Classifications

• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
  • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
  • D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
  • D06M11/09—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with free halogens or interhalogen compounds
• • A—HUMAN NECESSITIES
  • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
  • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
  • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
  • A01N25/32—Ingredients for reducing the noxious effect of the active substances to organisms other than pests, e.g. toxicity reducing compositions, self-destructing compositions
• • A—HUMAN NECESSITIES
  • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
  • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
  • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
  • A01N25/34—Shaped forms, e.g. sheets, not provided for in any other sub-group of this main group
• • A—HUMAN NECESSITIES
  • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
  • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
  • A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
  • A01N59/12—Iodine, e.g. iodophors; Compounds thereof
• • 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
  • A61L15/18—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing inorganic materials
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
  • A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
  • A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
  • A61L15/42—Use of materials characterised by their function or physical properties
  • A61L15/46—Deodorants or malodour counteractants, e.g. to inhibit the formation of ammonia or bacteria
• • 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
  • A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
  • A61L31/14—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
  • A61L31/16—Biologically active materials, e.g. therapeutic substances
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
  • C08K3/00—Use of inorganic substances as compounding ingredients
  • C08K3/02—Elements
• • D—TEXTILES; PAPER
  • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
  • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
  • D01F1/00—General methods for the manufacture of artificial filaments or the like
  • D01F1/02—Addition of substances to the spinning solution or to the melt
  • D01F1/10—Other agents for modifying properties
  • D01F1/103—Agents inhibiting growth of microorganisms
• • A—HUMAN NECESSITIES
  • A41—WEARING APPAREL
  • A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
  • A41D31/00—Materials specially adapted for outerwear
  • A41D31/04—Materials specially adapted for outerwear characterised by special function or use
  • A41D31/30—Antimicrobial, e.g. antibacterial
• • 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
  • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
  • A61L2300/20—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials
  • A61L2300/202—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials with halogen atoms, e.g. triclosan, povidone-iodine
• • 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
  • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
  • A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
  • A61L2300/404—Biocides, antimicrobial agents, antiseptic agents

Definitions

• This invention relates to anti-microbial, especially germicidal fibers, fabrics and articles of manufacture, especially those based on alloy fibers, such as for example, rayon-polyvinylpyrrolidone.
• An object of this invention is to provide improved fibers and fabrics having an anti-microbial activity, especially having a disinfectant activity against micro-organisms, particularly against pathogenic bacteria. Another object is to provide anti-microbicidal, especially germicidal articles of manufacture made from these fabrics.
• Still another object is to provide a method of effecting anti-microbial especially germicidal activity with the fibers, fabrics thereof, or articles of manufacture thereof.
• the alloy fiber consists essentially of a fiber-forming component and an alloying component capable of complexing an anti-microbial agent, especially a germicidal agent, e.g., iodine to a different degree of stability than the fiber-forming component.
• the fiber-forming component of the alloy fiber comprises regenerated cellulose, cellulose acetate, acrylonitrile copolymers, vinyl chloride copolymers and cross-linked algini ⁇ acid.
• rayon defined as a fiber composed of regenerated cellulose in which substituents have replaced not more than 15% of the hydrogens of the hydroxyl groups
• Viscose rayon produced from the viscose process is the preferred cellulose fiber-forming process of this invention. All other rayon processes are also contemplated, e.g., the cuproammonium process, the New Cell process, a solvent system based on liquid ammonia and thiocyanate salts, and others as reported in the literature. Proceedings of the Technical Association of the Pulp and Paper Industry, 1983 International Dissolving and Specialty Pulp Conference, Tappi Press, Atlanta, Georgia, Paper No.
• Iodophor alloy fibers of this invention containing regenerated cellulose as the base fiber-forming component are preferred because of their hydrophilic properties, ease of processability, and other beneficial characteristics.
• cellulose acetate is the fiber forming polymer
• acetate fibers which are defined as a fiber composed of cellulose acetate where less than 92% but at least 74% of the hydroxyl groups are acetylated, or triacetate fibers, which are defined as a fiber composed of cellulose acetate, where at least 92% of the hydroxylgroups are acetylated, is formed.
• Iodophor alloy fibers of this invention containing cellulose acetate as the base fiber-forming polymer are preferred in uses requiring dry cleaning.
• acrylic fibers defined as fibers in which the fiber-forming substance is any long chain synthetic polymer composed of at least 85% by weight of acrylonitrile units
• Modacrylic fibers defined as fibers made from a synthetic linear polymer that comprises less than 85%, but at least 35% by weight of acryl-onitrile units.
• Iodophor alloy fibers of this invention containing acrylonitrile copolymers as the base fiber-forming polymers are preferred by themselves or in blends with rayon to form blankets and the like.
• Vinyon fibers defined as fibers in which the fiber-forming substance is any long chain synthetic polymer composed of at least 85% by weight of vinyl chloride units, are formed.
• Iodophor alloy fibers of this invention containing vinyl chloride copolymers as the base fiber-forming polymer are preferred where there are used nonwoven textiles bonded by a thermal process, utilizing the relatively low softening point of the vinyl chloride copolymer to hold the fibers together in a fabric form.
• cross-linked alginic acid alginate fibers are formed. It is intended to include thereby, alginic acid cross linked by a polyfunctional agent, preferably a polyvalent metal or amine, especially calcium ion.
• All of the iodophor alloy fibers of this invention can be used in textile fabrics or in other shaped objects, either alone, or in blends with each other, or In blends with unalloyed fibers. All iodophor alloy fibers of this invention may be .either in staple fiber or in filament yarn form.
