binder.
C. .Alkaline anti-strippinq additive
In addition to polyphosphoric acid, the paving composition of the present invention
comprises an alkaline anti-stripping additive. It is contemplated that, typically, the alkaline antl-
stripping additive would be hydrated lime, which comprises calcium hydroxide (Ca(OH)2).
Commercial hydrated lime is a dry powder obtained by treating quicklime (calcium oxide, CaO)
with sufficient water to satisfy its chemical affinity for water, thereby converting the oxides to
hydroxides.
Preferably, the amount of lime added to the paving composition is an effective amount,
that is to say, an amount that increases the adhesion between the asphalt binder and the
aggregate compared to an identical paving composition that contains no lime. More preferably,
the lime is added to the paving composition in an amount that achieves the maximum anti-
stripping benefit. Although this optimum amount depends on several factors including the type
of asphalt (i.e., the chemical composition of the asphalt), the type of aggregate used to make
the paving composition, the moisture content of the asphalt and the aggregate, the inclusion of
polymer additives, etc.), it may be readily determined through routine empirical testing. In
general, it is believed that anti-stripping improvements may be observed by including as little
lime as about 0.5% by weight of the aggregate in the paving composition. Preferably, the
concentration of lime added to the paving composition is at least about 1% by weight of the
aggregate. Additionally, it is preferred that the concentration of lime added to the paving
composition is not so great as to be a detriment to other properties. Typically, the
concentration of lime is no greater than about 2.0% by weight of the aggregate. Preferably, the
concentration of lime is no greater than about 1.5% by weight of the aggregate. As such, in
one embodiment of the present invention the paving composition comprises lime at a
concentration that is between about 0.5 and about 2.0% by weight of the aggregate.
Preferably, the paving composition comprises lime at a concentration that is between about 1
and about 1.5% by weight of the aggregate.
When lime is added to hot mix asphalt, it reacts with the aggregate to strengthen the
bond between the bitumen and the stone. At the same time that it treats the aggregate, lime
also reacts with the asphalt binder. Specifically, it is believed that the lime reacts with highly
polar molecules that can otherwise react in the mix to form water-soluble soaps that promote
stripping. When those molecules react with lime, they form insoluble salts that no longer attract
water (see, e.g., Petersen, J.C , H. Plancher, and P.M. Harnsbergen, "Lime Treatment of


Asphalt to Reduce Age Hardening and Improve Flow Properties," Proceedings, AAPT, Vol. 56,
1987). Additionally, the dispersion of the tiny hydrated lime particles throughout the mix makes
it stiffer and tougher, reducing the likelihood the bond between the asphalt binder and the
aggregate will be broken mechanically, even if water is not present.
The hydrated lime that is used to prepare the paving composition of the present
invention may be added to the aggregate, asphalt, or both according to any appropriate
method. There are several proven and effective methods for adding hydrated lime to asphalt.
Examples of such methods include injecting hydrated lime into a drum mixer, adding the lime in
a pug mill, adding dry hydrated lime to moist aggregate with marination, adding slurry lime to
aggregate with orwithout marination (see, e.g., "How to Add Hydrated Lime to Asphalt," An
Overview of Current Methods, National Lime Association,
http://www.lime.org/publications.html). Typically, the method by which hydrated lime is added
is specified by the state departments of transportation. These state-developed specifications
and procedures are typically tailored to local materials and the capabilities of construction firms
and equipment.
D. Surface-active anti-stripping additives
Additionally, it has been discovered that the paving composition of the present invention
may comprise a surface-active anti-stripping additive. As mentioned above, most of such
additives are amine-type additives and this discovery is surprising because amine-type
additives are considered by some of skill in the art to be incompatible with phosphoric acid
modification. If: is important to note that type of surface-active anti-stripping additive that may
be included in a paving composition of the present invention is not limited to the amine-type, but
also includes, other commercially available surface-active materials that are known by those of
skill in the art to increase adhesion between aggregate and asphalt binder.
Typically, amine-type anti-stripping additives comprise, for example, primary amines,
diamines, triamines, tetramines, polyamines, amido amines, or ethoxylated diamines, etc.
Preferably, a surface-active anti-stripping additive is a liquid so that is more readily mixed
throughout the asphalt. Exemplary commercially available liquid amine anti-stripping additives
include the PAVEBOND and MORLIFE anti-strips commercially available from Rohm and Haas
and the AD-HERE anti-strip available from Arr-Maz Custom Chemicals, Inc.
If included, the concentration of surface-active anti-stripping additive in the paving
composition of the present invention is preferably consistent with the concentration(s)
considered appropriate for the particular application and the associated variables such as type
of asphalt, type of aggregate, etc. Typically, the concentration of surface-active anti-stripping
additives is between about 0.5 and about 1.0% by weight of the asphalt binder.


