Title of Invention

A FILTER MEDIUM AND PROCESS FOR MAKING IT

Abstract This invention discloses A filter medium comprising: a microporous structure having a mean flow path of 0.6 to 2 micron; and a microbiological interception enhancing agent comprising a cationic metal complex such as herein described capable of imparting a positive charge on at least a portion of said microporous structure. This invention also discloses a process for making said filter medium.
Full Text A FILTER MEDIUM AND PROCESS FOR MAKING IT
The present invention is directed to filter media having microbiological
interception capability, filtration systems containing such filter media, and
methods of making and using same.
Modern consumer water filters often provide 'health claims' including
reduction of particulates, heavy metals, toxic organic chemicals, and select
microbiological threats. These filtration systems have been able to intercept
microorganisms such as Cryptosporidium and Giardia using roughly 1.0
micron structures. However, in order to provide microbiological interception
of even smaller microbiological threats such as viruses, a filter medium having
a sub-micron microporous structure is required. Prior art filtration systems
often attempt to achieve broad microbiological interception using filter media
with insufficiently small pore size and with poor physical integrity. The
balance between the necessary pore structure required for successful
microbiological interception and satisfactory filter performance has not been
achieved. In addition, prior art systems did not provided devices capable of
operating in the presence of 'interferences' consisting of substances that cause
a loss of filtration performance.
Summary of the Invention
The present invention is directed to, in a first aspect, a filter medium
comprising: a microporous structure having a mean flow path of less than or
equal to about 1 micron; and a microbiological interception enhancing agent
comprising a catlonic metal complex capable of imparting a positive charge on
at least a portion of the microporous structure.
In another aspect, the present invention is directed to a composite filter
medium comprising: as adsorbent prefilter having immobilized therein a

material capable of removing charge-reducing contaminants; a microporous
structure, disposed downstream from the adsorbent layer, comprising a
plurality of nanofibers, the microporous structure having a mean flow path of
less than about 0.6 micron; and a microbiological interception enhancing
agent comprising a silver-cationic material-halide complex having a high
charge density, coated on at least a portion of a surface of at least some of the
plurality of fibers of the fiber matrix.
In yet another aspect, the present invention is directed to a filter system
comprising: a granular bed of particles capable of removing charge-reducing
contaminants; a microporous structure, disposed downstream from the
granular bed, having a mean flow path of less than about 0.6 micron; and a
microbiological interception enhancing agent comprising a silver-cationic
material-halide complex having a high charge density, coated on at least a
portion of a surface of the microporous structure.
In still yet another aspect, the present invention is directed to a filter
system comprising: a solid composite block comprising a material capable of
removing charge-reducing contaminants; a microporous structure, disposed
downstream from the block, having a mean flow path of less than about 2.0
microns; and a microbiological interception enhancing agent comprising a
silver-cationic material-halide complex having a high charge density, coated
on at least a portion of a surface of the microporous structure.
In still yet another aspect, the present invention is directed to a process
of making a filter medium comprising the steps of: providing a microporous
structure having a mean flow path of less than about 1 micron; and coating at
least a portion of the microporous structure with a microbiological interception
enhancing agent, the microbiological interception enhancing agent comprising
a cationic metal complex capable of imparting a positive charge on at least a
portion of the microporous structure.

In a further aspect, the present invention is directed to a process for
making a filter medium comprising the steps of. providing a plurality of
nanofibers; coating at least a portion of a surface of at lleast some of the
plurality of nanofibers with a microbiological interception enhancing agent,
the microbiological intercepting agent comprising a cationic metal complex;
and forming the fibers into a microporous structure having a mean flow path of
less than about 1 micron.
In still a further aspect, the present invention is directed to a process for
making a filter medium comprising the steps of: providing a plurality of
polymer nanofibers; coating at least a portion of a surface of at least some of
the plurality of polymer nanofibers with a microbiological interception
enhancing agent, the microbiological intercepting agent comprising a cationic
metal complex; and forming a microporous structure having a mean flow path
of less than about 1 micron.
In still a further aspect, the present invention is directed to a process for
making a filter medium comprising the steps of: providing a plurality of
cellulose nanofibers; coating at least a portion of a surface of at least some of
the plurality of cellulose fibers with a microbiological interception enhancing
agent, the microbiological intercepting agent comprising a cationic metal
complex; and forming a microporous structure having a mean flow path of less
than about 1 micron.
In still yet a further aspect, the present invention is directed to a process
of making a filter medium comprising the steps of: providing a membrane
having a mean flow path of less than about 1 micron; and coating at least a
portion of the membrane with a microbiological interception enhancing agent,
the microbiological interception enhancing agent comprising a cationic metal
complex capable of imparting a positive charge on at least: a portion of the
membrane.

In still yet a further aspect, the present invention is directed to a process
for making a filter medium comprising the steps of: providing a plurality of
nanofibers; coating at least a portion of a surface of at least some of the
plurality of the nanofibers with a microbiological interception enhancing
agent, the microbiological intercepting agent comprising a silver-amine-halide
complex having a medium to high charge density and a molecular weight
greater than 5000 Daltons; and forming a microporous structure having a
mean flow path of less than or about 0.6 microns.
In still yet a further aspect, the present invention is directed to a process
for making a filter system comprising the steps of: providing an adsorbent
prefilter comprising a material capable of removing charge-reducing
contaminants from an influent, wherein the material is immobilized into a
solid composite block; providing a plurality of nanofibers; coating at least a
portion of a surface of at least some of the plurality of the nanofibers with a
microbiological interception enhancing agent, the microbiological intercepting
agent comprising a silver-amine-halide complex having a medium to high
charge density and a molecular weight greater than 5000 Daltons; and forming
a microporous structure having a mean flow path of less than or about 0.6
microns.
In still yet a further aspect, the present invention is directed to a method
of removing microbiological contaminants in a fluid comprising the steps of:
providing a filter medium having a microporous structure having a mean flow
path of less than about 1 micron, the microporous structure having coated on
at least a portion thereof a microbiological interception enhancing agent
comprising a cationic metal complex wherein the cationic material has a
medium to high charge density and a molecular weight greater than about
5000 Daltons; contacting the fluid to the filter medium for greater than about 3
seconds; and obtaining at least about 6 log reduction of microbiological

contaminants smaller than the mean flow path of i:he filter medium, that pass
through the filter medium.
In still yet a further aspect, the present invention is directed to a gravity-flow
filtration system for treating, storing, and dispensing fluids comprising: a first
reservoir for holding a fluid to be filtered; a filter medium in fluid communication
with the first reservoir, the filter medium comprising a microporous structure with a
mean flow path of less than about 1 micron, and wherein the filter medium is so
treated as to provide at least about 4 log reduction of microbiological contaminants
smaller than the mean flow path of the filter medium; and a second reservoir in fluid
communication with the filter medium for collecting a filtered fluid.
Accordingly the present invention provides a filter medium comprising:
a microporous structure having a mean flow patn of 0.6 to 2 micron; and
a microbiological interception enhancing agent comprising a cationic metal
complex such as herein described capable of imparting a positive charge on at least
a portion of said microporous structure.
The invention also provides a process of making the filter medium of claim
1 comprising the steps of:
providing a microporous structure having a mean flow path of 1 micron;
and
coating at least a portion of the microporous structure with a
microbiological interception enhancing agent, the microbiological
interception enhancing agent comprising a cationic metal complex capable
of imparting a positive charge on at least a portion of the microporous
structure.
Brief Description of the / Drawings

The features of the invention believed to be novel and the elements
characteristic of the invention are set forth with particularly in the appended claims.
The figures are for illustration purposes only and are not drawn to scale. The
invention itself, however, both as to organization and method of operation, may
best be understood by reference to the description of the preferred embodiment(s)
that follows taken in conjunction with the accompanying drawings in that:
Fig. 1 is a side plan view of a filter incorporating the filter media of
the present invention.
Fig. 2 is a cross sectional view of the filter of Fig. 1 taken at lines 2-2.
Fig. 3 is a front plan view of an exemplary gravity flow filtration
system of the present invention.
Fig. 4 is a perspective view of another exemplary gravity flow
filtration system of the present invention.

Detailed Description of the Invention
In describing the preferred embodiment of the present invention,
reference will be made herein to Figs. 1 to 4 of the drawings in that like
numerals refer to like features of the invention. Features of the invention are
not necessarily shown to scale in the drawings.
Definitions
As used herein, "absorbent" shall mean any material that is capable of
absorbing impurities primarily by drawing the impurities into its inner
structure.
As used herein, "adsorbent" shall mean any material that is capable of
adsorbing impurities primarily by physical adsorption to its surface.
As used herein, "adsorbent filter medium" or "adsorbent prefiltration
medium" shall mean a filter medium made with an adsorbent such as, for
example, activated carbon. Exemplary of an adsorbent filter medium is
PLEKX®, commercially available from KX Industries, LP. of Orange,
Connecticut.
As used herein, "binder" shall mean a material used principally to hold
other materials together.
As used herein, "Canadian Standard Freeness"' or "CSF* shall mean a
value for the freeness or drainage rate of pulp as measured by the rate that a
suspension of pulp may be drained. This methodology is well known to one
having skill in the paper making arts.
As used herein, "composite filter medium" shall mean a filter medium
that combines a prefilter, an adsorbent prefiltration medium, and the
microbiological interception enhanced filter medium of the present invention,
into a single composite structure. In some cases, the prefilter may be absent or
its function assumed by the adsorbent prefiltration medium.

As used herein, "contaminant reduction" shall mean attenuation of an
impurity in a fluid that is intercepted, removed, or rendered inactive,
chemically or biologically, in order to render the fluid safer as, for example for
human use, or more useful, as in industrial applications.
As used herein, "fiber" shall mean a solid that is characterized by a high
aspect ratio of length to diameter of, for example, several hundred to one. Any
discussion of fibers includes whiskers.
As used herein, "filter medium" shall mean a material that performs
fluid filtration.
As used herein, "fluid" shall mean a liquid, gas, or combination thereof.
As used herein, "forming" shall mean converting a loose, unstructured
substance into a cohesive, uniform structure. For example, the conversion of
loose fibers into a paper.
As used herein, "intercept" or "interception" are taken to mean
interfering with, or stopping the passage of, so as to affect, remove, inactivate
or influence.
As used herein, "log reduction value" or "LRV shall mean the logio of
the number of organisms in the influent divided by the number of organisms in
the effluent of a fi Iter.
As used herein, "membrane" shall mean a porous medium wherein the
structure is a single continuous solid phase with a continuous pore structure.
As used herein, "microbiological interception enhanced filter medium"
shall mean a filter medium having a microporous structure where at least a
portion of its surface is treated with a microbiological interception enhancing
agent.
As used herein, "microorganism" shall mean any living organism that
may be suspended in a fluid, including but not limited to bacteria, viruses,
fungi, protozoa, and reproductive forms thereof including cysts and spores.