• the above-described alloy fibers of this invention are formed by mixing a solution of the base fiber-forming polymer with a compatible solution of the alloying polymer or copolymer.
• the solution can be aqueous or nonaqueous, depending on the base fiber-forming polymer.
• the present invention also contemplates the formation of melt-spun alloy fibers.
• the fiber-forming component and the alloying component must be sufficiently compatible and stable to form fibers by melt spinning.
• An example of such a system is a polyester or polyolefin fiber-forming component and a polyamide alloying component.
• Another example is a melt system of polypropylene and polyvinyl pyrrolidone; likewise polypropylene and polyethylene glycol (carbonwax 1540 or Polyox WSR 10) yield compatible meltspinnable systems, the resulting fibers forming iodophorswith iodine.
• the alloying component capable of complexing iodine it is preferred to utilize an alloying component capable of complexing iodine more firmly than the fiber-forming component.
• an alloying component capable of complexing iodine it is preferred to utilize either a polyvinylpyrrolidinone or a starch.
• polyvinylpyrrolidinone also called polyvinylpyrrolidone or poly-N-vinylpyrrolidinone
• the comonomer is any one or more of the following: vinyl acetate, vinyl propionate, styrene, alkyl vinyl ethers, alkyl acrylates or methacrylates, acrylic or methacryli ⁇ acid, acrylonitrile or methacrylonitrile, hydroxylethyl or hydroxypropyl acrylate or methacrylate, polyethoxy or polypropoxy or polyethoxypropyl acrylate or methacrylate, acrylamide or methacrylamide, N-alkyl or dialkyl acrylamide or methacrylamide, maleic acid or itaconic acid or their half or full esters or amides, allyl ethers, N-alkylaminoalkyl acrylate or me
• copolymers or modified polymers of vinyl pyrrolidone can be made with either partially or completely alkylated polyvinylpyrrolidone, e.g., Ganex V216.
• Especially preferred copolymers are 60:40 molar ratios of vinylpyrrolidinone and vinyl acetate, sold as GAF PVP/VA S-630, vinyl pyrrolidinone and dimethylaminoethyl methacrylate (sold as Gafquat series by GAF), and vinyl pyrrolidinone and styrene sold as Polectron series by GAF.
• starch By a starch is meant besides a conventional starch (ordinary cornstarch contains about 30% amylose and 70% amylopectin), high amylose starches such as Hylon VII containing 70% amylose and 30% amylopectin. Additional starches include but are not limited to dextrins, cationic starch, and amphoteric starch.
• the use of starch yields an iodophor more resistant to iodine extraction with carbon tetrachloride than the use of polyvinylpyrrolidone, all other conditions being equal.
• Such reversible iodine absorbers include but are not limited to polyacrylonitrile, polyethylene oxide of, e.g., a molecular weight of about 20,000, polyvinyl alcohol, polyvinyl acetate, partially hydrolyzed polyvinyl acetate copolymers of vinyl acetate and vinyl propionate, h ⁇ mopolymers and copolymers of alkyl and hydroxyalkyl acrylates and methacrylates, and polyamides wherein the alkyl is preferably of about 1-18 carbon atoms and the hydroxalkyl is preferably 2-3 carbon atoms, the polyamides including natural, e.g., albumin, and synthetic, e.g., nylon and polyacrylamide substances, all of these being found in the literature.
• Other alloying polymers found to be satisfactory include cationic polyamine Diamond Shamrock Product C, polyamide epichlorohydrin
• Patent 3,455,713 preferably a mixture of octapropoxytetracyclophosphazine and hexapropoxyphosphazine. It also appears that the binder used in a non-woven fabric, e.g., Rhoplex (copolymers of acrylic and methacrylic esters) or Vinyon by itself functions, to some extent, as an iodophor forming complexing agent when treated with iodine.
• Rhoplex copolymers of acrylic and methacrylic esters
• Vinyon by itself functions, to some extent, as an iodophor forming complexing agent when treated with iodine.
• the rayon alloy fibers are prepared by conventional methods, e.g., adding the alloying component compound to the viscous spinning solution prior to it being spun into fiber.
• U.S. 3,377,412 the original patent for rayon containing polyvinylpyrrolidinone, 4,041,121 (Smith) a method of making high fluid-holding fiber mass from a polyvinylpyrrolidinone having certain molecular weights and K values, and to 4,144,079 Reissue 31380 (Smith) directed to rayon fibers made by spinning of viscose containing dissolved starch.
• the alloying component present in a minor amount in the germicidal fiber, is distributed substantially uniformly along the length thereof.
• the alloying component is distributed throughout the fiber and is not concentrated at the surface thereof. This means that the normal and desirable surface characteristics of the fiber-forming portion of the germicidal fiber predominate, as opposed to a discrete coating, for example, of an iodiphor on the surface of the textile fiber which in turn would, in all likelihood, mask the beneficial surface properties of the fiber-forming component.
• Iodization of the rayon alloy can be conducted after any of fiber formation, fabric formation, article formation, or laundering stages. Consequently the term "fiber" in the following discussion refers to all of these stages.
• the technique of iodization can be conducted in a variety of ways. For example, it is possible to impregnate the resultant dried spun alloy rayon fiber with an aqueous solution of iodine and potassium iodide in the usual proportions required to solubilize iodine in water. After the impregnation step, the fiber is washed with water, preferably cold water having a temperature less than 25°C, to remove free iodine not associated with the alloying component.
• Reaction conditions such as, for example, concentration of I 2 in the KI solution, content of alloying component and residence time are selected so as to provide the fiber with a desired amount of iodophor.
• concentration of I 2 in the KI solution, content of alloying component and residence time are selected so as to provide the fiber with a desired amount of iodophor.