In another embodiment, however, the paving composition of the present invention is
preferably not modified with liquid anti-stripping additives, in general, and amine-type anti-
strips, in particular. Stated another way, in this embodiment the asphalt binder is preferably
substantially free of liquid amine anti-stripping additives. Specifically, the concentration of such
additives is, in order of increasing preference, less than about 0.5, 0.2, 0.1, 0.05, or 0.01 % by
weight of the asphalt binder, or even 0%.
E. Polymer asphalt modifiers
The pavement composition of the present invention may also comprise a polymer
modifier. Typical polymer asphalt modifiers include styrene-butadiene-styrene copolymers
(SBS), styrene-butadiene copolymers (SB), and elastomeric terpolymers. Commercially
available terpolymers include ELVALOY available from DuPont, which is an ethylene-glycidyl-
acrylate polymer (i.e., it comprises an ethylene backbone modified with a glycidyl functional
group to provide epoxy-like reactive properties and an acrylate functional group to provide
flexibility and elastomeric properties). Additional appropriate polymer modifiers may include
ethylene-vinyl-acetate (EVA) polymers, ethylene-methacrylate (EMA) polymers, styrene-
isoprene copolymers (SIS), epoxy resins, natural rubbers, and polydiolefins such as
polybutadiene and polyisoprene.
If included, the concentration of polymer modifier in the paving composition of the
present invention is preferably consistent with the concentration(s) considered appropriate for
the particular application and the associated variables such as type of asphalt, type of
aggregate, etc. Typically, the concentration of polymer modifiers is between about 2 and about
10% by weight of the asphalt binder. More typically, the concentration of polymer is between
about 2 and about 6% by weight of the asphalt, binder Terpolymers such as the commercially
available ELVALOY modifier typically comprise about 2% by weight of the asphalt binder and
sometimes as little as about 1 % by weight of the asphalt binder.
In another embodiment, however, the paving composition of the present invention is
preferably not modified with polymers. Stated another way, in this embodiment the asphalt
binder is preferably substantially free of polymer modifiers. Specifically, the concentration of
such additives is, in order of increasing preference, less than about 1.0, 0.5, 0.2, 0.1, 0.05, or
0.01% by weight of the asphalt binder, or even 0%.
In view of the foregoing embodiments, the paving composition may also be substantially
free of liquid anti-strips and polymer modifiers. Thus, in one embodiment of the present
invention the paving composition of present invention may consist essentially of asphalt binder,
polyphosphoric acid, lime, and aggregate at the concentrations that are preferably in
accordance with the values set forth herein.


F. Preparation of the Asphalt Binder
The preparation of the asphalt binder may be accomplished by any appropriate means
known in the art such as direct addition with agitation or in-line mixing. Regardless of the
method, the asphalt binder preparation is typically facilitated by increasing the temperature of
the asphalt binder, the polyphosphoric acid, and other additives. To facilitate mixing, the
temperature is increased to at least the softening point of the asphalt. Typically, the
temperature of the mixture is increased to between about 160 and about 200 °C. After the
asphalt is heated to a temperature sufficient for mixing purposes, the polyphosphoric acid and
any other constituents is/are typically introduced into the hot feed of asphalt with agitation
adequate to disperse the polyphosphoric acid and other optional constituents throughout the
asphalt.
Although asphalt binders that comprise asphalt, additives such as polyphosphoric acid,
and polymer modifiers (if present) may be prepared by blending the constituents in-line at the
hot mix plant (often referred to as post-blending), it is preferred that the asphalt, polyphosphoric
acid, and any optional polymer modifier be blended by the asphalt binder supplier before being
delivered to a hot mix asphalt plant (often referred to as pre-blending). Some combinations of
asphalt and additives may be mixed relatively easily using a mixing kettle, while others require
high shear milling or other special mixing operations. This preference, however, should not be
interpreted as an indication that the polyphosphoric acid cannot be mixed with an asphalt
binder (free of, or containing a polymer modifier) at a hot mix asphalt facility. In contrast,
surface-active anti-stripping additives are typically not pre-biended - they are typically blended
with the asphalt at the hot mix facility before the asphalt is mixed with the aggregate. Methods
for mixing surface-active anti-stripping additives and asphalt are well known to those of skill in
the art and any such method may be used to prepare an asphalt paving composition of the
present invention. Likewise, although it may be possible to pre-blend the alkaline anti-stripping
additive (e.g., lime) with the asphalt, such a practice would be atypical. As noted above, lime is
typically added to the paving composition by treating the aggregate before it is mixed with the
asphalt binder.
G. Aggregate
"Aggregate" is a collective term for the mineral materials such as sand, gravel, and
crushed stone that, are used with an asphalt binder to form compound materials such as a
asphalt paving composition. By volume, aggregate typically accounts for at least about 90% by
volume of an asphalt paving composition. For example, it is not uncommon for asphalt paving
compositions to comprise between about 92 and about 96% by volume of aggregate.