As used herein, 'microporous structure* shall mean a structure that has
a mean flow path less than about 2.0 microns, and often less than about 1.0
micron.
As used herein, "nanofiber" shall mean a fiber having a diameter less
than about 3.0 millimeters.
As used herein, 'natural organic matter" or "NOM" shall mean organic
matter often found in potable or non-potable water, a portion of which reduces
or inhibits the zeta potential of a positively charged filter medium. Exemplary
of NOM are polyanionic acids such as, but not limited to, humic acid and
fulvic acid.
As used herein, "nonwoven" means a web or fabric or other medium
having a structure of individual fibers that are interlaid, but not in a highly
organized manner as in a knitted or woven fabric. Nonwoven webs generally
may be prepared by methods that are well known in the art. Examples of such
processes include, but are not limited to, and by way of illustration only,
meltblowing, spunbonding, carding, and air laying.
As used herein, 'paper" or "paper-like" shall mean a generally flat,
fibrous layer or mat of material formed by a wet laid process.
As used herein, "particle* shall mean a solid having a size range from
the colloidal to macroscopic, and with no specific limitation on shape, but
generally of a limited length to width ratio.
As used herein, 'prefilter* shall mean a filter medium generally located
upstream from other filtration layers, structures or devices, and capable of
reducing particulate contaminants prior to the influent contacting subsequent
filtration layers, structures or devices.
As used herein, 'sheet" shall mean a roughly two-dimensional structure
having a length and a width that are significantly greater than its thickness.

As used herein, "whisker" shall mean a filament having a limited aspect
ratio and intermediate between the aspect ratio of a particle and a fiber. Any
discussion of fibers includes whiskers.
The Microbiological Interception Enhanced Filter Medium
A filter medium of the present invention includes a microporous
structure that provides microbiological interception capability using a
combination of an appropriate pore structure and a chemical treatment. The
microporous structure comprises any material that is capable of having a mean
flow path of less than about 2.0 microns. Preferably, the microporous
structure comprises nanofibers formed into a nonwoven or paper-like
structure, but may include whiskers, or be a membrane. The tight pore
structure of the microbiological interception enhanced filter medium of the
present invention provides short diffusion distances from the fluid to the
surface of the filter medium. The chemical treatment process used to treat the
surface of the microporous structure utilizes a synergistic interaction between a
cationic material and a biologically active metal, that when combined, provide
broad-spectrum reduction of microbiological contaminants on contact. The
charge provided by the cationic material to the filter medium aids in electro-
kinetic interception of microbiological contaminants, while the tight pore
structure provides a short diffusion path and, therefore, rapid diffusion kinetics
of contaminants in a flowing fluid to the surface of the microporous structure.
The microporous structure also provides supplemental direct mechanical
interception of microbiological contaminants. Due to the dominant role of
diffusion for the interception of extremely small particles, there is a direct
correlation between the log reduction value of viral particles and the contact
time of the influent within the filter medium, rather than a dependence upon
the thickness of the filter medium.

Characteristics of the Microbiological Interception Enhanced Filter
Medium
In order to provide full microbiological interception capability, the
microbiological interception enhanced filter medium of the present invention
has a mean flow path of less than about 2 microns, and preferably less than or
equal to about 1 micron, and more preferably less than or equal to about 0.6
microns. The volume of the microbiological interception enhanced filter
medium of the present invention compared to the flow rate of fluid through
the filter medium must be sufficient to provide a contact time adequate for the
contaminants to diffuse to the surface of the filter medium. To provide
enhanced electro-kinetic interception of microorganisms, of which the
majority are negatively charged, under most conditions, the microbiological
interception enhanced filter medium has a positive zeta potential generally
greater than about +10 millivolts at pH values of about 6 to about 7, and
retains a net positive zeta potential at pH values of about 9 or greater.
Natural organic matter (NOM), such as polyanionic acids, i.e., humic
acid or fulvic acid, that may reduce or remove the charge on the
microbiological interception enhanced filter medium, is preferably prevented
from contacting the charged microporous structure through the use of an
adsorbent prefilter that substantially removes the NOM. When used in the
context of a gravity-flow water filtration system, it is preferable that the
microbiological interception enhanced filter medium be made with
hydrophilic materials to provide good, spontaneous wettability. Alternatively,
in other applications, the microbiological interception enhanced filter medium
may be treated to provide either a hydrophilic or hydrophobic characteristic as
needed. It is possible that the microbiological interception enhanced filter
medium can have bom positively and negatively charged and uncharged
regions, and/or hydrophilic and hydrophobic regions. For example, the
negatively charged regions can be used to enhance the interception of less

common positively charged contaminants and uncharged hydrophobic regions
can be used to provide enhanced interception of contaminants that are
attracted to hydrophobic surfaces.
The Fibers/Whiskers Or Particulate Ingredients
The microbiological interception enhanced filter medium of the present
invention includes a microporous structure that may include a plurality of
nanofibers, including whiskers or microparticulate ingredients, of organic and
inorganic materials including, but not limited to, polymers, ion-exchange
resins, engineered resins, ceramics, cellulose, rayon, ramie, wool, silk, glass,
metal, activated alumina, carbon or activated carbon, silica, zeolites,
diatomaceous earth, activated bauxite, fuller's earth, calcium hydroxyappatite,
other adsorbent materials, or combinations thereof. Combinations of organic
and inorganic fibers and/or whiskers or micro-particules are contemplated and
within the scope of the invention as for example, glass, ceramic, or metal
fibers and polymeric fibers may be used together with very small particles
incorporated into the microporous structure.
When produced by a wet laid process from nanofibers such as cellulose
or polymer fibers, such fibers should also have a Canadian Standard Freeness
of less than or equal to about 100, and most preferably less than or equal to
about 45. Preferably, a significant portion of the fibers should have a diameter
less than or equal to about 1000 nanometers, more preferably less than or
equal to about 400 nanometers, and fibers less than or equal to about 250
nanometers in diameter are most preferred. It is preferable to chop the fibers
to a length of about 1 millimeter to about 8 millimeters, preferably about 2
millimeters to about 6 millimeters, and more preferably about 3 millimeters to
about 4 millimeters. Fibrillated fibers are most preferred due to their
exceptionally fine dimensions and potentially low cost.
Preferably, fibrillated synthetic cellulose fibers, processed in
accordance with the present invention, can produce an ultra-fine, hydrophilic

microporous structure for use as the microbiological interception enhanced
filter medium of the present invention. Such fibrillated cellulose fibers can be
made by direct dissolution and spinning of wood pulp in an organic solvent,
such as an amine oxide, and are known as lyocell fibers. Lyocell fibers have
the advantage of being produced in a consistent, uniform manner, thus
yielding reproducible results, which may not be the case for, for example,
natural cellulose fibers. Further, the fibrils of lyocell are often curled. The
curls provide a significant amount of fiber entanglement, resulting in a finished
filter medium with high dry strength and significant residual wet strength.
Furthermore, the fibrillated lyocell fibers may be produced in large quantities
using equipment of modest capital cost. It will be understood that fibers other
than cellulose may be fibrillated to produce extremely fine fibrils, such as for
example, artificial fibers, in particular, acrylic or nylon fibers, or other natural
celtulosic materials. Combinations of fibrillated and non-fibrillated fibers may
be used in the microporous structure.
Membranes
The microbiological interception enhanced filter medium of the present
invention can comprise a membrane of organic or inorganic composition
including, but not limited to, polymers, ion-exchange resins, engineered
resins, ceramics, cellulose, rayon, ramie, wool, silk, glass, metal, activated
alumina, activated carbon, silica, zeolites, diatomaceous earth, activated
bauxite, fuller's earth, calcium hydroxyappatite, titanates and other materials,
or combinations thereof. Combinations of organic and inorganic materials are
contemplated and within the scope of the invention. Such membranes may be
made using methods known to one of skill in the art.
The Microbiological Interception Enhancing Agent
The nanofibers or membrane that make up the microporous structure
are chemically treated with a microbiological interception enhancing agent
capable of creating a positive charge on the microbiological interception

enhanced filter medium. A cationic metal complex is formed on at least a
portion of the surface of at least some of the fibers or the membrane by treating
the fibers or membrane with a cationic material. The cationic material may be
a small charged molecule or a linear or branched polymer having positively
charged atoms along the length of the polymer chain.
If the cationic material is a polymer, the charge density is preferably
greater than about 1 charged atom per about every 20 Angstroms, preferably
greater than about 1 charged atom per about every 12 Angstroms, and more
preferably greater than about 1 charged atom per about every 10 Angstroms of
molecular length. The higher the charge density on the cationic material, the
higher the concentration of the counter ion associated therewith. A high
concentration of an appropriate counter ion can be used to drive the
precipitation of a cationic metal complex. The cationic material should
consistently provide a highly positively charged surface to the microporous
structure as determined by a streaming or zeta potential analyzer, whether in a
high or low pH environment. Zeta or streaming potentials of the microporous
structure after treatment with a high molecular weight charged polymer can be
greater than about +10 millivolts, and often up to about +23 millivolts at a
substantially neutral pH.
The cationic material includes, but is not limited to, quatemized
amines, quatemized amides, quaternary ammonium salts, quatemized imides,
benzalkonium compounds, biguanides, cationic aminosilicon compounds,
cationic cellulose derivatives, cationic starches, quatemized polyglycol amine
condensates, quatemized collagen polypeptides, cationic chitin derivatives,
cationic guar gum, colloids such as cationic melamine-formaldehyde acid
colloids, inorganic treated silica colloids, polyamide-epichlorohydrin resin,
cationic acrylamides, polymers and copolymers thereof, combinations thereof,
and the like. Charged molecules useful for this application can be small
molecules with a single charged unit and capable of being attached to at least

a portion of the microporous structure. The cationic material preferably has
one or more counter ions associated therewith which, when exposed to a
biologically active metal salt solution, cause preferential precipitation of the
metal in proximity to the cationic surface to form a cationic metal precipitate.
Exemplary of amines may be pyrroles, epichlorohydrin derived amines,
polymers thereof, and the like. Exemplary of amides may be those polyamides
disclosed in International Patent Application No. WO 01/07090, and the like.
Exemplary of quaternary ammonium salts may be homopolymers of diallyl
dimethyl ammonium halide, epichlorohydrin derived polyquaternary amine
polymers, quaternary ammonium salts derived from diamines and dihalides
such as those disclosed in United States Patent Nos. 2,261,002, 2,271,378,
2,388,614, and 2,454,547, all of which are incorporated by reference, and in
International Patent Application No. WO 97/23594, also incorporated by
reference, polyhexamethylenedimethylammonium bromide, and the like. The
cationic material may be chemically bonded, adsorbed, or crosslinked to itself
or to the fiber or membrane.
Furthermore, other materials suitable for use as the cationic material
include BIOSHIELD® available from BioShield Technologies, Inc., Norcross,
Georgia. BIOSHIELD® is an organosilane product including approximately 5%
by weight octadecylaminodimethyltrimethoxysilylpropyl ammonium chloride
and less than 3% chloropropyltrimethoxysilane. Another material that may be
used is SURFACINE®, available from Surfacine Development Company LLC,
Tyngsboro, Massachusetts. SURFACINE® comprises a three-dimensional
polymeric network obtained by reacting poly(hexamethylenebiguanide)
(PHMB) with 4,4'-methlyene-bis-N,N-diglycidylaniline (MBGDA), a
crosslinking agent, to covalently bond the PHMB to a polymeric surface.
Silver, in the form of silver iodide, is introduced into the network, and is
trapped as submicron-sized particles. The combination is an effective biocide,
which may be used in the present invention. Depending upon the fiber and