• the desired pick up of iodine for any given fiber can be controlled by conducting a series of routine tests, using different residence times for example.
• Additional techniques for incorporating the iodine into the alloy fiber include but are not limited to impregnation with a non-aqueous solution of 12, e.g., a solution of I2 in alcohol, CCI4, CHCI3, or perchloroethylene, as well as by vapor phase I2. Additional details are set forth in Japanese Kokai Patent No. SHO 54[1979]-91572 and Japanese Kokai Patent No.
• a prefered method of iodine treatment is to use water as the carrier, rather than air, aqueous KI solution, or organic solvent. Even though iodine has a low solubility in water, the concentration per unit volume is much greater than it is in air (0.336 g/1 of H 2 O at 25°C., compared with on the order of a milligram/1 of air).
• a fabric having only one half of a percent polyvinylpyrrolidone and as low as 0.3 milligram of iodine per gram of a total fiber provides a complete barrier to bacteria likely to cause infection in a hospital operating room, e.g., Staphylococcus aureus and others.
• the spin dope of the textile fiber is incorporated in the spin dope of the textile fiber.
• the solvent used for the spin dope is acetone, but other solvents can also be used. Any alloying component which is soluble or dispersible in the spin dope, and which is also capable of complexing iodine more firmly than cellulose acetate is contemplated by the present invention.
• alloying components include such diverse materials as Ganax V220 (an alkylated vinylpyrrolidone), copolymers of polyvinlypyrrolidinone and vinyl acetate having a molar ratio of 60:40 respectively a homopolymer of vinyl pyrrolidone, and Sandoflam.
• preferred alloying components include those useful for cellulose acetate, as well as other diverse materials such as, for example, polyvinylpyrrolidinone having a K value of 15.
• preferred alloying components include but are not limited to: polyvinylpyrrolidone K-15, Ganax V220, and polyvinylpyrrolidone/vinyl acetate S630. The iodization of the cellulose acetate, vinyon, or acrylic alloy fibers is conducted in the same manner as with rayon, as outlined above.
• the complexed iodine in any fiber, e.g., a starch alloyed rayon, can be substantially uniformly distributed therein e.g., the variation in concentration at any given section along the length of the fiber is not greater than 50% of the average concentration, preferably not more than 25% and, in particular, not more than 10%.
• the complexed iodine can be concentrated near the surface, e.g., at least 50% of the total iodine can be present in the outer 25% of the fiber cross-section.
• bromine will be complexed in substantially the same manner as iodine, especially into alloying components including but not limited to Ganax V216 and V220, PVP/VA S630 and PVP K-15. These components incorporated in rayon, cellulose acetate and Vinyon can be successfully brominated by immersion of the alloy fiber in bromine water. It is further contemplated that instead of bromine, other halogens and halogen compounds, such as, for example, chlorine, ICl, IBr, BrCl, ICI 3 and IBr 3 , can be complexed with an alloy fiber by the same methods employed for iodine. Such halogenated alloy fibers will also exhibit germicidal activity.
• halogenated alloy fabric preferably a chlorinated alloy fabric, e.g., containing at least about 10%, preferably about 20% polyvinyl pyrrolidone and substantially saturated with chlorine will oxidize certain deleterious air-borne compounds, e.g., those containing a phosphorus to oxygen or phosphorus to sulfur bond.
• the germicidal activity of the fibers of this invention is dependent on the environment in which they are employed. It is preferred that the complexed iodine be releasable, and in this case, the rate of release of iodine from the fiber is also a factor in the resultant degree of germicidal activity.
• the term "germicidal” is in accordance with its broad dictionary definition, i.e., synomonous to "microbicidal”. It is possible in this connection to employ a plurality of alloying components having different rates of release of the iodine, thereby yielding a predetermined desired continuous evolution of iodine.
• germicidal effectiveness of iodine is well known, reference being directed to the literature, for example the text "Disinfection, Sterilization, and Preservation", second edition, Seymour S. Block, Lea and Febiger, 1977, Phil., Pa. Chapter 11 "Iodine", Gershenfeld, pages 196-218, incorporated by reference herein.
• the germicidal activity includes bactericidal, fungicidal, viricidal, amebicidal, insecticidal, nematocidal and sporicidal activities.
• Example IV infra. The Barrier Test is likewise described in detail in Example VIII).
• fibers which are effective against at least one of the bacteria Staphylooccus aureus, Pseudomonas aeruginosa, Escherichia coli, and Proteus vulgaris. Fibers having disinfectant properties against the first two mentioned bacteria are particularly desirable, and those fibers which are disinfectant against all the mentioned bacteria are even more valuable in those areas where it is necessary to guard against infection. Even more valuable fibers are those which are not only a disinfectant against the aforementioned bacteria, but also against Streptoccus pyogenes.
• fibers have been found to be disinfectant not only against all of the mentioned bacteria, but also against the fungus Aspergillis niger which is indicative that most, if not all, fungi can be killed.
• fibers of the present invention will exhibit a wide spectrum of disinfectant activity, with the most valuable fibers being those which are disinfectant against all microorganisms against which iodine is germicidal.
• fibers embraced by the present invention and having a sufficiently high loading of releasable complexed iodine will exhibit the spectrum of germicidal activity as previously defined.
• the Kelsey-Sykes Test is not exclusive for the determination of germicidal activity inasmuch as the propriety of a given test will depend on the environment in which the fibers will be used.
• the fibers of the present invention can be formed into a wide variety of fabrics, there being substantially no limit to the particular fabric desired, e.g., the fibers of the present invention, in general, can be used in the same manner as the fiber-forming component.
