WO2001082986A9 - Ion-sensitive, water dispersible polymers - Google Patents
Ion-sensitive, water dispersible polymersInfo
- Publication number
- WO2001082986A9 WO2001082986A9 PCT/US2001/014339 US0114339W WO0182986A9 WO 2001082986 A9 WO2001082986 A9 WO 2001082986A9 US 0114339 W US0114339 W US 0114339W WO 0182986 A9 WO0182986 A9 WO 0182986A9
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- WO
- WIPO (PCT)
- Prior art keywords
- weight percent
- wetting composition
- binder
- ion
- water
- Prior art date
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Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/62—Compostable, hydrosoluble or hydrodegradable materials
Definitions
- Recent binder compositions have been developed which can be more dispersible and are more environmentally responsible than past binder compositions.
- One class of binder compositions includes polymeric materials having inverse solubility in water. These binder compositions are insoluble in warm water, but are soluble in cold water, such as found in a toilet. It is well known that a number of polymers exhibit cloud points or inverse solubility properties in aqueous media.
- binders of interest include a class of binders, which are ion-sensitive.
- Several U.S. and European patents assigned to Lion Corporation of Tokyo, Japan disclose ion-sensitive polymers comprising acrylic acid and alkyl or aryl acrylates. See U.S. Pat. Nos. 5,312,883, 5,317,063 and 5,384,189, the disclosures of which are incorporated herein by reference, as well as, European Pat. No. 608460A1.
- terpolymers are disclosed as suitable binders for flushable nonwoven webs.
- each calcium ion binds with two carboxylate groups either intramolecularly or intermolecularly.
- Intramolecular association causes the polymer chain to coil up, which eventually leads to polymer precipitation.
- Intermolecular association yields crosslinking.
- the terpolymer is not soluble in water containing more than about 15 ppm Ca 2+ and/or Mg 2+ . Due to the strong interaction between calcium ions and the carboxylate groups of the terpolymer, dissociation of the complex is highly unlikely because this association is irreversible.
- the polymer formulations of the present invention are relatively insensitive to calcium and/or magnesium ions. Consequently, flushable products containing the polymer formulations of the present invention maintain dispersibility in hard water. Furthermore, the ion-sensitive polymer formulations of the present invention can have improved properties of sprayability or reduced high-shear viscosity, improved product wettability or decreased properties of product stiffness and stickiness.
- the polymer formulations of the present invention are useful as binders and structural components for air-laid and wet-laid nonwoven fabrics for applications such as body-side liners, fluid distribution materials, fluid intake materials (surge) or cover stock in various personal care products.
- the polymer formulations of the present invention are particularly useful as a binder material for flushable personal care products, particularly wet wipes for personal use such as cleaning or treating skin, make-up removal, nail polish removal, medical care, and also wipes for use in hard surface cleaning, automotive care, including wipes comprising cleaning agents, disinfectants, and the like.
- the flushable products maintain integrity or wet strength during storage and use, and break apart or disperse after disposal in the toilet when the salt concentration falls below a critical level.
- Suitable substrates for treatment include tissue, such as creped or uncreped tissue, coform products, hydroentangled webs, airlaid mats, fluff pulp, nonwoven webs, and composites thereof.
- tissue such as creped or uncreped tissue, coform products, hydroentangled webs, airlaid mats, fluff pulp, nonwoven webs, and composites thereof.
- Methods for producing uncreped tissues and molded three-dimensional tissue webs of use in the present invention can be found in commonly owned U.S. patent application, Serial Number 08/912,906, "Wet Resilient Webs and Disposable Articles Made Therewith," by F.-J. Chen et al, filed Aug. 15, 1997; U.S. Pat. No. 5,429,686, issued to Chiu et al. on July 4, 1995; U.S. Pat. No. 5,399,412, issued to S.J. Sudall and S.A. Engel on
- the present invention further discloses an improved wetting composition for wet wipes.
- Wet wipes employing the polymer formulations of the present invention are stable during storage and retain a desired level of wet strength during use and are wetted with a wetting composition or cleaning agent that can be relatively free, or is substantially free, of organic solvents.
- Fig. 1 is a graph that depicts wet strength data for three binder formulations as a function of ionic environment and soak time.
- Fig. 2 is a chart showing how wet tensile strength (reported as CDWT in grams per 2.54 cm over a range of soak times) can change over time as a fabric, comprising 68 gsm softwood airlaid webs and ion-sensitive binders, are soaked in solutions comprising calcium ions.
- Fig. 3 compares two data sets with Lion SSB-3b product taken from FIG. 2 (labeled as Code 3300) with a sulfonated salt-sensitive binder blended with Dur-O-Set ® RB polymer in a 75/25 ratio.
- the formulations should desirably be (1) functional; i.e., maintain wet strength under controlled conditions and dissolve or disperse rapidly in soft or hard water such as found in toilets and sinks around the world; (2) safe (not toxic); and (3) relatively economical.
- the wetting composition with which the wet wipes of the present invention are treated can provide some of the foregoing advantages, and, in addition, can provide one or more of (7) improved skin care, such as reduced skin irritation or other benefits, (8) improved tactile properties, and (9) promote good cleaning by providing a balance in use between friction and lubricity on the slrin (skin glide).
- improved skin care such as reduced skin irritation or other benefits
- improved tactile properties and (9) promote good cleaning by providing a balance in use between friction and lubricity on the slrin (skin glide).
- the ion- sensitive polymer formulations of the present invention and articles made therewith, especially wet wipes comprising particular wetting compositions set forth below can meet many or all of the above criteria. Of course, it is not necessary for all of the advantages of the preferred embodiments of the present invention to be met to fall within the scope of the present invention.
- Suitable acrylic monomers include, but are not limited to, acrylic esters and methacrylic esters having an alkyl group of 1 to 18 carbon atoms or a cycloalkyl group of 3 to 18 carbon atoms and it is preferred that acrylic esters and/or methacrylic esters having a alkyl group of 1 to 12 carbon atoms or a cycloalkyl group of 3 to 12 carbon atoms be used singly or in combination.
- acrylic acid copolymers useful in the present invention include copolymers of 10 weight percent to 90 weight percent, desirably 20 weight percent to 70 weight percent of acrylic acid and/or methacrylic acid and 90 weight percent to 10 weight percent, desirably 80 weight percent to 30 weight percent of acrylic esters and/or methacrylic esters having an alkyl group of 1 to 18 carbon atoms or a cycloalkyl group of 3 to 18 carbon atoms in which 1 to 60 mole percent, desirably 5 to 50 mole percent of acrylic acid and/or methacrylic acid is neutralized to form a salt; or copolymers of 30 weight percent to 75 weight percent, desirably 40 weight percent to 65 weight percent of acrylic acid, 5 weight percent to 30 weight percent, desirably 10 weight percent to 25 weight percent of acrylic esters and/or methacrylic esters having an ahcyl group of 8 to 12 carbon atoms and 20 weight percent to 40 weight percent; desirably 25 weight percent to 35 weight percent
- Additional suitable sulfonate-containing monomers include, but are not limited to, 2-methyl-2-propene sulfonic acid, vinyl sulfonic acid, styrene sulfonic acid, 2-sulfopropyl methacrylate and 3- sulfopropyl acrylate, and organic or inorganic salts thereof, such as alkali earth metals and organic amine salts, such as alkyl ammonium hydroxide wherein the alkyl groups are C r C 18 .
- one or more hydrophobic monomers are added to the polymer.
- the ion-sensitive sulfonate anion modified acrylic acid copolymers of the present invention may be produced from monomers including the following monomers: acrylic acid, methacrylic acid, or a combination thereof; 2-acrylamido-2-methyl-l-propanesulfonic acid (AMPS) and organic or inorganic salts thereof, such as the sodium salt thereof (NaAJMPS); butyl acrylate; and 2-ethylhexyl acrylate.
- the ion-sensitive sulfonate anion modified acrylic acid copolymers of the present invention are produced from: acrylic acid; AMPS, NaAMPS or a combination thereof; butyl acrylate; and 2-ethylhexyl acrylate.
- the ion-sensitive polymer formulations of the present invention including sulfonate anion modified acrylic acid copolymers are insoluble in a salt solution containing at least about 1 weight percent of one or more inorganic and/or organic salts containing monovalent ions. More desirably, the ion-sensitive polymer formulations of the present invention including sulfonate anion modified acrylic acid terpolymers are insoluble in a salt solution containing from about 1 weight percent to about 5.0 weight percent of one or more inorganic and/or organic salts containing monovalent ions.
- the ion-sensitive polymer formulations of the present invention including sulfonate anion modified acrylic acid terpolymers are insoluble in salt solutions containing from about 1 weight percent to about 3.0 weight percent of one or more inorganic and/or organic salts containing monovalent ions.
- Suitable monovalent ions include, but are not limited to, Na + ions, K + ions, Li + ions,
- the ion-sensitive polymer formulations of the present invention are desirably soluble in water containing up to about 50 ppm Ca 2+ and/or Mg 2+ ions. More desirably, the ion-sensitive polymer formulations of the present invention are soluble in water containing up to about 100 ppm Ca 2+ and/or Mg 2+ ions.
- Proteins capable of being salted out, optionally modified to have additional soft ionic groups, can be useful as the ion-sensitive polymer of the present invention.