membrane material, the MBGDA may or may not crosslink the PHMB to the
fiber or the membrane.
The cationic material is exposed to a biologically active metal salt
solution such that the cationic metal complex precipitates onto at least a
portion of the surface of at least some of the fibers or the membrane. For this
purpose, the metals that are biologically active are preferred. Such
biologically active metals include, but are not limited to, silver, copper, zinc,
cadmium, mercury, antimony, gold, aluminum, platinum, palladium, and
combinations thereof. Most preferred are silver and copper. The biologically
active metal salt solution is preferably selected such that the metal and the
counter ion of the cationic material are substantially insoluble in an aqueous
environment to drive precipitation of the cationic metal complex.
A particularly useful microbiological interception enhancing agent is a
cationic silver-amine-halide complex. The cationic amine is preferably a
homopolymer of diallyl dimethyl ammonium halide having a molecular
weight of about 400,000 Daltons or other quaternary ammonium salts having
a similar charge density and molecular weight. A homopolymer of diallyl
dimethyl ammonium chloride useful in the present invention is commercially
available from Nalco Chemical Company of Naperville, Illinois, under the
tradename MERQUAT® 100. The chloride counter ion may be replaced with a
bromide or iodide counter ion. When contacted with a silver nitrate solution,
the silver-amine halide complex precipitates on at least a portion of the fibers
or membrane of the microporous structure of the filter medium.
The pH of the surrounding solution does affect the zeta potential of the
microbiological interception enhanced filter medium of the present invention.
An acidic pH will increase the charge on the filter medium while a basic pH
will decrease the charge on the filter medium. Under pH conditions typically
encountered in potable water, the microbiological interception enhanced filter
medium does retain a minimum positive charge and only at very high pH

values does the charge decline below zero millivolts. Exposure to NOM, such
as polyanionic acids, will decrease the zeta potential of the microbiological
interception enhanced filter medium. This will diminish its microbiological
interception capabilities. Therefore, in applications where high levels of NOM
are present, an adsorbent prefilter capable of removing the NOM extends the
useful life of the microbiological interception enhanced filter medium.
Methods Of Making The Microbiological Interception Enhanced Filter Medium
The microbiological interception enhanced filter medium may be made
in accordance with processes known to one of skill in the art. Dry laid
processes include spun bonding, electrospinning, spinning islands-in-sea
processes, fibrillated films, melt blowing, and other dry laid processes known
to one of skill in the art. An exemplary dry laid process; starts with staple
fibers, which can be separated by carding into individual fibers and are then
laid together to a desired thickness by an aerodynamic or hydrodynamic
process to form an unbonded fiber sheet. The unbonded fibers can then be
subjected to hydraulic jets to both fibrillate and hydroentangle the fibers. A
similar process can be performed on certain plastic films that when exposed to
high pressure jets of water, are converted into webs of fibrillated fibers.
In a preferred wet laid process, a fiber tow is chopped to a specific
length, usually in the range of about 1 millimeter to about 8 millimeters, and
in particular in the range of about 3 millimeters to about 4 millimeters. The
chopped fibers are fibrillated in a device having characteristics similar to a
blender, or on a large scale, in machines commonly referred to as a "hi-low", a
'beater* or a 'refiner'. The fiber is subjected to repetitive stresses, while
further chopping and the reduction of fiber length is minimized. As the fibers
undergo these stresses, the fibers split as a result of weaknesses between
amorphous and crystalline regions and the Canadian Standard Freeness (CSF),
which is determined by a method well known in the art, begins to decline.

Samples of the resulting pulp can be removed at intervals, and the CSF used as
an indirect measure of the extent of fibrillation. While the CSF value is slightly
responsive to fiber length, it is strongly responsive to the degree of fiber
fibrillation. Thus, the CSF, which is a measure of how easily water may be
removed from the pulp, is a suitable means of monitoring the degree of fiber
fibrillation. If the surface area is very high, then very little water will be
drained from the pulp in a given amount of time and the CSF value will
become progressively lower as the fibers fibritlate more extensively. The
fibrillated fiber of a given CSF value can be directly used for producing paper
or dewatered on a variety of different devices, including a dewatering press or
belt, to produce a dewatered pulp. The dewatered pulp can be subsequently
used to make a wet-laid paper. Generally, for application in the present
invention, a pulp with a CSF of below 100 is used, and preferably, the CSF
should be less than or equal to about 45.
The pulp is treated with a cationic material in such a manner as to
allow the cationic material to coat at least a portion of the surface of at least
some of the fibers thereby imparting a charge on the fibers. Methods of
applying the cationic material to the fibers are known in the art and include,
but are not limited to, spray, dip, or submergence coating to cause adsorption,
chemical reaction or crasslinking of the cationic material to the surface of the
fibers. The treated pulp is then rinsed in reverse osrnosis/deionized (RO/DI)
water, partially dewatered, usually under vacuum, to produce a wet lap that
can then be exposed to a biologically active metal salt solution. The use of
nearly ion-free rinse water causes the counter-ions associated with the cationic
material to be drawn tightly against the treated fiber surface and to eliminate
unwanted ions that may cause uncontrolled precipitation of the biologically
active metal into sites remote from the cationic surface.
The metal salt solution is infiltrated into the fibers to allow precipitation
of the cationic metal complex on a surface of at least a portion of the fibers.

The precipitation accurately deposits a metal colloid adjacent to the cationic
coating because the counter-ion associated with this coating reacts with the
applied metal salt to form colloidal particles. After sufficient exposure to the
biologically active metal salt solution, the fibers can be rinsed and excess
water is removed. Alternatively, the fibers can be directly sent to pulp
preparation systems to create a furnish suitable for paper making.
When silver nitrate is used as the metal salt solution, the presence of
precipitated silver can be confirmed by using a Kratos EDX-700/800 X-ray
fluorescence spectrometer available from Kratos Analytical, a Shimadzu Group
Company, Japan.
The microbiological interception enhanced filter medium comprising a
membrane may be made in accordance with processes known to one of skill
in the art. Raw material for the membrane may be treated prior to forming the
membrane or the cationic material may be applied to the membrane material
using known methods in the art and similar to those used to treat the fiber
surfaces.
Additives
The strength of the wet laid fiber sheet, especially when wet, may be
improved with the addition of various additives. It is well known in the art
that the addition of epoxy or acrylic or other resins to the paper making
process can provide enhanced wet strength, but these water-dispersed resins
often cause lower permeability to the final product, especially as fiber size
becomes very small. Although these resins and resin systems can be used in
the current invention, it is preferable to use thermoplastic or thermoset
materials known in the art, and in either powder, particulate or fiber form.
Useful binder materials include, but are not limited to, polyolefins,
polyvinyl halides, polyvinyl esters, polyvinyl ethers, polyvinyl sulfates,
polyvinyl phosphates, polyvinyl amines, polyamides, polyimides,
polyoxidiazoles, polytriazols, polycarbodiimides, polysulfones,

polycarbonates, polyethers, polyarylene oxides, polyesters, polyarylates,
phenol-formaldehyde resins, melamine-formaldehyde resins, formaldehyde-
ureas, ethyl-vinyl acetate copolymers, co-polymers and block interpolymers
thereof, and combinations thereof. Variations of the above materials and other
useful polymers include the substitution of groups such as hydroxyl, halogen,
lower alkyl groups, lower alkoxy groups, monocyclic aryl groups, and the like.
Other potentially applicable materials include polymers such as polystyrenes
and acrylonitrile-styrene copolymers, styrene-butadiene copolymers, and other
non-crystalline or amorphous polymers and structures.
A more detailed list of binder materials that may be useful in the
present invention include end-capped polyacetals, such as poly(oxymethylene)
or polyformaldehyde, polyftrichloroacetaldehyde), poly(n-valeraldehyde),
poly(acetaldehyde), and poly(propionaldehyde); acrylic polymers, such as
polyacrylamide, poly(acrylic acid), poly(methacrylic acid), poly(ethyl acrylate),
and poly(methyl methacrylate); fluorocarbon polymers, such as
poly(tetrafluoroethylene), perfluorinated ethylene-propylene copolymers,
ethylene-tetrafluoroethylene copolymers, poly(chlorotrifluoroethylene),
ethylene-chlorotrifluoroethylene copolymers, poly(vinylidene fluoride), and
polyvinyl fluoride); polyamides, such as poly(6-aminocaproic acid) or poly(e-
caprolactam), poly(hexamethylene adipamide), pcly(hexamethylene
sebacamide), and polyCM-aminoundecanoic acid); polyaramides, such as
poly(imino-1,3-phenyleneiminoisophthaloyl) or poly(m-phenylene
isophthalamide); parylenes, such as poly-2-xylylene, and poly(chloro-1-
xylylene); polyaryl ethers, such as poly(oxy-2,6-dimethyl-l,4-phenylene) or
poly(p-phenylene oxide); polyaryl sulfones, such as ,poly(oxy-1,4-
phenylenesulfonyl-1,4-phenyleneoxy-1,4-phenyl-eneisopropylide ne-1,4-
phenylene), and poly(sulfonyl-1,4-phenylene-oxy-1,4-phenylenesulfonyl4,4'-
biphenylene); polycarbonates, such as poly-(bisphenol A) or
poly(carbonyldioxy-1,4-phenyleneisopropylidene-1,4-phenylene); polyesters,

such as polyethylene terephthalate), poly(tetramethyiene terephthalate), and
poly(cyclohexyl-ene-1,4-dimethylene terephthalate) or polyfaxymethylene-i,^
cyclohexylenemethyleneoxyterephthaloyl); polyaryl sulfides, such as poly(p-
phenylene sulfide) or poly(thio-1,4-phenylene); polyirnides, such as
poly(pyromellitimido-1,4-phenylene); polyolefins, such as polyethylene,
polypropylene, poly(1-butene), poly(2-butene), polyd-pentene), poly(2-
pentene), poly(3-methyl-1-pentene), and poly(4-methyl-1-pentene); vinyl
polymers, such as poly(vinyl acetate), polyvinylidene chloride), and polyvinyl
chloride); diene polymers, such as 1,2-poly-1,3-butadiene, 1,4-poly-1,3-
butadiene, polyisoprene, and polychloroprene; polystyrenes; and copolymers
of the foregoing, such as acrylonitrilebutadiene-styrene (ABS) copolymers.
Polyolefins that may be useful include polyethylene, linear low density,
polyethylene, polypropylene, poly(1-butene), poly(2-butene), poly(1-pentene),
poly(2-pentene), poly(3-methyl-1-pentene), poly(4-methyl-1-pentene), and the
like.
A range of binder fibers, including polyethylene, polypropylene,
acrylic, or polyester-polypropylene or polypropylene-polyethylene bi-
component fibers, or others can be used. Certain types of treated polyethylene
fibers, when properly treated, as described below, are optimal, and have the
additional benefit of not significantly interfering with the hydrophilic nature of
the resulting filter medium when used in modest volumes. Preferred fiber
binder materials may include FYBREL® synthetic fibers and/or SHORT STUFF®
EST-8, both of which are polyolefin based. FYBREL.® is a polyolefin based
synthetic pulp that is a highly fibrillated fiber and is commercially available
from Mitsui Chemical Company, Japan. FYBREL® has excellent thermal
moldability and provides a smooth surface to the filter medium. SHORT
STUFF® EST-8 is commercially available from MiniFibers, Inc., Pittsburgh,
Pennsylvania, and is a highly fibrillated, high density polyethylene.