• iodine to form the iodophor which is incorporated in the fibers will result in different colored fabrics having different intensities of color, dependent on the concentration of the iodophor.
• iodophors for example, polyvinylpyrrolidonone on the one hand which yields a yellow color, and starch on the other hand which yields a blue color, different colors can be used to identify articles having disinfectant activity.
• the color intensities can be used as a standard to determine whether the required degree of germicidal activity remains in the fabric -- merely by color comparison.
• the desired degree of hydrophobicity, hydrophilicity fabric strength, and thermal plasticity can be achieved.
• Particular examples of blends include but are not limited to blends of 2, 3, 4 or 5 fibers so long as at least one is an iodophor fiber: rayon iodophor (RI) with regular rayon (RR); RI with polyester iodophor or non-iodophor, RR with polyester iodophor and so on, as demonstrated by the following Tables A and B :
• Such articles include but are not limited to: surgical applications, e.g., sponges, towels, dressings, face masks, gowns, drapes, wash cloths, booties, CSR wraps, scrub suits and air filters; hospital applications, e.g., bed linen including but not limited to sheets and pillow cases, towels, wash cloths, sponges, incontinent pads, adult diapers, wrapping packs for contagious patients, sterile burn and wound dressings, sterile gloves and draperies; conventional consumer items, e.g., handkerchiefs, tissues, face masks, vaginal tampons, sanitary napkins or pads, bandages including long term bandages, i.e., at least 1, 2, 3, 4, 5, 6 or 7 days, "Wet Ones", acne treatment pads, diaper covers, water filters, wiping cloths, "Q-Tips", "Coets", absorbent puffs,
• viscose rayon-alloy iodophor is the preferred fiber: sponges, towels, dressings, face masks, gowns, drapes, wash cloths, instrument covers, scrub suits, air filters, bed linen, incontinent pads, adult diapers, wrapping packs for contagious patients, filters, sterile burn and wound dressings, sterile gloves, handkerchiefs, vaginal and dental tampons, sanitary napkins and pads, dental packing, bandages, "Wet Ones", acne treatment pads, diaper covers, wiping cloths, "Q-Tips”, “Coets”, absorbent puffs, pill bottle stoppers, bath mats, headrests, upholstery, mattress tickings, nursing pads, diaper backing, and diaper absorbent.
• cellulose acetate alloy-iodophor is the preferred fiber: air filters, draperies, water filters, shoe linings, lining and containers for plants and seeds, carpet backing, upholstery, and mattress tickings.
• Vinyon-alloy iodophor as a binder is the preferred fiber: sponges, towels, dressings, face masks, gowns, drapes, wash cloths, instrument covers, scrub suits, air filters, bed linen, wrapping packs, blood filters, sterile burn and wound dressings, sterile gloves, handkerchiefs, face masks, vaginal tampons, sanitary napkins and pads, bandages, "Wet Ones", acne treatment pads, diaper covers, water filters, wiping cloths, "Q-Tips", "Coets", absorbent puffs, shoe linings, bath mats, headrests, dental sponges and liners, pet bed liners, bird cage liners, dog collars, lining and containers for plants and seeds, carpet backing, upholstery, mattress ticking
• Vinyon alloy iodophor as a structural fiber is the preferred fiber: face masks, air filters, blood filters, water filters and diaper backing.
• acrylic-alloy iodophor is the preferred fiber: air filters, socks, infant buntings, shoe linings, headrests, carpet backing, upholstery, mattress tickings and draperies.
• polyolefin and polyester alloy iodophors are preferred: diaper covers, sanitary napkins and pad covers, booties, sterile gloves, mattress tickings, filters and carpet backing.
• a particular blend of fibers for the production of non-woven fabrics is that of polypropylene and viscose rayon-alloy iodophor, the polypropylene functioning to bind the mass in the desired shape.
• the alloying component it is preferred in most applications for the alloying component to bind the iodine more firmly than the fiber-forming component, it is contemplated that certian applications will require the opposite effect wherein the iodine will be more weakly bound to the alloying component.
• any type of shaped object by conventional means from the combined fiber-forming and alloy components of this invention, e.g., films, sheets, foams, molded articles, etc.
• the resultant shaped object is then halogenized with iodine or the like.
• germicidal activity is effected to disinfect, sterilize, provide prophylaxis, or the like, to a locus by contacting the locus with a fiber, fabric or article of manufacture of this invention as aforesaid described.
• the locus can be anywhere, from the atmosphere of a space capsule to the interior of a small animal's intestines. Accordingly, with respect to ill animals, particularly immune-deficient animals or the like, the locus can be proximate to any animal having a pathological disorder -- so as to prevent the transmission of pathogenic microorganisms to said animal, e.g., a human patient in a hospital or the like.
• this invention contemplates the treatment or prevention of various diseases, including but not limited to toxic shock syndrome, vaginitis and female urinary tract infections, by utilizing, for example, the vaginal tampons, sanitary napkins and pads, etc. of the present invention.
• a porous, iodine-capturing protective layer is provided between the iodophor-containing fabric and the locus to be protected from harmful amounts of iodine.
• a protective layer include but are not limited to surgical masks, air filters, diapers and tampons.
• a germ-containing fluid can be passed through the fabric containing the iodophor, thereby disinfecting said fluid while completely or substantially preventing free iodine picked up by the fluid from escaping into the iodine-sensitive locus.
• porous iodine-capturing protective layers include but are not limited to fabrics capable of complexing iodine, e.g. in the form of an iodophor, fabrics containing activated carbon or other adsorption agents, e.g., molecular sieves, and/or fabrics containing chemicals capable of reacting with elemental iodine to form less harmful products thereof.
