Classifications

• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
  • A61F13/00—Bandages or dressings; Absorbent pads
  • A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
  • A61F13/53—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the absorbing medium
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
  • A61F13/00—Bandages or dressings; Absorbent pads
  • A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
  • A61F13/53—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the absorbing medium
  • A61F13/534—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the absorbing medium having an inhomogeneous composition through the thickness of the pad
  • A61F13/537—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the absorbing medium having an inhomogeneous composition through the thickness of the pad characterised by a layer facilitating or inhibiting flow in one direction or plane, e.g. a wicking layer
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
  • A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
  • A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
  • A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
  • A61L15/28—Polysaccharides or their derivatives
• • D—TEXTILES; PAPER
  • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
  • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
  • D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
  • D21C9/001—Modification of pulp properties
  • D21C9/002—Modification of pulp properties by chemical means; preparation of dewatered pulp, e.g. in sheet or bulk form, containing special additives

Definitions

• the present invention is directed to a method of making chemically cross- linked cellulosic fiber in the sheet form and to the product resulting from the process.
• Absorbent articles intended for personal care typically are comprised of at least a top sheet, a back sheet, an absorbent core disposed between the top sheet and back sheet, and an optional acquisition layer disposed between the top sheet and the absorbent core.
• the acquisition layer comprised of, for example, acquisition fibers, usually is incorporated in the absorbent articles to provide better distribution of liquid, increase the rate of liquid absorption, and reduce gel blocking.
• acquisition fibers are known in the art. Included among these are synthetic fibers, a composite of cellulosic fibers and synthetic fibers, and cross-linked cellulosic fibers. Cross-linked cellulose fiber is preferred because it is abundant, it is biodegradable, and it is relatively inexpensive.
• Cross-linked cellulose fibers and processes for making them have been described in the literature for many years (see, for example G. C.Tesoro, Cross-Linking of Cellulose, in Handbook of Fiber Science and technology, Vol. II, M. Lewis and S. B. Sello eds. pp 1-46, Mercel Decker, New York (1993)).
• the cross-linked cellulose fibers are typically made by reacting cellulose with polyfunctional agents that are capable of reacting with the hydroxyl groups of the anhydroglucose repeating units of the cellulose either in the same chain, or in neighboring chains simultaneously.
• Cross-linked cellulose fibers generally are characterized by their high absorbent capacity, and their high resiliency in the wet and dry states.
• Cellulosic fibers typically are cross-linked in fluff form.
• Processes for making cross-linked fiber in the fluff form comprise dipping swollen or non- swollen fiber in an aqueous solution of cross-linking agent, catalyst, and softener.
• the fiber so treated usually is then cross-linked by heating it at elevated temperatures in the swollen state as described in U.S. Patent No. 3,241,553, or in the collapsed state after defiberizing it as described in U.S. Patent No. 3,224,926, and European Patent No. 0,427,361 Bl, the disclosures of each of which are incorporated by reference herein in their entirety.
• Bernardin et al. in U.S. Patent 3,434,918 disclose a method of treating fiber in sheet form with a cross-linking agent and a catalyst. The treated sheet then is wet-aged to render the cross-linking agent insoluble. The wet-aged fibers are re-dispersed before curing and mixed with untreated fiber, and then sheeted and cured.
• Other documents describing methods of treating fiber in sheet form include, for example, U.S. Patent Nos. 4,204,054; 3,844,880; and 3,700,549 (the disclosures of which are incorporated by reference herein in their entirety).
• Fiber mercerization which is a treatment of fiber with an aqueous solution of sodium hydroxide (caustic), is one of the earliest known modifications of fiber. It was invented 150 years ago by John Mercer (see British Patent 1369, 1850). The process generally is used in the textile industry to improve cotton fabric's tensile strength, dyeability, and luster (see, for example, R. Freytag, J.-J. Donze, Chemical Processing of Fibers and Fabrics, Fundamental and Applications, Part A, in Handbook of Fiber Science and Technology Vol. I M. Lewis and S. B. Sello eds. pp. 1-46, Mercell Decker, New York (1983)).
• mercerization adds to fibers several other properties. Among these are: (1) mercerized fibers have high ⁇ - cellulose content, since caustic removes residuals such as lignin and hemicellulose from fiber leftover from pulping and bleaching processes; (2) mercerized fibers have a round, circular shape (rather than the flat, ribbonlike shape of conventional fibers) that reduces the contact and weakens the hydrogen-bonding between fibers in the sheet form; and (3) mercerization converts cellulose chains from their native structure form, cellulose I, to a more thermodynamically-stable and less crystalline form, cellulose II.
• the cellulosic chains in cellulose II are found to have an anti-parallel orientation rather than parallel orientation as in cellulose I (see, for example, R. H. Atalla, Comprehensive Natural products Chemistry, Carbohydrates And Their Derivatives Including Tannins, Cellulose, and Related Lignins Vol. Ill, D. Barton and K. Nakanishi eds. pp 529-598, Elsevier Science, Ltd., Oxford, U.K. (1999)).
• One feature of an embodiment of the present invention provides cross-linked fibers with enhanced bulking characteristics, porosity and rate of acquisition.
• An additional aspect of the present invention is to provide cross-linked cellulosic fiber having long shelf-life and high stability.
• another aspect of an embodiment of the present invention provides fibers useful in an acquisition layer and/ or in an absorbent core of absorbent products.
• Various aspects of the present invention also provide absorbent articles comprising the cross-linked fiber of the present invention.
• a cross-linked sheet of a blend of fibers and a method for cross-linking cellulose fibers in sheet form.