The aggregate may comprise natural aggregate, manufactured aggregate, or a
combination of the two. Natural aggregate is typically extracted rock from an open excavation
(i.e., a quarry) that is reduced to usable sizes by mechanical crushing. Natural aggregates
come from rock from three broad geological classifications: igneous, sedimentary, and
metamorphic. Igneous rocks are primarily crystalline that were formed by the cooling of molten
material beneath the earth's crust. Sedimentary rocks were formed from deposited insoluble
material on the bottom of an ocean or lake that was transformed to rock by heat and pressure.
Sedimentary rocks are layered in appearance and are further classified based on the
predominant mineral. For example, sedimentary rocks are generally classified as calcareous
(limestone, chalk, etc.), siliceous (chert, sandstone, etc.) or argillaceous (shale, etc.).
Metamorphic rocks are igneous or sedimentary rocks that have been subjected to enough heat,
pressure, or both that their mineral structure has changed from that of the original rock.
Manufactured aggregate is typically the byproduct of other manufacturing processes such as
slag from metallurgical processing (e.g., steel, tin, and copper production). Manufactured
aggregate also includes specialty materials that are produced to have a particular physical
characteristic not found in natural rock such as low density. The mineral composition of the
aggregate largely,determines the physical and chemical characteristics of the aggregate and
how it performs as a pavement material. In particular, the composition of the aggregate
significantly affects the susceptibility or propensity of a pavement composition to undergo
stripping. In fact, the physiochemical surface properties of the aggregate may play a much
larger role in stripping of hot mixed asphalt than the properties of the asphalt binder. Although
the complex phenomena related to the displacement of the asphalt binder from the surfaces of
the aggregate particles by water is not yet fully understood, it is known that the aggregate's
chemical composition or mineral content is a significant factor. For example, an aggregate's
affinity to water or asphalt plays a role. Some aggregates have an affinity for water over
asphalt (hydrophilic), which tends to make them more susceptible to stripping. These
aggregates tend to be acidic and examples include quartzite, sandstone, and granite. On the
other hand, aggregates with an affinity for asphalt over water (hydrophobic) tend to be less
susceptible to stripping. These aggregates tend to be basic and examples include marble,
limestone, basalt, and dolomite. The paving composition of the present invention may
comprise any appropriate type of paving aggregate. As indicated by the examples below,
however, the improvement in adhesion is particularly evident when using aggregate known to
be susceptible to stripping such as Lithonia granite.
Thus, aggregate may be selected to improve the anti-stripping property of the paving
composition. The selection of aggregate, however, typically is not based solely on its
propensity for stripping. Other factors such as hardness, toughness, abrasion resistance,