Preferably, the binder material is present in an amount of about 1 % to
about 10% by weight, more preferably about 3% to,about 6%, and most
preferably about 5%. It is preferable that the binder material have a softening
point that is significantly lower than a softening point of the nanofiber material
so that the filter medium can be heated to activate the binder material, while
the microporous structure does not melt and thereby lose porosity.
One or more additives either in a particulate, fiber, whisker, or powder
form may also be mixed with the nanofibers or incorporated into the
membrane to aid in adsorption of other contaminants or participate in the
formation of the microporous structure and interception of microbiological
contaminants. Useful additives may include, but are not limited to, metallic
particles, activated alumina, activated carbon, silica, polymeric powders and
fibers, glass beads or fibers, cellulose fibers, ion-exchange resins, engineered
resins, ceramics, zeolites, diatomaceous earth, activated bauxite, fuller's earth,
calcium sulfate, other adsorbent materials such as super adsorbent polymers
(SAPs), or combinations thereof. The additives can also be chemically treated
to impart microbiological interception capabilities depending upon the
particular application. Such additives are preferably present in a sufficient
amount such that the fluid flow in the resultant filter medium is not
substantially impeded when used in filtration applications. The amount of
additives is dependent upon the particular use of the filtration system.
Exemplary of a wet laid process includes mixing a pulp of 45 CSF
fibrillated lyocell fibers with 5% EST-8 binder fibers and dispersing the pulp
and binder fibers in deionized water with mixing in a blender to form a furnish
with about 1% to about 2% consistency. To this mixture is added about 3%
by weight of MERQUAT® 100, which is briefly dispersed Into the dilute pulp
furnish. The cationic material remains in contact with the pulp for about 4 to
about 12 hours until a significant portion has been adsorbed onto at least a
portion of the fibers to impart and maintain a positive zeta potential on the

fibers. Within about eight hours at room temperature, sufficient MERQUAT®
is adsorbed to provide a positive zeta potential on the fibers that is greater than
about +10 millivolts. Next, this pulp is partially dewatered under vacuum
and rinsed with deionized water to form a wet lap. A metal salt solution, such
as, for example, silver nitrate, in an amount equal to 0,5% by weight of the dry
nanofibers, is prepared with deionized water, and uniformly poured over the
sheet and allowed to stand for a short time to allow precipitation of the
biologically active metal with at least a portion of the counter ion associated
with the cationic material. Thereafter, the fibers can be directly used in the
production of wet laid filter medium.
Filtration Systems Utilizing the Microbiological Interception Enhanced Filter
Medium
Many types of filtration systems incorporating the current filter medium
can be imagined. Described below are certain specific embodiments.
However, these filtration systems are exemplary and should not be construed
as restricting the scope of the invention.
Precoat Filtration Systems Including Microbiological Interception
Enhanced Nanofiber
One filtration system of the present invention that utilizes nanofibers
treated with the microbiological interception enhancing agent, is an industrial,
commercial or municipal filter that uses a precoat applied to a porous septa.
This coating is produced by dispersing particles such as diatomaceous earth,
perlite or fibers as a precoat applied to the porous septa for filtering liquids
such as beer, wine, juices, and other liquids used in the food service or
pharmaceutical industry. As the liquid contacts the filter cake, unwanted
contaminants are removed while also clarifying the liquid. The charged
nanofibers not only remove negatively charged contaminants in the liquid
much smaller than the pores of the precoat but greatly improve the mechanical

interception of all particles. The nanofibers may be used in conjunction with
traditional precoat ingredients such as diatomaceous earth. Only a small
amount of nanofibers are needed in the precoat, generally about 1.5% to
about 10% by weight, to produce a significant effect. Preferably, a hydrophilic
microbiological interception enhanced filter medium is used in these
applications.
Filtration Systems Involving Multiple Layers Of Filter Medium
A microbiological interception enhanced filter medium of the present
invention can include configurations having more than one layer of the
microbiological interception enhanced filter medium.. A first microbiological
interception enhanced filter medium layer may be positively charged while a
second layer may be negatively charged. The negatively charged material can
be produced by contacting the nanofibers pulp with a negatively charged
compound or material such as a polycarboxylic acid mixed with a small
quantity of a crosslinking agent such as a glycerine. Heating the nanofibers
after soaking in such a mixture results in the formation of a coating on the
nanofibers of negatively charged carboxylic acid polymer crosslinked by the
glycerine. The multi-layer microbiological interception enhanced filtration
system is capable of intercepting both positively and negatively charged
microbiological targets. Again, in applications where NOM is present, an
adsorbent prefilter may be needed to preserve the charge on the
microbiological interception enhanced filter medium.
Filtration Systems With An Adsorbent Prefilter Combined With The
Microbiological Interception Enhanced Filter Medium
A microporous filter medium of the present invention treated with the
microbiological interception enhancing agent may be used as a flat sheet
medium, a pleated medium, or as a spiral wound medium depending upon the
application and the filter housing design. It may be used for just about any
type of fluid filtration including water and air.

However, the microbiological interception enhanced filter medium
may be less effective in the presence of moderate to high levels of NOM such
as polyanionic humic acid and fulvic acid, due to the decrease and eventual
loss of positive charge on the filter medium in the presence of such acids.
Therefore, such applications utilizing the microbiological interception
enhanced filter medium alone should be substantially free of or have low
levels of polyanionic acids.
In filtration systems containing the microbiological interception
enhanced filter medium that may come in contact with fluids that contain
NOM, it is prudent to use an adsorbent prefilter to remove the NOM in the
influent prior to it contacting the microbiological interception enhanced filter
medium. Alternatively, the positively charged filter medium can be formed
into a multitude of layers either as a stack of sheets or by conversion into a
structure. Under this type of arrangement, the outer layers of the filter medium
can be sacrificed to remove the NOM, while the inner layers are protected and
provide long-term reduction of microbiological contaminants. Additives that
adsorb or absorb NOM may be incorporated into the microporous structure,
including anion exchange resins. To avoid this costly loss of sacrificial
material, the following examples describe other alternative methods for
arranging the protection of the filter medium from the effects of NOM.
1. A Flat Adsorbent Filter Medium As A Prefilter
The microbiological interception enhanced filter medium may be used
in conjunction with adsorbent filtration media that serve to intercept NOM
interferences prior to their contact with the charged microbiological
interception enhanced filter medium. The microbiological interception
enhanced filter medium and one or more layers of an adsorbent filtration
medium may be used as a flat sheet composite, spiral wound together, or
pleated together. Such an adsorbent filtration medium may be manufactured
according to United States Patent Nos. 5,792,513 and 6,077,588, as well as

other processes in the prior art. A particularly suitable flat sheet adsorbent
filtration medium is commercially available as PLEKX® from KX Industries,
L.P., Orange, Connecticut. The flat sheet filtration medium may contain
hydrophilic or hydrophobic particles that can also be treated with the
microbiological interception enhancing agent, although not necessary, and
immobilized on a substrate to provide added microbiological interception
capabilities in addition to that provided by the microbiological interception
enhanced filter medium. At least one adsorbent layer is preferably placed
upstream from the microbiological interception enhanced filter medium to
reduce the deleterious effects of NOM on the microbiological interception
enhanced filter medium. The microbiological interception enhanced filter
medium can serve as one of the substrates used to support the adsorbent used
to filter NOM from the influent fluid. For example, the upper layer of the
PLEKX® structure can be a particulate prefilter. The core of the PLEKX®
composite can be primarily composed of an adsorbent with a high affinity for
NOM, and the lower, downstream layer can be the; microbiological
interception enhanced filter medium. The layers can be bonded into a single
cohesive composite structure using the PLEKX® process described in the
above-mentioned patents. The result is a hgh dirt capacity filter structure that
provides chemical, particulate, and microbiological interception in a single
material. The core of the PLEKX® structure can include a wide range of
ingredients useful for the adsorption of chemical contaminants.
2. GAC Filter Medium As An Adsorbent Prefilter
The microbiological interception enhanced filter medium may also be
used in conjunction with a bed of granular adsorbent such as, for example, a
granular activated carbon (GAC) bed. The granular bed filter should be placed
upstream from the microbiological interception enhanced filter medium to
remove any charge-reducing contaminants, such as NOM, from the influent
prior to contacting the charged microporous filter medium.

3. Solid Composite Block Filter Medium As An Adsorbent Prefilter
The microbiological interception enhanced filter medium may also be
used in conjunction with a solid composite block filter medium, preferably
comprising activated carbon, placed upstream from the microbiological
interception enhanced filter medium to remove any charge-reducing
contaminants, such as NOM, from the influent prior to contact with the
microbiological interception enhanced filter medium. The activated carbon
block may include, but is not limited to, such materials as activated alumina,
zeolites, diatomaceous earth, silicates, aluminosilicates, titanates, bone char,
calcium hydroxyapatite, manganese oxides, iron oxides, magnesia, perlite,
talc, polymeric particulates, clay, iodated resins, ion exchange resins,
ceramics, and combinations thereof to provide additional reduction of
contaminants such as heavy metals, arsenic, chlorine, and to improve taste and
odor. These materials, as well as the activated carbon,, may be treated with the
microbiological interception enhancing agent prior to being: converted into a
solid composite by extrusion, compression molding or other processes known
to one of skill in the art. Exemplary processes are described in United States
Patent Nos. 5,019,311, and 5,189,092. The solid composite block can
contain an anion-exchange resin that is specifically selected for its high
capacity to adsorb NOM.
Complete Filtration Devices Combining Adsorbent Prefilters And
Microbiological Interception Enhanced Filter Medim
One particular embodiment of a filtration system of the present
invention includes a composite filter medium, as described above, including
the microbiological interception enhanced filter medium and the adsorbent
filtration medium. This device is designated to operate as a gravity flow device
with a driving pressure of only a few inches water column to a maximum of a
few feet of water column. The composite filter medium is forced to first pass
through the adsorbent prefilter and then the microbiological iinterception layer.