• a fabric capable of forming an iodophor
• the fabric can be the same or different than the active germicidal fabric containing the iodine, e.g., a rayon-pvp alloy iodophor fabric protected by a rayon pvp alloy or rayon starch alloy fabric.
• the protective layer should preferably have at least or a greater affinity for iodine than the germicidal fabric.
• a sandwich is employed comprising a germicidal fabric surrounded on both sides by a protective layer; however, in certain cases, only one side of the germicidal fabric need be protected.
• the fabric can be formed of not only alloyed fibers but also non-alloyed fibers, examples of the latter including but not limited to those described in Japanese Kokai patents 54 [1979] 91572 and Kokai 57 [1982] 51725 as well as those iodophors described in Tables A and B, supra.
• a liter of aqueous iodine-potassium iodide (I-KI) solution was prepared containing 2 g. of iodine and 2.61 g. of potassium iodide. This solution was placed in the trough of a small padder.
• the needle punched fabric was placed on a piece of rayon challis as carrier and passed through the I-KI solution and the padder rolls to obtain about 100%, based on fabric weight, pick up of solution.
• the fabric was allowed to stand for 15 minutes and then with one liter of fresh distilled water in the padder each time, rinsed twice by passing through the padder using the same settings as before.
• the fabric was allowed to dry in air at room temperature.
• the fabrics were found to contain 2.1 and 4.9 mg. of titratable iodine per gram.
• the fabrics were evaluated in the Kelsey-Sykes test and found to be effective at dilutions of 1/1000 in water practically instantaneously against Proteus vulgaris, Pseudomonas aeruginosa, Escherichia coli, and Staphlococcus Aureus. They were effective practically instantaneously in organic soil at dilutions of 1/100 against the above listed organisms.
• a summary of data is presented in Table II.
• Example IV A lower range or PVP percentage is presented in Example IV.
• EXAMPLE III RAYON WITHOUT ALLOYING COMPONENT Needle-punched fabrics were prepared from rayon which contained no added polymer. These were treated with iodine-potassium iodide solution and washed as described in Example I. This fiber did not contain titrable iodine. Evaluation in the Kelsey-Sykes test showed no bactericidal activity, as seen in Table II.
• EXAMPLE IV POLYVINYLPYRROLIDONE ALLOYED RAYON (LOW RANGE) Fifty gram portions of rayon mixed polymer fibers were prepared to contain various concentrations of polyvinylpyrrolidone. These samples were then treated with a solution of 200 ml. of N/10 IKI and 150 ml. of water five minutes at 25°C. The samples were then washed with three portions of 10° water one minute each. The samples were dried and then subjected to the Kelsey-Sykes Test for the determination of bactericidal activity.
• the bacteria employed were Escherichia coli, Pseudomonas aeruginosa, Staphylococcus aureus, Proteus vulgaris, and Streptococcus pyogenes, the abbreviation in the tables being EC, PA, SA, PV and SP respectively.
• the Kelsey-Sykes Test procedure used was:
• test organisms were grown on Soybean-casein digest agar at 35°C for 18 to 24 hours and carried through three consecutive daily transfers to attain log growth phase. After the incubation period from the third transfer, each culture was harvested, washed with phosphate buffered saline (PBS), centrifuged, and resuspended in PBS to attain a concentration of approximately 1.0 X 10 8 cfu/ml. The suspensions were approximated by optical density and confirmed by plate count.
• PBS phosphate buffered saline
• Saccharomyces cerevisiae was grown to a concentration of 1.0 X 10 7 cfu/ml and heat-killed by boiling for 30 minutes.
• Each concentration of each sample was tested in the presence of 10% heat inactivated horse serum plus 1.0 X 10 6 cfu/ml of heat killed S. cerevisiae. 2. Each concentration of each sample was tested in sterile water.
• the contact times of bacterial cell suspensions (final concentration approximately 1.0 X 10 6 cfu/ml) with the test solutions were five minutes, one hour, four hours, twenty-four hours, and seven days.
• Table III and IIIA Dilutions in water achieved complete kill in 249 of 250 counts.
• the results from dilutions in organic soil are given in Table III and IIIA.
• Table III reports only complete kills wherein the "A" Table reports bacteria counts of less than 5 X 10 4 , the latter value representing only 5% of the original load of organisms applied.
• EXAMPLE V STARCH ALLOYED RAYON Fifty gram samples were prepared containing various concentrations of starch. These samples were then treated and evaluated as described in Example IV. Dilutions in water achieved complete kill in all 250 counts made. The results from dilution in organic soil are given in Tables IV and IV(A).
• EXAMPLE VI HIGH-AMYLOSE STARCH ALLOYED RAYON Hylon VII (National Starch and Chemical Corp.) is comprised of about 70% amylose and 30% amylopectin. (Ordinary cornstarch contains about 30% amylose and 70% amylopectin).
• a 50 g. sample of rayon with 10% Hylon VII boc was treated and evaluated as described in Example IV. This sample contained 11.1 mg. I 2 /g. All the dilutions in water (50 counts) achieved complete kill of the test organisms. The 1/50 dilutions in organic soil achieved total kill (25 counts). Dilutions at 1/100 in organic soil achieved total kill in 15 of 25 counts and substantial control in 21 of 25 counts.