• the cellulose fibers are a blend of mercerized fibers and conventional fibers that are cross-linked.
• the cross-linked fibers formed in accordance with the present invention can be easily defiberized without serious fiber breakage and with low knot- content and low nit-content. It will be appreciated, however, that knots and nits are advantageous for some applications, and accordingly, the present invention is not in any way limited to producing cross-linked cellulosic fibers substantially free of knots.
• a wet laid sheet of a blend of mercerized fibers and cellulose fibers are formed, and then treated a cross-linking agent to form a sheet impregnated with the cross-linking agent.
• the cross-linking agent then is dried and cured to form intra-fiber cross-links.
• Figures la and lb are photographs at 100X and 200X magnifications, respectively, of blends of fibers obtained as shown in Example 2 from Rayfloc ® -J-LD (southern pine Kraft pulp commercially available from Rayonier Performance Fibers Division, Jesup, GA) and mercerized fibers in about 1:1 weight ratio using glyoxylic acid (2%) cross-linking agent.
• Rayfloc ® -J-LD pine Kraft pulp commercially available from Rayonier Performance Fibers Division, Jesup, GA
• mercerized fibers in about 1:1 weight ratio using glyoxylic acid (2%) cross-linking agent.
• Figures 2a and 2b are photographs at 100X and 200X magnification, respectively, of a blend of fibers of the present invention prepared from Rayfloc ® -J-LD and mercerized fibers in 1:1 ratio and cross-linked in accordance with Example 3.
• the terms "absorbent garment,” “absorbent article” or simply “article” or “garment” refer to mechanisms that absorb and contain body fluids and other body exudates. More specifically, these terms refer to garments that are placed against or in proximity to the body of a wearer to absorb and contain the various exudates discharged from the body.
• absorbent garments includes diapers, diaper covers, disposable diapers, training pants, feminine hygiene products and adult incontinence products. Such garments may be intended to be discarded or partially discarded after a single use (“disposable” garments).
• Such garments may comprise essentially a single inseparable structure (“unitary” garments), or they may comprise replaceable inserts or other interchangeable parts.
• the present invention may be used with all of the foregoing classes of absorbent garments, without limitation, whether disposable or otherwise.
• Some of the embodiments described herein provide, as an exemplary structure, a diaper for an infant, however this is not intended to limit the claimed invention.
• the invention will be understood to encompass, without limitation, all classes and types of absorbent garments, including those described herein.
• component can refer, but is not limited, to designated selected regions, such as edges, corners, sides or the like; structural members, such as elastic strips, absorbent pads, stretchable layers or panels, layers of material, or the like.
• disposed and the expressions "disposed on,” “disposed above,” “disposed below,” “disposing on,” “disposed in,” “disposed between” and variations thereof are intended to mean that one element can be integral with another element, or that one element can be a separate structure bonded to or placed with or placed near another element.
• a component that is "disposed on” an element of the absorbent garment can be formed or applied directly or indirectly to a surface of the element, formed or applied between layers of a multiple layer element, formed or applied to a substrate that is placed with or near the element, formed or applied within a layer of the element or another substrate, or other variations or combinations thereof.
• top sheet and back sheet denote the relationship of these materials or layers with respect to the absorbent core. It is understood that additional layers may be present between the absorbent core and the top sheet and back sheet, and that additional layers and other materials may be present on the side opposite the absorbent core from either the top sheet or the back sheet.
• the term "impregnated" insofar as it relates to a cross-linking agent impregnated in a fiber denotes an intimate mixture of cross-linking agents and cellulosic fiber, whereby the cross-linking agent may be adhered to the fibers, adsorbed on the surface of the fibers, or linked via chemical, hydrogen or other bonding (e.g., Van der Waals forces) to the fibers. Impregnated in the context of the present invention does not necessarily mean that the cross-linking agent is physically disposed beneath the surface of the fibers.
• the present invention concerns chemically cross-linked blends of fibers that are useful in absorbent articles, and in particular, that are useful in forming acquisition layers or absorbent cores in the absorbent article.
• the particular construction of the absorbent article is not critical to the present invention, and any absorbent article can benefit from this invention.
• Suitable absorbent garments are described, for example, in U.S. Patent Nos. 5,281,207, and 6,068,620, the disclosures of each of which are incorporated by reference herein in their entirety including their respective drawings.
• Those skilled in the art will be capable of utilizing the chemically cross-linked cellulosic fibers of the present invention in absorbent garments, cores, acquisition layers, and the like, using the guidelines provided herein.
• Cross-linking of fibers in fluff form is beHeved to improve the physical and chemical properties of the fibers in many ways, such as improving the stiffness, increasing resiliency (in the dry and wet state), increasing the absorbency, reducing wrinkling, and improving shrinkage resistance.
• cross-linking if carried out on a fiber in sheet form, may create problems in the fiber which render it unsuitable for many appHcations. These problems include severe fiber breakage and increased amounts of knots and nits (hard fiber clumps). These problems are attributed to the inter-fiber (fiber-to-fiber) cross-linking that occurs between fibers in close contact during the curing process.
• fibers get into close contact in the dry state due to (a) mechanical entanglement; (b) hydrogen bonding between fibers; and (c) pulping and bleaching residuals such as Hgnin and hemiceUulose.
• fibers treated with a cross-linking agent are heated for curing, fibers in close contact tend to form inter-fiber cross-links rather than intra-fiber cross-links (chain-to-chain within the single fiber).
• the present invention is directed to a method of making cross-Hnked fibers in sheet form.