fatigue resistance, cost, availability, etc., are typically considered and may be of greater
importance than anti-stripping. For example, although limestone is generally considered to be
a good aggregate in terms of anti-stripping, it is considered a poor aggregate in terms of
hardness or toughness.
An aggregate is also selected based on the maximum size or mix size of its particles.
Examples of mix sizes include 4.75 mm, 9.5 mm, 12.5 mm, 19.0 mm, 25.0 mm, and 37.5 mm.
In addition to mix size, gradation (i.e., the relative amounts of different sized particles, which is
typically determined by sieve analysis) tends to be a selection factor. Examples of typical
gradations include: dense or well-graded, which is the most widely used in the U.S.; gap
graded, which tends to be prone to segregation during placement of the paving composition;
open graded, which may result in a greater percentage of voids because there are not enough
small particles in between larger particles; and uniformly graded in which all the particles are
essentially the same size.
The selection of an appropriate aggregate type and its properties (e.g., mix size,
gradation, moisture content, etc.) for a particular application is based on many factors such as
pavement location, traffic type, temperature, etc. and is known and understood by those of skill
in the art.
H. Method of Preparing an Asphalt Paving Composition
Because it is generally understood by those of skill in the art that the extent of
enhancement or detriment to properties such as anti-stripping and other properties such as
rutting, stiffness, abrasion resistance, oxidation and aging, and cracking depend in large part on
numerous variables such as the type(s) of asphalt(s), type(s) of aggregate(s), asphalt
modification parameters including the temperature, time, type(s) and concentration(s) of
modifying agents, an empirical determination of the optimum materials, concentrations,
processing conditions, or combinations thereof is preferred to produce an asphalt concrete
having the highest degree of anti-stripping behavior along other acceptable properties.
in general, an acceptable asphalt paving composition may be prepared by mixing the
asphalt binder, typically modified with the polyphosphoric acid and any other modifiers, and the
aggregate, typically treated with lime, at an elevated temperature (e.g., greater than about 165
°C) for a duration to coat the aggregate (e.g., between about 1 and about 4 hours) according
any method known in the art. Common methods include batch preparation, the parallel-flow
drum-mix, and the counter-flow drum mix. Although different methods may be used to combine
the aggregate with the asphalt binder, the resulting paving composition is essentially the same -
— aggregate and binder in an amount sufficient to coat the aggregate and adequately bind the
paving composition. Typically, the amount of asphalt binder is at least about 4% by weight with


the remainder of the paving composition comprising the aggregate, which is preferably treated
with lime. Additionally, the paving composition typically does not comprise more than about 7%
by weight of the asphalt binder because, among other things, it becomes significantly more
costly and typically more prone to deformation. In view of this, the concentration of asphalt
binder in the paving composition is preferably between about 4 and about 7% by weight. More
preferably, the concentration asphalt binder is between about 4.5 and about 6.5% by weight.
I. Use of an Asphalt Paving Composition
It is important to note that although the addition of phosphoric acid and lime may be
used to improve the adhesion between the asphalt and the aggregate, other factors related to
how a paving composition is applied play a significant role in the durability of a pavement. For
example, it is well known by those of skill in the art that the thickness of the pavement ("lift
thickness") and the degree of compaction, often measured as void percentage, affect the
permeability of the pavement to water. In general, it is believed that that lift thickness should be
between three and about four times that of the aggregate mix size. For example, the preferred
lift size for a paving composition containing a 9.5 mm mix size is about 38 mm (about 1.5
inches). The proper mix selection and the lift thickness aids the compaction of the paving
composition thereby reducing permeability. Preferably, the compaction of the paving
composition is to a void percentage that is less than about 7.5%. Typically, the compaction
may be such that a void percentage as low as about 4-5% may be attained.
Example 1 - Evaluation of Moisture Sensitivity using the Texas Boil Test
The Texas Boil Test (Texas Method Tex-530-C) or ASTM D 3625, "Effect of Water on
Bituminous-Coated Aggregate Using Boiling Water", is a subjective test that is widely used in
the asphalt binder industry to assess the adherence of an asphalt binder to a particular
aggregate. In this test the asphalt binder is mixed with the aggregate and the temperature of
the mixture is increased to about 135 °C. Upon reaching about 135 °C, the mixture is poured
into a container (e.g., a beaker) of boiling water and the contents are boiled for about ten
minutes. The asphalt binder is then separated from the water and allowed to dry at room
temperature. The dried asphalt is evaluated by visually estimating the percentage of aggregate
that is covered with adhering asphalt binder. Typically, a control sample of asphalt concrete
(i.e., a concrete without an anti-stripping additives) is simultaneously tested to more accurately
evaluate the effectiveness of the additive(s).
These tests were performed to evaluate the effect on stripping that different
concentrations of 105% polyphosphoric acid would have on three asphalts with significantly
different chemistries. Also evaluated was the effect of two liquid amine anti-stripping additives


and lime in conjunction with the polyphosphoric acid. The two liquid amine anti-stripping
additives were PAVEBOND (light grade) available from Rohm & Haas and ADHERE (HP plus)
available from Arr-Maz Custom Chemicals, Inc. The aggregate was 9.5 mm Lithonia granite
available from Martin Marietta. This aggregate was selected because it is known to be
particularly susceptible to stripping. The selected asphalts were a PG 64-22 from Valero/UDS,
a PG 67-22 available from Citgo, and a PG 58-22 available from Husky.
The concentrations of the constituents and the results of the Texas Boil Test are set
forth in Table A below.