As shown in Fig. 1, an exemplary filter design incorporates the composite filler
medium of the present invention in a filter housing 10 having a clam shell type
enclosure. Filter housing 10 has a top portion 12 having an inlet 14, and a
bottom portion 16 having an outlet 18. Residing within a sealed cavity
defined by the top portion and bottom portion is the composite filter medium
20 shown more accurately in the cross sectional view of Fig. 2. Top portion
12 and bottom portion 16 may be formed from a single sheet of a polymeric
material and folded over to provide a clam shell configuration.
To assemble the filter, composite filter medium 20 is cut into
substantially the size and shape of the clam shell enclosure. Composite filter
medium 20 is secured into bottom portion 16 and top portion 12 is placed
over bottom portion 16 and compressed together. The top and bottom shell
portions 12, 16 may be welded together creating a weldment 22 around the
entire periphery of filter medium 20. As illustrated in Fig. 2, there is shown a
substantially impermeable interface between the top and bottom portions and
the composite filter medium in the region directly adjacent weldment 22.
Excess material on the clam shell enclosure and composite filter medium is
simply cut off. It will be understood that other methods of sealing the filter
medium within the filter housing may be used such as, but not limited to,
adhesives, mechanical clamps, and the like. Although the filter design has a
clam shell enclosure, the filter design is not limited to such. Any enclosure
that may be sealed such that an influent will not bypass the filter medium
would be suitable.
In referring back to Fig. 2, the seal formed between composite filter
medium 20 and top portion 12 and bottom portion 16 is such that water being
filtered is forced to follow the path illustrated by arrows A and B, and cannot
bypass composite filter medium 20. In fact, at the periphery of composite filter
medium 20, the pressure exerted by the seal increases the density of the filter
medium so that contact time of the water being filtered with composite filter

medium 20 in this peripheral region is increased and filtration efficiency
enhanced.
During production of the filter, assurances concerning the seal and
assembly integrity may be obtained using a vision system, and gas or aerosol
pulse testing. The gas or aerosol pulse test uses a tiny pulse of dilute butane or
fog-oil smoke that is entirely adsorbed or intercepted by an intact filter, but
will significantly penetrate a defective filter. Other off-line test procedures
known to one of skill in the art may be used to methodically examine the
quality of the seal between the filter medium and the enclosure.
The wall of the filter housing may be sufficiently thin and flexible so
that when the filter is contacted with water, the modest pressure produced by
the hydrostatic load of the incoming water causes top portion 12 and bottom
portion 16 to bow away slightly from and provide a clearance space between
the inner surface of top portion 12 and bottom portion 16, and composite
filter medium 20. This clearance space assists in distributing the water across
the influent surface of composite filter medium 20 and provides drainage of
the effluent into outlet 18.
Referring to Fig. 3, there is shown a front plan view of a filtration
system 30 of the present invention useful in providing potable water in a
gravity flow device that may be useful in developing countries where safe,
potable water of suitable microbiological quality is scarce. Although water is
discussed as the liquid influent, it is within the scope of the invention to
contemplate the filtration of other liquids. Filtration system 30 has a first
reservoir 35 that is a raw water collection transport container. First reservoir
35 may be a bag configuration as shown constructed of a. substantially leak
proof material such as a polymeric material, i.e., polyester, nylon, a polyolefin
such as polyethylene, polyvinyl chloride, and multi-layer films of the like. For
ease of use, first reservoir 35 may have a reinforced opening and a handle 36
for carrying and hanging first reservoir 35 to provide a pressure head during

filtration. Preferably, first reservoir 35 has a resealable opening 37 that when
closed provides a substantially water-tight seal. Such resealable openings are
known to one of skill in the art or may include a threaded opening with a
screw-on cap.
First reservoir 35 is preferably equipped with an output hose 40 such
that water stored in the reservoir may be drained for filtration and eventual
use. Output hose 40 is preferably made with a food-safe grade of flexible
polymer. Output hose 40 may be opened and closed using a simple clamp.
Output hose 40 may be permanently attached to first reservoir 35 by ultrasonic
welding or retained simply by friction. Output hose 40 preferably has an
internal extension end 42 within first reservoir 35 such that internal extension
end 42 extends above the bottom of the first reservoir 35 to provide an area for
capturing sediment that can settle prior to water filtration. By limiting the
amount of sediment present in the influent prior to water filtration, the useful
life of the filtration system is prolonged.
Output hose 40 connects first reservoir 35 to a filter 10, described
above, including the composite filter medium of the present invention. A
clamp 45 may be fitted on output hose 40 at any point along the length of
output hose 40. Such clamps are well known in the art and may be a simple
one piece configuration made of a flexible polymer or metal. When the clamp
is in an open position, water from first reservoir 35 flows freely into filter 10.
Filter 10 is removably connected to output hose 40. The outlet of filter 10 is
then connected to a second reservoir 50. Second reservoir 50 serves as a
collection vessel for the filtered water or effluent. Alternatively, filter 10 and
second reservoir 50 may be connected together via a second output hose (not
shown). Second reservoir 50 generally is equipped with a means for
dispensing the filtered water.
The above filtration system may be used as follows. A user takes first
reservoir 35, with or without output hose 40 attached thereto, to a water

source. If output hose 40 is still attached to first reservoir 35, clamp 45 must
be in a closed position or first reservoir 35 must be sealed by other means.
First reservoir 35 is filled with a quantity of raw water and its opening again
sealed while the user carries first reservoir 35 back to a preferred location such
as a residence. It is possible that the raw water is contaminated with
microorganisms and chemical contaminants and may not be potable. To
facilitate filtration, first reservoir 35 is suspended or hung from a support
means. Depending upon any significant sediment present: as evidenced by
turbidity, the raw water is allowed to remain suspended for a period of time
sufficient for the sediment to settle below the height of internal extension end
42 of output hose 40 within first reservoir 35. Of course, should the water be
relatively clear, there is no need to suspend first reservoir 35 for such a period
of time. Output hose 40 is attached to first reservoir 35, if previously
detached, and secured to filter 10. Filter 10 is secured to second reservoir 50
for collecting the filtered water. Clamp 45 is then placed in an open position
and the water is allowed to flow into filter 10 wherein the water once treated
through composite filter medium 20, is rendered potable, and collected in
second reservoir 50. To preserve the potability of the filtered water, the
surfaces of second reservoir 50 may be made from or treated with a
disinfectant or with the microbiological interception enhancing agent.
Preferably, the disinfectant used would not alter or affect the taste of the water.
Typical water flow rates are about 25 to about 100 ml/minute for a
device equipped with a filter of about 3"x5" size and operated at about 6"
water column pressure. This provides one liter of potable water in about 10 to
40 minutes having at least about 6 log reduction in bacteria and at least about
4 log reduction in viral contaminants. Continual use of filter 10 will likely
develop, by progressive deposition thereon, a layer of particles that will slow
the flow rate until the filtration process takes an unacceptable amount of time.

Although the flow rate is diminished, the filter will maintain its microbiological
interception capabilities for an extended period.
Another gravity flow device incorporating a filter medium of the present
invention includes an exemplary carafe design as illustrated in Fig. 4 for
filtering, storing and dispensing filtered water or other fluids. Although the
carafe shown is primarily round, the carafe 60 may assume any shape
depending upon its use and environment, and is a matter of design choice. A
basic carafe has a housing 62 with a handle 64 and cover 66. Carafe 60 is
divided into a lower reservoir or storage chamber 68 and an upper reservoir
78 that are enclosed by lid 70 and cover 66 located within housing 62. Spout
72 facilitates the removal of filtered water through outlet 74 of storage
chamber 68.
Upper reservoir 78 and storage chamber 68 are separated by partition
80 that is provided with a filter receiving receptacle 85 having an opening (not
shown) in the bottom thereof. In one embodiment, a flat composite filter
medium 76 of the present invention is placed into filter receiving receptacle
85 with a water tight seal to segregate upper reservoir 78 and storage chamber
68. Placement of filter medium 76 into filter receptacle 85 may be
accomplished using means known to one of skill in the art including, but not
limited to, a snap or hinged mechanism. Filter medium 76 is preferably
manufactured as a replaceable cartridge. Other features of the carafe design
may be incorporated into the present invention without departing from the
scope of the invention. The filter medium may comprise any microporous
structure having a mean flow path of less than about 1 micron and so treated
as to provide at least about 4 log reduction of microbiological contaminants
smaller than the mean flow path of the filter medium. Preferably, the filter
medium has a volume of less than about 500 cm3 and has an initial flow rate
of greater than about 25 ml/minute.

A user would pour raw water into upper reservoir 78 and allow the raw
water to pass through filter medium 76 under the influence of gravity. Filtered
water is collected in storage chamber 68. As the raw water passes through the
filter medium of the present invention with sufficient contact time, the filter
medium renders the water potable by providing a high titer reduction of
microorganisms. The log reduction value (LRV) of microorganisms is
dependent upon the contact time of the filter medium with the flowing water.
To provide about 8 log reduction value of microorganisms, the required
contact time is about 6 to about 10 seconds,
Carafe 60 may also have an indicator (not shown) that allows a user to
keep track of the age of the filter to gauge when the useful life of the filter
medium has been expended. Other types of indicators may also be used such
as an indicator for indicating the number of refills of carafe 60, for measuring
the volume of water or liquid that passes through the filter medium, and the
like.
Other Filtration Systems
A filter medium of the present invention, in particular, the composite
filter medium, may also be incorporated into a point-of-use application such as
a sports bottle design for use as a personal water filtration system operating
under a slight pressure, about 1 psi. A suitable sports bottle design is disclosed
in International Patent Application No. WO 01/23306 wherein the filter
medium may be incorporated into the filter receptacle of the sports bottle.
For other point-of-use applications, the microbiological interception
enhanced filter medium of the present invention may further be incorporated
into end-of-tap (EOT), under-sink, counter-top, or other common consumer or
industrial filtration systems and configurations for use in pressurized systems.
The filter system may include a prefilter comprising a bed of adsorbent
particles or a solid adsorbent composite block. The microbiological
interception enhanced filter medium can be a pleated or a spiral wound

construction, or formed into a thick mat by vacuum formation on a suitable
mandrel to create a wet-formed or dry-formed cartridge.
Examples
The following examples are provided to illustrate the present invention
and should not be construed as limiting the scope of the invention.
Porometry studies were performed with an Automated Capillary Flow
Porometer available from Porous Materials, Inc., Ithaca, New York.
Parameters determined, using standard procedures published by the
equipment manufacturer, include mean flow pore size and gas (air)
permeability. The flow of air was assayed at variable pressure on both the dry
and wet filter medium. Prior to wet runs, the filter medium was initially
immersed in silicon oil for at least 10 minutes while held under high vacuum.
Zeta or streaming potential of various filter media was determined using
streaming potential and streaming current measured with a BI-EKA Electro-
Kinetic Analyzer available from Brookhaven Instruments, of Holtsville, New
York. This instrument includes an analyzer, a flat-sheet measuring cell,
electrodes, and a data control system. The analyzer includes a pump to
produce the pressure required to pass an electrolyte solution, generally
0.0015M potassium chloride, from a reservoir, through the measuring cell
containing a sample of the filter medium described herein. Sensors for
measuring temperature, pressure drop, conductivity and pH are disposed
externally of the cell. In accordance with this method the electrolyte solution
is pumped through the porous material. As the electrolyte solution passes
through the sample, a displacement of charge occurs. The resulting "streaming
potential and/or streaming current" can be detected by means of the
electrodes, placed at each end of the sample. The zeta (streaming) potential of
the sample is then determined by a calculation according to the method of