- the triggering mechanism which results in a pre-moistened wipe losing wet strength and becoming flushable even in hard water, can be due to the dilution of a monovalent or divalent metal ion, and particularly an alkali metal ion, with monovalent ions, such as sodium being preferred.
- a monovalent or divalent metal ion and particularly an alkali metal ion
- monovalent ions such as sodium being preferred.
- Natural polymers and gums which may be adapted for use as ion-sensitive binders, are described by R.L. Whistler and J.N. BeMiller in Industrial Gums, New York: Academic Press, Inc., 1973, incorporated herein by reference. Natural polymers, which become firm or form a gel in the presence of calcium ions, are described below.
- the co-binder polymer can have a glass transition temperature; i.e., T g , that is lower than the glass transition temperature of the ion-sensitive polymer.
- the co-binder polymer can be insoluble in water, or can reduce the shear viscosity of the ion-sensitive polymer.
- the co-binder can be present at a level relative to the solids mass of the triggerable polymer of about 45% or less, specifically about 30% or less, more specifically about 20% or less, more specifically still about 15% or less, and most specifically about 10% or less, with exemplary ranges of from about 1% to about 45% or from about 25% to about 35%, as well as from about 1% to about 20% or from about 5% to about 25%.
- the amount of co-binder present should be low enough, for co-binders with the potential to form water insoluble bonds or films, that the co-binder remains a discontinuous phase unable to create enough crosslinked, or insoluble bonds, to jeopardize the dispersibility of the treated substrate.
- the ion-sensitive polymer formulation of the present invention can comprise about 75 weight percent acrylic acid terpolymer and about 25 weight percent polyethylene- vinyl acetate) co-binder.
- the co-binder polymer can be in the form of an emulsion latex.
- the surfactant system used in such a latex emulsion should be such that it does not substantially interfere with the dispersibility of the ion-sensitive polymer.
- the combination of the ion-sensitive polymer and the co-binder polymer reduces the stiffness of the article to which it is applied compared to the article with just the ion-sensitive polymer.
- Co-binder polymers that can meet many or all of the foregoing criteria include, but are not limited to, poly(ethylene-vinyl acetate), poly(styrene-butadiene), poly(styrene-acrylic), a vinyl acrylic terpolymer, neoprene, a polyester latex, an acrylic emulsion latex, poly vinyl chloride, ethylene-vinyl chloride copolymer, a carboxylated vinyl acetate latex, and the like, all of which can be non-crosslinking (e.g., devoid of N-methylol acrylamide or other crosslinkers), crosslinking, or potentially crosslinking (i.e., prepared with a crosslinker present) but not substantially crosslinked in the final product.
- non-crosslinking e.g., devoid of N-methylol acrylamide or other crosslinkers
- crosslinking i.e., prepared with a crosslinker present
- a particularly preferred non-crosslinking poly(ethylene-vinyl acetate) is Dur-O-Set ® RB available from National Starch and Chemical Co., Bridgewater, NJ.
- a particularly preferred non-crosslinking polystyrene- butadiene) is Rovene ® 4817 available from Mallard Creek Polymers, Charlotte, NC.
- a particularly preferred non-crosslinking poly(styrene-acrylic) is Rhoplex ® JNM 1715K available from Rohm and Haas, Philadelphia, PA.
- filler-like approaches could include microparticles, microspheres, or microbeads of metal, glass, carbon, mineral, quartz, and/or plastic, such as acrylic or phenolic, and hollow particles having inert gaseous atmospheres sealed within their interiors. Examples include EJJXPANCEL phenolic microspheres from Expancel of Sweden, which expand substantially when heated, or the acrylic microspheres known as PM 6545 available from PQ Corporation of Pennsylvania. Foaming agents, including CO 2 dissolved in the ion-sensitive binder, could also provide helpful discontinuities as gas bubbles in the matrix of an ion-sensitive binder, allowing the dispersed gas phase in the ion-sensitive binder to serve as the co-binder.
- the T g of the co-binder polymer can be lower than the T g of the ion-sensitive polymer, which is believed to improve the flexibility of the treated substrate, especially in the dry state.
- Jm Table 1 shown below is a comparison of the glass transition temperature of some of the preferred polymers useful in the present invention.
- useful co-binder polymers can include a variety of commercial latex emulsions, including those selected from the Rovene ® series (styrene butadiene latices available from Mallard Creek Polymers of Charlotte, N.C.), the JRhoplex ® latices of Rohm and Haas Company, and the Elite ® latices of National Starch.
- Polymer emulsions or dispersions generally comprise small polymer particles, such as crosslinkable ethylene vinyl acetate copolymers, typically in spherical form, dispersed in water and stabilized with surface active ingredients such as low molecular weight emulsifiers or high molecular weight protective colloids.
- liquid binders can be applied to airlaid webs or other substrates by methods known in the art of binder treatment for nonwoven webs, including spray or foam application, flooded nip impregnation, curtain coating, etc., followed by drying.
- latex compounds and other resins or emulsions can be considered, including vinyl acetate copolymer latices, such as 76 RES 7800 from Union Oil Chemicals Divisions and Resyn ® 25-1103, Resyn ® 25-1109, Resyn ® 25-1119, and Resyn ® 25-1189 from National Starch and Chemical Corporation, ethylene-vinyl acetate copolymer emulsions, such as Airflex ® ethylene-vinylacetate from Air Products and Chemicals Inc., acrylic-vinyl acetate copolymer emulsions, such as Rhoplex ® AR-74 from Rohm and Haas Company, Synthemul ® 97-726 from Reichhold Chemicals Inc.
- DL650A available from Dow Chemical Company
- rubber latices such as neoprene available from Serva Biochemicals
- polyester latices such as Eastman AQ 29D available from Eastman Chemical Company
- vinyl chloride latices such as Geon ® 352 from B. F.
- an effective co-binder polymer replaces a portion of the ion-sensitive polymer formulation and permits a given strength level to be achieved in a pre-moistened wipe with at least one of lower stiffness, better tactile properties (e.g., lubricity or smoothness), or reduced cost, relative to an otherwise identical pre-moistened wipe lacking the co- binder polymer and comprising the ion-sensitive polymer formulation at a level sufficient to achieve the given tensile strength.
- These particles can be applied in highloft nonwovens by depositing them with the fibers during the airlaid process, and then later adding 10% to 30% moisture to cause the particles to swell and adhere to the fibers. This can be called the "chewing gum effect," meaning that the dry, non-tacky fibers in the web become sticky like chewing gum once moistened. Good adhesion to polar surfaces and other surfaces is obtained.
- These binders are available as free flowing particles formed from latex emulsions that have been dried and treated with agents to prevent cohesion in the dry state. They can be entrained in air and deposited with fibers during the airlaid process, or can be applied to a substrate by electrostatic means, by direct contact, by gravity feed devices, and other means.
- the commercial product can be used without reducing the amount of crosslinker by controlling the curing of the co-binder polymer, such as limiting the time and temperature of drying to provide a degree of bonding without significant crosslinking.
- dry emulsion binder powders have the advantage that they can easily be incorporated into a nonwoven or airlaid web during formation of the web, as opposed to applying the material to an existing substrate, permitting increased control over placement of the co-binder polymer.
- a nonwoven or airlaid web can be prepared already having dry emulsion binders therein, followed by moistening when the ion-sensitive polymer formulation solution is applied, whereupon the dry emulsion powder becomes tacky and contributes to binding of the substrate.
- the dry emulsion powder can be entrapped in the substrate by a filtration mechanism after the substrate has been treated with ion-sensitive binder and dried, whereupon the dry emulsion powder is rendered tacky upon application of the wetting composition.
- the dry emulsion powder is dispersed into the ion-sensitive polymer formulation solution either by application of the powder as the ion-sensitive polymer formulation solution is being sprayed onto the web or by adding and dispersing the dry emulsion powder particles into the ion-sensitive polymer formulation solution, after which the mixture is applied to a web by spraying, by foam application methods, or by other techniques known in the art.
- the polymer formulations of the present invention may be used as binders.
- the binder formulations of the present invention may be applied to any fibrous substrate.
- the binders are particularly suitable for use in water- dispersible products.
- Suitable fibrous substrates include, but are not limited to, nonwoven and woven fabrics. In many embodiments, particularly personal care products, preferred substrates are nonwoven fabrics.
- nonwoven fabric refers to a fabric that has a structure of individual fibers or filaments randomly arranged in a mat-like fashion (including papers).
- the binder composition may be applied to the fibrous substrate by any known process of application. Suitable processes for applying the binder material include, but are not limited to, printing, spraying, electrostatic spraying, coating, flooded nips, metered press rolls, impregnating or by any other technique.
- the amount of binder composition may be metered and distributed uniformly within the fibrous substrate or may be non-uniformly distributed within the fibrous substrate.
- the binder composition may be distributed throughout the entire fibrous substrate or it may be distributed within a multiplicity of small closely spaced areas. In most embodiments, uniform distribution of binder composition is desired.
- a desirable feature of the present invention is that the improvement in tensile strength is effected where the amount of binder composition present, "add-on", in the resultant fibrous substrate represents only a small portion by weight of the entire substrate.
- the amount of "addon” can vary for a particular application; however, the optimum amount of "add-on” results in a fibrous substrate which has integrity while in use and also quickly disperses when agitated in water.