The foregoing data indicates the following unexpected results. First, the combination of
about 0.5% polyphosphoric acid and about 2.0% lime-treated aggregate exhibited the best
overall anti-stripping properties. Second, the data indicates that the paving compositions that

comprised about 0.5% polyphosphoric acid with and without 0.5% of a liquid anti-strip additive
had similar degrees of adhesion. Third, high concentrations of polyphosphoric acid, by itself,
do not improve adhesion. As such, it is believed that exceeding a certain concentration of
polyphosphoric (e.g., about 2.0%), with lime or liquid anti-strip additives, decreases the
adhesion of the asphalt binder to the aggregate. Fourth, the control (untreated) asphalt
exhibited the worst adhesion. Fifth, aging the pavement composition (i.e., maintaining it at
about 49 °C for about one week) improved the anti-stripping nature cf the pavement
composition. Lastly, including about 0.5% polyphosphoric acid in the asphalt binder seemed to
have an equivalent effect as adding 2.0% lime to the aggregate. In summary, the an
improvement in adhesion is realized by selecting concentrations of polyphosphoric acid and
lime within readily determinable ranges.
Example 2 - Rheoloqical Evaluation with the Dynamic Shear Rheometer
Several of the asphalt binders set forth in Example 1 were tested according to the
standard dynamic shear rheometer test (AASHTO TP 5). The test involves measuring the
complex shear modulus (G*) and the phase angle (5), which is the time lag expressed in
radians between the maximum applied shear stress and the maximum resulting shear strain.
The complex shear modulus (G*) and the phase angle (8) are used as predictors for rutting and
fatigue cracking. To resist rutting, an asphalt binder should be stiff (not deform too much) and it
should be elastic (able to return to its original shape after load deformation), which corresponds
to a large elastic portion of the complex shear modulus (G*cos8). Intuitively, the higher the G*
value, the stifferthe asphalt binder is (resistant to deformation), and the lower the 5 value, the
greater the elastic portion of G* is (ability to rebound to its original shape). To resist fatigue
cracking, an asphalt binder should be elastic and not too stiff (excessively stiff substances will
crack rather than deform and rebound). The viscous portion of the complex shear modulus
(G*sin5) is preferably small. Although they appear similar, specifying a large G*cos8 and a
small G*sinS are not the same. They both typically require small phase angles (8), but the key
is having a complex shear modulus (G*) that is neither too large or too small.
The concentrations of the constituents and the results of the dynamic shear rheometer
testing are set forth in Table B below.


Among other things, the foregoing data indicates that the addition of 0.5% of a liquid
amine anti-strip additive (an ether amine) produced mixed results on the viscous portion of the
complex shear modulus (G*sinδ). Specifically, for the PG 64-22 asphalt, the G*sinδ was
decreased by adding the liquid amine additives, with the PAVEBOND additive providing a
larger decrease. For the PG 67-22 asphalt, the PAVEBOND increased the G*sinδ and the
ADHERE decreased the G*sinδ. Forthe PG 58-22 asphalt, both additives increased the
G*sinS, but the ADHERE provided a greater increase. Further, a significant increase to the
G*sinδ was observed by the addition of 0.5% polyphosphoric acid without a liquid amine
additive. In fact, the increase was large enough to raise the high temperature grade of the
binder. Additionally, the G*sinδ results from combining 0.5% polyphosphoric acid and liquid,
amine additives were mixed. Specifically, they were neutral for the PG 64-22 and PG 67-22
asphalts and significantly increased for the PG 58-22 asphalt. Still further, the addition of 2.0%
polyphosphoric acid, with and without liquid amine additives, significantly increased the G*sinδ.
Example 3 - Evaluation of Moisture Sensitivity using the Lottman Procedure

The Lottman Procedure, which is also known according to the AASHTO designation T
283-89(1993) and is entitled "Resistance of Compacted Bituminous Mixture-Induced Damage",
is performed to measure the effects of saturation and accelerated water conditioning on the
diametral tensile strength of compacted bituminous mixtures. The samples were prepared
using about 6.4% asphalt binder. The results of the Lottman Procedure may be used to predict
long-term stripping susceptibility of said mixtures and to evaluate the effectiveness of anti-
stripping additives that may be added to an asphalt binder or an aggregate.
The tensile strengths compacted samples are typically tested before and after being
conditioned. Typically, three samples are used for each test. The water conditioning process
comprises vacuum saturating them with moisture, maintaining the samples at about 60 °C for
about 24 hours, and then placing the samples in a water bath that is at about 25 °C for about
two hours. Additionally, a freeze-thaw cycle may be added to the conditioning process. The
tensile strengths of the unconditioned and conditioned samples are determined. Generally, if
the tensile strengths of the conditioned samples are at least about 70 percent of the
unconditioned samples the particular asphalt binder is considered to be resistant to moisture
induced damage. The different sample compositions and test results are set forth in Table C
beiow.