Fairbrother and Mastin that takes into account the conductivity of the
electrolyte.
Bacterial challenges of the filter media were performed using
suspensions of Escherichia coli of the American Type Culture Collection
(ATCC) No. 11775 to evaluate the response to a bacterial challenge. The
response to viral challenges was evaluated using MS-2 bacteriophage ATTC
No. 15597-B1. The Standard Operating Procedures of the ATCC were used
for propagation of the bacterium and bacteriophage, and standard
microbiological procedures, as well known in the art, were used for preparing
and quantifying the microorganisms in both the influent and effluent of filters
challenged with suspensions of the microbiological particles.
Examples 1-3: Filter Medium Made With Untreated Lyocell Fibers
(Comparative)
Filter medium made from untreated lyocell fibers having a mean flow
path of about 0.3 to about 0.6 microns were prepared in accordance with the
following method.
Dry EST-8 binder fibers having a weight of 0.45 g, commercially
available from MiniFibers, Inc., was fully dispersed in 1.0 L of deionized water
in a kitchen style blender on a pulse setting. Fibrillated lyocell fibers with a
Canadian Standard Freeness of 45 and having a dry weight of 120.0 g were
added as wet pulp to the dispersed binder fibers. The dispersed fiber mixture
was blended for another 15 seconds. The fiber mixture was poured into a
larger industrial Waring blender with an additional 1.0 L of deionized water
and blended for an additional 15 to 30 seconds. The fiber mixture was poured
into a 30.5 x 30.5 cm2 stainless steel FORMAX® paper deckle filled with about
12.0 L of deionized water and fitted with a 100 mesh forming screen. A 30 x
30 cm2 stainless steel agitator plate having 60 holes of 2 cm in diameter was
used to plunge the fiber mixture up and down from top to bottom about 8 to
10 times. The water was removed from the fiber mixture by pulling a slight

vacuum below the deckle to cause the fibers to form on the wire. Once the
bulk of the water is removed, supplemental dewatering is accomplished with a
vacuum pump to remove additional excess moisture and to create a relatively
smooth, flat, fairly thin paper-like sheet. The resulting sheet is separated from
the screen and combined with a blotter sheet on both top and bottom. The
combination of sheets is gently rolled with a 2.27 kg marble rolling pin to
remove excess water and smooth out the top surface of the sheet. The sheet is
then placed between two fresh and dry blotter sheets and placed on a
FORMAX® sheet dryer for about 10 to about 15 minutes at about 120°C. The
dried filter medium is separated from the blotter sheets and directly heated on
the FORMAX® sheet dryer for about 5 minutes on each side to activate the dry
binder fibers.
Table I shows the porometry and air permeability test results performed
on filter medium made from untreated lyocell fibers of varying thicknesses
made using the above process.

The resulting filter medium made with untreated lyocell fibers had a
reproducible streaming potential of about-9.0 millivolts.
Example 4: Filter Medium Made With Lyocell Fibers Treated With The
Microbiological Interception Enhancing Agent
To a blender were added 12.0 g dry weight lyocell fibers as a 10% by
weight wet pulp having a Canadian Standard Freeness of about 45, 0.45 g

SHORT STUFF® EST-8 binder fibers, and 1.0 L deionized water. The mixture
was blended until the fibers were fully dispersed. To the blender was added
3.0 ml of MERQUAT® 100 as a 30% aqueous solution and the fibers blended
with the MERQUAT® 100 for about 10 seconds and left to stand for at least
about 6 hours. After about 6 hours, the fibers were poured into a standard 8
inch Brit jar fitted with a 100 mesh forming wire and excess water removed
under vacuum. The resulting pulp sheet was rinsed with 500 ml of deionized
water. The excess water was again removed by vacuum.
A dilute silver nitrate solution was poured uniformly over the pulp sheet
to provide full exposure and saturation, providing about 0.1425 g of silver per
sheet. The silver nitrate solution was left on the pulp sheet for at least about
15 minutes and excess water removed under vacuum pressure. The silver-
treated pulp sheet was then torn into small pieces and placed in a WARING®
blender and re-dispersed in 2.0 L of deionized water. A second 3.0 ml portion
of the MERQUAT® 100 solution was added to the dispersion and the mixture
blended for about 10 minutes and the contents poured into a 30.5 x 30.5 cm2
stainless steel FORMAX® paper deckle fitted with a 100 mesh forming screen.
Paper-like sheets of the microbiological interception enhanced filter medium
were made in the same manner as the untreated lyocell filter media described
in Examples 1 to 3.
The zeta potential of the filter medium was consistently greater than
about +10 millivolts at a pH of about 7.0.
Examples 5-23: Comparison Of Microbiological Interception With The
Microbiological Interception Enhanced Filter Medium Of The Present
invention And The Untreated Lyocell Filter Medium
Sheets of fibrillated lyocell filter medium either untreated or treated
with MERQUAT® 100 and silver, as described in Examples 1 to 4, were folded
twice and cut into standard cone-shaped funnels and placed into small

sterilized glass funnels. Deionized water was used to pre-wet each filter
medium. Approximately 125 ml of various microbiological challenges were
poured through the filters and the effluents collected in sterile 250 ml
Erlenmeyer flasks. The effluents were subjected to serial dilution in duplicate
and plated on petri dishes following standard laboratory procedures as
required for each organism and left overnight in 37°C heated incubators. The
next day all test results were recorded. Table II summarizes the log reduction
values of a series of tests run using microbiological challenges made with de-
ionized water.

As illustrated in Table II, the filter medium made from lyocell fibers
treated with MERQUAT® 100 and silver provided significant microbiological
interception capabilities as compared to filter medium made from untreated

lyocell fibers. The efficacy of the microbiological interception enhanced filter
medium when challenged with MS2 viral particles illustrates that a filtration
system of the present invention would prove effective in removing nano-sized
pathogens such as viruses.
Examples 24-27: Microbiological Interception Capability Of The Filter Medium
Made With Treated Lyocell Fibers In the Presence Of Polyanionic Acids
As discussed above, NOM such as polyanionic acids reduce the
positive zeta potential and, thereby, reduce the efficacy of the microbiological
interception enhanced filter medium. After exposure to 500 ml humic acid
(0.005 g/1.0 L H2O), the zeta potential of the microbiological interception
enhanced filter medium decreased from +14.1 to -14.4. Likewise, after
exposure to 500 ml fulvic acid (0.005 g/1.0 L hhO), the zeta potential of the
microbiological interception enhanced filter medium decreased from +10.1 to
-8.9. Examples 24 to 27 show the reduction in microbiological interception
capabilities of the filter medium made with lyocell fibers treated with
MERQUAT® 100 and silver in the presence of humic and fulvic acid solutions.
Small discs of the filter medium treated with MERQUAT® 100 and
silver were folded and placed in small sterilized glass funnels to form a filter
and pre-wetted with de-ionized water. Challenge solutions of E. coli and MS2
viral particles were made with humic acid and fulvic acid, respectively.
Approximately 125 ml of the challenge solutions were poured through the
filters and the effluent collected in sterile 250 ml Erlenmeyer flasks. The
effluent was diluted and plated on petri dishes following standard laboratory
procedures. Log reduction values of E. coli and MS2 viral particles are
summarized in Tables III and IV below.


Clearly, the LRVs of the microbiological interception enhanced filter
media in the presence of NOM are significantly lower than the 7 to 9 log
reduction of E. coliand MS2 absent NOM interference as shown in Table II.
Examples 28-46: Microbiological Interception Capability Of The Filter Medium
Made With Treated Lyocell Fibers And An Adsorbent Layer In The Presence Of
Polyanionic Acids
In order to decrease the impact of NOM on the filter medium as shown
in Examples 24 to 27, an adsorbent prefilter was added to the filter to remove
or trap the NOM in the influent prior to contact with the filter medium. The
adsorbent layer is PLEKX® made with 600 g/m2 of finely ground coal-based
activated carbon having a surface area of 1000 m2/g, and is commercially
available from KX Industries, L.P.
A composite filter medium combining two (2) layers of a filter medium
made with the microbiological interception enhanced filter medium and one
(1) PLEKX® layer was fitted in ceramic Buchner funnels over a metal drainage
screen. The three (3) layers were secured in each Buchner funnels with a hot

melt adhesive to prevent any bypass of the influent. A head pressure of water
about 5 cm in depth was maintained in the Buchner funnel at all times. The
filters of examples 28 to 34 were charged with sterile deionized water prior to
the microbiological challenge and were not exposed to either humic or fulvic
acids. Results shown in Table V below show that the efficacy of the composite
filter medium with the addition of the adsorbent layer is similar to the results
shown in Table II above.
The filters of examples 35 to 40 were charged with 500 ml of a humic
acid solution (0.005 g/1 L H2O) prior to the microbiological challenge. Results
are shown in Table VI below. The filters of examples 41 to 46 were charged
with 500 ml of a fulvic acid solution (0.005 g/1 L H2O) prior to the
microbiological challenge. Results are shown in Table VII below.



The data shows that the use of an adsorbent prefilter such as PLEKX®,
placed upstream from the microbiological interception: enhanced filter
medium, maintained or improved the microbiological interception capabilities
of the filter medium by removing the NOM in the influent before the influent
contacted the microbiological interception enhanced filter medium. The
adsorbent prefilter medium does not need to be treated with the
microbiological interception enhancing agent to maintain the efficacy of the
microbiological interception enhanced filter medium. It may be a cost saving
measure not to treat the adsorbent prefilter medium. Thus, a composite filter
medium including the microbiological interception enhanced filter medium
and an adsorbent layer positioned upstream from the microbiological
interception enhanced filter medium would be robust enough to withstand
interference from NOM.
Examples 47-48: E co/i Challenges Of A Filtration System Of The Present
Invention
Two filtration systems of the present invention, as shown in Fig. 3,
including a composite filter medium comprising two (2) layers of an adsorbent
filter medium, PLEKX® made with 600 g/m2 of coal-based activated carbon
having a surface area of 1000 mVg, and a single layer of the microbiological
interception enhanced filter medium made from treated fibrillated lyocell
fibers as described in Example 4 were assembled using the clam shell filter
design of Figs. 1 and 2 described above. A supporting layer of PLEKX® was

placed in the bottom of each filter housing and glued into place using an
ethylene-vinyl acetate (EVA) hot melt. The layer of microbiological
interception enhanced filter medium was glued to the first PLEKX® layer,
followed by a second PLEKX® layer that was also glued into place atop the
microbiological interception enhanced filter medium. This configuration uses
only one of the PLEKX® layers as an adsorbent prefilter, while the other
PLEKX® layer serves primarily as a support for the microbiological interception
enhanced filter medium. The outside edges of the housing were also glued
and pressed firmly together to prevent any bypass leakage to the outside of the
housing. The dimensions of active filter area within the boundary defined by
the hot melt material was between 5 cm to 6 cm wide and 8 cm to 10 cm
long, providing an active filter area of between 40 cm2 and 60 cm2. While hot
melt was used during this prototype testing, filter assembly using ultrasonic or
other welding methods may be applied during commercial production.
A 0.635 cm (0.25 inch) inside diameter hose was attached to the inlet
of the filter housing using a plastic fitting and glued securely into place. The
outlet of the filter was open to allow fluid to exit the filter housing. The hose
attached to the filter inlet was attached to a glass Pyrex funnel to produce a
total inlet water column of approximately 30 cm to 60 cm. Test suspensions
were poured into the funnel to challenge the filter with various organisms.
Approximately 500 ml of de-ionized water was poured through the
filtration system to pre-wet the filter medium inside the housing. For £ coli
testing, a hose and funnel with a combined height of 60 cm was used to
provide head pressure. The flow rate at this influent: pressure was 70 ml/min.
A challenge suspension of £ coli was poured through the system and the
effluents collected in sterile 250 ml Erlenmeyer flasks. The effluents were
subjected to serial dilution in duplicate and plated on petri dishes following
standard laboratory procedures and left overnight in 37°C heated incubators.

The next day all test results were recorded and these are listed in Table VIII
below.

