EP3291984A1 - Articles de fibres de coton ignifuge - Google Patents

Articles de fibres de coton ignifuge

Info

Publication number
EP3291984A1
EP3291984A1 EP15891352.5A EP15891352A EP3291984A1 EP 3291984 A1 EP3291984 A1 EP 3291984A1 EP 15891352 A EP15891352 A EP 15891352A EP 3291984 A1 EP3291984 A1 EP 3291984A1
Authority
EP
European Patent Office
Prior art keywords
fiber
wax
regional
fibers
cotton
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP15891352.5A
Other languages
German (de)
English (en)
Other versions
EP3291984A4 (fr
Inventor
Francis P. Mccullough
David M. Hall
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Carbtex Technology Inc
Original Assignee
Carbtex Technology Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Carbtex Technology Inc filed Critical Carbtex Technology Inc
Publication of EP3291984A1 publication Critical patent/EP3291984A1/fr
Publication of EP3291984A4 publication Critical patent/EP3291984A4/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • B32B9/04—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B9/047—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material made of fibres or filaments
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06L—DRY-CLEANING, WASHING OR BLEACHING FIBRES, FILAMENTS, THREADS, YARNS, FABRICS, FEATHERS OR MADE-UP FIBROUS GOODS; BLEACHING LEATHER OR FURS
    • D06L4/00—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs
    • 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
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/02—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with hydrocarbons
    • 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
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/188—Monocarboxylic acids; Anhydrides, halides or salts thereof
    • 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
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/203—Unsaturated carboxylic acids; Anhydrides, halides or salts thereof
    • 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
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/224—Esters of carboxylic acids; Esters of carbonic acid
    • 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
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/224—Esters of carboxylic acids; Esters of carbonic acid
    • D06M13/2246—Esters of unsaturated carboxylic acids
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/60—Waxes
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
    • D21H21/34—Ignifugeants
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/02—Synthetic macromolecular fibres
    • B32B2262/0276—Polyester fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/06—Vegetal fibres
    • B32B2262/062—Cellulose fibres, e.g. cotton
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/14—Mixture of at least two fibres made of different materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/306—Resistant to heat
    • B32B2307/3065—Flame resistant or retardant, fire resistant or retardant
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2437/00—Clothing
    • 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
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/04—Vegetal fibres
    • D06M2101/06—Vegetal fibres cellulosic
    • 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
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/30—Flame or heat resistance, fire retardancy properties

Definitions

  • the present invention is directed to ignition resistant and/or flame retardant whole cotton fibers, and whole cotton fibers having a bleached cellulose region at the core and an outer region comprised a wax sheath or surface.
  • the invention is also directed to methods for the manufacture of the ignition resistant whole cotton fiber, and to articles made from a multiplicity of said whole cotton fibers.
  • Cotton is a natural fiber and is renewable. That is, a new crop can be grown each year. Most synthetic fibers are made from petroleum which is not a renewable resource. Cotton has been known for thousands of years, and accordingly, the physical and chemical properties about cotton are well known. Because of a unique chemical nature, cotton can be made to be fire retardant, have wash-wear qualities, and be wrinkle free, among other properties. Cotton also can be blended with other textile fibers to enhance the overall performance of the blended fabric.
  • Raw cotton in other words the unprocessed material obtained from plants, like all vegetable matter contains minerals, resins, gums, protein, tannins, oils and waxes and carbohydrates in addition to cellulose.
  • Cotton normally has to be purified to remove these products from the primary cellulose polymer substrate.
  • Natural cotton is typically bleached in either the yarn form or the fabric form. This involves boiling the cotton for 30 plus minutes in a strong alkaline solution. This process cleanses the cellulosic part of the cotton and removes the natural wax on the outside of the cotton. Most of the unwanted portions of the cotton plant material are removed in a "Kier" boil process.
  • the wax in the cotton fiber is not one having a single component, but is thought to have a blend of complex esters, acids and alcohols.