• the method preferably comprises treating ceUulose fibers in sheet or roU form with an aqueous solution of a polyfunctional cross-linking agent, foUowed by drying and curing at sufficient temperature for adequate time to accelerate the formation of covalent bonding between hydroxyl groups of cellulose fibers and functional groups of the cross-linking agent.
• the method of an embodiment of the invention preferably comprises reacting a blend of fibers in sheet form with one or more reagents selected from organic molecules having carboxyHc acid, an aldehyde and carboxyHc acid (e.g., an acid aldehyde), or epoxy functional groups.
• the method of the present invention provides cross-Hnked fibers in sheet form that can be readily defiberized with low knot-content and without significant fiber breakage.
• the method of the present invention provides cross-linked fibers that are characterized by an enhanced acquisition rate, resiHency, and absorbency under load.
• cross- linked fibers of the present invention display a reduction in centrifuge retention capacity which makes the fiber especiaUy suited for use in acquisition, distribution and acquisition-distribution layers in absorbent articles intended for fluid management.
• the fiber in sheet form comprises a blend of mercerized fibers and conventional fibers.
• conventional fibers denotes cellulose fibers of diverse origins, especiaUy those primarily derived from wood pulp. Suitable wood pulp can be obtained from any of the chemical processes known by those of ordinary skill in the art such as Kraft, and sulfite processes. Preferred fibers are those obtained from various soft wood pulp such as Southern pine, White pine, Caribbean pine, Western hemlock, various spruces, (e.g. Sitka Spruce), Douglas fir or mixtures and combinations thereof.
• Fibers obtained from hardwood pulp sources such as gum, maple, oak, eucalyptus, poplar, beech, and aspen, or mixtures and combinations thereof can also be used in the present invention.
• Other ceUulose fibers derived form cotton linter, bagasse, kemp, flax, and grass may also be used in the present invention.
• the fiber can be comprised of a mixture of two or more of the foregoing cellulose pulp products.
• Particularly preferred "conventional" fibers for use in forming the cross- linked fibers of the present invention are those derived from wood pulp prepared by Kraft and sulfite-pulping processes.
• the fibers of the present invention preferably have a high surface purity of ceUulose, but it is not necessarUy required that the cellulosic fibers have a high ceUulose bulk purity. It is preferred that the ceUulosic fiber be cross- linked in the sheet form, and more preferably, be fiber with "high ceUulose purity.”
• the high ceUulose purity refers to the surface purity of the ceUulosic fibers. Throughout this description, the expression "high ceUulose purity” refers to pulp comprising at least about 65%, preferably at least 75%, and most preferably, at least about 90% -ceUulose.
• the preferred fibers in sheet form that are cross-linked in accordance with the present method are blends of conventional ceUulose and "mercerized fibers."
• the expression "mercerized fibers” denotes any of wood pulp fibers or fibers from any source described, previously treated with an aqueous solution of alkaH metal.
• Fiber mercerization can be carried out by any method known in the art such as those described in, for example, Cellulose and Cellulose Derivatives, Vol. V, Part 1, Ott, SpurHn, and Grafllin, eds., Interscience PubHsher (1954). Fiber mercerization can be performed by mixing pulp in an aqueous solution of alkaH metal (i.e. sodium hydroxide), washing, neutralizing, or washing and neutralizing, and optionaUy drying the pulp.
• alkaH metal i.e. sodium hydroxide
• Reagents suitable for mercerization include but are not Hmited to, alkaH metal hydroxides, such as sodium hydroxide, potassium hydroxide, calcium hydroxide, and rubidium hydroxide, Hthium hydroxide, and benzyltrim.ethylamm.oniurn hydroxide.
• Sodium hydroxide is a particularly preferred reagent for use in fiber mercerization in accordance with the present invention.
• the pulp of the invention preferably is treated with an aqueous solution containing from about 8 to about 30% by weight sodium hydroxide, more preferably from about 12 to about 20%, and most preferably 13% to about 16% .
• Mercerization may be performed during or after bleaching, purification, and drying.
• the cellulose fibers Preferably contain at least about 80% by weight ⁇ -ceUulose, preferably at least about 90% by weight, more preferably at least about 95% by weight, and even more preferably at least about 97% by weight ⁇ -ceUulose.
• CommerciaUy available caustic extractive pulp suitable for use in the present invention includes, for example, Porosanier-J- HP, avaUable from Rayonier Performance Fibers Division (Jesup, GA), and Buckeye's HPZ products, available from Buckeye Technologies (Perry, FL).
• the pulp fibers be in sheet or roU form.
• the sheet or roU form of ceUulose preferably is a blend of mercerized fiber and conventional fiber containing about 10% to about 60% by weight conventional fiber, more preferably from about 20% to about 60% by weight conventional fiber, and most preferably from about 30% to about 50% by weight conventional fiber, based on the total weight of the mixture of fibers.
• the fiber in another aspect of the invention, can be used in wet or dry state. It is preferred in the present invention that the ceUulosic fibers be employed in the dry state.
• Cross-linking agents suitable for use in the present invention are polyfunctional molecules.
• polyfunctional molecule refers to a polymeric or monomeric molecule able to form a bridge between adjacent ceUulose chains. Accordingly, any material capable of reacting with more than one hydroxyl group of ceUulose chains can be suitable for use in the present invention.
• Particularly suitable cross-linking agents for use in the present invention are those carrying functional groups such as, for example, carboxyl, aldehyde and epoxy.
• the cross- Hnking agents include dialdehydes, acid aldehydes, polycarboxyHc acids, and polyepoxides.
• Cross-Hnking agents preferred for use in the present invention include acid aldehydes.