Thus, a filtration system of the present invention utilizing a composite
filter medium including a PLEKX® prefilter and the microbiological
interception enhanced filter medium will provide greater than 8.5 log
reduction of E. coli at a flow rate of approximately 1 to 2 ml/minute»cm2.
Example 49-51: MS2 Challenges Of A Filtration System Of The Present
Invention
Three filters were constructed in a similar fashion as for the £ coli
challenge as described in examples 47 and 48 above, for determining the viral
interception capability of a filtration system of the present invention. In two
filters, Examples 49 and 50, a layer of netting was installed at the bottom,
effluent side, of the filter housing, followed by a layer of the microbiological
interception enhanced filter medium, followed by a single top layer of PLEKX®
made with 600 g/m2 of coal-based activated carbon having a surface area of
1000 m2/g. For the third filter, Example 51, the plastic netting was replaced
with a metal 100 mesh screen as the bottom support layer. For the MS2
challenge, a hose and funnel of 30 cm was used to reduce the flow rate and
allow for longer contact time through the composite filter medium. De-
ionized water was poured through the system to pre-wet the layers and verify

that the housing had no leaks. A flow rate of 38 ml/ minute was recorded for
the 30 cm high water column. After the de-ionized water exited through the
system, the MS2 challenge solution was poured through the system. The
effluent was collected in sterile Erlenmeyer flasks, diluted and plated on Petri
dishes following standard procedures for MS2 and left overnight. The next day
all test results were recorded and listed in Table IX below.

A filtration system of the present invention utilizing a composite filter
medium including a PLEKX® prefilter and the microbiological interception
enhanced filter medium is shown to provide greater than 3.5 log reduction of
MS2 at a flow rate of approximately 0.75 ml/minute«cm2.
Examples 52 and 53: Long Term MS2 Challenges Of A Filtration System Of
The Present Invention
These examples assess the effectiveness of a filtration system of the
present invention when challenged with MS2 bacteriphage and having a
composite filter medium including two (2) layers of the microbiological
interception enhanced filter medium and two (2) layers of PLEKX® as described
earlier.
Two filtration systems of the present invention were prepared by
securing a 100 mesh screen inside a filter enclosure as shown in Figs. 1 and 2.
Two layers of the microbiological interception enhanced filter medium were

placed atop the mesh screen followed by two layers of PLEKX®. Each layer
was glued securely in place to prevent bypass. The filter enclosure was sealed
with the glue as well. A 0.635 cm (0.25 inch) inner diameter hose was
attached securely to the inlet of the filter housing. The outlet of the filter
housing was open to allow the passage of fluid. A funnel was securely
attached to each filter to provide one with a 25.4 cm (10 inches) water
column, and the other filter with a 10.2 cm (4 inches) water column for testing
of microbiological challenges.
Deionized water, approximately 500 ml, was passed through each
filtration system to pre-wet the filter medium and verify that no bypass was
occurring. Subsequently 500 ml of an MS2 challenge, prepared in deionized
water, was passed through each system. The effluents were collected in sterile
Erlenmeyer flasks, diluted and plated on Petri dishes following standard
procedures for the organism and left overnight. After 24 hours, an additional
500 ml of deionized water was passed through the system followed by another
500 ml MS2 challenge. This protocol was continued every 24 hours until the
filter media no longer provided an LRV above 4. The results are shown in
Tables X and XI below.



The useful life of the filtration system of Example 52 with a pressure
head of 25.4 cm provided an acceptable MS2 log reduction for 6.0 L of water
for 120 hours. However, when the pressure head was 10.2 cm, as in Example
53, the useful life of the filtration systems was extended, providing acceptable
log reduction values of MS2 for a volume of 13.0 L of water and 364 hours. It
is apparent that the flow rate will affect the microbiological interception
capabilities of the filtration system. From the results of Examples 52 and 53, a
lower flow rate will provide more effective microbiological interception due to
greater contact time of the microorganisms with the filter medium.

Example 54: Long Term E coli Challenges Of A Filtration System Of The
Present Invention
This example assesses the effectiveness of a filtration system of the
present invention having a composite filter medium including two (2) layers of
the microbiological interception enhanced filter medium and two (2) layers of
PLEKX® as described earlier.
Deionized water, approximately 500 ml, was passed through the
filtration system to pre-wet the filter medium and verify that no bypass was
occurring. Subsequently, 500 ml of the £ coli challenge, prepared in
deionized water, was passed through the filter. The effluent was collected in a
sterile Erlenmeyer flasks, diluted and plated on Petri dishes following standard
procedures for £ coli and left overnight. After 24 hours, an additional 500 ml
of deionized was passed through the system followed by another 500 ml £
coli challenge. This protocol was continued every 24 hours until the filter
medium no longer provided an LRV above 4. The results are shown in Table
XII below.


The filtration system of Example 50 provided acceptable performance
after 6.0 L of water had passed through the system at an average flow rate of
about 24 ml/minute wherein the head pressure was caused by a 25.4 cm water
column.
While the present invention has been particularly described, in
conjunction with a specific preferred embodiment, it is evident that many
alternatives, modifications and variations will be apparent to those skilled in
the art in light of the foregoing description. It is therefore contemplated that
the appended claims will embrace any such alternatives, modifications and
variations as falling within the true scope and spirit of the present invention.

We Claim:
1. A filter medium comprising:
a microporous structure having a mean flow path of 0.6 to 2 micron; and
a microbiological interception enhancing agent comprising a cationic metal
complex such as herein described capable of imparting a positive charge
on at least a portion of said microporous structure.
2. A filter medium as claimed in claim 1 wherein said microporous
structure comprises a plurality of nanofibers having a fiber diameter of 1000
nanometers.
3. A filter medium as claimed in claim 2 wherein the nanofibers comprise
organic nanofibers, inorganic nanofibers,, or a mixture thereof.
4. A filter medium as claimed in claim 2 wherein the nanofibers comprise
substantially fibrillated lyocell nanofibers.
5. A filter medium as claimed in claim 4 wherein the fibrillated lyocell
nanofibers have a Canadian Standard Freeness of 45.
6. A filter medium as claimed in claim 1 wherein said microporous
structure is a membrane comprising an organic material, an inorganic material,
or a mixture thereof.
7. A filter medium as claimed in claim 6 wherein the membrane comprises
a polymer material.
8. A filter medium as claimed in claim 1 wherein said microbiological
interception enhancing agent consists of a cationic metal complex wherein a

cationic material on a surface of said microporous structure has an associated
counter ion therewith and wherein a biologically active metal is caused to
precipitate with at least a portion of the counter ion associated with the cationic
material.
9. A filter medium as claimed in claim 8 wherein the cationic material
having a counter ion associated therewith is selected from the group consisting
of amines, amides, quaternary ammonium salts, imides, benzalkonium
compounds, biguanides, aminosilicon compounds, polymers thereof, and
combinations thereof.
10. A filter medium as claimed in claim 1 wherein the cationic metal
complex includes a biologically active metal selected from the group consisting
of silver, copper, zinc, cadmium, mercury, antimony, gold, aluminum,
platinum, palladium, and combinations thereof.
11. A filter medium as claimed in claim 1 wherein the cationic metal
complex is formed by treating at least a portion of said microporous structure
with a cationic material comprising a homopolymer of diallyl dimethyl
ammonium halide followed by precipitation of silver with at least a portion of
the halide counter ion associated with the homopolymer of diallyl dimethyl
ammonium halide.
12. A filter medium as claimed in any one of claims 1 through 11 wherein
said microporous structure is combined with an adsorbent prefilter medium
containing activated carbon, activated alumina, zeolites, diatomaceous earth,
silicates, aluminosilicates, titanates, bone char, calcium hydroxyapatite,
manganese oxides, iron oxides, magnesia, perlite, talc, polymeric particulates,
clay, iodated resins, ion exchange resins, ceramics, or combinations thereof.

13. A filter medium as claimed in claim 1 comprising:
an adsorbent prefilter having immobilized therein a material capable of
removing charge-reducing contaminants;
a microporous structure, disposed downstream from said adsorbent layer,
comprising a plurality of nanofibers, said microporous structure having a
mean flow path of 0.6 micron; and
a microbiological interception enhancing agent comprising a silver-cationic
material-halide complex having a high charge density, coated on at least
a portion of a surface of at least some of the plurality of nanofibers of
said microporous structure.
14. A filter medium as claimed in claim 13 wherein said microbiological
interception enhancing agent consists of a- silver-cationic material-halide
complex wherein a homopolymer of diallyl dimethyl ammonium halide on
surface of said microporous structure
has a halide counter ion associated therewith and wherein silver is precipitated
with at least a portion of the halide counter ion.
15. A filter medium as claimed in any one of claims 1,12, and 13 wherein
the homopolymer of diallyl dimethyl ammonium halide has a molecular weight
of 400,000 Daltons.
16. A filter medium as claimed in any one of claims 1, 13, 14, and 15
wherein said microporous structure incorporates one or more materials selected
from the group consisting of activated carbon, activated alumina, zeolites,
diatomaceous earth, silicates, aluminosilicates, titanates, bone char, calcium
hydroxy apatite, manganese oxides, iron oxides, magnesia, perlite, talc,

polymeric particulates, clay, iodated resins, ion exchange resins, ceramics, and
combinations thereof.
17. A filter medium as claimed in any one of claims 1 and 13 wherein said
microporous structure is optionally provided with a binder.
18. A filter medium as claimed in any one of claims 1 and 13 optionally
having a particulate prefilter.
19. A filter medium as claimed in any one of claims 2 and 13 wherein the
plurality of nanofibers are made from material selected from the group
consisting of polymers, ion-exchange resins, engineered resins, ceramics,
cellulose, rayon, a wool, silk, glass, metal,
activated alumina, activated carbon, silica, zeolites, diatomaceous earth,
activated bauxite, fuller's earth, calcium hydroxyapatite, and combinations
thereof.
20. A filter medium as claimed in claim 1 comprising:
a bed of granular material capable of removing charge-reducing
contaminants;
a microporous structure, disposed downstream from said granular bed,
having a mean flow path of 0.6 micron; and
a microbiological interception enhancing agent comprising a silver-cationic
material-halide complex having a high charge density, coated on at least
a portion of a surface of said microporous structure.
21. A filter medium as claimed in claim 1 comprising:
a solid composite block comprising a material capable of removing charge-
reducing contaminants;

a microporous structure, disposed downstream from said block, having a
mean flow path of 2.0 microns; and
a microbiological interception enhancing agent comprising a silver-cationic
material-halide complex having a high charge density, coated on at least
a portion of a surface of said microporous structure.
22. A filter system as claimed in any one of claims 20 and 21 optionally
having a particulate prefilter.
23. A filter medium as claimed in any one of claims 20 and 21 wherein the
silver-cationic material-halide complex comprises a homopolymer of dially
dimethyl ammonium halide, on a surface of said microporous structure having a
halide counter ion associated therewith and wherein silver is precipitated with
at least a portion of the halide counter ion.
24. A filter medium as claimed in any one of claims 20 and 21 wherein the
silver-cationic material-halide complex comprises a homopolymer of dially
dimethyl ammonium halide on a surface of said microporous structure having a
halide counter ion associated therewith wherein the homopolymer of diallyl
dimethyl ammonium halide has a molecular weight of 400,000 Daltons, and
wherein silver is precipitated with at least a portion of the halide counter ion.
25. A filter medium as claimed in any one of claims 20 and 21 wherein the
material capable of removing charge-reducing contaminants comprises
activated carbon, activated alumina, zeolites, diatomaceous earth, silicates,
aluminosilicates, titanates, bone char, calcium hydroxyapatite, manganese
oxides, iron oxides, magnesia, perlite, talc, polymeric particulates, clay, iodated
resins, ion exchange resins, ceramics, or combinations thereof.

