MXPA00007311A - Wet-like articles comprising a multi-phase, multi-component emulsion and an activation web - Google Patents
Wet-like articles comprising a multi-phase, multi-component emulsion and an activation webInfo
- Publication number
- MXPA00007311A MXPA00007311A MXPA/A/2000/007311A MXPA00007311A MXPA00007311A MX PA00007311 A MXPA00007311 A MX PA00007311A MX PA00007311 A MXPA00007311 A MX PA00007311A MX PA00007311 A MXPA00007311 A MX PA00007311A
- Authority
- MX
- Mexico
- Prior art keywords
- emulsion
- activation
- phase
- article
- cleaning
- Prior art date
Links
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Abstract
Disclosed are disposable cleansing articles (1) which comprise a multi-phase, multi-component emulsion (5) and an activation web (2) that facilitates activation of the emulsion during use. In a preferred embodiment, the multi-phase emulsion is a high internal phase inverse emulsion having a continuous external lipid phase and a discontinuous internal polar phase. During use, the activation web facilitates breakage of the emulsion's external phase, thereby releasing the internal phase for its desired use. Because the internal liquid phase may account for up to about 97%of the emulsion, significant levels of fluid (e.g., water or a polar liquid) may be delivered from a"dry"wipe.
Description
WET ARTICLES THAT COMPRISE A MULTIPLE PHASE, A MULTI-COMPONENT EMULSION, AND A TISSUE ACTIVATOR
FIELD OF THE INVENTION The present invention relates to articles that are useful in a wide variety of cleaning applications. In particular, the invention relates to fabrics for wet cleaning, made of a textured carrier substrate, treated with a multi-component, multi-phase emulsion, which can be activated to release a liquid phase.
BACKGROUND OF THE INVENTION In the technique of personal cleaning and for domestic use, several approaches have been developed aimed at cleaning needs. These approaches can be broadly classified into two main categories: those that use a practically dry substrate and a separate cleaning agent, and those that use a combination of integrated substrate agent / cleaner.
The first approach is usually one in which the user uses a dry substrate of the choice for him or her that has the desired absorption and texture properties. Commonly used substrates include disposable and reusable paper towels, cloths of natural and / or synthetic origin, and the like. The user then applies an emulsion of the desired composition to either the target surface and / or the dry substrate and then applies the substrate to the target surface for the rubbing or cleaning activity. 'While this approach has been used for many years, it requires the user to keep supplies separate from substrates and emulsions. In addition, it is often not convenient to transport the emulsion to remote locations in the types of containers normally used. Additionally, it is a matter of trial and error to determine the amount of effective emulsion suitable to apply. In an effort directed to these consumer needs, in more recent times products have been developed with integrated substrate / cleaning agent where the substrate is packaged to be used with the desired amount of the emulsion already applied. An example of a product of this kind is the pre-packaged, pre-moistened towel often available at the nearest store or shop to clean hands before or after eating. Another example is pre-moistened "baby fabrics" frequently used for child care activities. While these products have enjoyed a considerable degree of commercial success, they require a certain degree of packaging to avoid evaporation, contamination, or degradation of the emulsion before being used. Furthermore, depending on the desired context, it is a disadvantage to eliminate the packaging and in the case of packaging multiple products, separate the wet substrates for individual use. More recently, products have been developed with integrated substrate / cleaning agent that address what is related to the conservation of a "wet" or activated implement in a usable condition. These articles use a textured carrier substrate treated with a multi-phase emulsion having a dispersed polar phase and a continuous lipid phase. These articles have several significant advantages over previous cleaning products, especially when they are in the form of wet cleaning fabrics. These items release significant amounts of the internal polar phase (eg, water) during use for effective cleaning. The continuous lipid phase of the emulsion is sufficiently weak to easily break through low shear contact (e.g., during rubbing of the skin) to easily release this internal phase, although sufficiently firm to prevent premature release of the internal phase during the rigors of processing. The continuous lipid phase of these articles is also sufficiently stable during storage to avoid significant evaporation of the internal polar phase. These articles can be used in many applications that require the release of a polar or liquid internal phase such as, for example, water, as well as assets that are dispersible in these polar materials. These applications include the cleaning of hard surface floors, contractors, sinks, bath tubs, toilets and the like, as well as the release of antimicrobial or pharmaceutical active ingredients that are soluble or dispersible in polar liquids. These articles can also perform multiple functions. For example, the emulsion applied to these articles can be formulated to provide cleaning and waxing benefits at the same time when they are used in articles such as, for example, furniture, shoes, automobiles and the like. While the articles of this variety have been successful in use, it is often difficult to activate either a sufficient amount of emulsion to meet the need of the end user or to efficiently release the capacity of the emulsion loaded in the article. As a consequence, it is often necessary to compensate by increasing the emulsion charge of the carrier material to ensure an adequate amount of internal polar phase that will be available for use. Accordingly, it would be desirable to provide an article for cleaning with integrated / active substrate agent that provides efficient utilization of the active agents. In addition, it would be desirable to provide an article for cleaning that provides an activation facility for releasing and depositing the active agent.
BRIEF DESCRIPTION OF THE INVENTION The present invention relates to cleaning articles that are supplied in a dry state but are capable of releasing a significant amount of liquid upon activation by the end user. In particular, the invention relates to an article for cleaning, comprising: (a) an activation pattern having a first surface and having one or more regions exhibiting a textured, three-dimensional surface topography and a second surface, the plot of activation has a ratio of wet gauge to dry bore (resilience ratio) of at least about 0.9; and (b) a multi-component, multi-phase emulsion that is in direct contact with the first surface of the activation screen. During use, the textured activation pattern facilitates the breaking of the continuous external phase of the emulsion and liberates the internal polar phase for the desired use.
BRIEF DESCRIPTION OF THE DRAWINGS While the specification concludes with the claims that are particularly directed and clearly claim the present invention, it is believed that the present invention will be better understood from the following description of the preferred embodiments, taken in conjunction with the accompanying drawings, in which like reference numbers identify identical elements and wherein: Figure 1 is an elevated sectional view of a preferred embodiment of an article for cleaning according to the present invention; Figure 2 is a perspective illustration, partially segmented, enlarged of a macroscopically-expanded, three-dimensional formed film web suitable for use as an activation web in an article for cleaning according to the present invention; Figure 3 is an elevated sectional view of another embodiment of an article for cleaning according to the present invention; Figure 4A is an illustration of a plan view of a mode of an activation pattern useful in the articles of the present invention, the
activation pattern comprises a continuous network of a polymeric material printed on a substrate; Figure 4B is a cross-sectional illustration of the activation frame shown in Figure 4A, taken along the direction indicated by line 4-4. The figure illustrates the textured, three-dimensional surface resulting from the printing of the polymer on the substrate to form the activation pattern; Figure 5 is a schematic representation illustrating a spray system suitable for use in the application of a high internal phase reverse emulsion to a carrier substrate; and Figure 6 is a schematic representation
illustrating a rotogravure coating system suitable for use in the application of a high internal phase reverse emulsion to a carrier substrate.
DETAILED DESCRIPTION OF THE INVENTION A. Definitions In the sense in which it is used herein, the term "comprising" means that the various components, ingredients, or steps, are
can be used together in the practice of the present invention. Accordingly, the term "comprising" embraces the more restrictive terms "consisting essentially of" and "consisting of". As used herein, the terms "detergent", "detersive surfactant" and "detergent surfactant" are used interchangeably, and refer to any substance that reduces the surface tension of water, specifically a surfactant that it concentrates in the interfaces oil in water, exerts an emulsifying action and in this way helps in the elimination of dirt. In the sense in which it is used in the present, the term "polar" refers to a molecule that possesses a dipole moment, that is, a molecule in which the positive and negative electric charges are permanently separated, while they oppose to a non-polar molecule in which the charges coincide. A "polar liquid" is a liquid comprising one or more polar constituents. In the sense in which it is used herein, the terms "activated" and "activation" refer to the breaking of the continuous external phase of the emulsion and the release of the internal phase thereof.
All percentages, ratios and proportions used herein are by weight unless otherwise specified.
B. Structure of the Representative Article Figure 1 represents a currently preferred embodiment of an article for cleaning according to the present invention. More particularly, Figure 1 depicts an article for cleaning 1 including an activation frame 2, a first sub-frame 3 peripherally linked with the activation frame 2 to define an internal zone 4, and a multi-component, multi-component emulsion 5. phase, which occupies at least partially the inner zone 4. A second secondary frame 3 'forms the other surface of the fabric in its final form. The activation frame 2 and the first secondary frame 3 are preferably substantially unbonded inward of their peripheries in order to allow some degree of lateral relative movement between them in response to externally applied shear forces, as will be discussed in FIG. more detail later.
As used herein, the term "activation screen" refers to a web-like material frame that is structured to provide an activation property when used in direct contact with a multi-component emulsion. , multi-phase, during use. By activation property, it is meant that the activation frame works to break the external phase of the emulsion and release the internal liquid phase. This allows to transfer at least one of the emulsion phases (preferably the internal liquid phase) from the article. "Secondary frames", on the other hand, refers to the present frames that form other surfaces or elements of the articles for cleaning in accordance
• with the present invention and lack either (i) direct contact with the multi-component emulsion, multi-phase during use, (ii) activation properties, or both. The multi-component, multi-phase emulsion 5 can be provided in the form of a uniformly distributed layer or can be applied by regions or by zones as depicted in Figure 1. Multi-component, multi-phase emulsion can be applied as a unitary deposition or it can be applied progressively as multiple thin layers or it can even be applied by regions sequentially more than simultaneously. Preferably, the emulsion is applied to at least one activation web or to the secondary web before the web is assembled, although other means for introducing the emulsion into the article that are within the scope of the present invention may also be contemplated. . For purposes of analysis, in particular with respect to the methods and apparatuses for manufacturing the articles according to the present invention, the web to which the emulsion is initially applied can be referred to as a "carrier web". The individual elements or components of the cleaning article depicted in Figure 1 will be described in greater detail in the subsequent sections.