• acid aldehyde refers to organic molecules having carboxyHc acid and aldehyde functional groups, such as, for example, glyoxyHc acid and succinic semialdehyde.
• a particularly preferred acid aldehyde cross-Hnking agent is glyoxyHc acid.
• suitable cross-linking agents include polycarboxylic acids.
• EspeciaUy suitable polycarboxyHc acids are those having at least two carboxyl groups, such as, 1,2,3,4-butanetetracarbocyHc acid, 1,2,3-propanetricarboxylic acid, oxydisuccinic acid, citric acid, itaconic acid, maleic acid, tartaric acid, glutaric acid.
• Particularly preferred polycarboxyHc acids are 1,2,3,4- butanetetracarbocyHc acid and citric acid.
• polycarboxyHc acids include polymeric polycarboxyHc acids such as those speciaUy prepared from monomers such as, for example, acrylic acid, vinyl acetate, maleic acid, maleic anhydride, carboxy ethyl acrylate, itanoic acid, fumaric acid, methacryUc acid, crotonic acid, aconitic acid, acryHc acid ester, methacryUc acid ester, acryHc amide, and methacryHc amide, butadiene, styrene, or combinations thereof.
• polymeric polycarboxyHc acids such as those speciaUy prepared from monomers such as, for example, acrylic acid, vinyl acetate, maleic acid, maleic anhydride, carboxy ethyl acrylate, itanoic acid, fumaric acid, methacryUc acid, crotonic acid, aconitic acid, acryHc acid ester, me
• CommerciaUy available examples of these polymers and co-polymers include polyacryHc acid, polymaleic acid, polyitaconic acid, polyaspartic acid, polymethacryHc acid, poly(acryHc acid-co-maleic acid), poly(acrylamide-co-acryHc acid), poly(etheylene-co-acryHc acid), and poly(styrene-co-maleic acid).
• Particularly preferred polycarboxyHc acids are polymaleic acid, polyacryHc acid, and a co-polymer of acryHc acid and maleic acid.
• cross-Hnking agents suitable for use in the present invention include polyepoxides, particularly those containing hydrophobic saturated, unsaturated, branched and un-branched alkyls. Examples of these include 1,4-cyclohexanedimethanol diglycidyl ether, diglycidyl 1,2- cyclohexanedicrboxylate, N,N-diglycidylar ⁇ line, N,N-diglcidyl-4- glycidyloxyaniline, and diglycidyl 1,2,3,4-tetrahydrophthalate and glycerol propoxylate triglycidyl ether.
• a particularly preferred polyepoxide is 1,4- cyclohexanedimethanol diglycidyl ether.
• a mixture or combination of cross-Hnking agents may be used.
• the present invention provides chemicaUy cross-linked fibers in sheet form, that are cross-Hnked with a blend of cross-Hnking agents including those described above.
• the cross-linking agent may be appHed to the ceUulose fiber in an aqueous solution.
• the aqueous solution has a pH of from about 1 to about 5, more preferably from about 2 to about 3.
• the present inventors have discovered that an aqueous solution of acid aldehyde cross-Hnking agent can be used as is without any adjacent or additional pH control agent.
• a water insoluble cross-linking agent e.g. polyexpoxide
• a minor amount of surfactant e.g., a few drops — less than 1% by weight
• the cross-Hnking agent may then be appHed to the fiber as a dispersion, instead of an aqueous solution.
• any type of surfactant capable of forming a dispersion with the water insoluble cross-Hnking agent can be used.
• Suitable surfactants include nonionic, anionic, or cationic surfactant or mixtures and combinations of surfactants that are compatible with each other.
• the surfactant is selected from Triton X-100 (Rohm and Haas), Triton X-405 (Rohm and Haas), sodium lauryl sulf ate, and lauryl bromoethyl ammonium chloride, ethoxylated nonylphenols, polyoxyethylene alkyl ethers, polyoxyethylene alkyl ethers, and polyoxyethylene fatty acid esters.
• the ceUulosic fiber preferably is treated with an effective amount of cross- linking agent to achieve the absorbent properties and physical characteristics described herein.
• the concentration of the cross-Hnking agent in aqueous solution is sufficient to provide from about 0.5 to 10.0 weight percent cross-Hnking agent on fiber, more preferably from about 1 to 6 weight percent, and most preferably from about 2 to 5 weight percent.
• the method of forming the ceUulosic fiber in accordance with the invention includes a catalyst to accelerate the formation of an ester linkage between the hydroxyl groups of the ceUulose and the carboxyl groups of the polycarboxyHc acid and acid aldehyde cross-Hnking agents.
• a catalyst also may be used to accelerate the formation of acetal cross-links between hydroxyl groups of ceUulose and aldehyde functional groups of acid aldehyde cross-Hnking agents.
• a catalyst is not required.
• any catalyst known in the art that is capable of accelerating the formation of an ester cross-link between a hydroxyl group and an acid group, or capable of accelerating the formation of an acetal cross-link between a hydroxyl group of ceUulose and an aldehyde group could be used in the present invention.
• Suitable catalysts for use in the present invention to accelerate the formation of ester cross-links include alkali metal salts of phosphorous containing acids such as alkali metal hypophosphites, alkali metal phosphites, alkaH metal polyphosphonates, alkali metal phosphates, and alkaH metal sulfonates.
• a particularly preferred catalyst of this type is sodium hypophosphite.
• Suitable catalysts for use in the present invention to accelerate the formation of acetal cross-links are Lewis acids consisting of a metal and a halogen, such as for example FeCk, AICI3, and MgCl 2 .
• a catalyst may also be used to promote the reaction between polyepoxides and ceUulose hydroxyl groups, to the extent a ciOss-linking agent containing polyepoxide groups is used as a cross-Hnking agent.