The data in Table C is consistent with some generally known trends such as the
understanding that amine anti-strips tend to reduce the viscosity of an asphalt binder and are
expected to decrease the strength of a paving composition. It is also generally known that lime,
alone, and polyphosphoric acid, alone, tend to increase the viscosity of an asphalt binder and
are expected to increase the strength of a paving composition. Unexpectedly, however, the
combination of polyphosphoric acid and lime provided the greatest strength increase. Also
unexpectedly, the combination of amine anti-strip and polyphosphoric acid had a strength that
was significantly less than the other modified samples.
Example 4 - Hamburg Wheel Test
In this procedure, specimens comprising an asphalt binder and aggregate are prepared
in the form of compacted slabs that are mounted and placed in temperature controlled water
bath (e.g., 50-60 °C). The slabs are compacted using a linear kneading compactor that
achieves the desired density without fracturing aggregate. The prepared samples are placed in
the device and the wheels are set in motion and data recording starts. This data, which may be
collected automatically per wheel pass, includes rut depth and bath temperature. Often this
test is performed until 20,000 cycles or 20 mm of deformation, whichever is reached first. For

this evaluation, however, the test was performed for 8,000 cycles and the rut depth was
determined. A 10 mm rut depth was the criteria to determine if a sample passed or failed.
These parameters are currently in use by several state Departments of Transportation because
they provide a quicker and more cost effective evaluation. It is to be noted that a test failure
does not necessarily mean that such a paving composition would actually fail if used in the
field. The results of the test are merely a method of predicting a paving composition's
resistance to rutting and stripping under extreme conditions of moisture exposure and
evaluating relative performance of different paving compositions.
The asphalt binder compositions and their dynamic shear rheometer data are set forth ir
Table D below.

The data in Table D is consistent with the data of the other examples and demonstrates the
rheological effects induced by the polyphosphoric acid and the other additives at relatively smal
concentrations. It was expected that there would be an indirect correlation of rut depth to
complex shear modulus (G*). Specifically, it was expected that at greater the G* values the rut
depth would be reduced.

The pavement compositions, which were made with the asphalt binders set forth in
Table D, and the Hamburg Test results are set forth in Table E below. The initial evaluations
were directed to establishing a test temperature that would result in the control (a neat or
untreated asphalt binder mixed with the Lithonia granite aggregate) failing and a sample that
comprised a neat asphalt binder and lime treated Lithonia granite aggregate passing. The
temperature that differentiated the samples was about 50 °C. In addition to the rut depth
measurement, each of the samples was visually inspected to determine the percent of stripping
caused by the testing.


Among other things, the data in Table E generally indicates that the addition of
polyphosphoric acid has a significant effect on the potential performiance of a paving

composition. Another general observation was that there was some correlation between the rut
depth and the degree of stripping. Further, it appears that resistance to deformation may be
more complex than simply being related to the complex shear modulus. More specifically, it
was determined that the combination of polyphosphoric acid modified asphalt binder and lime
treated aggregate provided the best overall results (i.e., the second smallest rut depth and the
less than about 5% stripping). Additionally, there did not seem to be a significant performance
difference between the 105% and the 115% phosphoric acids. It was also observed that the
relatively high concentration of asphalt binder (i.e., about 6.5%) produced a rut depth resulting
in failure.
All references cited in this specification, including without limitation all journal articles,
brochures, manuals, periodicals, texts, manuscripts, website publications, and any and all other
publications, are hereby incorporated by reference. The discussion of the references herein is
intended merely to summarize the assertions made by their authors and no admission is made
that any reference constitutes prior art. Applicants reserve the right to challenge the accuracy
and pertinence of the cited references.
It is lo be understood that the above description is intended to be illustrative and not
restrictive. Many embodiments will be apparent to those of skill in the art upon reading the
above description. The scope of the invention should therefore be determined not with
reference to the above description alone, but should be determined with reference to the claims
and the full scope of equivalents to which such claims are entitled.
When introducing elements of the present invention or an embodiment thereof, the
articles "a", "an", "the" and "said" are intended to mean that there are one or more of the
elements. The terms "comprising", "including" and "having" are intended to be inclusive and
mean that there may be additional elements other than the listed elements. Additionally, it is to
be understood an embodiment that "consists essentially of or "consists of specified
constituents may also contain reaction products of said constituents.
The recitation of numerical ranges by endpoints includes all numbers subsumed within
that range. For example, a range described as being between 1 and 5 includes 1, 1.6, 2,2.8,
3,3.2,4,4.75, and 5.