C. Multiphase, Multi-Component Emulsion Composition The articles of the present invention comprise an emulsion that is applied to a carrier substrate. This emulsion comprises: (1) a lipid phase; (2) an internal polar phase dispersed in the lipid phase; and (3) an emulsifier which forms the emulsion when the lipid phase is liquid. In particular, the emulsion comprises: (1) from about 2 to about 60% of a solidified, continuous lipid phase, comprising a waxy lipid material having a melting point of about 30 ° C or greater; (2) from about 39 to about 97% of an internal polar phase dispersed in the lipid phase; and (3) an effective amount of an emulsifier capable of forming the emulsion when the lipid phase is in a fluid state. Because the internal phase contains a high level of one or more polar liquids, this emulsion is usually referred to as a "high internal phase reverse emulsion". The continuous lipid phase is very low at ambient temperatures such that the emulsion ruptures and releases the internal polar phase when subjected to low shear during use, eg, wiping of the skin or other surface. The continuous lipid phase must also be stable at ambient temperatures in such a way as to stabilize the emulsion structure of the present invention. In particular, this continuous lipid phase prevents the dispersed internal polar phase from being released prematurely from the article before being used, such as, for example, during the rigors of processing. The continuous lipid phase may comprise from about 2 to about 60% of the emulsion of the present invention. Preferably, this continuous lipid phase will comprise from about 5 to about 30% of the emulsion. More preferably, this lipid phase will comprise from about 6 to about 15% of the emulsion. The main constituent of this continuous lipid phase is a waxy lipid material. This lipid material is characterized by a melting point of about 30 ° C or higher, that is, it is solid at ambient temperatures. Preferably, this lipid material has a melting point of about 40 ° C or greater, more preferably about 50 ° C or higher. Typically, this lipid material has a melting point in the range of about 40 ° to about 80 ° C, more typically in the range of about 50 ° to about 80 ° C, still more typically in the range of about 60 ° to about 70 ° C. The lipid material is solid at ambient temperatures and fluid or plastic at those temperatures in which the high internal phase reverse emulsion is applied to the carrier substrate. It is also desirable that the lipid material be stable (ie, minimum coalescence of the emulsion droplets), for extended periods of time at elevated temperatures (e.g., about 50 ° C or higher) that are normally encountered during storage and storage. distribution of the articles of the present invention. This lipid material also needs to be sufficiently weak at the shear conditions of use of the article in such a way that it ruptures and releases the dispersed internal polar phase. These lipid materials should also desirably provide a good skin feel when used in personal care products such as, for example, wet cleaning fabrics used in perianal cleaning. Suitable lipid materials for use in the high internal phase reverse emulsion of the present invention include natural and synthetic waxes, as well as other oil soluble materials having a waxy consistency. As used herein, the term "waxes" refers to mixtures or organic compounds which are generally insoluble in water and tend to exist as amorphous or crystalline solids at room temperatures (eg, at about ° C). Suitable waxes include various types of hydrocarbons as well as esters of certain fatty acids (eg, "saturated" triglycerides) and fatty alcohols.They can also be derived from natural sources (ie, animal, vegetable or mineral) or can be synthesized. Mixtures of these various waxes can also be used, some representative animal and vegetable waxes that can be used in the present invention include beeswax, carnauba, spermaceti, lanolin, shellac wax, candelilla and the like. Particularly preferred vegetables are beeswax, lanolin and candelilla Representative waxes from mineral sources that can be used in the present invention include petroleum-based waxes such as, for example, paraffin, petrolatum and microcrystalline wax, and fossil or terrestrial waxes such as, for example, white ceresin wax, yellow ceresin wax, white ozocerite wax, and the like. Particularly preferred mineral waxes are petrolatum, microcrystalline wax, yellow ceresin wax, and white ozocerite wax. Representative synthetic waxes that can be used in the present invention include ethylenic polymers such as, for example, polyethylene wax, chlorinated naphthalenes such as, for example, "Halowax", hydrocarbon type waxes manufactured by the Fischer-Tropsch synthesis and the like. Particularly preferred synthetic waxes are polyethylene waxes. In addition to the waxy lipid material, the continuous lipid phase may include minor amounts of other lipophilic or lipid miscible materials. These other lipophilic / lipid miscible materials are usually included for the purpose of stabilizing the emulsion to minimize the loss of the polar internal phase or improve the aesthetic feel of the emulsion on the skin. Suitable materials of this type that may be present in the continuous lipid phase include hot melt adhesives such as, for example, Findley 193-336 resin, long chain alcohols such as, for example, cetyl alcohol, stearyl alcohol, and cetaryl alcohol water-insoluble soaps such as, for example, aluminum stearate, silicone polymers such as, for example, polydimethylsiloxanes, hydrophobically modified silicone polymers such as, for example, phenyl trimethicone and the like. Other suitable lipophilic / miscible lipid materials include polyol polyesters. By "polyol polyester" is meant a polyol having at least 4 ester groups. By "polyol" is meant a polyhydric alcohol containing at least 4, preferably from 4 to 12 and more preferably from 6 to 8 hydroxyl groups. The polyols include monosaccharides, disaccharides and trisaccharides, sugar alcohols and other sugar derivatives (e.g., alkyl glycosides), polyglycerols (e.g., diglycerol and triglycerol), pentaerythritol, and polyvinyl alcohols. Preferred polyols include xylose, arabinose, ribose, xylitol, erythritol, glucose, methyl glucoside, mannose, galactose, fructose, sorbitol, maltose, lactose, sucrose, raffinose and maltotriose. Sucrose is an especially preferred polyol. With respect to the polyol polyesters useful herein, it is not necessary that all of the hydroxyl groups of the polyol be esterified, however, the disaccharide polyesters should not have more than 3, and more preferably more than 2, unesterified hydroxyl groups. Typically, virtually all hydroxyl groups (eg, at least about 85%) of the polyol are esterified. In the case of the sucrose polyesters, usually from about 7 to about 8 of the hydroxyl groups of the polyol are esterified. By "liquid polyester polyol" is meant a polyester polyol derived from the groups described above having a liquid consistency or less than about 37 ° C. By "solid polyester polyol" is meant a polyester polyol derived from the groups described above having a plastic or solid consistency at about 37 ° C or higher at that temperature. The liquid polyol polyesters and the solid polyol polyesters can be used successfully as emollients and immobilizing agents, respectively, in the emulsions of the present invention. In some cases, solid polyol polyesters may also provide some emolliency functionality. Typically, the main component of the high internal phase reverse emulsions of the present invention is the dispersed internal polar phase. This internal phase can provide several different benefits when it is released. In preferred embodiments, the polar phase will contain a significant percentage of water. For example, in fabrics for wet cleaning for perianal cleaning, the internal polar phase will comprise a significant level of water; This internal aqueous phase released is what provides the main cleaning action for these fabrics. In these preferred embodiments, the polar phase will contain a significant percentage of water, preferably at least about 60% by weight of the internal polar phase, more preferably at least 75% by weight and still more preferably at least about 85% by weight. weight . The internal polar phase may comprise from about 39 to about 97% of the emulsion of the present invention. Preferably, this internal polar phase will comprise from about 67 to about 92% of the emulsion. More preferably, this polar phase will comprise from about 82 to about 91% of the emulsion. In preferred embodiments, where the internal phase comprises significant amounts of water, this internal polar phase may comprise other water soluble or dispersible materials that do not adversely affect the stability of the high internal phase reverse emulsion. A material that is typically included in the internal aqueous phase is a water-soluble electrolyte. The dissolved electrolyte minimizes the tendency of the materials present in the lipid phase to also dissolve in the aqueous phase. Any electrolyte capable of imparting ionic resistance to the aqueous phase can be used. Suitable electrolytes include water-soluble mono-, di-, or trivalent inorganic salts such as, for example, water-soluble halides, for example, chlorides, nitrates, and sulfates of alkali metals and alkaline earth metals. Examples of these electrolytes include sodium chloride, calcium chloride, sodium sulfate, magnesium sulfate and sodium bicarbonate. The electrolyte will typically be included in a concentration in the range of about 1 to about 20% of the aqueous phase. Other soluble or water dispersible materials that may be present in the internal aqueous phase include thickeners and viscosity modifiers. Suitable thickeners and viscosity modifiers include water-soluble polyacrylic resins and hydrophobically modified polyacrylic resins such as, for example, Carbopol and Pemulen, starches such as, for example, corn starch, potato starch, tapioca, gums such as, for example, gum guar, gum arabic, cellulose esters such as, for example, hydroxypropyl cellulose, hydroxyethyl cellulose, carboxymethyl cellulose, and the like. These thickeners and viscosity modifiers will typically be included in a concentration in the range of about 0.05 to about 0.5% of the aqueous phase. Other soluble or water dispersible materials that may be present in the internal aqueous phase include polycationic polymers to provide spherical stabilization at the water-lipid interface and non-ionic polymers that also stabilize the water emulsion in lipid. Polycationic polymers include Reten 201, Kymene® 557H and Acco 711. Suitable nonionic polymers include polyethylene glycols (PEG) such as, for example, Carbowax. These polycationic and nonionic polymers will typically be included in a concentration in the range of from about 0.1 to about 1.0% of the aqueous phase. In addition to containing water or alternatively, the internal polar phase may comprise polar materials, among which are included solvents such as, for example, ethanol, isopropanol, butanol and hexanol; glycols or