  • the waxes are thought to have a composition involving C 24 _ C 34 primary alcohols as well as other complex mixtures and a melting point of about 77° C, a density of 0.976, an acid value of 29, saponification value of 57 (after acetylation, 137), an acetyl value of 84, an iodine number of 27, and 68% of un-saponifiable material (having an acetyl value of 123 - indicating an absence of wax esters and a large proportion of free wax alcohols).
  • cotton fiber can be combined with flame and/or ignition resistant fibers, such as synthetic fibers.
  • flame and/or ignition resistant fibers such as synthetic fibers.
  • modacrylic fibers and matrix fibers of vinyl/vinyon among others, have been used.
  • the resulting fabrics frequently lack the performance properties and consumer appeal of pure cotton fabric.
  • Another disadvantage of this method of producing fire resistant fabric is that yams containing two or more fibers with different flammability characteristics which tends to produce fabrics having non-uniform cross-sectional areas, and therefore, non-uniform fire resistant characteristics.
  • cotton fabric can be treated with flame retardant chemicals and/or chemicals that promote ignition resistance that change or interrupt the burning process known as pyrol sis.
  • flame retardant chemicals and/or chemicals that promote ignition resistance that change or interrupt the burning process known as pyrol sis.
  • cotton fabric treated with such chemicals lack the performance properties and consumer appeal of pure cotton fabric. Most of these treatments involve harsh chemicals which are very unfriendly to the environment. Several have also been linked to health problems in infants and newborns. For this reason most of the newborn and infant bedding and sleepwear has been switched to 100 percent polyester.
  • flame retardant chemicals or chemicals that provide ignition resistance interrupt pyrolysis.
  • the flame retardant or ignition resistance may be converted upon heating into acids and bases that catalyze decomposition of the textile at lower temperatures than are required for the formation of volatile combustibles.
  • Compounds containing phosphorus are converted to acidic materials that catalyze the thermal decomposition of the polymer.
  • the flame retardant or ignition resistance chemicals may decompose or sublime upon heating to release large amounts of nonflammable vapors which exclude oxygen from the flame,
  • a need exists for a cotton fiber chat is inherently flame and/or ignition resistant such that fabric made from these fiber complies with flammability and safety regulations without application of harsh chemicals, or with application of reduced amounts of chemical compared to fabric made from untreated cotton fibers,
  • the present invention comprises a major departure from the present state of the art by discovering that bi-regional cotton fiber which has a wax sheath unexpectedly has flame retardant and/or ignition resistant properties, even after being dyed under low temperature and alkaline conditions.
  • One embodiment of the invention is directed to bi-regional cotton fiber comprised of a cellulosic center and an outer surface comprised of a wax.
  • the bi-regional fiber is bleached and preferably bleached with chlorine, ozone, peroxide, hypochlorite or a combination thereof.
  • the wax comprises at least 0.4 percent by weight of said fiber, more preferably the wax comprises from about 0.4 percent to about 25 percent by weight of said fiber, and more preferably from about 14 percent to about 16 percent by weight of said fiber.
  • the wax comprises is a natural wax, a synthetic wax, an emulsified wax or a mixture thereof, wherein the natural wax is preferably a cotton wax, a jojoba wax, a soy wax, a carnauba wax, or a combination thereof, and also preferably the wax has a melting point temperature of about 70°C or greater or about 90°C or greater.
  • the fibers have at least 10 percent greater tensile strength as compared to natural cotton fibers, and more preferably at least 20 percent greater tensile strength as compared to natural cotton fibers.
  • the bi-regional fibers further comprise a saponified acid or derivative thereof on the outer surface of the fiber.
  • the saponified acid or derivative thereof comprises lauric acid, myristic acid, palmitic acid, stearic acid, oleic acid or combinations thereof.
  • the bi-regional fiber is fire retardant and/or ignition resistant and/or meets or exceeds a vertical burn test conducted according to FAR 25.853(b).
  • the fire retardant and/or ignition resistant bi- regional fiber contains no harmful chemicals such as organohalogens.
  • the bi-regional fiber has reduced water absorption as compared to a natural cotton fiber.
  • Another embodiment of the invention is directed to materials comprised of a plurality of the bi-regional fibers of the invention.
  • the materials are fire retardant and/or ignition resistant and, also preferably, the materials have reduced water absorption as compared to a natural cotton fiber.