- the binder components typically are from about 5 to about 65 percent, by weight, of the total weight of the substrate. More particularly, the binder components may be from about 10 to about 35 percent, by weight, of the total weight of the substrate. Even more particularly, " the binder components may be from about 17 to about 22 percent by weight of the total weight of the substrate.
- the binder formulations of the present invention are particularly useful for binding fibers of air-laid nonwoven fabrics.
- These airlaid materials are useful for body-side liners, fluid distribution materials, fluid in-take materials, such as a surge material, absorbent wrap sheet and cover stock for various water-dispersible personal care products.
- Air-laid materials are particularly useful for use as a pre-moistened wipe (wet wipe).
- the basis weights for air-laid non-woven fabrics may range from about 20 to about 200 grams per square meter ("gsm") with staple fibers having a denier of about 0.5-10 and a length of about 6-15 millimeters.
- the nonwoven fabrics of the present invention may also be incorporated into such body fluid absorbing products as sanitary napkins, diapers, surgical dressings, tissues and the like.
- the binder is such that it will not dissolve when contacted by body fluids since the concentration of monovalent ions in the body fluids is above the level needed for dissolution; i.e., greater that 0.3 % by weight and/or greater than 1% by weight.
- the nonwoven fabric retains its structure, softness and exhibits a toughness satisfactory for practical use.
- a drying step can be avoided, if desired, or replaced with low-temperature water removal operations such as room-temperature drying or freeze drying. Elevated temperature is generally helpful for drying, but the drying can be done at temperatures below what is normally needed to drive crosslinking reactions.
- the peak temperature to which the substrate is exposed or to which the substrate is brought can be below any of the following: 180° C, 160° C, 140° C, 120° C, 110° C, 105° C, 100° C, 90° C, 75° C, and 60° C, with an exemplary range for peak web temperature of from about 50° C. to about 110° C, or from about 70° C. to about 140° C. Of course, higher temperatures can be used, but are not necessary in most embodiments.
- the wipe may desirably contain from about 10 percent to about 400 percent of the wetting composition, more desirably from about 100 percent to about 300 percent of the wetting composition, and even more desirably from about 180 percent to about 240 percent of the wetting composition.
- the wipe maintains its desired characteristics over the time periods involved in warehousing, transportation, retail display and storage by the consumer. Accordingly, shelf life may range from two months to two years.
- the pre-moistened wipes of the present invention are wetted with an aqueous wetting composition, which has one or more of the following properties:
- salts that have been disclosed as having urease inhibition properties include ferric and aluminum salts, especially the nitrates, and bismuth salts.
- Other urease inhibitors are disclosed by Trinh, including hydroxamic acid and its derivatives; thiourea; hydroxylamine; salts of phytic acid; extracts of plants of various species, including various tannins, e.g.
- carob tannin and their derivatives such as chlorogenic acid derivatives; naturally occurring acids such as ascorbic acid, citric acid, and their salts; phenyl phosphoro diamidate/diamino phosphoric acid phenyl ester; metal aryl phosphoramidate complexes, including substituted phosphorodiamidate compounds; phosphoramidates without substitution on the nitrogen; boric acid and/or its salts, including especially, borax, and/or organic boron acid compounds; the compounds disclosed in European Patent Application 408,199; sodium, copper, manganese, and/or zinc dithiocarbamate; quinones; phenols; thiurams; substituted rhodanine acetic acids; alkylated benzoquinones; formarnidine disulphide; 1 :3-diketones maleic anhydride; succinamide; phthalic anhydride; pehenic acid; /N,N-dihalo-2- imidazolidinones; N-halo2-
- the wetting composition contains from about 0.01 weight percent to about 2 weight percent of odor control additives. Even more desirably, the wetting composition contains from about 0.03 weight percent to about 1 weight percent of odor control additives.
- the wetting composition and/or pre-moistened wipes comprise derivatized cyclodextrins, such as hydroxypropyl beta-cyclodextrin in solution, which remain on the sldn after wiping and provide an odor-absorbing layer.
- the odor source is removed or neutralized by application of an odor-control additive, exemplified by the action of a chelant that binds metal groups necessary for the function of many proteases and other enzymes that commonly produce an odor. Chelating the metal group interferes with the enzyme's action and decreases the risk of malodor in the product.
- Deposition may be by spray, coating, electrostatic deposition, impingement, filtration (i.e., a pressure differential drives a particle-laden gas phase through the substrate, depositing particles by a filtration mechanism), and the like, and may be applied uniformly on one or more surfaces of the substrate or may be applied in a pattern (e.g., repeating or random patterns) over a portion of the surface or surfaces of the substrate.
- the detackifier may be present throughout the thickness of the substrate, but may be concentrated at one or both surfaces, and may be substantially only present on one or both surfaces of the substrate.
- Polymers and other additives having low surface energy may also be used, including a wide variety of fluorinated polymers, silicone additives, polyolefins and thermoplastics, waxes, debonding agents known in the paper industry including compounds having alkyl side chains such as those having 16 or more carbons, and the like.
- Compounds used as release agents for molds and candle making may also be considered, as well as, dry lubricants and fluorinated release agents.
- the detackifier comprises polytetrafluorethylene (PTFE), such as PTFE telomer (KRYTOX ® DF) compound, used in the PTFE release agent dry lubricant MS-122DF, marketed by Miller-Stephenson (Danbury, CT) as a spray product.
- PTFE particles may be applied by spray to one side of the substrate prior to winding of the pre-moistened wipes.
- a detackifying agent is applied to only one surface of the substrate prior to winding into a roll.
- the wetting composition desirably contains less than about 25 weight percent of detackifying agents based on the total weight of the wetting composition.
- the wetting composition contains from about 0.01 weight percent to about 10 weight percent of detackifying agents, more specifically about 5% or less. Even more specifically, the wetting composition contains from about 0.05 weight percent to about 2 weight percent of detackifying agents.
- Starch may be applied by adding the starch to a suspension of laponite to improve the dispersion of the starch within the wetting composition.
- microparticulates The wetting composition of the present invention may be further modified by the addition of solid particulates or microparticulates.
- Suitable particulates include, but are not limited to, mica, silica, alumina, calcium carbonate, kaolin, talc, and zeolites.
- the particulates may be treated with stearic acid or other additives to enhance the attraction or bridging of the particulates to the binder system, if desired.
- two-component microparticulate systems commonly used as retention aids in the papermaking industry, may also be used.
- Such two-component microparticulate systems generally comprise a colloidal particle phase, such as silica particles, and a water-soluble cationic polymer for bridging the particles to the fibers of the web to be formed.
- the presence of particulates in the wetting composition can serve one or more useful functions, such as (1) increasing the opacity of the pre-moistened wipes; (2) modifying the rheology or reducing the tackiness of the pre-moistened wipe; (3) improving the tactile properties of the wipe; or (4) delivering desired agents to the skin via a particulate carrier, such as a porous carrier or a microcapsule.
- the wetting composition contains less than about 25 weight percent of particulate based on the total weight of the wetting composition. More specifically, the wetting composition may contain from about 0.05 weight percent to about 10 weight percent of microparticulate. Even more specifically, the wetting composition may contain from about 0.1 weight percent to about 5 weight percent of microparticulate.
- Microcapsules and other delivery vehicles may also be used in the wetting composition of the present invention to provide skin-care agents; medications; comfort promoting agents, such as eucalyptus; perfumes; skin care agents; odor control additives; vitamins; powders; and other additives to the skin of the user.
- the wetting composition may contain up to about 25 weight percent of microcapsules or other delivery vehicles based on the total weight of the wetting composition. More specifically, the wetting composition may contain from about 0.05 weight percent to about 10 weight percent of microcapsules or other delivery vehicles. Even more specifically, the wetting composition may contain from about 0.2 weight percent to about 5.0 weight percent of microcapsules or other delivery vehicles.
- Microcapsules and other delivery vehicles are well known in the art.
- POLY-PORE ® E200 Chemical Corp., Arlington
- IL is a delivery agent comprising soft, hollow spheres that can contain an additive at over 10 times the weight of the delivery vehicle.
- additives reported to have been used with POLY-PORE ® E200 include, but are not limited to, benzoyl peroxide, salicylic acid, retinol, retinyl palmitate, octyl methoxycinnamate, tocopherol, silicone compounds (DC
- the wetting composition of the present invention may also contain preservatives and/or anti-microbial agents.
- preservatives and/or anti-microbial agents such as Mackstat H 66 (available from Mclntyre Group, Chicago, IL), have been found to give excellent results in preventing bacteria and mold growth.
- preservatives and anti-microbial agents include, but are not limited to DJMDM hydantoin (e.g., Glydant PlusTM, Lonza, Inc., Fair Lawn, NJ), iodopropynyl butylcarbamate, Kathon (Rohm and Hass, Philadelphia, PA), methylparaben, propylparaben, 2-bromo-2- nitropropane-l,3-diol, benzoic acid, and the like.
- the wetting composition contains less than about 2 weight percent on an active basis of preservatives and/or anti-microbial agents based on the total weight of the wetting composition.
- the wetting composition contains from about 0.01 weight percent to about 1 weight percent of preservatives and/or anti-microbial agents. Even more desirably, the wetting composition contains from about 0.01 weight percent to about 0.5 weight percent of preservatives and/or anti-microbial agents.