WE CLAIM :
1. An asphalt paving composition comprising an asphalt binder, aggregate, and
an alkaline anti-stripping additive, wherein the asphalt binder comprises asphalt
and polyphosphoric acid.
2. The asphalt paving composition as claimed in claim 1 wherein the asphalt
binder is at a concentration that is between 4 and 7% by weight of the asphalt
paving composition.
3. The asphalt paving composition as claimed in claim 1 wherein the aggregate
is at a concentration that is at least 90% by volume of the asphalt paving
composition.
4. The asphalt paving composition as claimed in claim 1 wherein the
polyphosphoric acid is at a concentration that is at least 0.05% by weight of the
asphalt binder.
5. The asphalt paving composition as claimed in claim 1 wherein the
concentration of the polyphosphoric acid is no greater than 2.0% by weight of the
asphalt binder.
6. The asphalt paving composition as claimed in claim 1 wherein the alkaline
anti-stripping additive comprises calcium hydroxide.
7. The asphalt paving composition as claimed in claim 1 wherein the alkaline
anti-stripping additive is at a concentration that is at least 0.5% by weight of the
aggregate.


8. The asphalt paving composition as claimed in claim 6 wherein the
concentration of the alkaline anti-stripping additive is no greater than 2% by weight
of the aggregate.
9. The asphalt paving composition as claimed in claim 1 wherein the asphalt
binder comprises a surface-active anti-stripping additive.
10. The asphalt paving composition as claimed in claim 8 wherein the surface-
active anti-stripping additive comprises an amine.
11. The asphalt paving composition as claimed in claim 8 wherein the surface-
active anti-stripping additive is at a concentration that is between 0.5 and 1.0% by
weight of the asphalt binder.
12. The asphalt paving composition as claimed in claim 1 wherein the asphalt
binder comprises a polymer modifier.
13. The asphalt paving composition as claimed in claim 11 wherein the polymer
modifier is selected from the group consisting of a styrene-butadiene-styrene
copolymer, a styrenebutadiene copolymer, a terpolymer, an ethylene-vinyl-acetate
polymer, an ethylenemethacrylate polymer, a styrene-isoprene copolymer, an epoxy
resin, a natural rubber, a polydiolefin, and combinations thereof.
14. The asphalt paving composition as claimed in claim 11 wherein the polymer
modifier is at a concentration that is at least 1.0% by weight of the asphalt binder.
15. The asphalt paving composition as claimed in claim 1 wherein the
concentration of the polymer modifier is no greater than 10.0% by weight of the
asphalt binder.


16. The asphalt paving composition as claimed in claim 1 consisting essentially
of the asphalt, the aggregate, the polyphosphoric acid, and the alkaline anti-
stripping additive.
17. A method for improving the resistance to stripping of an asphalt pavement
prepared using an asphalt paving composition that comprises asphalt and
aggregate, the method comprising modifying the asphalt paving composition by
adding polyphosphoric acid and an alkaline anti-stripping additive to the asphalt
paving composition.
18. A method for preparing an asphalt paving composition, the method
comprising mixing a modified asphalt binder that comprises an asphalt and
polyphosphoric acid with aggregate and an alkaline anti-stripping additive to
produce the asphalt paving composition.
19. The method as claimed in claim 18 wherein the modified asphalt binder is at
a concentration that is between 4 and 7% by weight of the asphalt paving
composition, the aggregate is at a concentration that is at least 90% by volume of
the asphalt paving composition, the polyphosphoric acid has an H3PO4 equivalent
concentration of at least 100% and is at a concentration that is between 0.05% and
2.0% by weight of the modified asphalt binder, and the alkaline anti-stripping
additive is a concentration that is between 0.5 and 2.0% by weight of the
aggregate.
20. The method as claimed in claim 18 wherein the modified asphalt binder
consists essentially of asphalt and polyphosphoric acid.