  • the materials have a wrinkle resistance greater than conventional cotton.
  • Another embodiment of the invention comprises fibers and/or materials of the invention further comprising additional fibers such as, for example, natural fibers, synthetic fibers, carbonaceous fibers, and combinations thereof.
  • the synthetic fibers comprise polyester and the carbonaceous fibers comprise flexible bi-regional carbonaceous fibers.
  • the synthetic fibers comprise about 50 to about 90 percent polyester and about 10 to about 50 percent bi-regional fibers.
  • apparel comprised of materials and/or fibers of the invention as for infants, toddlers, children and adults.
  • the apparel comprises shirts, socks, pants, sweaters, hats, coats, undergarments, sportswear, skirts, sweats, scarves, gators, dresses, tops, blankets, and designs and combinations thereof.
  • the apparel is suitable for wear in environments wherein conditions are greater than and/or less than body temperature including for sports activities such as for example, snow sports, hiking in mountains, jungles and deserts, , running, and rock and mountain climbing. At least in part due to immediate transfer of water and water vapor through the material, apparel of the invention is suitable for wear in both ambient and extremes of temperature environments.
  • Another embodiment of the invention comprises methods for manufacture of a fiber comprising: bleaching a cotton fiber; and applying a wax to the fiber and, also preferably, no wash step is performed after bleaching and before application of the wax.
  • bleaching comprises treating the fiber with chlorine, ozone, peroxide, hypochlorite or a combination thereof and, also preferably, bleaching is performed at about 40°C or less, or at room or ambient temperature and at a pH of between about 6 and about 8.
  • the fibers comprise ignition resistance without added harmful chemicals.
  • the manufacturing combines fibers of the invention with polyester fibers and also preferably, the polyester fibers are treated with a solution of a hydrolyzed partial condensation of trimethoxy methyl silane.
  • Cotton fabric can be made flame retardant or ignition resistant by treating with certain chemicals that change or interrupt pyrolysis (e.g., organohalogens, compounds containing bromine or chlorine). These treatments typically involve harsh chemicals which are unfriendly to the environment and linked to health problems. Many of these compounds are known to be harmful and may be carcinogenic and/or toxic. In addition, cotton fabrics so treated lack the performance properties and consumer appeal of pure cotton.
  • chemicals that change or interrupt pyrolysis e.g., organohalogens, compounds containing bromine or chlorine.
  • bi-regional fibers of the invention can be made fire retardant and/or ignition resistant without the need for harsh or harmful chemical treatments by creating bi-regional fibers of the invention.
  • These bi-regional fibers of the invention preferably contain substantially reduced or no harsh and/or harmful chemicals.
  • Bi- regional cotton fibers of the invention are made from regular, ecru (i.e., raw) or unbleached cotton either in the yarn or in fabric form.
  • the resultant bi-regional cotton that preferable has at least about a ten percent or more greater tensile strength as compared to untreated or conventionally treated cotton fibers, more preferable about 20 percent or greater, more preferably about 30 percent or greater, more preferably about 50 percent or greater.
  • Bi-regional cotton fibers of the invention are preferably ignition resistant and flame retardant and pass the 45 degree angle flame impingement test as prescribed for children sleepwear in the United States.
  • the bi-regional cotton has no harsh chemicals in contact with the infant skin and requires no additional ignition resistance or flame retardant treatment such as that required by traditional cotton.
  • bi-regional cotton retains the natural waxes and oils of raw cotton and requires no additional finishes or lubricants and has superior handling compared with traditional cotton fabrics.
  • the intended consequence of the Kier process which is the standard processing of cotton, is that it removes all of the wax from the cotton fibers.
  • a low alkaline and low temperature process has been developed that does not remove the waxes. It was surprisingly discovered that an unexpected result of such a treatment allows the wax to either migrate to the surface of the cotton fiber or does not remove the surface wax thereby markedly increasing the ignition resistance of the final cotton fabric. Also the method with mild heating migrates the wax to the surface forming the bi-regional fiber. Other properties such as an enhanced hand feel and smoothness of the fiber assemblies, is also obtained.