26. A filter medium as claimed in any one of claims 20 and 21 wherein said
microporous structure incorporates one or more materials selected from the
group consisting of activated carbon, activated alumina, zeolites, diatomaceous
earth, silicates, aluminosilicates, titanates, bone char, calcium hydroxyapatite,
manganese oxides, iron oxides, magnesia, perlite, talc, polymeric particulates,
clay, iodated resins, ion exchange resins, ceramics, and combinations thereof.
27. A filter medium as claimed in any one of claims 20 and 21 wherein said
microporous structure is optionally provided with a binder.
28. A process of making the filter medium of claim 1 comprising the steps
of:
providing a microporous structure having a mean flow path of 1 micron;
and
coating at least a portion of the microporous structure with a
microbiological interception enhancing agent, the microbiological
interception enhancing agent comprising a cationic metal complex
capable of imparting a positive charge on at least a portion of the
microporous structure.
29. A process as claimed in claim 28 wherein the step of providing a
microporous structure comprises forming a plurality of nanofibers having a fiber
diameter of 1000 nanometers into the microporous structure.
30. A process as claimed in claim 28 wherein the step of providing a
microporous structure comprises forming a plurality of nanofibers, wherein the
nanofibers comprise organic nanofibers, inorganic nanofibers, or a mixture
thereof, into the microporous structure.

31. A process as claimed in claim 28 wherein the step of providing a
microporous structure comprises forming a plurality of substantially fibrillated
lyocell nanofibers wherein at least a portion of the fibrillated lyocell nanofibers
are 1 millimeter to 8 millimeters in length having a diameter of 250
nanometers, into the microporous structure.
32. A process as claimed in claim 28 wherein the step of forming a plurality
of substantially fibrillated lyocell nanofibers comprises forming a plurality of
substantially fibrillated lyocell nanofibers having a Canadian Standard Freeness
of 45, into the microporous structure.
33. A process as claimed in claim 28 wherein the step of providing a
microporous structure comprises providing a membrane comprising an organic
material, an inorganic material, or a mixture thereof.
34. A process for making a filter medium as claimed in claim 28 comprising
the steps of:
providing a plurality of nanofibers;
coating at least a portion of a surface of at least some of the plurality of
nanofibers with a microbiological interception enhancing agent, the
microbiological intercepting agent comprising a cationic metal complex;
and
forming said nanofibers into a microporous structure having a mean flow
path of 1 micron.
35. A process for making a filter medium as claimed in claim 28 comprising
the steps of:
providing a plurality of polymer nanofibers;

coating at least a portion of a surface of at least some of the plurality of
polymer nanofibers with a microbiological interception enhancing agent,
the microbiological intercepting agent comprising a cationic metal
complex; and
forming a microporous structure having a mean flow path of 1 micron.
36. A process for making a filter medium as claimed in claim 28 comprising
the steps of:
providing a plurality of cellulose nanofibers;
coating at least a portion of a surface of eit least some of the plurality of
cellulose nanofibers with a microbiological interception enhancing
agent, the microbiological intercepting agent comprising a cationic metal
complex; and
forming a microporous structure having a mean flow path of 1 micron.
37. A process for making a filter medium as claimed in claim 28 comprising
the steps of:
providing a membrane having a mean flow path of 1 micron; and
coating at least a portion of the membrane with a microbiological
interception enhancing agent, the microbiological interception
enhancing agent comprising a cationic metal complex capable of
imparting a positive charge on at least a portion of the membrane.
38. A process as claimed in claim 37 wherein the step of coating comprises:
treating at least a portion of the membrane with a cationic material having a
counter ion associated therewith to form a canonically charged
membrane;
exposing the cationically charged membrane to a biologically active metal
salt; and

precipitating a biologically-active metal complex with at least a portion of
the counter ion associated with the cationic material on at least a portion
of the membrane.
39. A process for making a filter medium as claimed in claim 28 comprising
the steps of:
providing a plurality of nanofibers;
coating at least a portion of a surface of at least some of the plurality of said
nanofibers with a microbiological interception enhancing agent, the
microbiological interception enhancing agent comprising a silver-amine-
halide complex having a medium to high charge density and a molecular
weight of 5000 Daltons; and
forming a microporous structure having a mean flow path of 0.6 microns.
providing an adsorbent prefilter comprising a material capable of removing
charge-reducing contaminants from an influent, and placing said
adsorbent prefilter upstream of said microporous structure.
40. A process for making a filter medium as claimed in claim 28 comprising
the steps of:
providing an adsorbent prefilter comprising a material capable of removing
charge-reducing contaminants from an influent, wherein the material is
immobilized into a solid composite block;
providing a plurality of nanofibers;
coating at least a portion of a surface of at least some of the plurality of said
nanofibers with a microbiological interception enhancing agent, the
microbiological interception enhancing agent comprising a
silver-amine-halide complex having a medium to high charge density and a
molecular weight of 5000 Daltons; and

forming a microporous structure comprising the plurality of nanofibers
having a mean flow path of 0.6 microns, wherein the microporous
structure is downstream from the adsorbent prefilter.
41. A process as claimed in any one of claims 28, 34, 35, 36, 37, 39, and
40 optionally comprising the step of incorporating one or more ingredients to
the filter medium selected from the group consisting of activated carbon,
activated alumina, zeolites, diatomaceous earth, silicates, aluminosilicates,
titanates, bone char, calcium hydroxyapatite, manganese oxides, iron oxides,
magnesia, perlite, talc, polymeric particulates, clay, iodated resins, ion
exchange resins, ceramics, and combinations thereof.
42. A process as claimed in any one of claims 34, 36, 39, and 40 wherein
the step of providing a plurality of nanofibers comprising forming a plurality of
fibrillated lyocell nanofibers and forming the fibriillated lyocell nanofibers into
the microporous structure.
43. A process as claimed in any one of claims 34, 35, and 36 wherein the
step of coating comprises:
treating at least a portion of the plurality of nanofibers with a cationic
material having a counter ion associated therewith to form a cationically
charged fiber material;
exposing the cationically charged fiber material to a biologically active
metal salt; and
precipitating a biologically-active metal complex with at least a portion of
the counter ion associated with the cationic material on at least a portion
of the canonically charged fiber material.

44. A process as claimed in any one of claims 34, 35, and 36 wherein in the
step of coating, at least a portion of the plurality of nanofibers are treated with a
cationic material having a counter ion associated therewith to form a
canonically charged fiber material, wherein the cationic material is selected
from the group consisting of amines, amides, quaternary ammonium salts,
imides, benzalkonium compounds, biguanides, pyrroles, aminosilicon
compounds, polymers thereof, and combinations thereof.
45. A process as claimed in any one of claims 34, 35, and 36 wherein in the
step of coating, the canonically charged fiber material is exposed to a
biologically active metal salt, wherein the biologically active metal is selected
from the group consisting of silver, copper, zinc, cadmium, mercury, antimony,
gold, aluminum, platinum, palladium, and combinations thereof.
46. A process as claimed in any one of claims 34, 35, and 36 wherein in the
step of coating, the cationic metal complex comprises a metal-amine-halide
complex.
47. A process as claimed in any one of claims 34, 35, and 36 wherein in the
step of coating, the cationic metal complex comprises a silver-amine-balide
complex.
48. A process as claimed in any one of claims 34, 35, 36, 37, 39, and 40
optionally comprising the step of providing a prefilter capable of removing
charge-reducing contaminants from an influent prior to the influent contacting
the microporous structure.
49. A process as claimed in any one of claims 29, 30, 34, 39, and 40
wherein the step of providing a plurality of nanofibers, the nanofibers are made

from a material selected from the group consisting of polymers, ion-exchange
resins, engineered resins, ceramics, cellulose, reiyon, wool, silk, glass, metal,
activated alumina, activated carbon, silica, zeolites, diatomaceous earth,
activated bauxite, fuller's earth, calcium hydroxyapatite, and combinations
thereof.
50. A process as claimed in any one of claims 34, 35, 36, 39, and 40
wherein the step of forming the microporous structure comprises a wet laid
process, a dry laid melt blown, or dry laid spun-bonding.
51. A process as claimed in any one of claims 34, 35, 36, 39, and 40
wherein the step of forming the microporous structure includes incorporating
into the microporous structure one or more ingredients selected from the group
consisting of activated carbon, activated alumina, zeolites, diatomaceous earth,
silicates, aluminosilicates, titanates, bone char, calcium hydroxyapatite,
manganese oxides, iron oxides, magnesia, perlite, talc, polymeric particulates,
clay, iodated resins, ion exchange resins, ceramic;, and combinations thereof.
52. A filter medium substantially as herein described particularly with
reference to the foregoing examples and illustrations in the accompanying
drawings.
53. A process for making a filter medium substantially as herein described
particularly with reference to the foregoing examples.

This invention discloses A filter medium comprising:
a microporous structure having a mean flow path of 0.6 to 2 micron; and
a microbiological interception enhancing agent comprising a cationic metal
complex such as herein described capable of imparting a positive charge on at least
a portion of said microporous structure.
This invention also discloses a process for making said filter medium.

Documents:

956-KOLNP-2004-(03-01-2012)-FORM-27.pdf

956-KOLNP-2004-CORRESPONDENCE 1.1.pdf

956-KOLNP-2004-CORRESPONDENCE.pdf

956-KOLNP-2004-FORM 27 1.1.pdf

956-KOLNP-2004-FORM 27.pdf

956-kolnp-2004-granted-abstract.pdf

956-kolnp-2004-granted-assignment.pdf

956-kolnp-2004-granted-claims.pdf

956-kolnp-2004-granted-correspondence.pdf

956-kolnp-2004-granted-description (complete).pdf

956-kolnp-2004-granted-drawings.pdf

956-kolnp-2004-granted-examination report.pdf

956-kolnp-2004-granted-form 1.pdf

956-kolnp-2004-granted-form 18.pdf

956-kolnp-2004-granted-form 3.pdf

956-kolnp-2004-granted-form 5.pdf

956-kolnp-2004-granted-form 6.pdf

956-kolnp-2004-granted-gpa.pdf

956-kolnp-2004-granted-reply to examination report.pdf

956-kolnp-2004-granted-specification.pdf


Patent Number 225990
Indian Patent Application Number 956/KOLNP/2004
PG Journal Number 49/2008
Publication Date 05-Dec-2008
Grant Date 03-Dec-2008
Date of Filing 07-Jul-2004
Name of Patentee KX TECHNOLOGIES, LLC
Applicant Address 269 SOUTH LAMBERT ROAD, ORANGE, CT 06477
Inventors:
# Inventor's Name Inventor's Address
1 KOSLOW EVAN E 14 TWELVE O'CLOCK ROAD, WESTON, CT 06883
PCT International Classification Number B01D 61/00
PCT International Application Number PCT/US03/00067
PCT International Filing date 2003-01-02
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 10/286,695 2002-11-01 U.S.A.
2 60/354,062 2002-03-31 U.S.A.