• Any catalyst known in the art to accelerate the formation of an ether bond or linkage between the hydroxyl groups of ceUulose and an epoxide group can be used in the present invention.
• the catalyst is a Lewis acid selected from aluminum sulfate, magnesium sulfate, and any Lewis acid consisting of a metal and a halogen, including, for example FeCk, AICI3, and MgCk.
• the catalyst can be appHed to the fiber as a mixture with the cross-Hnking agent, before the addition of the cross-Hnking agent, or after the addition of cross- Hnking agent to ceUulosic fiber.
• the ratio of catalyst to cross- linking agent is, for example, from about 1:2 to 1:10, more preferably from about 1:4 to 1:8.
• finishing agents such as water repeUent, softening, and wetting agents also can be used to treat the ceUulosic fiber.
• softening agents include fatty alcohols, fatty acids amides, polyglycol ethers, fatty alcohols sulfonates, and N-stearyl-urea compounds.
• wetting agents include fatty amines, salts of alkylnaphthalenesulfonic acids, alkaH metal salts of dioctyl sulf osuccinate, and the like.
• any method of applying the cross-Hnking agent(s) to the fiber can be used in carrying out the cross-linking method of the invention.
• Acceptable methods include, for example, spraying, dipping, impregnation, and the like.
• the fiber is impregnated with an aqueous solution of cross- Unking agent. Impregnation usuaUy creates a uniform distribution of cross- Hnking agent on the sheet and provides a better penetration of cross-linking agent into the interior part of the fiber.
• a sheet including a blend of mercerized and conventional fibers in roll form is conveyed through a treatment zone where a cross-linkmg agent(s) is appHed on both surfaces by conventional methods such as spraying, roUing, dipping, knife-coating or other manners of impregnation.
• a preferred method of applying the aqueous solution of the cross-linking agent(s) to fiber in roU form is by puddle press, size press, and blade coater.
• a blend of fibers in sheet or roU form after having been treated with a solution of cross-Hnking agent then preferably is transported by a conveying device such as a belt or a series of driven roUers through a two-zone oven for drying and curing.
• Fibers in roll or sheet form after treatment with the cross-Hnking agent preferably are dried and cured in a two stage process, and even more preferably dried and cured in a one stage process. Such drying and curing removes water from the fiber, thereupon beHeved to induce the formation of an ester and an ether linkage between hydroxyl groups of fiber and cross- linkmg agent(s).
• Curing usuaUy is carried out in a forced draft oven preferably from about 300 °F to about 450 °F, and more preferably from about 320 °F to about 430 °F, and most preferably from about 350 °F to about 420 °F.
• Curing preferably is carried out for a certain period of time that permits complete fiber drying and efficient cross-linking. It is preferred that the ceUulosic fiber is cured for a period of time ranging from about 5 min to about 25 min, and more preferably from about 7 min to about 20 min, most preferably from about 10 min to about 15 min.
• the blend of ceUulosic fibers cross-Hnked in accordance with the present invention can be characterized as having an absorbent capacity within the range of about 7.0 g/g to about 12.0 g/g.
• the fibers Preferably, the fibers have an absorbent capacity of at least 8.0 g/g, more preferably at least 9.0 g/g, even more preferably at least 10.0 g/g or higher.
• the cross-linked ceUulosic fibers can have a centrifuge retention as determined by the Hanging CeU Test method within the range of about 0.4 g/g to about 0.6 g/g.
• the fibers have a centrifuge retention of less than about 0.6 g/g, more preferably less than about 0.55 g/g, and most preferably less than about 0.5 g/g.
• the ceUulosic fibers cross-Hnked in accordance with the present invention preferably possess characteristics that are deshable in absorbent articles.
• the cross-linked ceUulosic fibers preferably have a centrifuge retention capacity of less than about 0.6 grams of synthetic saline per gram of fiber (hereinafter "g/g")-
• the chemicaUy cross-Hnked ceUulose fibers also have desirable properties, such as a free sweU of greater than about 10 g/g, an absorbent capacity of greater than about 8.0 g/g, an absorbency under load of greater than about 8.0 g/g, less than about 10% of knots, less than about 6.5% of fines, and an acquisition rate upon the third insult (or third insult strike-through) of less than about 13.0 seconds.
• the particular characteristics of the cross-Hnked ceUulosic fibers of the invention are determined in accordance with the procedures described in more detaU in the examples.
• the centrifuge retention capacity measures the abiHty of the fiber to retain fluid against a centrifugal force. It is preferred that the blend of fibers of the invention have a centrifuge retention capacity of less than about 0.6 g/g, when cross-Hnked with any cross-Hnking agent, more preferably, less than about 0.55 g/g, even more preferably less than 0.5 g/g.
• the cross-linked ceUulosic fibers of the present invention can have a centrifuge retention capacity as low as about 0.40 g/g.
• the fibers of the invention have a centrifuge retention capacity of less than about 0.60 g/g when cross-Hnked with an acid aldehyde cross-Hnking agent, more preferably, less than about 0.55 g/g, even more preferably less than 0.50 g/g, and most preferably less than about 0.45 g/g.
• the fibers of the invention have an absorbent capacity of more than about 8.0 g/g, more preferably, greater than about 8.5 g/g, even more preferably greater than about 9.0 g/g, and most preferably greater than about 10.0 g/g.
• the absorbency under load measures the abUity of the fiber to absorb fluid against a restraining or confining force of 0.3 psi over a given period of time. It is preferred that the blend of fibers of the invention have an absorbency under load of greater than about 7.0 g/g, more preferably, greater than about 7.5 g/g, and most preferably, greater than about 8.0 g/g.