  • the process requires that all treatments must be performed at a low temperature and alkalinity so as not to result in unintended saponification which could solubilize and result in removal of the wax.
  • Dye-ability is an important asset for any textile fiber. Cotton is fortunate that it can be colored by numerous different dyeing classes. Unfortunately, many of these such as vat, sulfur and/or naphthol, are performed employing high alkaline conditions. The choice of dye class varies in the fastness properties they are able to impart to the finished dyed cotton such as light fastness, wash fastness, fastness to perspiration and the like. To achieve uniformity of dyeing, the cotton is first prepared so that a uniform uptake and leveling of the applied dyestuff is achieved. The normal preparation step involves a Kier type treatment followed by bleaching to remove natural colored impurities. The most desirable dyeing conditions which insure survivability of the residual wax is a low temperature/low alkali reactive dyeing process.
  • the normally employed Kier/bleach process can be replaced with either a low temperature - peroxide/catalyst or low alkalinity hypochlorite process.
  • These bleaching steps employ an oxidative rather than a high heat/alkalinity process to remove cotton impurities.
  • the result is a process that retains essentially all of the waxy composition of the cotton fiber.
  • the wax appears un-expectantly to either migrate to the surface of the fiber or remain on the surface and is not removed by these oxidative processes.
  • This process creates a wax layer on the outer surface of the cotton, thereby causing fibers to be bi-regional. This surface wax contributes to improving the ignition resistance of the fabric.
  • the bleach temperature preferably does not exceed 60°C.
  • Normal peroxide processes are done at the boil or employ a steaming step, for example, by saturated steam at 100°C or greater for continuous operations.
  • a steaming step for example, by saturated steam at 100°C or greater for continuous operations.
  • a stabilizer e.g., Crosprep HES
  • a catalyst that is active at the lower temperature e.g., Crosprep CAT
  • Any remaining peroxide is neutralized employing a non alkaline agent (e.g., Croszyme PEK). Crosprep and Croszyme can be obtained commercially from Eurodye- CTC S.A., Jodoigne, Belgium.
  • chlorine bleach preferably 1 g/1 Cl 2 is employed in the bleach bath to prevent over bleaching and pH is maintained at 7.5 to 8.0.
  • sodium carbonate is used as buffering the bleach bath instead of caustic soda. This reduces the potential saponification of the wax.
  • the temperature can also be increased, but should preferably not exceed 40°C.
  • the temperature is 40°C or below, more preferably 30°C or below, more preferably 25°C or below, and more preferably at about ambient or room temperature. In such cases it is preferred to employ the weaker (1 g/1 Cl 2 ) bleach solution at a higher temperature than to use stronger bleach solutions at lower
  • Acidic products are produced as the oxidation process proceeds which reduce the normal alkalinity present.
  • Ordinary bleaching with chlorine requires additional alkali to insure neutralization of the HC1 which is formed during bleaching. This results in excessive alkali being present after bleaching which is removed usually by a post treatment with acetic acid.
  • Another advantage of this bi-regional cotton process is that an acetic acid wash step, to remove residual alkali, can usually be omitted since very little residual base should be present after the bleaching process. This saves processing time and also expense.
  • the pH of the fabric will be sufficiently low after rinsing so as not to interfere with subsequent dyeing processes.
  • J boxes can be employed to store the padded cloth but the dwell time preferably does not exceed 20 minutes.
  • any residual chlorine is preferably neutralized with either sodium thiosulfate or sodium bisulfite antichlor.
  • Bleaching with bromine is faster than with chlorine but generally the method is not as cost effective as with chlorine. Small amounts (e.g., 1-2 percent of bromine on weight of chlorine content) added to the chlorine bleach solutions also measurably improves bleaching efficiency (see, R. H. Peters, Textile Chemistry, Vol II, Elsevier, New York, 1967).
  • cellulosic fibers that do not have a natural wax content similar to bi-regional cotton of the invention are preferably treated with a topical wax and receive the same or similar ignition resistance.
  • These other cellulosic fibers include the Rayon's, Linen, although non-prepared Linen has a natural wax content of 0.5-2.0 percent (having a melting point of about 62°C) as well as blends. In these cases it is possible to
  • blends of cellulosic fibers will benefit from a post application of an emulsified wax or combination of waxes.