substituted glycols such as, for example, propylene glycol, butylene glycol, 2,2,4-tr imet ilpentan-1,3-diol or hexylene glycol; polyglycols such as, for example, diethylene glycol or triethylene glycol; glycol ethers such as, for example, short chain derivatives (for example, Ci-Ce) of oxyethylene glycol and oxypropylene glycol, such as mono- and di-ethylene glycol n-hexyl ether, mono-, di- and tri-propylene glycol n-butyl ether; and the similar. Also, solvents such as tetrahydrofuran, dimethyl sulfoxide, acetone and the like can be included in the internal polar phase. Another key component of the high internal phase reverse emulsion of the present invention is an emulsifier. In the emulsions of the present invention, the emulsifier is included in an effective amount. What constitutes an "effective amount" will depend on several of the factors including the respective amounts of the polar and internal polar phase components, the type of emulsifier used, the level of impurities present in the emulsifier, and the like. Typically, the emulsifier comprises from about 1 to about 10% of the emulsion. Preferably, this emulsifier will comprise from about 3 to about 6% of the emulsion. More preferably, this emulsifier will comprise from about 4 to about 5% of the emulsion. While the single "emulsifier" is used to describe this component, more than one emulsifier can be used when the emulsion is being formed. Indeed, as discussed below, it may be desirable to use both a primary emulsifier and a secondary emulsifier when certain materials are used. Although it is not intended to limit the scope of the invention, when two emulsifiers are used, it is preferred when the primary emulsifier comprises from about 1 to about 7%, more preferably from about 2 to about 5%, still more preferably about 2. to approximately 4% of the emulsion; and the secondary emulsifier comprises from about 0.5 to about 3%, more preferably from about 0.75 to about 2%, still more preferably from about 0.75 to about 1.5% by weight of the emulsion. This emulsifier needs to be practically soluble or miscible in lipids with the materials in the lipid phase, especially at temperatures at which the lipid material melts. A relatively low HLB value must also be obtained to facilitate the formation of the required inverse emulsion. Suitable emulsifiers for use in the present invention have HLB values typically in the range of about 2 to about 5 and may include mixtures of different emulsifiers. Preferably, these emulsifiers will have HLB values in the range of about 2.5 to about 3.5. Suitable emulsifiers for use in the present invention include polymeric silicone emulsifiers such as, for example, alkyl dimethicone copolyols (e.g., Dow Corning Q2-5200 laurylmethylol copolyol). These emulsifiers are described in detail in copending U.S. Patent Application No. 08 / 430,061, filed April 27, 1995 by L. Mackey (Case 5653), which is incorporated herein by reference. Other suitable emulsifiers are described in copending U.S. Patent Application No. 08 / 336,456, filed November 9, 1994 by L. Mackey et al. (Case 5478), which is incorporated herein by reference. Emulsifiers described herein include certain sorbitan esters, preferably sorbitan esters of saturated, unsaturated or branched chain Ci6-C22 fatty acids. Due to the manner in which they are typically manufactured, these sorbitan esters usually comprise mixtures of mono-, di-, tri-, etc. esteres. Representative examples of suitable sorbitan esters include sorbitan monooleate (e.g., SPAN® 80), sorbitan sesquioleate (e.g., Arlacel® 83), sorbitan thearate monoisoes (e.g., CRILL® 6 manufactured by Croda), stearates sorbitan (for example, SPAN® 60), triooleate (for example, SPAN® 85), sorbitan tristearate (for example, SPAN® 65) and sorbitan dipalmitates (for example, SPAN® 40). The laurylmethylone copolyol is a particularly preferred emulsifier for use in the present invention. Other emulsifiers described herein include certain glyceryl monoesters, preferably glyceryl monoesters of saturated, unsaturated or branched C16-C22 fatty acids such as, for example, glyceryl monostearate, glyceryl monopalmitate, and glyceryl monobehenate; certain fatty acid esters of sucrose, preferably sucrose esters of the saturated, unsaturated and branched C C2-C22 fatty acids such as, for example, sucrose trilaurate and sucrose tristearate (eg, Crodesta® FIO), and certain polyglycerol esters of saturated, unsaturated or branched C 16 -C 22 fatty acids such as, for example, diglycerol monooleate and tet raglycerol monooleate. In addition to these primary emulsifiers, co-emulsifiers can be used to provide stability of the water emulsion in additional lipid. Suitable coemulsifiers include phosphatidyl cholines and phosphatidyl choline containing compositions such as, for example, lecithins; C.sub.6 -C.sub.22 long chain fatty acid salts such as, for example, sodium stearate, long chain Ci.sub.6 -C.sub.2 dialiphatic quaternary ammonium salts, short chain C? -C dialiphatic salts such as dimethyl ammonium and dimethyl ammonium chloride. methylisulfate dimethyl ammonium; long chain dialkoyl (alkenoyl) -2-hydroxyethyl dialkyl quaternary ammonium salts of short chain C 1 -C 4 dialiphatic such as, for example, ditallow-2-hydroxyethyl dimethyl ammonium chloride, imidazolinium quaternary ammonium salts C? 6-C22 long chain dialiphatics such as for example, methyl-1-tallowamido-ethyl-2-tallow imidazolinium methylisulfate and methyl-1-oleyl amidoethyl-2-oleyl imidazolinium methylisulfate, dialiphatic quaternary ammonium salts C? -C4 of short chain, monoaliphatic benzyl of C? 6 Long chain C22 such as, for example, dimethyl stearyl benzyl ammonium chloride, and synthetic phospholipids such as for example, stearamidopropyl PG-diammonium chloride (Phospholipid PTS from Mona Industries) Interfacial tension modifiers may also be included such as, for example, cetyl and stearyl alcohol for final packaging at the water-lipid interface. Other emulsifiers useful in making the articles of the present invention include the high viscosity emulsifiers described in copending U.S. Patent Application Number 08 / 640,268, filed April 30, 1996 by L. Mackey and B. Hird. , which is incorporated herein by reference. These emulsifiers preferably have a viscosity at 55 ° C of at least about 500 centipoise. (Viscosity can be measured using a rotary disk viscometer of the Lab-Line Instruments Brookfield type.) This application describes the use of emulsifiers such as, for example, those designed by The Lubrizol Corporation (Wickliffe, OH) as OS-122102, OS -121863, OS-121864, OS-80541J and OS-80691J, which are reaction products of (i) a carboxylic acid substituted with hydrocarbyl or anhydride (preferably a succinic acid or anhydride substituted with polyisobutylene); and (ii) an amine or alcohol, to form an ester or amide product. The materials and methods for their manufacture are described in U.S. Patent No. 4,708,753, issued November 24, 1987 to Forsberg [see especially Column 3, lines 32-38; and Column 8, line 10, to Column 26, line 68], and United States Patent Number 4,844,756, issued July 4, 1989 to Forsberg, both are incorporated herein by reference. Other materials known to be useful in the present invention include hydrocarbon substituted succinic anhydrides such as, for example, those described in U.S. Patent 3,215,707, issued November 2, 1965 to Rense; U.S. Patent 3,231,587, issued January 25, 1996 to Rense; U.S. Patent Number 5,047,175, issued to Forsberg on September 10, 1991; and World Patent Publication Number O87 / 03613, published by Forsberg on June 18, 1987. These publications are all incorporated herein by reference. Still other useful materials such as the emulsifier, in particular as a co-emulsifier with a high viscosity primary emulsifier, are ABA block copolymers of 12-hydroxyacetic acid and polyethylene oxide. These materials are described in U.S. Patent 4,875,927, issued to T. Tadros on October 24, 1989, which is incorporated herein by reference. A representative material of this class useful as an emulsifier herein is available from Imperial Chemical Industries PLC as Arlacel P135. As indicated, while all of the materials described in the foregoing can be used as an individual emulsifier, it may be desirable to employ more than one emulsifier when the emulsion is being formed. In particular, when a high viscosity emulsifier is used, a certain "sticky" feeling may result when the treated article is subjected to shear stresses in use that break the emulsion. In this case, it may be desired to use a co-emulsifier of relatively low viscosity with the primary emulsifier, to allow the use of a lower amount of a main emulsifier, thereby decreasing stickiness. In one embodiment of the present invention, a primary emulsifier available from Lubrizol (ie, the reaction product of succinic acid substituted with polyisobutylene and an amine) and a secondary emulsifier which is an ABA block copolymer of polyhydric acid are used. 12-hydroxystearic and polyethylene oxide (for example, ICI's Arlacel P135) to provide an emulsion with beneficial water retention levels over time, as well as beneficial reduced tack (by reducing the level of primary emulsifier). The expert technician will recognize that. the different uses and desired final product designs will be dictated if multiple emulsifiers are adequate, and the appropriate relative amounts of each if appropriate. This determination will require only routine experimentation by the skilled artisan in view of the present disclosure. The high internal phase reverse emulsions of the present invention may also comprise other optional components typically present in emulsions containing moisture of this type. These optional components may be present in either the continuous lipid phase or the internal polar phase and include perfumes, antimicrobial (eg, antibacterial) actives, pharmaceutical actives, deodorants, opacifiers, astringents, skin conditioners, cosmetics, cleansers. , surface conditioners, insect repellents, pH regulators, and the like, as well as mixtures of these components. All of these materials are well known in the art as additives for these formulations and can be employed in suitable and effective amounts in the emulsions of the present invention. A particularly preferred optional component that is included in fabric emulsions for wet cleaning according to the present invention is glycerin as a skin conditioning agent. The emulsion component of the articles of the present invention is described and claimed herein in terms of components (i.e., lipid phase components, internal polar phase components, emulsifying components, etc.), and the corresponding amounts of these components, which are present after the formation of the emulsion. That is, when the stable emulsion is formed and applied to the carrier. It should be understood, however, that the description (components and amounts) of the emulsion also covers the emulsions formed by combining the described components and the levels described, with respect to the chemical identity of the components after emulsification and application to the emulsion. carrier.