• Sample 16 was a fifty gram portion of regular rayon which was immersed in excess of a solution of
• Betadine in water such that 50 g. of the solution would contain 1 g (2% of the fiber weight) of polyvinylpyrrolidone. After 2 minutes immersion, the sample was centrifuged 1 minute at 3000 rpm in a five inch basket type centrifuge. The sample was then dried and submitted for microbiological testing. The results are given in Tables V and VI. It is further to be noted that topical treatment with Betadine of fiber or fabric results in bonds between fiber such that processing of fiber would be very difficult. The fabric is stiffened. Apparently most of the retained PVP applied (in the Betadine) remains on the fiber surface or in the spaces between fibers.
• the mixed polymer fiber containing PVP By contrast, in the mixed polymer fiber containing PVP, most of the PVP is contained (encapsulated the fiber.
• the fiber is not self-bonded, and is readily processable into fabric structures which are not stiff.
• An advantage of the alloyed polymer fiber is that iodine carried by it (complexed with, the contained PVP component) would be released more slowly than that held by PVP present on the surface.
• the secretions natural to the events could remove PVP from the fiber surface whereas PVP in the fiber structure would not be removed. The iodine is nonetheless still available.
• Sample 7 was 50 g. of regular rayon treated and washed as described in Example IV.
• Sample 17 was 50 g. of regular rayon with no exposure to iodine in any form.
• Sample 6 was 50 g. of 2% PVP alloyed rayon without iodine.
• Sample 14 was 50 g. of 20% Starch alloyed rayon without iodine.
• Sample 15 was 50 g. of 10% Hylon VII alloyed rayon without iodine.
• the test apparatus was a simple commercial frame generally designed for incorporating a conventional microporous filter, said frame being mounted on a receiving flask. The sample was inserted in the frame, the exposed area of the sample being 42 mm in diameter. A 100 ml. suspension of test organism 10 4 organisms per ml. was poured on the fabric and passed through within two to thirty seconds. The liquid was then examined for presence of living organisms.
• This Barrier Test is considered to be a simulated use of fabric for surgical masks inasmuch that irrespective of the fact that the surgical mask is contacted with an aerosol, the microenvironment of the microorganism is water.
• Sample 14 was similar to sample 13, but contained only 10 parts of rayon - 20% Hylon VII staple.
• Sample 15 was similar to sample 13, but contained 10 parts of a 20% PVP rayon staple with 90 parts of bright regular rayon.
• Sample 16 was prepared from a mixture of 10 parts of iodine pretreated PVP rayon staple and 90 parts of bright regular rayon.
• Cellulose acetate and Vinyon spin dopes are solutions of the respective polymers in acetone. Some of the iodine complexing polymers are soluble in acetone and soluble or dispersible in cellulose acetate and in vinyon spin dope. In the attached table are listed several polymers which were dissolved or dispersed in acetone or in cellulose acetate or Vinyon spin dope. Four of the cellulose acetate and three of the Vinyon mixtures were spun by pumping the mixture through a small jet into water. The fiber was stretched a little and collected. The fiber was cut about 1 1/2 inches long and air dried. Five gram portions were then treated by immersion in 150 ml. of N/10 IKI solution at room temperature.
• EXAMPLE XII RAYON IODOPHOR AND NONWOVEN BINDER Rayon fiber is used to make nonwoven fabrics, many of which are bonded using latex emulsions such as Rhoplex HA8 (Rohm & Haas). Rayon iodophor precursor fiber has been formed into a web, needle-punched (for handling in the laboratory) and then Rhoplex HA8 applied. After washing with water, the fabric was dried and submitted for iodine and binder analysis. The results are shown in the following table.
• the presence of the binder increased stiffness and apparently caused slower release of iodine.
• the differences in binder content resulted from changing dilution of the emulsion applied.
• EXAMPLE XIII Efficacy of Fabrics in the Barrier Test Bacteria
• the barrier test described in Example VIII was modified in order to find limits of effective control of the microorganisms used. The modifications were to use one layer of 4 oz/sq yd test fabric and to vary the concentration of organisms used in the test. The concentration variations selected were based on the results reported in Examples VII, IX, and X. Sample fabrics were selected from the group used in the above named experiments.
• the bacteria used were Escherichia coli, Pseudomonas aeruginosa, Staphylococcus aureus and Proteus vulgaris. The results were as shown in Table XIII.
• Polyvinylpyrrolidone (PVP) mixed polymer fibers prepared as described in U.S. 4,136,697 containing 2% PVP were treated with IKI solution as described above.
• a needle punched nonwoven was prepared from that fiber and a portion simulating a bandage or dressing evaluated by applying portions to a bacterial lawn on a soybean-casein digest agar in 100 mm x 15 mm Petri dishes. After 24 hours (48 for Aspergillis niger) at 35°C., these assemblies were evaluated for areas of growth, no growth, and width of any clear area around the fabric. Results for this experiment are shown in Table XV. EXAMPLE XV
• Example XIV was repeated except that a cover stock of 1/2 oz. (17 g./sq.meter) rayon nonwoven was placed on the iodophor fabric and became the contact surface with the bacterial lawn. Results for this experiment are shown in Table XV. EXAMPLE XVI
• Example XIV was repeated except that a protective layer became the surface which contacted the bacterial lawn.
• the protective layer was a 1 oz. (34 g./sq. meter) needle punched nonwoven made from rayon-starch fiber prepared as described in U.S. Patent 4,144,079. Results from this experiment are shown in Table XV.