  • the application of the saponified acid derivatives such as, for example, lauric, myristic, palmitic, stearic, oleic and combinations thereof provide ignition resistance to treated fabrics. These products are removable in a conventional laundry cycle, but are preferably useful for fabrics that are not intended to be laundered.
  • the fabric is preferably dyed.
  • the dyeing method of choice is with reactive dyes that can be dyed at temperatures not exceeding 60°C and at low alkalinity.
  • the dyes form a covalent dye with active hydrogen on the cotton fiber.
  • the dye is preferably salted on with high concentrations of sodium chloride. The amount employed depends upon the dye level required to produce the required shade. Table 3 provides levels of salt to employ and concentration of alkali.
  • a preferred alkali is soda ash and can be employed to achieve the fixation of the dye. Once the dye reaches the desired equilibrium, for example the proper shade, 2 gpl soda ash is added to fix the dye within the fibers. This level of alkalinity does not result in saponification of the surface wax. Dyeing is continued at the 60° C until fixation is assured.
  • the invention comprises a bi-regional cotton fiber, fiber assembly or fabric.
  • the cotton or cellulose (e.g., cellulosic) core fiber comprises the fiber core at least 70 percent of the fiber by weight and have a wax sheath or coating (also referred to as the outer core) comprising at least 2/10 of a percent to 25 percent of the whole cotton fiber by weight.
  • the wax coating may be high temperature (high melting point) wax which is preferably a melting point at or above 70°C. Alternatively, the wax coating may be of lower temperature melting wax.
  • This bi-regional fiber contains a unique blend of cellulose with wax.
  • the wax may be a naturally occurring wax from the processed cotton ball or it may be an emulsified wax added to the fiber surface. This wax can be added to the fibers after a low temperature processing, preferably less than 70°C. In another embodiment, the wax may be coated on the fibers after standard process such as, for example, Kier processing.
  • the wax may constitute about 0.4 to 1 percent by weight of the cotton fiber. In another embodiment the wax may constitute about 10 to 25 percent by weight of the cotton fiber. In another embodiment, the wax may comprise about 14 to 16 percent of the cotton fiber by weight.
  • the fibers or woven fabric made from such fibers become an ignition resistant fiber. This is attributed to the high wax content of the fibers coating the exterior (see Example 4).
  • the fibers or fabric preferably exhibit a smooth, silky texture and enhanced moisture (water wetting) resistance as a result of the wax coating.
  • Fiber of the invention is preferably stronger than standard cotton fibers because of the milder processing conditions employed, such as, for example, lower processing temperature.
  • the cotton of the invention preferably possesses flame resistance (flame retardant and/or ignition resistance) to meet flammability safety regulation without application chemical additives or with application of reduced amounts of flame resistant chemicals.
  • blends of the cotton fiber of the invention can be made with flexible bi-regional carbonaceous fibers (BRCF) as described in U.S. Patent No 5,700,573.
  • Blends comprising preferably from 10 to 90 percent of the cotton fibers of the invention with the balance of the fibers being BRCF.
  • untreated cellulose core fiber comprises at least 70 percent of the fiber by weight and the wax sheath comprises from at least 0.2 percent to 15 percent of the cotton fiber by weight.
  • the low-energy room temperature method of cleaning and bleaching leaves the natural wax sheath around the cotton resulting in significant energy savings and carbon dioxide emission reductions, in comparison to the traditional high pH effluent process.
  • the process of the invention produces smarter cotton which reduces C0 2 emissions by 560 pounds and reduces energy consumption by 906 kWh.
  • C0 2 emissions can be reduced by up 4.43 MM tons and up to 14GWh.
  • the superior smarter cotton is up to 30 percent stronger, shows inherent reduced ignitability, enhanced moisture wicking, stain and easy care properties.
  • Clothing and articles made from the smarter cotton are environmentally green and made from a sustainable material compared to synthetic materials. For example, 5.7 million metric tons of cotton will save 906 kWh (kilowatt hours) and 506 lbs. per metric ton. Two forms of smarter cotton are released to the market.