- Suitable non-ionic surfactants include, but are not limited to, the condensation products of ethylene oxide with a hydrophobic (oleophilic) polyoxyalkylene base formed by the condensation of propylene oxide with propylene glycol.
- the hydrophobic portion of these compounds desirably has a molecular weight sufficiently high so as to render it water-insoluble.
- the addition of polyoxyethylene moieties to this hydrophobic portion increases the water- solubility of the molecule as a whole, and the liquid character of the product is retained up to the point where the polyoxyethylene content is about 50% of the total weight of the condensation product.
- Nonionic surfactants include, but are not limited to, the condensation products of C 8 -C 22 alkyl alcohols with 2-50 moles of ethylene oxide per mole of alcohol.
- Examples of compounds of this type include the condensation products of C n -C 15 secondary alkyl alcohols with 3-
- non-ionic surface active agents include, but are not limited to, alkyl polyglycosides (APG), derived as a condensation product of dextrose (D-glucose) and a straight or branched chain alcohol.
- APG alkyl polyglycosides
- D-glucose dextrose
- a straight or branched chain alcohol derived as a condensation product of dextrose (D-glucose) and a straight or branched chain alcohol.
- the glycoside portion of the surfactant provides a hydrophile having high hydroxyl density, which enhances water solubility. Additionally, the inherent stability of the acetal linkage of the glycoside provides chemical stability in alkaline systems.
- Silicones are another class of wetting agents available in pure form, or as microemulsions, macroemulsions, and the like.
- One exemplary non-ionic surfactant group is the silicone-glycol copolymers. These surfactants are prepared by adding poly(lower)alkylenoxy chains to the free hydroxyl groups of dimethylpolysiloxanols and are available from the Dow
- Anionic surfactants may also be used in the wetting compositions of the present invention.
- Anionic surfactants are useful due to their high detergency include anionic detergent salts having alkyl substituents of 8 to 22 carbon atoms such as the water-soluble higher fatty acid alkali metal soaps, e.g., sodium myristate and sodium palmitate.
- a preferred class of anionic surfactants encompasses the water-soluble sulfated and sulfonated anionic alkali metal and alkaline earth metal detergent salts containing a hydrophobic higher alkyl moiety (typically containing from about 8 to 22 carbon atoms) such as salts of higher alkyl mono or polynuclear aryl sulfonates having from about 1 to 16 carbon atoms in the alkyl group, with examples available as the Bio-Soft series, i.e. Bio-Soft D-40 (Stepan Chemical Co.).
- anionic surfactants include, but are not limited to, the alkali metal salts of alkyl naphthalene sulfonic acids (methyl naphthalene sodium sulfonate, Petro AA, Petrochemical Corporation); sulfated higher fatty acid monoglycerides such as the sodium salt of the sulfated monoglyceride of cocoa oil fatty acids and the potassium salt of the sulfated monoglyceride of tallow fatty acids; alkali metal salts of sulfated fatty alcohols containing from about 10 to 18 carbon atoms (e.g., sodium lauryl sulfate and sodium stearyl sulfate); sodium C 14 -C 16 -alphaolefin sulfonates such as the Bio-Terge series (Stepan Chemical Co.); alkali metal salts of sulfated ethyleneoxy fatty alcohols (the sodium or ammonium sulfates of the condensation products of about 3
- the wetting composition may further comprise an aqueous microemulsion of silicone particles.
- an aqueous microemulsion of silicone particles for example, U.S. Pat. No. 6,037,407, "Process for the Preparation of Aqueous Emulsions of Silicone Oils and/or
- the wetting composition contains less than about 5 weight percent of a microemulsion of silicone particles based on the total weight of the wetting composition. More desirably, the wetting composition contains from about 0.02 weight percent to about 3 weight percent of a microemulsion of silicone particles. Even more desirably, the wetting composition contains from about 0.02 weight percent to about 0.5 weight percent of a microemulsion of silicone particles.
- the wetting composition of the present invention may also contain one or more emollients.
- Suitable emollients include, but are not limited to, PEG 75 lanolin, methyl gluceth 20 benzoate, C 12 -C 15 alkyl benzoate, ethoxylated cetyl stearyl alcohol, products marketed as Lambent wax WS - L, Lambent WD - F, Cetiol HE (Henkel Corp.), Glucam P20 (Amerchol), Polyox WSR N-10 (Union Carbide), Polyox WSR N-3000 (Union Carbide), Luviquat (BASF), Finsolv SLB 101 (Finetex Corp.), mink oil, allantoin, stearyl alcohol, Estol 1517 (Unichema), and Finsolv SLB 201 (Finetex Corp.).
- An emollient can also be applied to a surface of the article prior to or after wetting with the wetting composition.
- Such an emollient may be insoluble in the wetting composition and can be immobile except when exposed to a force.
- a petrolatum-based emollient can be applied to one surface in a pattern, after which the other surface is wetted to saturate the wipe.
- Such a product could provide a cleaning surface and an opposing skin treatment surface.
- the emollient composition in such products and other products of the present invention can comprise a plastic or fluid emollient such as one or more liquid hydrocarbons (e.g., petrolatum), mineral oil and the like, vegetable and animal fats (e.g., lanolin, phospholipids and their derivatives) and/or a silicone materials such as one or more alkyl substituted polysiloxane polymers, including the polysiloxane emollients disclosed in U.S. Pat. No. 5,891,126, issued Apr. 6, 1999 to Osborn, III et al.
- a hydrophilic surfactant may be combined with a plastic emollient to improve wettability of the coated surface.
- liquid hydrocarbon emollients and/or alkyl substituted polysiloxane polymers may be blended or combined with one or more fatty acid ester emollients derived from fatty acids or fatty alcohols.
- the emollient material is in the form of an emollient blend.
- the emollient blend comprises a combination of one or more liquid hydrocarbons (e.g., petrolatum), mineral oil and the like, vegetable and animal fats (e.g., lanolin, phospholipids and their derivatives), with a silicone material such as one or more alkyl substituted polysiloxane polymers.
- Water-soluble, self-emulsifying emollient oils which are useful in the present wetting compositions, include the polyoxyalkoxylated lanolins and the polyoxyalkoxylated fatty alcohols, as disclosed in U.S. Pat.
- the polyoxyalkoxy chains desirably will comprise mixed propylenoxy and ethyleneoxy units.
- the lanolin derivatives will typically comprise about 20-70 such lower-alkoxy units while the C 12 -C 20 - fatty alcohols will be derivatized with about 8-15 lower- alkyl units.
- One such useful lanolin derivative is Lanexol AWS (PPG-1)
- a useful poly(15-20)C 2 -C 3 - alkoxylate is PPG-5-Ceteth-20, known as Procetyl AWS (Croda, Inc.).
- the wetting composition contains less than about 25 weight percent of emollients based on the total weight of the wetting composition. More specifically, the wetting composition may comprise less than about 5 weight percent emollient, and most specifically less than about 2% emollient. More desirably, the wetting composition may contain from about 0.01 weight percent to about 8 weight percent of emollients. Even more desirably, the wetting composition may contain from about 0.2 weight percent to about 2 weight percent of emollients.
- the wetting composition and/or pre- moistened wipes of the present invention comprise an oil-in-water emulsion comprising an oil phase containing at least one emollient oil and at least one emollient wax stabilizer dispersed in an aqueous phase comprising at least one polyhydric alcohol emollient and at least one organic water-soluble detergent, as disclosed in U.S. Pat. No. 4,559,157, issued Dec. 17, 1985 to Smith et al., the entirety of which is herein incorporated by reference.
- Suitable surface feel modifiers include, but are not limited to, commercial debonders; and softeners, such as the softeners used in the art of tissue making including quaternary ammonium compounds with fatty acid side groups, silicones, waxes, and the like.
- Exemplary quaternary ammonium compounds with utility as softeners are disclosed in U.S. Pat. No. 3,554,862, issued to Hervey et al. on Jan. 12, 1971; U.S. Pat. No. 4,144,122, issued to Emanuelsson et al., Mar. 13, 1979, U.S. Pat. No. 5,573,637, issued to Ampulski et al. Nov.
- the wetting composition contains less than about 2 weight percent of surface feel modifiers based on the total weight of the wetting composition. More desirably, the wetting composition contains from about 0.01 weight percent to about 1 weight percent of surface feel modifiers. Even more desirably, the wetting composition contains from about 0.01 weight percent to about 0.05 weight percent of surface feel modifiers.
- the wetting composition of the present invention contains less than about 2 weight percent of fragrances based on the total weight of the wetting composition. More desirably, the wetting composition contains from about 0.01 weight percent to about 1 weight percent of fragrances. Even more desirably, the wetting composition contains from about 0.01 weight percent to about 0.05 weight percent of fragrances.
- fragrance solubilizers may be used in the wetting composition of the present invention.
- Suitable fragrance solubilizers include, but are not limited to, polysorbate 20, propylene glycol, ethanol, isopropanol, diethylene glycol monoethyl ether, dipropylene glycol, diethyl phthalate, triethyl citrate, Ameroxol OE-2 (Amerchol Corp.), Brij 78 and Brij 98 (ICI Surfactants), Arlasolve 200 (ICI Surfactants), Calfax 16L-35 (Pilot Chemical Co.), Capmul POE-S (Abitec Corp.), Finsolv SUBSTANTIAL (Finetex), and the like.