• EXAMPLE XVII
• Example XVI was repeated except that the protective layer was made from a mixed polymer fiber comprising a matrix of cellulose acetate including 10% of polyvinylpyrrolidone. (This fiber was spun in water from a solution in acetone of cellulose acetate and PVP K-15). Results from this experiment are shown in Table XV. EXAMPLE XVIII
• Example XVI was repeated except that the protective layer was made from rayon PVP fiber. Results from this experiment are shown in Table XV. EXAMPLE XIX
• Example XIV A piece of fabric like that in Example XIV was inserted into a commercial diaper (Pampers, Newborn size, P&G) between the coverstock and the layer of fluff. Data for this example are shown in Table XV. EXAMPLE XX
• Example XVIII was repeated except that a cover stock was placed on the protective layer, which in turn lay on the iodophor fabric. Data for this example are shown in Table XV. EXAMPLE XXI
• Example XV was repeated except that the cover stock was a polyester nonwoven instead of rayon nonwoven. Results from this experiment are shown in Table XV. EXAMPLE XXII
• Example XV was repeated except that the iodophor fiber used was rayon-starch fiber treated with IKI solution as previously described. Results from this experiment are shown in Table XV.
• Example XV was repeated except that the iodophor fiber used was cellulose acetate-PVP mixed polymer fiber treated with IKI solution as previously described. Results from this experiment are shown in Table XV. EXAMPLE XXIV
• Example XIV was repeated except that there was no iodine present. Results from this experiment are shown in Table XV.
• any measurable width of clear zone means that germicidal activity was effected.
• Example XXV was repeated using samples of higher iodine content as shown in Table XVI. Results for these examples are shown in Table XVII.
• Examples XXV through XXIX were repeated except there was added between the iodophor fabric and the test organism a protective layer of a 2 oz. (68 g./sq. meter) needle punched nonwoven prepared from 16% PVP-rayon fiber. Results for these examples are given in Table XVII.
• Example XXXV An air mask or filter material like that of Example XXXV was prepared with a 1/2 oz. (17 g./sq. meter) rayon nonwoven cover stock on either side. It was evaluated as described in Example XXXV and data are. given in Tables XVIII, XIX and XX. EXAMPLE XXXVII
• the fabric was like that in Example XXXVI, except that a 1 oz. (17 g./sq.yd.) protective layer of a rayon-starch needle punched nonwoven was inserted between the iodophor fabric layer and the upstream cover stock.
• the rayon-starch fiber was prepared as described in U.S. Patent 4,144,079 and contained 20% starch based on cellulose in the viscose. Data are given in Tables XVIII, XIX and XX as well as the data for the remaining examples through XLV. EXAMPLE XXXVIII
• Example XXXVII The fabric was like that in Example XXXVII, except that the protective rayon-starch fabric layer was inserted downstream of the iodophor fabric layer.
• the fabric was like that in Example XXXVIII except that the protective layer was a needle punched nonwoven prepared from cellulose acetate - polyvinylpyrrolidone (PVP) mixed polymer fiber. This fiber contained 10% PVP. It was made by dissolving PVP in cellulose acetate spin dope and then spinning fiber from the solution.
• PVP polyvinylpyrrolidone
• EXAMPLE XL The fabric was like that in Example XXXIX except that the protective layer was prepared from rayon-PVP mixed polymer fiber.
• EXAMPLE XLI cellulose acetate - polyvinylpyrrolidone
• the fabric was like that of Example XL except that the iodophor fabric was rayon containing starch (20% boc).
• Example XXXVI This fabric was like that of Example XXXVI, except that the iodized component was prepared from cellulose acetate fiber, treated with iodine and processed as described in Japanese Patent 57-51725, Example I, except that the sample was not laundered.
• EXAMPLE XLIII EXAMPLE XLIII
• Example XXXVI The fabric was like that of Example XXXVI, except that the iodophor component was prepared from a cellulose acetate-PVP mixed polymer fiber prepared as described in Example XXXIX and then treated with iodine using 0.1 N IKI solution. The fiber was washed in three portions of water and dried.
• EXAMPLE XLIV the iodophor component was prepared from a cellulose acetate-PVP mixed polymer fiber prepared as described in Example XXXIX and then treated with iodine using 0.1 N IKI solution. The fiber was washed in three portions of water and dried.
• Example XLII The fabric was like that in Example XLII, except that the iodized component was based on polypropylene fiber treated and processed as described in Japanese Patent 57-51725, Example VII.
• EXAMPLE XLV EXAMPLE XLV
• Example XLV compared with the control.
• Example XLV were all successful in reduction of passage of live organisms.
• an iodine absorber in this example is introduced in the form of a layer of fiber of a type similar to that which supplies iodine, except that it contains no iodine. This constitutes the protective layer.
• the following examples relate to the use of the invention for diapers and incontinent pads and the like of sponges, cosmetic puffs and tampons.
• PVP polyvinylpyrrolidone
• 2 oz. 68 g/sg. meter
• a commercial disposable diaper was opened and one layer of the above fabric inserted between the cover stock (a porous nonwoven) and the absorptive layers. This structure was then tested as follows: A 2X2 inch (5X5 cm.) square of the diaper was wetted using 5 ml.
• the fabric structure was like that in Example XLVIII except that the rayon-PVP portion had been treated by immersing in 0.1 N IKI solution (for 1g. of fiber 7 ml. of solution) for 5 minutes. The fiber was separated from the above solution and washed with three portions of 10° water, 1 minute each and a volume of 3.5 ml. per gram of fiber. Dry at 70°C. Data for this sample are given in Table XXII. EXAMPLE L
• the fabric structure was like that in Example XLIX except that the iodophor fabric was made from rayon-starch fiber prepared as described in U.S. Patent 4,144,079 and then treated with 0.1 N IKI solution as described in Example XLIX. Data for this sample are given in Table XXII.
• Cosmetic puffs were prepared from Rayon-PVP fiber such as is described in Example XLIX. This material contained 10 mg. of iodine per gram of fiber. It was tested by wetting with 5 m l. of physiological saline solution containing 2X10 4 Staphylococcus aureous. Within 5 minutes, the liquid was separated from the fiber and evaluated for presence of live organisms. None were found.