D. Activation Frames In accordance with the present invention, the article for cleaning also comprises a sheet of material that forms an activation frame to assist in the release of a liquid from the multi-component, multi-phase emulsion when " is activated "by a user. • In order to "activate" the multi-component, multi-phase emulsion, it has been found that two physical properties in combination improve the effectiveness of these articles for cleaning by increasing the degree of breakdown of the continuous phase of the emulsion and increasing the release of the active portion of the emulsion from the interior of the article to the exterior surface where it can be used effectively for its intended function. One property that has been found to be important in the activation frames of the present invention is a textured surface on the side of a portion thereof, of the activation screen that comes into direct contact with the multi-component emulsion, multi-phase during use. By "textured" is meant that the surface of the frame has extensions beyond the two-dimensional plane defined by the macroscopic frame. In other words, the activation frame comprises a surface having three-dimensionality. Without attempting to be bound by a theory, the applicants assume that a surface provides a degree of abrasion to the surface of the weft to help provide a frictional activation property for the breaking of the continuous external lipid phase and to release the internal liquid phase. from the emulsion. Variant abrasion grades can be provided by properly selecting the activation weft material and the surface geometry. However, the preferential activation frame must allow a sufficiently relative lateral movement between the activation frame and the optional additional subjacent frame in order to provide a shearing action on the multi-phase emulsion to assist in the release of the internal liquid phase. Another property that has been found to be important in the activation frames of the present invention is resilience. Activation frames according to the present invention must exhibit a resilient property, at least for a period of time corresponding to the typical use period for the article, which makes it possible for the frames to retain their textured or three-dimensional character during the activation of the emulsion.
For the purposes of the present invention, the resilience of the activation web is described in terms of its wet gauge for the dry gauge ratio (hereinafter referred to as the "resilience ratio"). Wet resilience is measured according to the procedure described in the Test Method section below. The activation frames of the present invention will have a resilience ratio of at least about 0.9. Preferably, the activation frames will have a resilience ratio of about 0.95, more preferably at least about 0.98. As indicated, the activation frame must have the resilience ratio required during a period of time corresponding to the period of typical use of the article. In this way, the activation frame does not need to exhibit the required resilience ratio indefinitely. As will be discussed later, in certain modalities, the activation pattern will comprise a synthetic material
(for example, a polymer network) printed on a cellulosic material. It is evident that while the cellulose component of the activation member may collapse (ie, it will not be "resilient") to some degree when it is wetted, the polymer network will maintain its textured, t-dimensional character and provide the desired activation of the emulsion. . In these embodiments, the resilience ratio will be adjusted to exclude the reduced resilience caused solely by the cellulosic component. In addition to providing the abrasive character through a textured surface and exhibit the required resilience ratio, the textured surface of the activation screen, in direct contact with the multi-component, multi-phase emulsion during use, will preferably provide a significant amount of void volume in the embodiment that is accessible to the emulsion. This void volume provides a containment or confinement space to capture and retain the solid phase of the emulsion when it is separated from the active liquid phase during the activation process, such that this proportion of the emulsion does not interfere with the release or operation of the liquid phase and / or leave the item for cleaning where it may contaminate the external surfaces during use. Another property that has been found to provide optional desirable attributes in articles for cleaning according to the present invention is permeability. In accordance with the present invention, the activation screen does not need to be permeable and in fact may be impermeable to liquids, at least for the liquid formation of the multi-component, multi-phase emulsion. In this embodiment, the activation frame could form a barrier and ensure that the released liquid remains on a single side of the activation frame. However, a liquid-permeable activation pattern allows the liquid to penetrate the activation web and depending on the construction of the article for total cleaning, moisten the outer layer or layers of the article on both opposite sides of the activation web for used as desired. For activation frames that are permeable, it is believed that an additional property that is advantageous for certain applications is capillarity. With the liquid characteristics of the particular liquid component of the multi-component, multi-phase emulsion taken into account, liquid activation passages extending from one surface to the other surface acting as capillary structures can be provided to the activation grid. the particular liquid used. Accordingly, the activation frame can provide a preferential liquid flow direction for directing the liquid from one side of the activation frame to the other side of the activation frame. This motive force of the liquid also tends to resist liquid flow in the opposite direction. These capillary properties can be used for various functions, such as, for example, providing an item for single-side cleaning where one side becomes wet by the liquid to provide an active cleaning surface, while the other side remains practically unchanged. moisten by the internal liquid. In addition, it has been found advantageous to use an activation screen comprising a thermoplastic material. These materials, which are not essential to the present invention, provide an additional benefit over and above those provided by non-thermoplastic materials in that the weft provides a material that can be easily bonded with heat to other components of the invention. article for cleaning such as, for example, non-thermoplastic secondary screens in the absence of adhesives and other binding agents.
A material suitable for use in accordance with the present invention comprises a macroscopically, three-dimensional expanded, formed film web of a polymeric material, such as, for example, polyethylene, polypropylene or other suitable material, as a carrier for the emulsion. Films formed with perforations are preferred because they are liquid permeable and even non-absorbent and also have a tendency to exhibit a preferential liquid flow in one direction. Suitable formed films are described in U.S. Patent No. 3,929,135, issued to Thompson on December 30, 1975; U.S. Patent No. 4,324,246 issued to Mullane, et al. on April 13, 1982; U.S. Patent No. 4,342,314 issued to Radel. et al. on August 3, 1982; U.S. Patent No. 4,463,045 issued to Ahr et al. on July 31, 1984; 4,637,819 issued to Ouellette, et al. on January 20, 1987; and U.S. Patent No. 5,006,394 issued to Baird on April 9, 1991. Each of these patents is incorporated herein by reference. Other suitable shaped films include hydroformed films such as those described in U.S. Patent No. 4,629,643, issued December 16, 1986 to Curro et al., And U.S. Patent No. 4,609,518, issued September 2. from 1986 to Curro, both of which are also incorporated herein by reference. Preferably formed films could have microperforations formed thereof. Figure 2 is a perspective illustration, partially segmented, "enlarged, of a particularly preferred embodiment of a polymeric web, liquid permeable, fiber-like, three-dimensional, macroscopically expanded, perforated, generally in accordance with the teachings "of the United States Patent assigned jointly No. 4,342,314 to Radel et al., on August 3, 1982, which has been found suitable for use as a main document of the absorbent articles .The term" macroscopically expanded " ", when used to describe the three-dimensional plastic frames of the present invention, refers to frames, bands and films that have been the cause of shaping the surface of a three-dimensional formation structure in such a way that both surfaces of the same exhibit a pattern of three-dimensional formation of the surface aberrations that correspond to the macroscopic cross section of the forming structure, the surface aberrations that comprise the pattern are visible individually to the naked eye, that is, a simple normal view that has a 20/20 vision without the aid of an instrument that changes the apparent size or distance of an object or otherwise alters the visual power of the eye, when the perpendicular distance between the eye of the observer and the plane of the frame is approximately 12 inches (30.48 cm). The term "fiber-like", in the sense in which it is used herein, describes the appearance of plastic wefts of the present invention, refers in general to any fine-scale pattern of perforations, randomized or non-randomized, reticulated or non-reticular, which implies a general appearance and impression of an interwoven or non-woven fibrous web when viewed by the human eye. As can be seen in Figure 2, the fiber-like appearance of the weft consists of a continuous medium of fiber-like elements, the opposite ends of each of the fiber-like elements are interconnected with each other of the fiber-like elements. In the embodiment set forth in Figure 2, the interconnected fiber-like elements form a pattern network of capillaries 41 with a pentagonal shape. The web 40 exhibiting a fiber-like appearance incorporates a three-dimensional microstructure extending from the webs of the first surface 42 in the plane 43 to its second surface 44 in the plane 45 that is used in the absorbent articles to stimulate the transport of fast liquid from the first Surface 42 to the second surface 44 of the frame without lateral transmission of the liquid between the adjacent capillaries 41. In the sense in which it is used in the present, the term "microstructure" refers to a fine scale structure whose precise detail is easily observed by the human eye only when magnified by a microscope or other means well known in the art. The perforations 47 in the first surface 42 are formed by a multiplicity of intersecting fiber-like elements, for example, the elements 48, 49, 50 and 52, interconnected with each other in the body facing the surface of the weft. Each fiber-like element comprises a base portion, for example, a base portion 54, located in the plane 43. Each base portion has a side wall portion, for example, side wall portions 56, attached to each edge of the walls. same. The side wall portions 56 extend generally in the direction of the second surface 44 of the weft. The intersecting side wall portions of the fiber-like elements interconnect with each other in the middle of the first and second surfaces of the weft and terminate substantially concurrently with each other in the plane 45 of the second surface. In the particularly preferred embodiment shown in Figure 2, the interconnected side wall portions 56 terminate substantially concurrently with each other in the plane 45 of the second surface 44 to form the perforations 58 in the second surface 44 of the weft. The network of capillaries 41 formed in the side wall portions 56 interconnected between the perforations 47 and 58 allows the free transfer of liquids from the uppermost surface of the weft directly to the lowermost surface of the weft without the lateral transmission of the liquid between the adjacent capillaries.