- the wetting composition contains less than about 2 weight percent of fragrance solubilizers based on the total weight of the wetting composition. More desirably, the wetting composition contains from about 0.01 weight percent to about 1 weight percent of fragrance solubilizers. Even more desirably, the wetting composition contains from about 0.01 weight percent to about 0.05 weight percent of fragrance solubilizers.
- Suitable opacifiers include, but are not limited to, titanium dioxide or other minerals or pigments, and synthetic opacifiers such as REACTOPAQUE ® particles (available from Sequa Chemicals, Inc., Chester,
- the wetting composition contains less than about 2 weight percent of opacifiers based on the total weight of the wetting composition. More desirably, the wetting composition contains from about 0.01 weight percent to about 1 weight percent of opacifiers. Even more desirably, the wetting composition contains from about 0.01 weight percent to about 0.05 weight percent of opacifiers.
- the wetting composition contains from about 0.01 weight percent to about 0.05 weight percent of a pH adjuster.
- a variety of wetting compositions, formed from one or more of the above-described components, may be used with the wet wipes of the present invention, in one embodiment, the wetting composition contains the following components, given in weight percent of the wetting composition, as shown in Table 2 below:
- the wetting composition comprises the following components, given in weight percent of the wetting composition, as shown in Table 3 below:
- tensile testing is performed according to the following protocol. Testing of dry product should be conducted under Tappi conditions (50% relative humidity, 73 °F) with a procedure similar to ASTM-1117-80, section 7. Tensile tests are performed with a constant crosshead speed tensile tester such as the Thwing Albert 1256- 100 tensile tester with an RSA-2 10-kg load cell. Specimens are cut to 3-inch widths and 6 inch lengths, and mounted between jaws with a 4-inch gauge length. The crosshead speed is 12 inches per minute. Peak load (for tensile strength) and elongation at peak load (for stretch) are measured. For cross direction (CD) tensile tests, the sample is cut in the cross direction. For machine direction (JMD) tensile tests, the sample is cut in the cross direction.
- CD cross direction
- JMD machine direction
- a container having dimensions of 200 mm by 120 mm and deep enough to hold 1000 ml is filled with 700 ml of the selected soak solution. No more than 108 square inches of sample are soaked in the 700 ml of soaking solution, depending on specimen size.
- the premoistened specimens, that have equilibrated overnight, are immersed in the soak solution and then allowed to soak undisturbed for a specified time period (typically 1 hour).
- CDWT the sample is immersed in deionized water for 1 hour and then tested.
- S-CDWT-M M indicating divalent metal ions
- MS-CD WT-M the sample is immersed in water containing 50 ppm of Ca ++ /Mg ++ in a 2:1 ratio, soaked for one hour and then tested. Testing done with other time increments or soaking solutions should be so indicated to prevent confusion with the S- CDWT or S-CDWT-M tests.
- wet wipes are produced using the above- described wetting composition in Table 3 and an air-laid fibrous material comprising 90 weight percent of softwood fibers and 10 weight percent of an ion-sensitive binder compositions comprising acrylic acid terpolymers or a copolymer substantially free of acrylic acid monomers, wherein the weight percentages are based on the total weight of the dry nonwoven fabric.
- the amount of wetting composition added to the nonwoven fabric, relative to the weight of the dry nonwoven fabric in these embodiments, is desirably about 180 percent to about 240 weight percent.
- the wet wipes possess an in-use wet tensile strength of at least 300 g/in, and a tensile strength of less than about 20 g/in after being soaked in water having a concentration of Ca 2+ and/or Mg 2+ ions of about 200 ppm for about one hour (S-CDWT-M).
- the wet wipes treated with the binder material of the present invention including the acrylic acid terpolymer possess an in-use wet tensile strength of at least 100 g/in for a 1 inch width sample in the cross machine direction when soaked with 10% to 400% by weight wet wipes solution containing more than 0.3% by weight monovalent ion (NaCl) concentration and a tensile strength of less than about 30 g/in after being soaked in deionized water for about one hour.
- the acrylic acid terpolymer possess an in-use wet tensile strength of at least 100 g/in for a 1 inch width sample in the cross machine direction when soaked with 10% to 400% by weight wet wipes solution containing more than 0.3% by weight monovalent ion (NaCl) concentration and a tensile strength of less than about 30 g/in after being soaked in deionized water for about one hour.
- the wet wipes treated with the binder material of the present invention including the acrylic acid terpolymer possess an in-use tensile strength of at least 200 g/in for a 1 inch width sample in the cross machine direction when soaked with 10% to
- wet wipes solution containing more than 0.3 % by weight monovalent ion (NaCl) concentration and a tensile strength of less than about 30 g/in after being soaked in deionized water for about one hour.
- NaCl monovalent ion
- the wet wipes treated with the binder material of the present invention including the sulfonate anion modified acrylic acid terpolymer desirably possess an in-use tensile strength of at least 200 g/in for a 1 inch width sample in the cross machine direction when soaked with 10% to 400% by weight wet wipes solution containing more than 1% by weight monovalent ion (NaCl) concentration and a tensile strength of less than about 30 g/in after being soaked in water having a concentration of Ca 2+ and/or Mg 2+ ions of about 50 ppm for about one hour.
- the binder material of the present invention including the sulfonate anion modified acrylic acid terpolymer desirably possess an in-use tensile strength of at least 200 g/in for a 1 inch width sample in the cross machine direction when soaked with 10% to 400% by weight wet wipes solution containing more than 1% by weight monovalent ion (NaCl) concentration and a
- the wet wipes treated with the binder material of the present invention including the sulfonate anion modified acrylic acid terpolymer possess an in- use tensile strength of at least 200 g/in for a 1 inch width sample in the cross machine direction when soaked with 10% to 400% by weight wet wipes solution containing more than 1% by weight monovalent ion (NaCl) concentration and a tensile strength of less than about 30 g/in after being soaked in water having a concentration of Ca 2+ and/or Mg 2+ ions of about 200 ppm for about one hour.
- the binder material of the present invention including the sulfonate anion modified acrylic acid terpolymer possess an in- use tensile strength of at least 200 g/in for a 1 inch width sample in the cross machine direction when soaked with 10% to 400% by weight wet wipes solution containing more than 1% by weight monovalent ion (NaCl) concentration and a tensile strength of less than about
- Products with high basis weights or wet strengths than flushable wet wipes may have relatively higher wet tensile strength.
- products such as pre-moistened towels or hard-surface cleaning wipes may have basis weights above 70 gsm, such as from 80 gsm to 150 gsm.
- Such products can have CDWT values of 500 g/in or greater, with S- CDWT values of about 150 g/in or less, more specifically about 100 g/in or less, and most specifically about 50 g/in or less, with similar ranges possible for S-CDWT-M.
- the product may not be fully wetted with water from the toilet bowl when it is flushed, or rather, there may not have been adequate time for the wetting composition of the product to have been replaced with the water of the toilet bowl when the momentary shear of flushing is applied.
- previous measurements of dispersibility could suggest that a product is dispersible when, in fact, it may be poorly suited for septic system.
- the second solution can be either deionized water for determination of the "Deionized Dispersibility” value or hard water (according to the S-CDWT-M test) for determination of the "Hard Water Dispersibility” value.
- the Dispersibility is defined as (1 minus the ratio of the cross-direction wet tensile strength in the second solution divided by the original cross-direction wet tensile strength) * 100%.
- the articles of the present invention can have a Deionized Dispersibility of 80% or greater, more specifically 90% or greater, specifically still 95% or greater, and can have a Deionized
- the articles of the present invention can have a Hard Water Dispersibility of 70% or greater, more specifically 80% or greater, specifically still about 90% or greater, and can have a Deionized Dispersibility of about 100%.
- the pre-moistened wipes of the present invention can be made in several ways.
- the ion-sensitive polymer composition is applied to a fibrous substrate as part of an aqueous solution or suspension, wherein subsequent drying is needed to remove the water and promote binding of the fibers.
- the binder migrates to the crossover points of the fibers and becomes activated as a binder in those regions, thus providing acceptable strength to the substrate.
- the following steps can be applied: 1. Providing an absorbent substrate that is not highly bonded
- the substrate may be dried such that the peak substrate temperature does not exceed 160° C, or 140° C, or 120° C, 110° C, or 100° C. In one embodiment, the substrate temperature does not exceed 80° C or 60° C.
- Application of the co-binder polymer can be done simultaneously with application of the binder composition by previously mixing the two, or the co-binder polymer can be added before or after the binder is applied.
- the other steps are desirably conducted in the order shown above.
- Application of the ion-sensitive polymer composition to the substrate can be by means of spray; by foam application; by immersion in a bath; by curtain coating; by coating and metering with a wire-wound rod; by passage of the substrate through a flooded nip; by contact with a pre-metered wetted roll coated with the binder solution; by pressing the substrate against a deformable carrier containing the ion-sensitive polymer composition such as a sponge or felt to effect transfer into the substrate; by printing such as gravure, inkjet, or flexographic printing; and any other means known in the art.
- foams In the use of foams to apply a binder or co-binder polymer, the mixture is frothed, typically with a foaming agent, and spread uniformly on the substrate, after which vacuum is applied to pull the froth through the substrate.