• the third insult strikethrough measures the abiHty of the fiber to acquire fluid, and is measured in terms of seconds. It is preferred that the fibers of the invention have a third insult strike-through of less than about 15.0 seconds, more preferably, less than about 14 seconds, even more preferably less than 13 seconds, and most preferably less than about 12 seconds.
• the cross-Hnked fibers of the present invention preferably have less than about 10% of knots, more preferably less than about 8% knots, and most preferably, less than about 5% knots.
• the cross-Hnked fibers of the present invention also preferably have less than about 8.0% of fines, preferably less than about 7.0% fines, and most preferably, less than about 6.0% fines.
• Fibers cross-linked in sheet form have typicaUy been expected to have an increased potential for inter-fiber cross-linking which leads to "knots" and "nits” resulting in poor performance in some appHcations.
• the "knot” content increases substantiaUy, indicating increased deleterious inter-fiber bonding. Examination of these "knots” recovered by classification showed they contained true “nits” (hard fiber bundles).
• a blend of mercerized pulp and conventional pulp cross-Hnked in sheet or roU form actuaUy yields fewer knots and nits than control pulps having conventional ceUulose purity cross-Hnked under the same conditions.
• a blend of fibers in sheet or roll form that were cross-Hnked in accordance with the present invention were found to contain fewer knots than commercial individuahzed cross-Hnked ceUulose fibers, like those produced by the Weyerhaeuser Company, commonly referred to as HBA (for high-bulk additive), and by The Proctor & Gamble Company (“P&G").
• knots to a certain level in the cross-linked fiber of the present invention enhances the performance of the cross-Hnked fiber when used as an acquisition layer in hygiene products.
• the knots present in the cross-linked fiber are within the range of 2% to 15%, more preferably from 3% to 12%, and most preferably from 5% to 10% .
• ceUulose fibers cross-Hnked in sheet form in accordance with the present invention enjoy equal performance characteristics to conventional individualized cross-linked ceUulose fibers, but avoid the processing problems associated with dusty individuahzed cross-Hnked fibers.
• the cross-Hnked fibers of the present invention are twisted and curled.
• the photographs show a mixture of round, circular- shaped fibers and flat, ribbon-like fibers.
• the round, circular-shaped fibers represent the mercerized fibers while the flat, ribbon-like fibers represent the conventional fiber Rayfloc ® -J-LD.
• Cross-Hnked ceUulosic fibers prepared in accordance with the present invention can be utilized, for example, as a bulking material in the manufacture of high bulk specialty fiber appHcations that require good absorbency and porosity.
• the cross-Hnked fibers can be used, for example, in non-woven, fluff absorbent appHcations.
• the fibers can be used independently, or preferably can be incorporated with other ceUulosic fibers to form blends using conventional techniques, such as air laying.
• the cross-Hnked fibers of the present invention either alone or blended with other fibers, are blown onto a forming screen.
• a wet laid process may also be used, combining the cross-Hnked fibers of the invention with other ceUulosic fibers to form sheets or webs of blends.
• the cross-Hnked fibers of the present invention can be incorporated into various absorbent articles intended for body waste management such as adult incontinent pads, feminine care products, and infant diapers.
• the cross-Hnked fibers can be used in an acquisition layer in the absorbent articles.
• the cross-Hnked fibers also can be utilized in the absorbent core of the absorbent articles.
• Towels, wipes and other absorbent products such as filters also may be made with the cross-Hnked fibers of the present invention.
• an additional feature of the present invention is to provide an absorbent core and an absorbent article that includes the chemically cross- Hnked fibers of the present invention.
• absorbent cores typicaUy are prepared using fluff pulp to wick the Hquid, and an absorbent polymer (oftentimes a superabsorbent polymer ("SAP")) to store Hquid.
• SAP superabsorbent polymer
• the cross-linked blend of fibers of the present invention have high resiHency and high free sweU capacity.
• the blend of cross-Hnked fibers are highly porous.
• the cross-Hnked fibers of the present invention can be used in combination with the SAP to make an absorbent composite (or core) having improved porosity, bulk, resiHency, wicking, softness, absorbent capacity, absorbency under load, low third insult strikethrough, low centrifuge retention capacity, and the like.
• the absorbent composite could be used as an absorbent core in absorbent articles intended for body waste management.
• the cross-Hnked fibers be present in the absorbent composite in an amount ranging from about 10% to about 80% by weight, based on the total weight of the composite. More preferably, the cross-linked fibers are present in an amount ranging from about 20% to about 60% by weight.
• a mixture of ceUulosic fibers and cross-linked fibers of the present invention along with the SAP may also be used to make the absorbent composite.
• the cross-Hnked fibers of the present invention are present in the mixture in an amount ranging from about 1% to about 70% by weight, based on the total weight of the fiber mixture, and more preferably present in an amount from about 10% to about 40% by weight.
• Suitable additional conventional ceUulosic fibers include any of the wood fibers mentioned previously, cold caustic treated fibers, conventional fibers, mercerized fibers and mixtures and combinations thereof.
• Any suitable superabsorbent polymer, or other absorbent material can be used, to form the absorbent composite.
• the SAP can be in the form of, for example, fiber, flakes, or granules capable of absorbing several times its weight of saline (0.9% solution of NaCl in water) and/ or blood.
• the SAP also preferably is capable of retaining the Hquid when it is subjected to load.