Base portion 54 may include a microscopic pattern of surface aberrations 60, generally in accordance with the teachings of co-assigned United States Patent No. 4,463,045 to Ahr et al. on July 31, 1984. When used in a visible configuration, the microscopic pattern of the surface aberrations 60 provides a virtually dull visible surface when the screen 40 is affected by incidental light rays. When used as an activation pattern as shown in the embodiment of Figure 1, the formed film web of Figure 2 can be used with the first surface oriented and brought into direct contact with the multi-component emulsion 5, multi-phase. However, it is currently preferred to use the second surface 44 as the surface that is directly contacted with the emulsion during use. In this configuration, the three-dimensional nature of the film formed with its perforations 58 broken unevenly in the second surface provides an enhanced abrasive property compared to the first surface to provide an enhanced activation property in accordance with the present invention. Accordingly, when a material is used as an activation pattern in accordance with the present invention (i) it provides a three-dimensional surface topography on the lateral part of the material that initially comes into direct contact with the multi-component, multi-emulsion. -phase, during use, (ii) it provides an accessible three-dimensional void volume for the emulsion, (iii) it is wet resilient, (iv) it comprises a capillary structure and (v) it provides a hot sealable material useful in the assembly of the article for cleaning. In addition to using thermoplastic films as activation frames, the relatively untexturized webs can be modified in such a way as to significantly increase the amount of texture that will come into contact with the emulsion and thereby improve the fluid release performance of the article. A particular method for modifying this untextured plot is to print on a more texturized element to a relatively untextured plot. The printed component can cover the entire surface or only a portion of the surface in contact with the emulsion. Potential embodiments include, for example, printed polymeric networks, unbonded particles or particles adhered to the substrate, printed polymeric "hooks", which are described in detail in U.S. Patent Nos. 5,230,851, 5,318,741, 5,058,247, 5,116,563, 5,180,534 , 5,540,673, 5,326,415, 5,325,569, 5,392,498, 5,300,058, 5,385,706, 5,397,317 and 5,5 ^ 86,979, the teachings of which are incorporated herein by reference. It will be understood by one skilled in the art that this technique can be applied to any of a wide variety of substrates in such a way that the total resilience ratio of the material increases in total texture in contact with the emulsion that has been increased. For the purpose of this invention, any modified web, as described herein, will require the calculation of the wet resilience ratio that will be modified as described in the Test Method section below. In a particular embodiment, the activation pattern may be in the form of a polymer network printed on a substrate (eg, a cellulosic substrate) in a predetermined binding pattern to provide a plurality of t-dimensional regions, you turi zada s, on the substrate. An embodiment of an activation frame is generally represented in Figure 4A as the frame 200. The frame 200 comprises a substrate 114 having printed thereon a polymer, which is designated 110. In this preferred embodiment, the adhesive 110 it is applied to substrate 114 by stenciling or screening of an adhesive in a crosslinked pattern in general as shown in Figure 4A. A suitable screen for this mode is a 40 mesh Galvano screen manufactured by Rothtec Engraving Corp., New Bedford, MA. A suitable adhesive is a hot melt adhesive commercially available as H1382-01 from Ato-Findley Adhesives of Wauwatosa, Wisconsin. A suitable screen printer is available from ITW Dynatec, Model SP-117. The adhesive is preferably insoluble in water, so that the printed structure maintains its geometrical integrity when it is wetted. The adhesive is preferably also tolerant to the surfactant. By "surfactant tolerant" it is meant that the agglutination characteristics of the adhesive are not degraded by the presence of surfactants. Suitable adhesives include EVA (ethylene vinyl acetate) based on hot melt adhesives. Referring further to Figure 3, the hot melt adhesive can be applied to the substrate (e.g., the cellulosic layer) 114 in a continuous network defining a discontinuous plurality of unjoined regions. In a preferred embodiment, as shown, the adhesive is applied as separate lines, parallel in a first direction, intersected by separate parallel lines in a second direction. The intersecting lines define diamond-shaped patterns of unconnected regions in the activation frame.
E. Secondary Frames The articles of the present invention may also comprise one or more secondary frames. The weft or sheet materials useful in the present invention as secondary frames together with the activation screen (as shown in Figure 1) containing the multi-component, multi-phase emulsion before being used, can take a variety of forms of substrate. Suitable substrates include woven materials, non-woven materials, foams, sponges, wadding, beads, tassels, films and the like. Particularly preferred substrates for use in the present invention are of the non-woven types. These nonwoven substrates may comprise any conventionally formed nonwoven web or sheet having a suitable basis weight, caliper (thickness), absorbency characteristics and strength. Nonwoven substrates can be defined in general as bonded fibrous or filamentary products having a weft structure, in which the fibers or filaments are randomly distributed according to the processes of "laying in the air" or certain processes of "wet laying" "or with a degree of orientation, as in certain processes of" wet laying "or" carded ". The fibers or filaments of these non-woven substrates can be natural (for example, wood pulp, wool, silk, jute, hemp, cotton, linen, henequen or ramin) or synthetic (for example, rayon, cellulose ester, derivatives of polyvinyl, polyolefins, polyamides or polyesters) and may be bonded together with a polymeric binder resin. Examples of suitable commercially available nonwoven substrates include those sold under the trade name Sontara® by DuPont and Polyweb® by James River Corp. For reasons of cost, ease of manufacture and disposable characteristics of the article (eg, ability to be disposed of by the product). odorless), the preferred type of the nonwoven substrate used in the fabrics of the present invention comprises those made of wood pulp fibers, i.e., paper webs. As noted, paper webs can be prepared by either air-laying or wet-laying techniques. Air-laid paper webs such as, for example, Air Tex® SC130 are commercially available from James River Corp. More conventionally, paper webs are manufactured by wet laying processes. In these processes, a web is made by forming an aqueous pulp, which deposits this paste on a foraminous surface, such as for example, a Fourdrinier mesh, and by the subsequent removal of water from the pulp, for example by gravity, by drying assisted by vacuum and / or by evaporation, with or without pressing, to thereby form a paper web of desired fibrous consistency. In many cases, the papermachine apparatus is adjusted to rearrange the fibers in the pulp of the pulp as drainage proceeds to form the paper substrates of particularly desirable strength, handling, bulk, appearance, absorbency, etc. . The pulp used to form the preferred paper weave substrates for the articles of the present invention essentially comprises an aqueous pulp of papermaking fibers (ie, paper pulp) and may optionally contain a wide variety of chemicals such as, for example, wet strength resins, surfactants, pH control agents, softness additives, disintegrating agents and the like. You can use wood pulp in all its variations to form the pulp. The wood pulps useful herein include both sulphite and sulfate pulps, as well as mechanical, thermo-mechanical and chemo-thermo-mechanical pulps, all of which are known to those skilled in the papermaking art. Pulps derived from both deciduous and coniferous trees can be used. Preferably, the pulp used to form the preferred paper web substrates for fabrics of the present invention comprises Kraft pulp derived from soft northern woods. • Several of the papermaking processes using a papermaking apparatus that forms paper webs having particularly useful or desirable fiber configurations have been developed. These configurations can serve to impart these paper weave characteristics as improved volume, absorbency and strength. One of these processes employs a printing cloth in the papermaking process which serves to impart a high density knuckle pattern and low density areas on the resulting paper web. A process of this type, and the papermaking apparatus for carrying out this process, is described in greater detail in U.S. Patent 3,301,746 (Sanford et al.), Issued January 31, 1967, which is incorporated by reference. . Another papermaking process employs a through-drying fabric having print knuckles that rise above the plane of the fabric. These impressions create protrusions in the through-drying sheet and provide the sheet with stretching in the transverse direction of the machine. A process of this type is described in European Patent Publication No. 677,612A2, published October 18, 1995 by G. Wendt et al., The disclosure of which is incorporated herein by reference. Even another papermaking process carried out with a special papermaking apparatus is one that provides a paper web having a continuous, distinct network region formed by a plurality of scattered "domes" through the network region of the substrate. These domes are formed by compressing an embryonic web such as that formed during the papermaking process into a foraminous deflection member having a patterned network surface formed by a plurality of discrete isolated deflection conduits on the surface of the deflection member. A process of this type, and the apparatus for carrying out this process is described in more detail in U.S. Patent 4,529,480 (Trokhan), issued July 16, 1985.; U.S. Patent 4,637,859 (Trokhan), issued January 20, 1987; and U.S. Patent 5,073,235 (Trokhan), issued December 17, 1991, all of which are incorporated by reference. Another type of