  • NuGard is a form of cotton fibers of the invention that has significantly improved properties compared to conventional forms of cotton. NuGard maximizes the wearer's comfort in addition to reduced ignitability without adding flame resistant chemicals. Articles composed of NuGard are extremely cool in warm weather, have a naturally ultimate soft silky hand, and show reduced tendency to staining and wrinkling as compared with conventionally treated cotton and polyester. Sweat rings with Nugard are not present thanks to its micro- evaporation power. The natural wax repels instant spills, facilitates vapor transport inside- out keeping the wearer cool and dry to the skin.
  • Bi-regional cotton fibers of the invention including Nugard cotton can be made into most any apparel including apparel for infants, toddlers, children and adults such as, for example, shirts, socks, pants, sweaters, hats, scarves, gators, sweats, coats, undergarments, sportswear, skirts, dresses, tops, and blankets.
  • Other embodiments of the invention comprise materials composed of fibers of the invention combined with additional fibers and other materials, such as, for example, leathers, metals, plastics and other polymers in creating most any design and style of clothing and apparel.
  • Workhorse cotton fabric products such as underwear, denim jeans, sheeting, bedding, children's clothing, and the like can be referred to as DuraGard products.
  • Treated cotton because of the wax coated surfaces has the following preferred characteristics: (i) increased staining resistance and improved soil release characteristics; (ii) natural softness and hand; (iii) natural water repellency providing greater dry sleeping comfort; (iv) when blended with diamondown will provide superior thermal comfort by blocking 91 percent of radiant heat loss; (v) enhanced fabric wick ability; and (vi) less problems associated with dyeing.
  • Fabrics manufactured employing the so treated cotton will experience a greater degree of polymerization (DP) in the final fabric because of the less harsh preparation and process treatments normally employed.
  • DP polymerization
  • the fabrics possess increased tenacity (about 14 percent) and elongations (about 14 percent).
  • the milder processing reduces the associated energy costs (about 20 percent minimum) as well as lower water consumption and waste water treatment requirements.
  • ignition resistant refers to fibers or fiber assemblies that satisfactorily pass the (a) FAR 25.853(b) Flammability of Aircraft Seat Cushions, or (b) flammability test or the 45 degree angle flame impingement test (16 CFR 1610, Standard for the Flammability of Clothing Textiles).
  • fiber assembly used herein applies to a multiplicity of fibers that are in the form of a yarn, a wool like fluff, batt, mat, web or felt, and comprising a formed sheet, screen or panel, a braided, knitted or woven cloth or fabric, or the like.
  • high temperature high alkalinity processed cotton means cotton processed by the Kier process or similar processes conducted at temperatures of near 100°C.
  • the fabric and solution is heated to 60° C over 15 minutes.
  • One gpl of a catalyst suitable for low temperature peroxide bleaching (such as Crosprep CAT) is added and the fabric heated in this mixture at the 60°C temperature for 45 minutes followed by draining and refilling.
  • Acetic acid is added over 5 minutes until the pH stabilizes to 6.5-7.0.
  • the fabric is then treated for 10 minutes with a stabilized liquid catalase (such as Croszyme PEK) to neutralize any residual peroxide.
  • the fabric is rinsed, drained and dried.
  • Cotton yarns can be bleached effectively in a pressure dyeing machine.
  • the pH of the bleach liquors can be easily adjusted to control the pH with soda ash.
  • the bleach solution is automatically programed to give alternate inside out and outside in of the yarn package in to insure bleach uniformity.
  • the acetic acid rinse can be controlled to keep the cloth near neutral. This is followed by treatment with the catalase to remove residual peroxide and a final rinse.
  • the fabric is padded to 100 percent wet pick up in a solution containing 0.2 g/1 wetting agent and lgpl chlorine bleach at a pH of 7.5-8.0 and stored in a J Box for 20 minutes at room temperature.
  • the temperature may be increased but may not exceed 40°C.
  • soda ash is preferred because of its buffering effect and so the cloth will not need an acetic acid rinse to obtain a final pH of 6.8-7.2.