- Any known foam application method can be used, including that of U.S. Pat. No. 4,018,647, "Process for the Impregnation of a Wet Fiber Web with a Heat Sensitized Foamed Latex Binder," issued Apr. 19, 1977 to Wietsma, the entirety of which is herein incorporated by reference.
- Wietsma discloses a method wherein a foamed latex is heat-sensitized by the addition of a heat-sensitizer such as functional siloxane compounds including siloxane oxyalkylene block copolymers and organopolysiloxanes.
- a heat-sensitizer such as functional siloxane compounds including siloxane oxyalkylene block copolymers and organopolysiloxanes.
- Specific examples of applicable heat-sensitizers and their use thereof for the heat sensitization of latices are described in the U.S. Pat. Nos. 3,255,140; 3,255,141; 3,483,240 and 3,484,394, all of which are incorporated herein by reference.
- the use of a heat-sensitizer is said to result in a product having a very soft and textile-like hand compared to prior methods of applying foamed latex binders.
- the "thickness" of a web is measured with a 3- in acrylic plastic disk connected to the spindle of a Mitutoyo Digimatic Indicator (Mitutoyo Corporation, 31-19, Shiba 5-chome, Minato-ku, Tokyo
- Water-dispersible substrates of the present invention can have any suitable thickness, such as from about 0.1 mm to 5 mm.
- thicknesses can be in the range of 0.2 mm to about 1 mm, more specifically from about 0.3 mm to about 0.7 mm. Thickness can be controlled, for example, by the application of compaction rolls during or after web formation, by pressing after binder or wetting composition has been applied, or by controlling the tension of winding when forming a roll good.
- the use of the platen method to measure thickness gives an average thickness at the macroscopic level. Local thickness may vary, especially if the product has been embossed or has otherwise been given a three-dimensional texture.
- Acrylic acid (43.3 g, 0.60 mol), AMPS (10.7 g, 0.052 mol), butyl acrylate (35.2 g, 0.27 mol), and 2-cthylhexyl acrylate (20 g, 0.11 mol) were dissolved in 55 g of acetone/water (70/30) mixture.
- AIBN 2,2-azobisisobutyronitrile
- EJXAMPLE 2 Preparation of an Acrylic Acid Terpolymer
- An acrylic acid terpolymer was produced using the polymerization procedure outlined in Example 2 of U.S. Patent No. 5,312,883. The following monomers were used: acrylic acid (50 g, 0.69 mol), butyl acrylate (25 g, 0.20 mol), and 2-ethylhexyl acrylate (25 g, 0.14 mol). The polymer was neutralized with 0.1 mole sodium hydroxide.
- EJXAMPLE 4 Solubility of Ion-sensitive Polymer Formulation The sensitivity of the polymer formulations of Example 3 to divalent cations present in hard water were measured. Samples 1-10 of Example 3 are placed in a number of CaCl 2 solutions with a Ca 2+ concentration varying from ⁇ 10 to 200 ppm. Following soaking for an hour, the solubility of each polymer is noted. The solubility results are given below in Table 7.
- CDWT Cross machine Direction Wet Tensile strength.
- Tensile results for Examples 5 through 7 were obtained with an MTS tensile test device, the MTS 500/S unit (MTS Systems, Research Park, North Carolina) using the TestworksTM 3.10 for Windows software. Instead of the normal 3 -inch strip for testing, a 1-inch wide strip was used, cut to 6 inches in length. The gauge length between the rubber-coated jaws of the test device was 3 inches. Testing was operated at the specified crosshead speed of 12 in/min. The MTS device with the modified test procedure generally gives comparable results to the tensile test protocol previously described using 3- inch wide samples and the Thwing- Albert tester.
- EXAMPLE 8 The addition of the co-binder polymer to the ion-sensitive polymer reduces the shear viscosity of the polymer blend compared to the shear viscosity of the ion-sensitive polymer alone.
- Table 10 illustrates the effect of the addition of various co-binder polymers to an acrylic acid terpolymer (SSB-2) in accordance with the present invention.
- the web was then transferred to an oven wire and sprayed on the top side with ion-sensitive polymer formulation mixture on the exposed surface of the web, applying 10% ion-sensitive polymer formulation solids relative to the dry fiber mass of the web.
- the ion-sensitive polymer formulation mixture comprised water as the carrier with 12% binder solids, wherein the binder comprised 75% SSB-4 as the ion-sensitive polymer formulation and 25% Rhoplex ® JNW- 1715K latex emulsion (Rohm and Haas Corp.) as the co-binder polymer.
- Spray was applied with a series of Quick Neejet® nozzles, Nozzle No. 730077, manufactured by Spraying Systems Co. (Wheaton,
- a spray boom over the web provided 13 such nozzles on 5.5-inch centers with a tip-to-wire distance of 8 inches. This arrangement yields 100% overlap of spray cones for the ion-sensitive polymer formulation solution of this trial.
- the web then was transferred onto the underside of another oven wire, upon which it passed over another spray boom where more ion-sensitive polymer formulation solution was applied to the bottom side of the web to add another 10 weight percent solids relative to the dry fiber mass of the web.
- the web then passed through two successive dryer units where through-air drying with air at about 225° C. completed drying of the web.
- the pressure differential across the web was approximately 10 inches of water.
- the length of the three dryer sections, from first to third, respectively, was about 9, 10, and 6 feet.
- the thickness of the web after drying was 1.14 mm (this number, like other physical properties reported here, can vary depending on the fibers, basis weight, and so forth).
- MDDT machine direction dry tensile
- CDDT cross direction dry tensile
- EJXAMPLE 11 The sheet formed was identical to that of Example 10 except that the fibers in the airlaid web were 75% softwood kraft and 25% PET fibers. The thickness of the web after drying was 1.35 mm.
- the machine direction dry tensile (MDDT) strength of the web was measured at 3.87 kg/3 in.
- the cross direction dry tensile (CDDT) strength of the web was measured at 2.84 kg/3 in with a CD stretch of 11.31%.
- the cross direction wet tensile (CDWT) at 4% saline was measured at 0.82 kg/3 in. The Soaked CDWT strength was effectively 0, as was the Soaked CD Stretch.
- EJXAMPLE 12 Additional examples were conducted according to Example 10, with the exception that Rovene latex emulsion was used as the co-binder polymer and the basis weight and fiber composition varied as shown in Table 11. The Soaked CDWT results were all 0, indicating a complete loss of tensile strength. Other results are shown in Table 11, where Pulp/PET designates the ratio of softwood to synthetic fibers in the substrate, BW is the basis weight in gsm, TH is the thickness in mm, and S-CDWT-M is the one- hour soak CD wet tensile test for a sample soaked in water containing 200 ppm of Ca ++ /Mg H' in a 2: 1 ratio.
- EJXAMPLE 13 A pre-moistened wipe was made similar to that of Example 10, except that the co-binder polymer was a modified Elite® latex emulsion substantially free of crosslinking agents provided by National Starch.
- the basis weight of the web was 61.35, the thickness 1.21 mm, the MDDT 5.09 kg/3-in, the MD stretch 7.89%, the CDDT 3.90 kg/3-in, the CD stretch 9.50%, the CDWT in 4% saline 0.78 kg/3-in, the CDWT stretch 32.96%, and the residual strengths after one hour in both deionized water (S-CDWT) and hard water (S-CDWT-M) were 0 kg/3-in.
- S-CDWT deionized water
- S-CDWT-M hard water
- Pre-moistened wipes comprising the basesheet of Example 10 were prepared with a wetting composition comprising a slurry of particles.
- the particles were selected from the following products marketed by
- each particle type in Table 12 five 1000-gram batches of wetting composition were prepared with particle concentrations of 0.5%, 1%, 2%, 5%, and 10% by weight. Each batch was prepared by adding the appropriate amount of deionized, filtered water to a 1.15-liter beaker (for the 5 batches, the water amounts were, respectively, 926.3 g, 921.3 g, 911 g, 881 g, and 831 g).
- a 2.5-inch magnetic stirring rod stirred the contents of the jar while residing on a Thermolyne Cimarec 2 stirrer, with stirring speed set to maximum to provide a strong central vortex in each of 5 jars.
- the powder was added to the solution as it was being stirred and allowed to wet and become suspended over a period of about 30 minutes after addition of the powder. Some additional stirring by hand was needed for some of the powders to promote mixing.
- the pH was adjusted to 5.0 by adding malic acid, prepared at a strength of 50 weight percent in water. The pH was measured with a Cole Parmer Model 59002-00 pH/mN/° C. meter, with a Model 59002- 72 KK8 electrode.
- Each of the particle suspensions was then added to dried airlaid basesheets that had been treated with NaAMPS binder and a co-binder polymer according to Example 13.
- the add level was 200%, with application by spray on one side of the web.
- the moistened web was then sealed in plastic to sit overnight.
- Examination of the pre-moistened wipes treated with particulate suspensions as the wetting composition revealed that the particles generally remained in the wet wipe without the need for additional thickeners or polymeric retention aids. Squeezing the pre-moistened wipes, for example, yielded a mostly clear fluid apparently substantially devoid of particulates, in contrast to the milky suspensions used to wet the wipes. Generally, no visible residue appeared to be left of the hands after using the wipes. The particulates also generally improved opacity and appeared to slightly provide tactile property improvements (reduced tack, better rheological feel).