papermaking process, and apparatus for carrying it out that is suitable for the manufacture of laminated paper substrates is described in U.S. Patent 3,994,771 (Morgan et al.); granted on November 30, 1976, which is incorporated as a reference. Yet another papermaking process carried out with a special papermaking apparatus is one that provides a paper web having regions of multiple basis weight. This process is described in U.S. Patent 5,245,025, issued September 14, 1993 to Trokhan et al., U.S. Patent No. 5,503,715, issued April 2, 1996 to Trokhan et al., And U.S. Patent No. 5,534,326, issued July 9, 1996 to Trokhan et al., the description of each of which is incorporated herein by reference. See also co-pending US Patent Application Serial No. 08 / 886,764, filed by Nissing et al. on July 1, 1997, the description of which is incorporated herein by reference. These substrates provide a carrier that has regions that are more permeable (i.e. regions of relatively lower basis weight) than other regions (i.e., regions of higher basis weight). In addition to papermaking fibers, the pulp used to make these paper weave substrates may "have other components or materials added thereto as may or may later become known in the art." The types of desirable additives will depend on the particular end use. For example, in fabric products such as toilet paper, paper towels, facial tissues, baby fabrics and other similar products, high wet strength is a desirable attribute. It is often desirable to add to the pulp chemicals known in the art as "wet strength" resins.A general thesis on the types of wet strength resins used in the paper art can be found in the TAPPI monograph No. Series 29, Wet Stength in Paper and Paperboard, Technical Association of the Pulp and Paper Industry (New York, 1965). Most useful wet strength resins have been cationic in nature. For the generation of permanent wet strength, the polyamide-epichlorohydrin resins are cationic wet strength resins which have been found to be of particular utility. Suitable types of these resins are described in U.S. Patent No. 3,700,623 (Keim), issued October 24, 1972, and U.S. Patent No. 3,772,076 (Keim), issued November 13, 1972. 1973, both of which are incorporated by reference. A commercial source of a useful polyamide-epichlorohydrin resin is Hercules, Inc. of Wilmington, Delaware, which markets these resins under the trademark Kymene® 557H. It has been found that polyacrylamide resins are useful as wet strength resins. These resins are described in U.S. Patent Nos. 3,556,932
(Coscia et al.), Granted on January 19, 1971, and
3,556,933 (Williams et al.), Granted on January 19, 1971, both of which are incorporated by reference. A commercial source of polyacrylamide resins is American Cyanamid Co. of Stamford, Connecticut, which markets one of these resins under the Parez® 631 NC brand. Still other water-soluble cationic resins which find utility as wet strength resins are resins of urea formaldehyde and melamine formaldehyde. The most common functional groups of these polyfunctional resins are nitrogen-containing groups such as, for example, amino groups and methylol groups attached to nitrogen. Resins of the polyethylenimine type can also find utility in the present invention. In addition, temporary wet strength resins such as, for example, Caldas 10 (manufactured by Japan Carlit), CoBond 1000 (manufactured by National Starch and Chemical Company), and Parez 750 (manufactured by American Cyanamide Co.) Can be used in the present invention. It should be understood that the addition of chemical compounds such as, for example, wet strength resins and temporary wet strength discussed in the foregoing for pulp pulp is optional and is not necessary for the practice of the present invention. In addition to the wet strength additives, it may also be desirable to include in the papermaking fibers certain additives to control the wet strength and lint formation known in the art. With respect to this, it has been found that starch binders are particularly suitable. In addition to reducing the lint formation of the paper substrate, low levels of starch binders also impart a modest improvement in dry tensile strength without imparting stiffness that could result from the addition of high levels of starch. Normally the starch binder is included in an amount such that it is retained at a level of from about 0.01 to about 2%, preferably from about 0.1 to about 1% by weight of the paper substrate. In general, suitable starch binders * for these paper web substrates are characterized by water solubility and hydrophilicity. Although it is not intended to limit the scope of suitable starch binders, representative starch materials include starch and potato starch, with waxy maize starch known industrially as amioca starch which is particularly preferred. Amioca starch differs from common corn starch in that it is completely amylopectin, while common corn starch contains both amylopectin and amylose. Various unique characteristics of amioca starch are further described in "Amioca-The Starch From Waxy Corn," H. H. Schopmeyer, Food Industries, December 1945, p. 106-108 (Vol. Pp. 1476-1478) The starch binder may be in granular or dispersed form, the granular form is especially preferred.The starch binder should preferably be cooked sufficiently to cause swelling of the particles. Most preferably, the starch granules swell, as they are being cooked, to a point just before the starch granule dispersion.These fairly swollen starch granules are referred to as "fully cooked." for the dispersion in general they can vary depending on the size of the starch granules, the degree of crystallinity of the granules and the amount of amylose present.The fully cooked amioca starch, for example, can be prepared by heating an aqueous pulp of about 4% consistency of starch granules at about 190 ° F (about 88 ° C) for between about 30 and about 40 minutes. Employable starch enzymes that can be used include modified cationic starches such as, for example, those modified to have nitrogen-containing groups, including amino groups and methylol groups attached to nitrogen, available from National Starch and Chemical Company , (Bridgewater, New Jersey), which have been previously used as additives for pulp pulp to increase their wet and / or dry strength.
F. Other Optional Fabric Components Along with the high internal phase reverse emulsion, there are other optional components that can be included in the articles of the present invention, normally for the purposes of improving the cleaning performance of the article when the phase is released. internal polar emulsion. Certain of these optional components may not be present in the emulsion at significant levels (e.g., more than 2% of the internal polar phase) because they may cause a premature breakdown of the emulsion. These include various anionic detergent surfactants having relatively high HLB values (eg, HLB values of about 10 to about 25), such as, for example, sodium linear alkyl benzene sulphonates (LAS) or ethoxy alkyl sulfates (AES), as well as non-ionic detergent surfactants such as, for example, alkyl ethoxylates, alkyl amine oxides, alkyl polyglycosides, zwitterionic detergent surfactants, ampholytic detergent surfactants, and cationic detergent surfactants such as, for example, salts of cetyl trimethyl ammonium salts and lauryl trimethyl ammonium. See U.S. Patent 4,597,898 (Van der Meer), issued July 1, 1986 (incorporated herein by reference), especially columns 12 through 16 for anionic, nonionic, zwitterionic, ampholytic and cationic detergent surfactants. , representative. In contrast, these detergent surfactants of high HLB values can be applied or included in the article separately from the emulsion. For example, an aqueous emulsion of these detergent surfactants of high HLB value can be applied to only one side of the carrier substrate, with the high internal phase inverse emulsion which will be applied to the other side of the substrate. During rubbing, the emulsion breaks down, releasing the internal polar phase (e.g., water) so that it can be combined with the high HLB detergent surfactant to provide improved cleaning on hard surfaces.
Although the description of the invention in general relates to the application of an individual emulsion to the carrier, it is recognized that two or more different emulsions can be used to prepare an individual article. In these embodiments, the emulsions may be different in a variety of ways, including, but not limited to, the ratio of the internal polar phase to the external lipid phase, the emulsifiers used, the components used for the internal and external phases. lipids or both, and the similar. The use of multiple emulsions in an article may be particularly desirable when two or more components are incompatible with each other, but each may be included in the emulsions separately. Alternatively, if a particular reaction is desired at the time of use, the reagents may be provided in separate emulsions. During the shearing stress of the emulsions during use, the desired reaction will occur. For example, when foaming is desired during the rubbing processes, a mild acid can be incorporated into the internal polar phase of the emulsion, while the bicarbonate is incorporated into the internal polar phase of a second emulsion. With the shear stress of the emulsions during use, the reagents interact to provide the desired foam.
G. Other Modalities of Items for Cleaning 'In addition to the configuration represented in the
Figure 1, items for cleaning according to the present invention can be assembled in a variety of other alternative configurations so long as they maintain the advantages of the present invention. Figure 3 represents an alternative configuration, wherein the article for cleaning 1 is similar in structure to that shown in Figure 1, but where the activation pattern 2 itself forms an external surface of the article. In a configuration, if the activation pattern is liquid permeable such as, for example, the formed film web of Figure 2, the article can function as an article for double side cleaning and release the active emulsion either through the web activation and the secondary frame 3 or both. Alternatively, if the activation pattern is impervious to liquids, the article functions as an item for single-side cleaning by distributing an active emulsion only through the secondary screen.