• Non-Hmiting examples of superabsorbent polymers applicable for use in the present invention include any SAP presently avaUable on the market, including, but not Hmited to, polyacrylate polymers, starch graft copolymers, ceUulose graft copolymers, and cross-Hnked carboxymethylceUulose derivatives, and mixtures and combinations thereof.
• An absorbent composite made in accordance with the present invention preferably contains superabsorbent polymer in an amount from about 20% to about 60% by weight, based on the total weight of the composite, and more preferably from about 30% to about 60% by weight.
• the SAP may be distributed throughout an absorbent composite within the voids in the cross- linked fiber or the mixture of cross-linked fibers and ceUulosic fibers.
• the SAP is attached to the fiber via a binding agent that includes, for example, a material capable of cross-linking the SAP to the fiber via hydrogen bonding (see, for example, U.S. Patent No. 5,614,570, the disclosure of which is incorporated by reference herein in its entirety).
• a method of making an absorbent composite of the present invention may include forming a pad comprising cross-linked fibers or a mixture of cross- Hnked fibers and ceUulosic fibers and incorporating particles of superabsorbent polymer in the pad.
• the pad can be wet laid or airlaid, preferably the pad is airlaid. It also is preferred that the superabsorbent polymer and cross-Hnked fibers, or mixture of cross-linked fibers and ceUulosic fibers, are air laid together.
• Absorbent cores containing cross-Hnked fibers and superabsorbent polymer preferably have dry densities ranging from about 0.1 g/cm 3 to 0.50 g/cm 3 and more preferably from about 0.2 g/cm 3 to 0.4 g/cm 3 .
• the absorbent core can be incorporated into a variety of absorbent articles intended for body waste management, such as diapers, training pants, adult incontinence, ferriinine care products, and toweling (e.g. wet and dry wipes).
• the invention wiU be iUustrated but not limited by the foUowing examples.
• aU percentages are by weight and aU temperatures in degrees Celsius, unless otherwise noted. Also, when referring to pulp weight, the measurement includes equihbrium moisture content. When subjected to testing, aU fiber contains about 5% to 7% moisture.
• the absorbency test method was used to determine the absorbency under load, absorbent capacity, and centrifuge retention capacity of the cross- Hnked fibers of the present invention.
• the absorbency test was carried out in a one inch inside diameter plastic cylinder having a 100-mesh metal screen adhering to the cylinder bottom "ceU," containing a plastic spacer disk having a 0.995 inch diameter and a weight of about 4.4 g.
• the weight of the ceU containing the spacer disk was determined to the nearest 0.0001 g, and then the spacer was removed from the cylinder and about 0.35 g of cross-linked fibers having a moisture content within the range of from about 4% to about 8% by weight were air-laid into the cylinder.
• the spacer disk then was inserted back into the cylinder on the fiber, and the cylinder group was weighed to the nearest 0.0001 g.
• the fiber in the ceU was compressed with a load of 4 psi for 60 seconds, the load then was removed and the fiber pad was aUowed to equiHbrate for 60 seconds.
• the pad thickness was measured, and the result was used to calculate the dry bulk of the cross-Hnked fiber.
• the ceU was aUowed to stand in the Petri dish for 10 minutes, and then it was removed and hung in another empty Petri dish and aUowed to drip for 30 seconds. Wrule the pad stiU was under the load, its thickness was measured.
• the absorbent capacity of the cross-Hnked fiber was determined in the same manner as the test used to determine absorbency under load above, except that this experiment was carried out under a load of 0.01 psi. The results are used to determine the weight of the saline solution absorbed per gram fiber and expressed as the absorbent capacity (g/g).
• Op Test Fiber QuaHty Analyzer is an optical instrument that has the capabiHty of measuring the average fiber length, kink, curl, and fines content.
• Fluff Fiberization Measuring Instrument is used to measure nits and fine contents of fiber.
• a sample of fiber in fluff form was continuously dispersed in an air stream.
• loose fibers passed through a 16 mesh screen (1.18 mm) and then through a 42 mesh (0.36 mm) screen.
• Pulp bundles (knots) which remained in the dispersion chamber and those that were trapped on the 42-mesh screen were removed and weighed. The former are caUed "knots" and the latter "accepts.” The combined weight of these two was subtracted from the original weight to determine the weight of fibers that passed through the 0.36 mm screen. These fibers were referred to as "fines.”
• This example iUustrates a method for making mercerized fibers and a method for forming handsheets from a blend of mercerized and Rayfloc ® -J- LD fibers.
• Fiber mercerization was carried out as follows: A sample of Rayfloc ® -J-LD
• Rayfloc ® -J-LD is an untreated southern pine Kraft pulp CommerciaUy avaUable from Rayonier Performance Fibers Division, Jesup, GA.
• a 70.0 g (dry weight base) sample of Rayfloc ® -J-LD was treated with an aqueous solution of 16% (w/w) sodium hydroxide at room temperature at a consistency of about 3.5%. The mixture was agitated for about 10 min, then excess NaOH was removed by suction fUtration or centrifuge. The resulting mercerized pulp then was washed with excess water, neutraHzed to a pH of 6.4 with acetic acid solution (0.01 M) at a consistency of about 3.5%, and optionaUy sheeted and dried.
• Handsheets of blends of fibers then were formed by thoroughly agitating a slurry of Rayfloc ® -J-LD and mercerized fiber in water at consistency of about 3% for about 10 min.
• the blend of fibers then was formed into sheets on a standard 12X12 inch laboratory sheet mold.
• the wet sheets were optionaUy dried.
• the formed sheets had approximately the same basis weight (762 gsm) and had a density in the range of 3.2 to 4.6 g/cm 3 .