  • An antichlor treatment with sodium bisulfite or sodium thiosulfate to remove any unreacted chlorine completes the bleaching process.
  • Fibers derived from raw cotton fiber (ecru) are bleached at less than 70°C, preferably at ambient or room temperature, with a bleaching solution comprising an OX " system, where X is a halogen and where the pH is 6.5 to 8.
  • the dye bath is set with the proper concentration of dye on the fabric, 1 gpl of antifoam such as Croscolor SLR New, lgpl of Croscour HP -JS and the salt concentration from Table 3.
  • the temperature is raised to 60°C and dye for 20 minutes. Soda ash (see Table 3) is added and dyeing continued for 40 additional minutes.
  • the bath is dropped and the fabric is given a hot (60°C) rinse containing 1 gpl acetic acid.
  • the bath is dropped and the fabric soaped 10 minutes at 60°C with 1 gpl Croscolor BCSR followed by a hot (60°C) rinse for 10 minutes and a cold rinse (20°C) for 10 minutes.
  • Treatment of cellulose containing fabrics continues after a standard preparation treatment.
  • Another method of chlorine bleaching is to employ package dyeing equipment.
  • This method offers considerable advantages over continuous bleaching in a finishing plant.
  • the pH of the process is continuously monitored via the add tank and corrections can be made while running. After the antichlor treatment the yarn packages do not need to be dried but the dyeing operation can be started immediately.
  • This bleach method can be employed on small runs in order to make and test product changes, for example, in the color line or for product modifications. Further, this method provides better shrinkage control of the yarns since normal shrinkage will have occurred during the package bleaching/dyeing process.
  • a desized and bleached cotton print cloth (Testfabrics style 400 weighing 3.03 osy
  • Example 3 An army carded cotton sateen which had been desized and bleached (Testfabrics style 428 weighing 6.93 osy, and a bleached, mercerized, and carded cotton broad cloth (Testfabrics' style 453, weighing 3.53 osy) and a cotton sheeting (Testfabrics' style 493, weighing 4.45 osy) gave the same results (passed the 45°C flammability test) after treating in the fabrics in the manner described above, (treated at 100 percent wet pickup with a solution of a 0.75 percent owf (on weight of fabric) emulsified candelilla wax, and 0.1 percent nonionic wetting agent).
  • a Cotton/Linen 56/44 blended fabric (Testfabrics' style L5040, weighing 6.4 osy) treated as above did not ignite even after a 4 second flame impingement.
  • the same results were obtained when bees wax was substituted for the candelilla wax.
  • the same results were obtained when a 50/50 emulsified blend of Jojoba and Carnauba was employed.
  • the desized and bleach print cloth (Testfabrics' style 400) cited above was treated with 1.0 percent blend (50/50 w/w) mixture of oleic and stearic acid at 75 percent wet pickup. After drying, fabric did not ignite even after a 4 second flame impingement. The ignition resistance protection did not occur after the fabric was laundered to remove the acid blend.
  • the non-flammability and ignition resistance of the bi-regional cotton fibers of the disclosure is determined following the test procedure set forth in 14 C.F.R. ⁇ 25.853(b). The test is performed as follows:
  • a minimum of three 1 inch x 6 inch x 6 inch (2.54 cm x 15.24 cm x 15.24 cm) specimens (derived from a batting of the bi-regional whole cotton fibers as prepared above.
  • the specimens are conditioned by maintaining them in a conditioning room maintained at a temperature of 70°C ⁇ 3°C and 5 percent relative humidity for 24 hours preceding the test.
  • Each specimen is supported vertically and exposed to a Bunsen or Turill burner with a nominal I.D. tube of 1.5 inches (3.8 cm) in height.
  • the minimum flame temperature is measured by a calibrated thermocouple pyrometer in the center of the flame and is 1550°F (843°C).
  • the lower edge of the specimen is 0.75 inch (1.91 cm) above the top edge of the burner. The flame is applied to the cluster line of the lower edge of the specimens for 12 seconds and then removed.
  • the material is self-extinguishing.
  • the average burn length does not exceed 8 inch (20.32 cm), the average after flame does not exceed 15 seconds and flaming drippings did not continue to burn for more than 5 seconds after falling to the burn test cabinet floor.