H. Test Method-Wet Resilience Wet resilience (ie, wet-gauge to dry gauge ratio) of an activation pattern is measured using an Electronic Thickness Tester Model II from Thwin-Albert Instrument Co. , according to the following procedure. The samples are conditioned at 70 ° Ft [sic] and 50% relative humidity for two hours before the test. The dry gauge of activation is measured using a confining pressure of 95 g / in2 and a loading foot that has a diameter of 2 inches. The dry caliber is measured for eight samples. The measurements of the eight calibers are averaged to provide an average dry caliber. Each sample is then moistened by immersing it in a bath of distilled water for 30 seconds. The sample is then removed from the water bath and allowed to drain for 5 seconds while hanging vertically. The size of the wet sample is measured within 30 seconds of removal of the sample from the bath. The wet caliber is measured in the same location in which the dry caliber was previously measured. The eight wet-gauge measurements are averaged to provide an average wet gauge. The ratio of wet caliber to dry caliber is the average wet caliber divided by the average dry caliber. If the activation pattern is a composite of multiple sheets or materials, for the purposes of this measurement it will be necessary to calculate the resilience ratio of the individual components. For the purposes of this calculation, the following definitions apply:
a = initial dry bore of the complete screen b = initial dry bore of the screen distal to the emulsion c initial dry bore of the screen next to the emulsion
A = initial wet calibration of the complete screen B = initial wet calibration of the screen distal to the emulsion C = initial wet calibration of the screen close to the emulsion
where the resilience ratio is defined as A / a; and where it is assumed that a, A and either b, B or c, C can be measured. For this measurement, it should be understood that a component of the composite screen must be removed to facilitate the measurement of b, B; c, C; or both independently. If a component of the composite frame can not be measured after it has been removed from the composite the resilience ratio can be calculated using the following expressions:
B / b = (A-C) / (a-c) C / c = (A-B) / (a-b)
I. Preparation of Representative Cleaning Items To prepare the articles according to the present invention, the high internal phase inverse emulsion is initially formulated. Normally, this is achieved by mixing or melting together the lipid phase components and the emulsifier. The particular temperature at which this lipid / emulsifier mixture is heated will depend on the melting point of the lipid phase components. Typically, this lipid / emulsifier mixture is heated to a temperature in the range of from about 60 ° to about 90 ° C, preferably from about 70 ° to about 80 ° C, before being mixed, bound or otherwise combined with the components in polar phase. The melted lipid / emulsifier mixture is then mixed with the components of the internal polar phase and then mixed together, usually under low shear conditions to provide the emulsion. This high internal phase reverse emulsion is then applied in a fluid or plastic state at the temperatures indicated above to the carrier substrate, for example, a paper web. Any of a variety of methods can be used that apply materials that have a fluid or plastic consistency to apply this emulsion. Suitable methods include scrubbing, printing (eg, flexographic or screen printing), coating (eg, photo-etched coating), extrusion, or combinations of these application techniques, for example, spraying the detergent surfactant onto a paper web, followed by photo-etched coating of the emulsion on the weft treated with detergent. The emulsion can be applied to either one side or both sides of the carrier web, or, in the case of multiple webs, it can be applied to the surface or internal surfaces of the layers. Once the emulsion has been applied to the carrier web, it is allowed to cool and form a typically discontinuous coating or film, solidified on the surface of the web. The high internal phase reverse emulsion is typically applied to the carrier web after the web has dried, i.e., a "dry web" addition method, for initially wet webs. The emulsion can also be applied uniformly to the surface or surfaces of the weft. By "non-uniform" it is meant that the quantity, pattern of distribution, etc. of the emulsion may vary on the surface of the carrier web. For example, some portions of the surface of the carrier web may have greater or lesser amounts of the emulsion, including portions of the surfaces that do not have any emulsion therein. The high internal phase reverse emulsion can be applied to the carrier web at any point after it has dried. For example, the emulsion can be applied to the surface of a paper web after it has been creped in a Yankee dryer. Usually, it is preferred to apply the emulsion to the carrier web while it is being unwound from a main roll and before rolling into smaller finished product rolls. In the application of the high internal phase reverse emulsions of the present invention to the carrier webs, the spray coating methods are currently preferred. Figure 5 illustrates one of these preferred methods wherein the emulsion is sprayed onto the carrier web 10. Referring to Figure 5, this spray system has a spray head 12 which applies a dispersed spray of the emulsion on the web 10. This spray system is actuated by a unit consisting of a ball screw driver 16 which is connected by coupling 18 to a piston 26 of the hydraulic cylinder 22. A portion of the cylinder 22 is shown in Figure 5 while is filling with the high internal phase reverse emulsion as indicated by 30. The cylinder 22 is heated to maintain the emulsion 30 in a fluid or plastic state. The emulsion 30 enters the cylinder 22 through a 4-way coupling 34 having a line 38 connected to a hot fill port 42. The coupling 34 also has a line 46 which is connected to the pressure gauge 50 and the spray head 12. There are three valves indicated as 56, 58 and 60 that control the flow of the emulsion in lines 38 and 46. The spray system shown in Figure 5 also has a line 64 connected to the spray head 12 which allows the air indicated in general, 68 is admitted to the spray head. Line 64 also has a manometer and regulator 72 for controlling and measuring the air pressure in the line. Lines 64 and 46 are heated to maintain the emulsion in a molten state before it is applied to the web. To load cylinder 22 with emulsion 30, valves 56 and 60 are closed and valve 58 is opened. The actuator with ball thread 16 is driven in such a way that the piston 26 moves to the left. The vacuum created in the cylinder 22 extracts the emulsion from the filling port 42 through the line 38 and into the interior of the cylinder 22. To provide the emulsion from the cylinder 22 to the spray head 12, the valve 58 closes and valves 56 and 60 open. The actuator with ball thread 16 is driven in such a way that the piston 26 moves to the right. This forces the emulsion 30 out of the cylinder 22 and into the interior of the coupling line 46. The emulsion then passes through the valve 60 and into the interior of the dew head 12 where it is dispersed by the incorporation of air from line 64 to provide a dispersed spray 14 which is then applied to the weft 10. Figure 6 illustrates an alternative method for applying the high internal phase reverse emulsion involving a rotogravure coating system. Referring to Figure 6, a carrier plot. 110 is unrolled from the main roller 112 (rotating in the direction indicated by the arrow 112a) and is advanced around the rotating rollers 114, 116 and 118. From the rotary roller 118, the weft 110 is advanced towards a rotating station 110. coating by engraving indicated in general as 120 where the emulsion is then applied to both sides of the weft. After leaving the station 120, the web 110 becomes a treated web indicated by 122. The treated web 122 is advanced to the surface rewind roller 126 (by rotating in the direction indicated by the arrow 126a) and then wound onto the roller of finished product 128 (rotating in the direction indicated by arrow 128a). The station 120 comprises a pair of hot, coupled pressings 130 and 134 for engraving. The press 130 consists of a smaller anilox cylinder 138 and a plate cylinder 142 for larger printing; the press 134 similarly consists of a smaller anilox cylinder 146 and a plate cylinder 150 for larger ping. The anilox cylinders 138 and 146 each have a ceramic or chromium surface, while the ping plate cylinders 142 and 150 each have a rubber, urethane or photopoly surface with a raised pattern. These anilox and ping plate cylinders rotate in the direction indicated by the arrows 138a, 142a, 146a and 150a, respectively. As shown in Figure 6, the ping plate cylinders 142 and 150 are opposite each other and provide a contact point area indicated by 154 through which the screen 110 passes. The molten, hot emulsion (e.g. , 60 ° C) is pumped into each of these presses 130 and 134 of bonded or sprayed on them in the contact point areas indicated by arrows 158 and 162, respectively, at a constant volumetric flow rate. (The emulsion distributed to the presses 130 and 134 may be the same or different.) In other words, the emulsion is added to the engraving presses 130 and 134 joined at the same speed as the emulsion is being applied to the frame 110. This Eliminates "emulsion buildup" in the system. As the anilox cylinders 138 and 146 rotate in the direction indicated by the arrows 138a and 146a, they act as rotating scraper blades to spread the emulsion evenly across the surfaces of the ping plate cylinders 142 and 150, respectively. and to remove the excess emulsion from the ping plates of the cylinders 142 and 150. The emulsion which is spread on the ping plate cylinders 142 and 150 (rotating in the opposite direction to that indicated by the arrows 142a and 150b) is then transferred to both sides of the frame 110 in the area of contact point 154. The amount of the emulsion transferred to the frame
110 can be controlled by: (1) adjusting the width of the contact area 154 between the printing plate cylinders 142 and 150, (2) "adjust the width of the contact areas 158 and 162 between the pairs of cylinders 138 / 142 and 146/150 anilox / printing plate; (3) the relief of the printed image (ie, valley depth) of the printed plate on the cylinders 142 and 150; (4) the printed area
(i.e., valley area) of the printed plate on the cylinders 142 and 150; and / or (6) the printed pattern of the printed plate on the cylinders 142 and 150.
EXAMPLE 1 This example illustrates the preparation of a cleaning article comprising an emulsion contained between two sheets of a compound activation frame. The activation pattern is prepared by printing a polymer network on the surface of a cellulosic web. This activation frame is represented in Figure 4A. The emulsion is printed on the activation web in such a way that the polymer network comes into direct contact with the emulsion in the finished article.
A) Activation Screen (1) Preparation of the Cellulose Screen The cellulosic screen component of the activation screen is a tissue paper substrate. The base paper is a sheet without layers, 100% NSK with a basis weight of 20 pounds / ream (approximately 32.5 gsm). The paper has a plurality of areas of high basis weight and areas of low basis weight. The paper was produced in accordance with the teachings of U.S. Patent 5,506,715 (Trokhan, et al.) With the following specific data:
1) The forming mesh contained 100 protuberances per square inch. 2) The protuberances occupied approximately 50% of the surface area of the forming mesh. 3) The protuberances extended above the forming mesh reinforcing the structure approximately 0.004 inches.
4) The perforations of each protuberance occupied approximately 10% of the surface area of the forming mesh. 5) In the final wetting stage of the conventional papermaking process, 2% aminosilicone (available from General Electric as CM 22666D1) was injected into the pulp NSK pulp in a proportion of _ 0.004 pounds of amino silicone solids per pound of dry paper. 6) In the final moistening stage of the conventional papermaking process, 1% of Kymene 2064 (available from Hercules Inc.) was injected into the NSK pulp at a rate of 20 pounds of Kymene solids per tonne of dry paper.
(2) Addition of Polymer An adhesive polymer is printed on the paper substrate in a predetermined pattern to provide texturized, three-dimensional regions to the substrate. Referring to Figure 4A, the printed regions are designated 110, and the unprinted regions are designated 114. In particular, in a preferred embodiment, the polymer is applied by screen printing. A suitable stencil stamping is Model SP-117 of ITW Dynatec. The polymer used is a
Hot melt EVA in general available as H1382-01 from Ato-Findley Adhesives of Wauwatosa, Wisconsin. A stencil suitable for this mode is a 40 mesh Galvano screen manufactured by Rothtec Engraving Corp., New Bedford, MA. The macroscopic printing pattern used is a cross-linked pattern of straight intersecting lines. The lines are approximately 0.0625 inches wide and are separated by approximately 0.5 inches. These lines intersect at approximately an 80 degree angle thus forming a pattern of untreated, diamond-shaped, discrete regions.