• Tampons were prepared and tested as follows: A blend of 1 part of rayon-PVP fiber was made with 9 parts of high absorbency rayon (prepared as described in U.S. Reissue 30029). The blend of fibers was then formed into a batt by use of a sample card. The batt was then cut across the grain into six inch sections. Portions of these sections weighing 2.5 grams were rolled to give a six inch long roll. A string was then looped around the center of the rolled sample. The string was passed through a forming tool (see below) and the fiber sample pulled into the tool. Excess string was cut off, the forming tool capped and the plunger inserted. This assembly was then placed in a cabinet maker's clamp and the sample compressed to one inch (2.54 cm.) length. After 30 seconds, the clamp was released and the tampon removed from the forming tool.
• the tampon forming tool is of brass and comprises a heavy walled tube, 1/2 inch inside diameter and 5-7/8 inches (14.9 cm.) long, having screw threads on one end for securing a cap and fitted with a plunger which may be inserted into the open end of the tube and is long enough to completely f il l it .
• the plunger is close f itting in the tube and both cylinder and plunger have polished surfaces.
• the tampons were evaluated as follows: 1. Place 10 ml. of a 60/40 blood/saline mixture in a 125 mm. culture tube having a screw cap.
• Tampons having antimicrobial properties were prepared as in Example LVII, using rayon-PVP fiber which had been treated with IKI solution as described in Example XLIX. Results of evaluation are given in Table XXIV.
• EXAMPLE LIX Tampons were prepared and evaluated as described above except that the high absorbency rayon was replaced with regular rayon. Results of the evaluation are given in TableXXIV.
• EXAMPLE LX Tampons were prepared as described in Example LVIII, except that a protective cover was included. The protective layer was a 1 oz. (34 g./sq.m.) rayonstarch needle punched nonwoven which was wrapped around the rolled blend of fibers just before putting the string on it during the tampon preparation process described in Example LVII.
• EXAMPLE LXI Tampons were prepared as in Example LVII, except that the fiber used was 100% rayon-PVP iodophor instead of a blend. Results of evaluation are given in Table XXIV. EXAMPLE LXII
• Tampons were prepared as in Example LIX except that a rayon-starch iodophor like that described in Example LI was used instead of rayon-PVP fiber. Results of the evaluations are given in Table XXIV.
• Tampons were prepared and tested as follows: The fibers were formed into a batt by use of a sample card. The batt was then cut across the grain into six inch sections. Portions of these sections weighing 2.5 grams were rolled to give a six inch long roll. A string was then looped around the center of the rolled sample. The string was passed through a forming tool (see below) and the fiber sample pulled into the tool. Excess string was cut off, the forming tool capped and the plunger inserted. This assembly was then placed in a cabinet maker's clamp and the sample compressed to one inch (2.54 cm.) length. After 30 seconds, the clamp was released and the tampon removed from the forming tool.
• the tampon forming tool is of brass and comprises a heavy walled tube, 1/2 inch inside diameter and 57/8 inches (14.9 cm.) long, having. screw threads on one end for securing a cap and fitted with a plunger which may be inserted into the open end of the tube and is long enough to completely fill it.
• the plunger is close fitting in the tube and both cylinder and plunger have polished surfaces.
• the tampons were evaluated as follows: A sterile 50 ml. capped tube was inoculated with
• the plates and tube were incubated at 37°C. for 24 to 48 hours. The plates were enumerated, the tubes scored for growth (+), or no growth (-).
• the releasable iodine of this invention has virucidal activity, e.g., against Herpes II. Consequently, the germicidal fabrics of this invention are useful when in the form of undergarments, handkerchiefs and kleenex type throwaways, for example.
• Iodine treatment using water as the iodine carrier An apparatus was assembled as follows: A one liter flask was placed on a magnetic stirrer, a stir bar placed in the flask and ten grams of iodine crystals added. The flask was fitted with a two hole stopper. A 100 ml. coarse fritted funnel was fitted into the rubber stopper. This funnel had a long stem so that it would discharge just above the stir bar. Into the other hole of the rubber stopper was fitted a tube which connected to a small pump. The discharge from the pump was into the funnel. Water was added to the funnel with the pump running until the system was filled and the depth in the funnel was sufficient to cover the fiber placed therein.
• Example LXVIII was repeated except that an 8% PVP-rayon was used and treatment times were varied giving the following results: Treatment Time, Minutes mg. I 2 /g.
• Example LXVIII The treatment described in Example LXVIII was repeated, using an 8% PVP-rayon and varying the temperature using a treatment time of 10 minutes. At the end of the treatment time, the fiber was removed and allowed to stand 10 minutes, then squeezed and dried at 70°C. The results were as follow:
• Example LXVIII was repeated except that the water used contained 0.5% Tween 20. The uniformity of treatment was improved and the solution had greater capacity for iodine. This example shows that an ethoxylated non-ionic surfactant improves the treatment substantially. Furthermore, it is expected that most, if not all surfactants will improve the treatment, and the selection of a particular surfactant can be conducted by routine experimentation.

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• 1984
  • 1984-08-13 KR KR1019850700098A patent/KR850700145A/ko not_active Application Discontinuation
  • 1984-08-13 AU AU33912/84A patent/AU3391284A/en not_active Abandoned
  • 1984-08-13 HU HU843552A patent/HUT38684A/hu unknown
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• 1985
  • 1985-07-16 FI FI852791A patent/FI852791L/fi not_active Application Discontinuation
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