- the pre-moistened wipes comprising starch displayed reduced tackiness when handled with the human hand than did similar pre-moistened wipes without the starch.
- the wipes containing starch also felt smoother.
- EJXAMPLE 16 Additional pre-moistened wipes were prepared using the wetting compositions displayed in Table 14, one of which comprised starch as an additive and the other which comprised botanicals.
- the wetting composition was added to an airlaid fibrous substrate comprising an ion- sensitive binder.
- the wetting composition was added at add-on levels of 300 and 200 weight percent, respectively.
- binders were prepared according to the methods of Example 1, but scaled up as a batch process capable of producing several hundred gallons per batch.
- EJXAMPLE 18 Typical Wetting Solution A wetting composition was prepared by combining the following ingredients according to the specific weight percent: 92.88 weight percent deionized water, 4 weight percent NaCl, 1 weight percent Mackstat H-
- a Treated Substrate An airlaid substrate was made with the equipment described for Example 10. Basis weight was 65 gsm and the fibers were 100% Weyerhaeuser CF405 bleached softwood kraft pulp. The binder solution had 12.8 weight percent binder solids, 75 weight percent of which was SSB Code
- MDDT was 5.55 kg/3-in
- CCDT was 4.83 kg/3-in
- CDWT in 4% NaCl solution
- S-CDWT as well as S-CDWT-M (1 hour soak tests) gave 0 kg/3-in.
- Some of the dried web was slit to a 4.25-inch width and treated with wetting composition at 225% add-on, comprising 4% NaCl in deionized water without surfactant.
- the moistened web was perforated with a perf-knife operating with a depth of 0.070 inches to perforate every 4.5 inches.
- the perforated web was rolled into a coreless roll with 100 perforated sheets per roll (approximately 37.5 feet per roll) and placed in a white plastic cartridge for subsequent use in a dispenser for pre-moistened wipes.
- EJXAMPLE 21 A portion of the dried, treated web of Example 20 was wetted with the wetting composition of Example 18 and converted into perforate roll form for use as pre-moistened wipes to be dispensed from a bathroom dispenser.
- COMPARATIVE EJXAMPLE 22 A conventional, adhesively bonded airlaid substrate with a basis weight of 60.1 gsm was created using the methods described in Example 10.
- Dur-O-Set E-646 National Starch
- wood pulp CF405
- the substrate was wetted with a 4% NaCl solution and tested using the methods described.
- the binder was entirely the self-crosslinking Dur-O-Set E-646 compound; no salt-sensitive binder was applied.
- the binder solids mass was 17% of the substrate mass. Dry thickness of the web was 1.4 mm, and the CDWT value was 1.3 kg/3-in, while S-CDWT was 1.2 kg and S_CDWT-M was 1.15 kg, indicating that the web maintained nearly all of its strength after soaking, and suggesting that the crosslinked latex provided the majority of the tensile strength of the web and that the latex bonds did not weaken substantially in water.
- EJXAMPLE 23 A variety of binder/co-binder combinations were prepared, as described below, using the salt-sensitive binders of Table 15 and co-binders as shown in Table 16 which are not self-crosslinkable. Table 16. Latex co-binders that are not self-crosslinkable.
- airlaid substrates were made from bleached kraft fibers.
- the substrate was wetted with a 4% NaCl solution and tested using the methods described. All subsfrates were comprised of wood pulp (CF405) and binder. Results are shown in Table 17, where the binder mixture consistently comprised 75% of a salt-sensitive binder selected from Table 15 and 25% of a co-binder selected from Table 16.
- the binder/co-binder column refers to the binder and co-binders listed in Table 15 and 16, respectively. For example, "A/1" refers to a mixture of SSB Code A in Table 15 and co-binder 1 of Table 16.
- the comparative Example 22 lost less than 15% of its strength after soaking for 1 hour in either deionized water or 200 ppm divalent ion solution. All of the subsfrates in Table 17 lost more tensile sfrength on soaking than the comparative Example 22.
- EJXAMPLE 24 Different co-binders from Table 16 were blended with the salt- sensitive binder Code F from Table 15. The binder blend was then applied using the methods described in Example 10 to create the airlaid substrates listed in Table 18. In each case, 20% binder solids were applied to the substrate in a blend of 75% SSB/25% co-binder
- EXAMPLE 25 Measurements were made of the peel force required to unroll the product from the outer layers of a coreless roll of pre-moistened wipes suitable for use as a moist toilet paper product.
- the product was made according to Example 10 with an add-on level of 200% wetting composition.
- the dried web was slit to a 4.25-inch width and treated with wetting composition at 200% add-on, comprising 4% NaCl in deionized water with surfactants, silicone, and lanolin as listed in Table 19 for wetting composition Q, R, and S.
- the moistened web was perforated with a perf-knife operating to perforate every 4.5 inches.
- the perforated web was rolled into a coreless roll with 100 perforated sheets per roll (approximately 37.5 feet per roll) and sealed in a plastic cartridge for subsequent use in a dispenser for pre- moistened wipes.
- the roll rested freely in a plastic tub with a rounded, ribbed bottom that held the roll in place with a minimum of friction when the roll was unwound by pulling vertically upwards on the tail end of the roll.
- Adjacent plies adhered to each other such that some force was required to separate the layers.
- the peel force needed was less than the weight of the roll and appeared to be substantially greater than the frictional resistance offered by the tub as the roll turned, evidenced in part by angle between the web and the roll at the point of separation. With no peel force, the angle between the web being pulled up and a line normal to the roll at the point of separation would be 90 degrees, but in unwinding the moist roll with the salt-sensitive binder, the angle was substantially less than 90 degrees, thus imparting peel force to separate the web.
- the peel force was measured with an MTS Sintech 1/G test machine with Test Works 3.10 software. All testing as done in a conditioned laboratory under Tappi Standard conditions. A 4.5-inch wide clamp with rubber surfaces gripped the tail of a roll, with the roll position directly underneath the clamp such the tail would remain vertical as it was unwound from the roll if there were no peel force causing the web to wrap a portion of the roll and deflect from the vertical.
- the clamp was attached to the crosshead, which pulled the tissue web upward at a speed of 100 cm/minute. Peel force was measured by a 50 N load cell. The average load to pull 18 sheets away from the roll was recorded by averaging two runs in which 4 sheets each were separated and two runs in which 5 sheets each were separated. Only the first 18 sheets from the roll were used in the measurement. The average peel force for two rolls per condition (for an overall average taken over a total of 36 sheets) is reported in Table 20 below.
- Peel forces for a roll having a width between 7 and 15 cm are desirably are less than 500 g, more specifically less than 300 g, more specifically less than about 200 g, more specifically still less than about 160 g, most specifically less than about 120 g, with an exemplary range of from about 50 g to about 350 g, or from about 80 g to about 200 g. More generally, the peel force per 4-inch width of a moist roll can be any of the aforementioned values of ranges.
- EJXAMPLE 26 Additional samples were prepared according to Example 24 above, except that 15 weight % of the fiber blend consisted of 6-mm, crimped PET fibers (KoSa). Different co-binders from Table 16 were blended with the salt-sensitive binder Code F from Table 15. The binder blend was then applied using the methods described in Example 10 to create the airlaid substrates whose properties are listed in Table 21. hi each case, 20% binder solids were applied to the substrate in a blend of 75% SSB/25% co-binder. The properties of these substrates were measured after wetting with a 4% NaCl solution. All three co-binders perform comparably. All of the substrates have lost their tensile strength in 200 ppm divalent cation solution independent of co-binder type. Compared to the parallel results in Example 24, incorporation of the synthetic fibers impart a slight to modest strength improvement (CDWT) and a modest increase in dry bulk.
- CDWT modest strength improvement
- Table 21 Data for substrates with PET fibers and various co-binders.
- Table 22 Data for substrates with PET fibers and various co-binders.
- EXAMPLE 28 The substrates shown in Table 23 were all made according to the methods of Example 10 and prepared according to the methods described in Example 23. All of the substrates in Table 23 were formed from airlaid pulp (CF405). All binder blends were 75% SSB and 25% co-binder. The dry thickness of the sheet was controlled by adjusting the level of web compaction by the two compaction rolls prior to the first spray application of binder. SSB Codes O and Q from Table 15 were used.
- Sheet dispersibility can be managed by choosing lower molecular weight SSBs in combination with synthetic fibers and dry web densification.
- EJXAMPLE 30 The substrates listed in Table 25 were prepared, wetted with 4% NaCl solution, and tested according to the methods described in Example 29. Each substrate was comprised of the fiber blend noted and 20% binder with the SSB / co-binder blend noted in Table 25.
- Dur-O-Set RB was the co- binder used in all of the samples listed in Table 25. All codes used 100% softwood fiber except the last one, Code 2813, which comprised 15% PET fiber (the 6 mm, crimped fiber obtained from KoSa). Basis weight was generally held constant to about 60 gsm.
- the thickness of the airlaid web was controlled by adjusting the level of web compaction by the two compaction rolls prior to the first spray application of binder.
- the dry CD stiffness of selected substrates in Table 25 were measured using a Handle-o-meter and reported as stiffness.