  • Ozone has been found to be effective in the de-colorization of dyes such as indigo (see Wasinger/Hall U.S. Patent Nos. 5,313,811, 5,366,510 and 5,531,796). Ozone is also effective as a bleaching agent on desized and prepared goods in a finishing plant operation (see, Wasinger/Hall U.S. Patent No. 5,376,143). Ozone may not have been used as a bleaching agent on raw cotton goods because the usual finishing plant preparation procedures involve the removal of the wax.
  • Raw cotton yarn can be bleached in a package dyeing machine using ozone without removal of the cotton wax to a degree of whiteness ranging from 75-85 (AATCC Method 110 "American Association of Textile Chemists and Colorists") depending upon the time, ozone concentration and water temperature of the treatment.
  • the so bleached goods were found to have retained almost all of its initial tensile strength along with an increase in the wet-ability of the goods without any measurable wax removal. After treatment the package is ready for dyeing.
  • Ozone creates hydroxyl (OH ) radicals which although they are short lived at elevated temperatures are sufficiently stabile in cold water to effectively facilitate in the bleaching along with the ozone itself.
  • the use of the package machine is also useful for bleaching employing essentially the same low temperature process that is described for fabric bleaching.
  • the advantage of this process is that the yarn is now ready for dyeing without a pre-drying step employed with fabric bleaching.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Ceramic Engineering (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Woven Fabrics (AREA)
  • Mechanical Engineering (AREA)
  • Professional, Industrial, Or Sporting Protective Garments (AREA)

Abstract

L'invention concerne une fibre bi-régionale avec un noyau cellulosique et une gaine externe de cire. La gaine peut comprendre une cire à température de fusion élevée. La fibre peut être produite par traitement de la fibre naturelle à des températures inférieures à 70 °C. La fibre peut être traitée de manière classique selon, par exemple, un processus de Keir qui peut consister à blanchir approximativement à 100 °C à l'aide d'une cire ajoutée par la suite à une température suffisante pour disperser la cire sur la surface de la fibre. Les fibres résistent à l'inflammation de la manière mesurée par les tests classiques du secteur. La cire peut comprendre entre au moins environ 0,4 et 25 pour cent de la fibre en poids. La cire peut être une cire naturelle, une cire synthétique ou émulsifiée ou leurs mélanges. Les fibres bi-régionales peuvent être mélangées avec d'autres fibres y compris des fibres BRCF afin de créer des tissus ignifuges compris des vêtements, des couvertures et des matériaux ménagers.
EP15891352.5A 2015-05-04 2015-05-04 Articles de fibres de coton ignifuge Withdrawn EP3291984A4 (fr)

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JP (1) JP2018523026A (fr)
KR (1) KR20180022658A (fr)
CN (1) CN107949474A (fr)
AU (1) AU2015393998A1 (fr)
CA (1) CA2988885A1 (fr)
MX (1) MX2017014154A (fr)
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US11905630B2 (en) 2019-02-22 2024-02-20 Jess Black Inc. Fire-resistant double-faced fabric of knitted construction
US11987926B2 (en) * 2021-01-25 2024-05-21 Energy Ogre Llc Launderable activated cotton
US20220389650A1 (en) * 2021-01-25 2022-12-08 Energy Ogre Llc Launderable activated cotton
WO2024044164A1 (fr) * 2022-08-22 2024-02-29 Energy Ogre Llc Vêtement en coton activé blanchissable

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AT409144B (de) * 1996-06-21 2002-05-27 Chemiefaser Lenzing Ag Verfahren zur behandlung von cellulosefasern und von gebilden aus diesen fasern
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WO2016178662A1 (fr) 2016-11-10
ZA201708203B (en) 2020-07-29
EP3291984A4 (fr) 2018-11-14
KR20180022658A (ko) 2018-03-06
AU2015393998A1 (en) 2017-12-21
CN107949474A (zh) 2018-04-20
JP2018523026A (ja) 2018-08-16
CA2988885A1 (fr) 2016-11-10
MX2017014154A (es) 2018-07-06

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