• Example 2 This example iUustrates a method for cross-Hnking a blend of fibers in the sheet form prepared in the manner described above in example 1.
• sheets with various proportions of Rayfloc ® -J-LD and mercerized fibers were prepared as described in example 1 and used in this example. Sheets were soaked in a bath of 2% solution of glyoxyHc acid (obtained as 50% solution in water CommerciaUy avaUable from Clarinet Corporation, Charlotte, NC) for about 1 to 2 min and then pressed to a pick-up that affords about 2% of glyoxyHc acid on fiber. Sheets then were dried and cured in one step process at 190°C for 15 min.
• glyoxyHc acid obtained as 50% solution in water CommerciaUy avaUable from Clarinet Corporation, Charlotte, NC
• Example 3 This example iUustrates a method for cross-linking a blend of fibers in sheet form using DP-60 as a cross-Hnking agent
• Belclene ® DP-60 is a mixture of polymaleic acid terpolymer with the maleic acid monomeric unit predominating (molecular weight of about 1000) and citric acid commerciaUy avaUable from BioLab Industrial Water Additives Division).
• Sheets with various proportions of Rayfloc ® -J-LD and mercerized fibers were prepared as described above in Example 1, and then were soaked in a bath of DP-60 solution (5%) for about 1 to 2 min and then pressed to a pick-up that affords about 5% of DP-60 on fibers. Sheets were then dried and cured in a one step process at 190 °C for about 15 min.
• Porosanier-J-HP 70% by weight (mercerized fiber available from Rayonier Performance Fibers Division (Jesup, GA)) and Rayfloc ® -J-LD 30% by weight.
• Cross-Hnking was carried out using glyoxyHc acid in the presence and in the absence of a catalyst. Sheets were soaked in a bath of an aqueous solution of glyoxyHc acid (2%) and magnesium chloride hexahydrate (0.25%) for about 1 to 2 min and then pressed to a pick-up that affords about 2% of glyoxyHc acid and 0.25% of magnesium chloride hexahydrate on fiber. [0099] Sheets after treatment were dried in a 50°C oven to about 5 to 7% moisture contents then cured at various temperatures for about 5 min. The above experiment was repeated without a catalyst.
• This example iUustrates the effect of curing time on absorbent properties of representative cross-Hnked fibers formed in accordance with the present invention.
• This example iUustrates the effect of using various amounts of cross-Hnking agent on absorbent properties of produced fibers.
• Sheets used in this experiment were formed as described above in example 1 using 70% by weight Porosanier-J-HP and 30% by weight Rayfloc ® -J-LD. Fiber treatment was carried out as shown in Example 2 except that in this example various amounts of cross-Hnking agents were used. GlyoxyHc acid was used as a cross-Hnking agent in the presence of a constant amount of the catalyst magnesium chloride hexahydrate (0.25%). Treated sheets were dried at 50°C then cured at 150 °C for 5 min. The results are summarized below in Table 6.
• Example 7 This example iUustrates the effect of using varying amounts of catalyst on the absorbent properties of cross-linked fiber.
• the sheets used in this example were prepared as described in example 1 using 70% Porosanier-J- HP by weight and 30% Rayfloc ® -J-LD by weight.
• Fiber treatment was carried out as described above in Example 2 except that in this example, glyoxyHc acid (2%) was used as a cross-Hnking agent in the presence of various amounts of magnesium chloride hexahydrate. Treated sheets were dried at 50°C, and then cured at 150°C for 5 min.
• This example iUustrates an airlaid method for forming a representative absorbent structure of the present invention.
• An airlaid absorbent core formed in accordance with the present invention was prepared using an airlaid apparatus known to experts in the art. Fiber (Rayfloc ® -J-LD) and superabsorbent particles (P-02-055-01 obtained from BASF), were loaded into the airlaying apparatus. Vacuum then was appHed, fibers and superabsorbent particles traveled through plastic tubing and were combined through an air vortex into a plastic cylinder having a 100-mesh metal screen adhering to the cylinder bottom. After fibers and superabsorbent particles were completely combined, the vacuum was discontinued and the resulting pad was removed from the cylinder. The pad was then compressed by a hydraulic press to a pressure of 700 PSI for 3 min.
• This example iUustrate the acquisition times of cross-Hnked fibers made in accordance with the present invention.
• the acquisition time was determined by the SART test method.
• the test evaluates the performance of cross-linked fibers as an acquisition layer in absorbent article.
• the test measures the time required for a dose of saline to be absorbed completely into the absorbent article.
• the test is conducted on a sample of absorbent core made in accordance with the method described in example 8.
• the core included about 45% by weight fiber (Rayfloc ® -J-LD) and 55 % by weight superabsorbent particles (P-02-055-01 obtained from BASF) based on the total weight of the core.
• the core had a circular shape with a diameter of 60.0 mm, a density of 0.2, and weighed about 3.0 g ( ⁇ 0.1 g).
• a sample of cross-linked fibers made in accordance with the present invention was airlaid into a 60.0 mm pad.
• the pad weighed about 0.7 g and was compressed with a load of a 7.6 PSI for 60 seconds before being tested.
• the core was placed into the testing ceU, which consisted of a plastic base and a funnel cup.
• the base used to hold the sample was a plastic cy Under with an inside diameter of 60.0 mm.
• the funnel cup was a plastic cylinder with a star shape hole, the outside diameter of the funnel cup was 58 mm.
• the funnel cup was placed inside the plastic base on top of the sample and a load of 0.6 PSI having a donut shape was placed on top of the funnel cup.
• blends of the invention therefore preferably are useful in absorbent articles as an acquisition layer and/ or an absorbent core.

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