- EXAMPLE 31 The substrates listed in Table 26 were prepared according to the method described in Examples 10 and 23. Each substrate comprised pulp (CF405) and 20% binder. The binder had the SSB / co-binder blend given in Table 26. Dur-O-Set RB was the co-binder. The substrate was converted into roll form and wetted with solution Q of Table 19 (solution D). Measurements were made of the peel force required to unroll the product from the outer layers of the coreless roll of pre-moistened wipes according to the method described in Example 25. The results of these tests are recorded in Table 26 below.
- EJXAMPLE 33 Samples were made generally as in Example 10 using 75/25 blends of SSB binder (see Table 15) and co-binder (see Table 16) as noted in Table 28. All substrates contain 6 mm crimped, 2.4 dtex Lyocell (Accordis) as 15% of the fiber blend with 85% softwood pulp (CF405). All substrates are comprised of 19% binder and 81% of the binder blend. Table 28. Tensile results for a range of binders and basesheet properties.
- Reducing the salt sensitive binder's molecular weight can be used to make the substrate more dispersible as is shown by subsfrate AB/1.
- changing the salt sensitive binder's composition can be used to make the substrate more dispersible as demonstrated by L/l and E/2.
- fully dispersible blends can be made.
- by selecting a different co-binder chemistry to be more compatible with the salt sensitive binder fully dispersible binder blends can be made as demonstrated by substrates AB/2 and AB/1.
- EXAMPLE 34 A latex emulsion comprising about 6% JNMA crosslinker, AirFlex 105 (Air Products, Allentown, PA), was combined with SSB Code H of Table 15 at a ratio of 75 parts SSB to 25 parts latex solids and cast into 8 bars with dimensions 1 cm x 4 cm x 3 mm as described in Example 9. Four bars were prepared by drying in air at 60° C. overnight, while the other four bars were dried at 167°C for 3 hours. Two bars from each set were then each placed in 30 ml of 4% NaCl solution and allowed to sit for one hour, after which solubility was determined gravimetrically. Bars from both sets (the two drying conditions) were essentially completely insoluble in the saline solution.
- the remaining bars from each set were each placed in 30 ml of hard water containing 200 ppm calcium and magnesium ions at a 2:1 ratio at about 23° C. and allowed to sit for one hour.
- the two bars dried at 167° C. and placed in hard water were essentially completely insoluble (0% soluble).
- the two bars dried at 60° C. and placed in hard water were 54% and 53% soluble, respectively, which was unexpectedly low given that the latex should be substantially uncrosslinked for drying at this temperature.
- some coagulation occurred when the latex was mixed with the SSB, suggesting a possible compatibility problem between the two mixtures, and thus solubility may be impaired, or some coagulated particles may not have passed through the filter paper.
- J MA crosslinker in the Airflex latex may have promoted crosslinking or gelling of the blend. While it is believed that a more compatible latex emulsion would have yielded higher solubility, it is also believed that co-binders that are relatively low in crosslinking agents (e.g., less than 6%, specifically less than 2%, more specifically less than 1%, and most specifically less than 0.3% crosslinker on a solids mass basis) can be helpful in maintaining high solubility of the dried polymer blend.
- crosslinking agents e.g., less than 6%, specifically less than 2%, more specifically less than 1%, and most specifically less than 0.3% crosslinker on a solids mass basis
- Figure 1 shows the wet tensile results for treated airlaid basesheets, wherein the tests have been carried out in different saline solutions or hard water.
- the airlaid basesheets were prepared according to Example 10 and provided with 20% add-on of salt-sensitive binder compositions labeled as Code X, Code Y, and Code Z.
- Code X is a binder polymer comprising 60% acrylic acid, 10.5% 2-ethylhexyl acrylate, 24.5% butyl acrylate, and 5% NaAMPS, polymerized according to Example 1 with a molecular weight of 1.3 million, corresponding to Code B in Table 15.
- Code Y is similar but with a molecular weight of about 550,000, corresponding to Code D in Table 15.
- Code Z is similar but has 62% acrylic acid and 8.5% 2-ethylhexyl acrylate as monomers, with a molecular weight of about 1.2 million, corresponding to Code G in Table 15. All binders were blended with Dur-O-Set RB co-binder in a 75:25 ratio. The treated webs were dried, as in Example 10, and then wetted with either a 4% or 1.5% NaCl solution. Wet tensile testing was conducted according to the CDWT protocol with the exceptions described in
- Example 5 e.g., a 1-inch wide strip and a MTS tensile tester were used. Soaked CD tensile tests were conducted on samples prepared with the 4% solution. The four columns shown for each code (some of which are not visible due to zero values) correspond to the results from the four different tests. The first two columns are the CDWT values "as is" for the web in either the 4% or 1.5% NaCl solution. The third and fourth columns are the S-CDWT-M (hard water soak) results at 1 hour and 3 hours for each web that had been wetted with the 4% solution.
- Fig. 2 is a chart showing how wet tensile sfrength (reported as CDWT in grams per 2.54 cm over a range of soak times) can change over time as 68 gsm softwood airlaid webs comprising ion-sensitive binders are soaked in solutions comprising calcium ions.
- the moistened webs were prepared with 20% binder by weight comprising 85% Lion (Tokyo, Japan) SSB-3b acrylic-acid based terpolymer and 15% Dur-O-Set RB (National Starch) co- binder. After being dried, the webs were wetted with a solution containing
- Code 3300 (labeled as Code 3300) with a sulfonated salt-sensitive binder blended with Dur-O-Set JRB polymer in a 75/25 ratio.
- the data set labeled as Code 2102 refers to a 65-gsm web containing the sulfonated salt-sensitive binder, which corresponds to SSB Code H in Table 15. This web was wetted with the solution described in Table 4. Solution add-on was 225% based on the dry weight of the web.
- This binder formulation displayed a rapid drop in tensile strength - hence good triggerability - when immersed in hard water, even at a calcium ion concentration of 257 ppm.
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Priority Applications (6)
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MXPA02010427A MXPA02010427A (en) | 2000-05-04 | 2001-05-03 | Ion sensitive, water dispersible polymers, a method of making same and items using same. |
AU2001259442A AU2001259442A1 (en) | 2000-05-04 | 2001-05-03 | Ion-sensitive, water dispersible polymers |
CA002406631A CA2406631C (en) | 2000-05-04 | 2001-05-03 | Wetting composition having ion-sensitive, water dispersible polymers |
EP01932963A EP1278557B1 (en) | 2000-05-04 | 2001-05-03 | Ion-sensitive, water dispersible polymers |
DE60131959T DE60131959T2 (en) | 2000-05-04 | 2001-05-03 | ION-SENSITIVE WATER DISPERSIBLE POLYMERS |
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US09/564,939 US6444214B1 (en) | 2000-05-04 | 2000-05-04 | Ion-sensitive, water-dispersible polymers, a method of making same and items using same |
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WO2001082986A2 WO2001082986A2 (en) | 2001-11-08 |
WO2001082986A3 WO2001082986A3 (en) | 2002-05-23 |
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EP (2) | EP1886700A3 (en) |
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BR (1) | BR0110582B1 (en) |
CA (1) | CA2406631C (en) |
DE (1) | DE60131959T2 (en) |
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-
2000
- 2000-05-04 US US09/564,939 patent/US6444214B1/en not_active Expired - Fee Related
-
2001
- 2001-05-03 BR BRPI0110582-5B1A patent/BR0110582B1/en not_active IP Right Cessation
- 2001-05-03 MX MXPA02010427A patent/MXPA02010427A/en active IP Right Grant
- 2001-05-03 KR KR1020027014733A patent/KR100849312B1/en not_active IP Right Cessation
- 2001-05-03 EP EP07022936A patent/EP1886700A3/en not_active Withdrawn
- 2001-05-03 AU AU2001259442A patent/AU2001259442A1/en not_active Abandoned
- 2001-05-03 WO PCT/US2001/014339 patent/WO2001082986A2/en active IP Right Grant
- 2001-05-03 DE DE60131959T patent/DE60131959T2/en not_active Expired - Lifetime
- 2001-05-03 EP EP01932963A patent/EP1278557B1/en not_active Expired - Lifetime
- 2001-05-03 CA CA002406631A patent/CA2406631C/en not_active Expired - Fee Related
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2002
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BR0110582B1 (en) | 2013-12-24 |
CA2406631C (en) | 2009-10-27 |
CA2406631A1 (en) | 2001-11-08 |
US20020176877A1 (en) | 2002-11-28 |
KR100849312B1 (en) | 2008-07-29 |
EP1886700A3 (en) | 2008-08-27 |
WO2001082986A2 (en) | 2001-11-08 |
EP1886700A2 (en) | 2008-02-13 |
US6444214B1 (en) | 2002-09-03 |
DE60131959T2 (en) | 2008-12-11 |
BR0110582A (en) | 2004-08-10 |
DE60131959D1 (en) | 2008-01-31 |
EP1278557B1 (en) | 2007-12-19 |
MXPA02010427A (en) | 2004-09-06 |
KR20020093119A (en) | 2002-12-12 |
US6814974B2 (en) | 2004-11-09 |
EP1278557A2 (en) | 2003-01-29 |
AU2001259442A1 (en) | 2001-11-12 |
WO2001082986A3 (en) | 2002-05-23 |
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