C) Preparation of the Emulsion A batch of lOOOg of an emulsion was prepared
(internal phase at 88.65%) from the ingredients shown in Table I.
To formulate the internal polar phase, all components of the polar phase are mixed together and then heated to 140 ° F (45.8 ° C). Separately, the lipid phase ingredients are heated, with mixing, at a temperature of about 140 ° F until they melt. The polar phase lipid components are then combined in a stainless steel vessel and mixed with a Model 100-C Hobart mixer in a low speed setting while allowing the ingredients to cool slowly. The mixing continues until the emulsion is formed. The formation of the emulsion is manifested by an increase in viscosity of more than 2000 centipoise as measured by a rotating disk viscometer from Lab-Line Instruments.
D) Application of the Emulsion to the Activation Screen The emulsion prepared in stage C is applied to the activation screen using a rotogravure printing process practically in the manner as shown in Figure 6, except that it is only used an engraving press (130). (The rewinding roller 126 is also not used in the preparation of the article described by this example.) The emulsion was maintained at a temperature of 135 ° F such that it is liquid or molten. A positive displacement pump drives the emulsion towards the engraving press 130 in the area of contact point indicated by the arrow 158 at a constant volumetric flow rate of 380 ml / minute. The anilox cylinder 138 spreads the emulsion evenly across the surface of the impression cylinder 142 (rotating at approximately 40 feet per minute). Cylinder 142 then transfers the emulsion to one side of frame 110 (cylinder 150 is used in a return cylinder to maintain constant printing on frame 110). The coated activation web (ie, the polymer network and the paper web) are then folded in such a way that the emulsion is contained within the interior of the article. The surface of the composite web with the polymer network is also contained within the article, in contact with the emulsion. The combination, perforation and sealing can be carried to ca'bo using techniques known in the art.
EXAMPLE 2 This example illustrates the preparation of a fabric for releasing moisture comprising an emulsion contained between a secondary paper web and an activation web. The activation pattern consists of a laminated formed film for a paper web. The emulsion is applied to the side of the formed film of the laminate. The additional processing could include the emulsion between the secondary screen and the lateral part of the film of the activation screen, as shown in Figure 1.
A) Preparation of the Secondary Plot The secondary plot is a tissue paper substrate. The base paper is a sheet without layers, 100% NSK with a base weight of 20 lbs / ream (approximately 32.5 gsm). The paper has a plurality of areas of high basis weight and areas of low basis weight. The paper was produced in accordance with the teachings of U.S. Patent 5,506,715 (Trokhan, et al.) With the following speci fi c data:
1) The forming mesh contained 100 protuberances per square inch. 2) The protuberances occupied approximately 50% of the surface area of the forming mesh. 3) The protuberances extended above the forming mesh reinforcing the structure to approximately 0.004 inches. 4) The perforations of each protuberance occupied approximately 10% of the surface area of the forming mesh. 5) In the final wetting stage of the conventional papermaking process, a 2% amino silicone (available from General Electric as CM 22666D1) was injected into the NSK pulp at a rate of 0.004 pounds of amino silicone solids per pound of dry paper. 6) In the final wetting stage of the conventional papermaking process, 1% of Kymene 2064 (available from Hercules Inc.) was injected into the NSK pulp at a rate of 20 pounds of Kymene solids per tonne of dry paper.
B) Preparation of the Activation Screen The activation screen is prepared by laminating a web of film formed with a paper layer similar in composition to the secondary screen described above, the formed film being approximately half the width of the paper plot. The difference in width is to allow bending after the emulsion has been applied in such a way that the finished product has an activation pattern on only one side of the emulsion, as shown in Figure 1. The formed film is a macroscopically expanded, three-dimensional grid, of polymeric materials prepared in accordance with the teachings of U.S. Patent No. 4,342,314 issued to Radel. et al. on August 3, 1982. The formed film has a three-dimensional microstructure comprising a continuous regulated medium of tapered capillary networks originating in the first surface 42 and extending therefrom in the plane 43 and ending in the second surface 44 in plane 45, forming perforations in both surfaces. The size of the perforations is approximately 0.040 inches on one surface and approximately 0.016 inches on the other surface. The total height between the plane 43 and the plane 45 is approximately 0.012 inches. The microstructure has a density of approximately 625 capillaries per square inch. The base portion 54, located in the plane 43, may include microscopic aberrations 60, generally in accordance with the teachings of the co-assigned United States Patent No. 4,463,045, issued to Ahr et al. on July 31, 1984. Surface aberrations 60 may be outwardly projecting protrusions or inwardly projecting depressions, and measure at least 0.0002 inches from the plane that causes the aberrations. The average distance between the adjacent surface aberrations is less than 0.0004 inches. This formed film is laminated to the paper layer using a hot melt adhesive, H2031, generally available from Ato-Findley Adhesives of Wuwatosa, Wisconsin. In this example, the more textured side of the formed film is oriented towards the emulsion (ie, the glue used in the lamination process is applied to the less textured side). The melt adhesive on. hot is applied using a stencil stamper (Model SP-117 from ITW Dynatec) in a continuous pattern.
C) Preparation of the Emulsion A batch of lOOOg of an emulsion (internal phase at 88.65%) of the ingredients shown in Table II is prepared.
Table II
To formulate the internal polar phase, all the polar phase components are mixed together and then heated to 140 ° F (45.8 ° C). Separately, the lipid phase ingredients are heated, with mixing, to a temperature of about 140 ° F until they are melted. The polar and lipid phase components are then combined in a stainless steel vessel and mixed with a Hobart Model 100-C mixer set at low speed while allowing the ingredients to cool slowly. The mixing continues until the emulsion is formed. The formation of the emulsion is manifested by an increase in viscosity above 2000 centipoise as measured by a rotating disk viscometer from Lab-Line Instruments.
D) Application of the Emulsion to the Activation Screen The emulsion prepared in stage C is applied to the more textured lateral part (that is, the lateral part of the formed film) of the activation screen using a spray process similar to the shown in Figure 5. The emulsion is maintained at a temperature of 135 ° F such that it is liquid or molten. A positive displacement pump drives the emulsion towards the spray head indicated by arrow 12 at a constant volumetric flow rate of 625 ml / minute during an in-line speed of 25 feet per minute. No airflow passes through line 64 to allow continuous ridges to be applied to the paper web. Next, the secondary web is a laminated activation web, as shown in Figure 1. The finished article 10 is then perforated (in Figure 4A the apparatus for sealing, bending and punching is not illustrated) to provide the product web. finished. While the particular embodiments of the present invention have been illustrated and described, it will be apparent to those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention, and it is intended to cover all the appended claims These modifications are within the scope of the invention.
Claims (12)
- CLAIMS 1. An article for cleaning comprising: (a) an activation pattern having a first surface having one or more regions that exhibit a three-dimensional, textured surface topography and a second surface, the activation pattern has a ratio of wet gauge at dry gauge (resilience ratio) of at least 0.9; and (b) a multi-component, multi-phase emulsion that is in direct contact with the first surface of the activation screen during use.
- 2. An article for cleaning comprising: (a) an activation pattern having a first surface having one or more regions exhibiting a three dimensional, textured surface topography and a second surface, the activation pattern having a wet size ratio to dry caliber (resilience ratio) of at least 0.9; (b) a secondary frame, the activation frame and the secondary frame are linked at least peripherally to each other; (c) a multi-component, multi-phase emulsion which is in direct contact with the first surface of the activation screen during use.
- 3. The article for cleaning according to claim 1 or 2, characterized in that the activation pattern has a resilience ratio of preferably at least 0.95, more preferably at least 0.98.
- 4. The article for cleaning according to any of the preceding claims, characterized in that the activation frame comprises a macroscopically expanded, three-dimensional formed film.
- 5. The article for cleaning according to any of the above indications, characterized in that the activation frame comprises a capillary frame structure.
- 6. The article for cleaning according to any of the preceding claims, characterized in that the activation frame comprises a thermoplastic material.
- 7. The article for cleaning according to any of the preceding claims, characterized in that the activation pattern is permeable to fluids.
- 8. The cleaning article according to any of the preceding claims, characterized in that the activation screen is impermeable to fluids.
- 9. The article for cleaning according to any of the preceding claims, characterized in that the article for cleaning comprises at least one additional frame opposite to the secondary frame and peripherally joined to the activation frame.
- 10. The article for cleaning according to any of the preceding claims, characterized in that one or more regions of the activation pattern that are textured comprise a particulate material.
- 11. The cleaning article according to any of the preceding claims, characterized in that one or more regions of the activation web that are textured comprise an adhesive polymeric material.
- 12. The article for cleaning according to any of the above indications, characterized in that the emulsion comprises: (1) from 2 to 60% of a solidified, continuous lipid phase, comprising a waxy lipid material having a melting point of 30 ° C or older; (2) from 39 to 97% of an internal polar phase dispersed in the lipid phase; and (3) an effective amount of an emulsifier capable of forming the emulsion when the lipid phase is in a fluid state.
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US60/072,448 | 1998-01-26 |
Publications (1)
Publication Number | Publication Date |
---|---|
MXPA00007311A true MXPA00007311A (en) | 2001-07-09 |
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