An asphalt paving composition and method of preparation thereof are
disclosed. The asphalt paving composition comprises an asphalt binder, aggregate,
and an alkaline anti-stripping additive, wherein the asphalt binder comprises
asphalt and polyphosphoric acid. The method for improving the resistance to
stripping of an asphalt pavement prepared using an asphalt paving composition
that comprises asphalt and aggregate involves modifying the asphalt paving
composition by adding polyphosphoric acid and an alkaline anti-stripping additive to
the asphalt paving composition.

Documents:

03898-kolnp-2006 abstract.pdf

03898-kolnp-2006 claims.pdf

03898-kolnp-2006 correspondence others.pdf

03898-kolnp-2006 description(complete).pdf

03898-kolnp-2006 form-1.pdf

03898-kolnp-2006 form-3.pdf

03898-kolnp-2006 form-5.pdf

03898-kolnp-2006 international publication.pdf

03898-kolnp-2006 international search authority report.pdf

03898-kolnp-2006 pct others form.pdf

03898-kolnp-2006 priority document.pdf

03898-kolnp-2006-assignment.pdf

03898-kolnp-2006-correspondence-1.1.pdf

03898-kolnp-2006-correspondence-1.2.pdf

03898-kolnp-2006-form-3-1.1.pdf

03898-kolnp-2006-g.p.a.pdf

3898-KOLNP-2006-ABSTRACT 1.1.pdf

3898-KOLNP-2006-ABSTRACT.pdf

3898-KOLNP-2006-AMANDED CLAIMS 1.1.pdf

3898-KOLNP-2006-AMANDED CLAIMS.pdf

3898-KOLNP-2006-AMANDED PAGES OF SPECIFICATION 1.1.pdf

3898-KOLNP-2006-AMANDED PAGES OF SPECIFICATION.pdf

3898-kolnp-2006-assignment.pdf

3898-KOLNP-2006-CORRESPONDENCE 1.5.pdf

3898-KOLNP-2006-CORRESPONDENCE 1.6.pdf

3898-KOLNP-2006-CORRESPONDENCE-1.3.pdf

3898-KOLNP-2006-CORRESPONDENCE-1.4.pdf

3898-KOLNP-2006-CORRESPONDENCE-1.7.pdf

3898-kolnp-2006-correspondence.pdf

3898-KOLNP-2006-DESCRIPTION (COMPLETE).pdf

3898-kolnp-2006-examination report.pdf

3898-KOLNP-2006-FORM 1.1.1.pdf

3898-KOLNP-2006-FORM 1.pdf

3898-kolnp-2006-form 18.1.pdf

3898-kolnp-2006-form 18.pdf

3898-KOLNP-2006-FORM 2.1.1.pdf

3898-KOLNP-2006-FORM 2.pdf

3898-KOLNP-2006-FORM 3-1.1.pdf

3898-KOLNP-2006-FORM 3-1.2.pdf

3898-kolnp-2006-form 3.2.pdf

3898-KOLNP-2006-FORM 3.pdf

3898-kolnp-2006-form 5.pdf

3898-KOLNP-2006-FORM-27.pdf

3898-kolnp-2006-gpa.pdf

3898-kolnp-2006-granted-abstract.pdf

3898-kolnp-2006-granted-claims.pdf

3898-kolnp-2006-granted-description (complete).pdf

3898-kolnp-2006-granted-form 1.pdf

3898-kolnp-2006-granted-form 2.pdf

3898-kolnp-2006-granted-specification.pdf

3898-KOLNP-2006-OTHERS.pdf

3898-kolnp-2006-others1.1.pdf

3898-KOLNP-2006-PETITION UNDER RULE 137 1.1.pdf

3898-KOLNP-2006-PETITION UNDER RULE 137.pdf

3898-KOLNP-2006-REPLY TO EXAMINATION REPORT.pdf

3898-kolnp-2006-reply to examination report1.1.pdf


Patent Number 249233
Indian Patent Application Number 3898/KOLNP/2006
PG Journal Number 41/2011
Publication Date 14-Oct-2011
Grant Date 12-Oct-2011
Date of Filing 22-Dec-2006
Name of Patentee ICL PERFORMANCE PRODUCTS LP
Applicant Address 622 EMERSON ROAD ST. LOUIS MISSOURI
Inventors:
# Inventor's Name Inventor's Address
1 FALKIEWICZ, MICHAEL 63 MUIRFIELD SPRING COURT ST.CHARLES MISSOURI-63304
PCT International Classification Number C08L 95/00
PCT International Application Number PCT/US2005/021355
PCT International Filing date 2005-06-16
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 60/582,118 2004-06-23 U.S.A.