WO2010082063A1 - Procédé de traitement de la laine - Google Patents

Procédé de traitement de la laine Download PDF

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Publication number
WO2010082063A1
WO2010082063A1 PCT/GB2010/050060 GB2010050060W WO2010082063A1 WO 2010082063 A1 WO2010082063 A1 WO 2010082063A1 GB 2010050060 W GB2010050060 W GB 2010050060W WO 2010082063 A1 WO2010082063 A1 WO 2010082063A1
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WO
WIPO (PCT)
Prior art keywords
composition
acid
wool
fabric
vessel
Prior art date
Application number
PCT/GB2010/050060
Other languages
English (en)
Inventor
Jamie Anthony Hawkes
David Malcolm Lewis
Paul Webb
Yong Lu
Original Assignee
Perachem Limited
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 Perachem Limited filed Critical Perachem Limited
Publication of WO2010082063A1 publication Critical patent/WO2010082063A1/fr

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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
    • 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
    • D06M13/322—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 nitrogen
    • D06M13/402—Amides imides, sulfamic acids
    • D06M13/432—Urea, thiourea or derivatives thereof, e.g. biurets; Urea-inclusion compounds; Dicyanamides; Carbodiimides; Guanidines, e.g. dicyandiamides
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K21/00—Fireproofing materials
    • C09K21/06—Organic materials
    • C09K21/12—Organic materials containing phosphorus
    • 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
    • D06M11/58—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 nitrogen or compounds thereof, e.g. with nitrides
    • D06M11/66—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 nitrogen or compounds thereof, e.g. with nitrides with sulfamic acid or its salts
    • 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
    • D06M11/68—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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
    • D06M11/70—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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with oxides of phosphorus; with hypophosphorous, phosphorous or phosphoric acids or their salts
    • 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
    • D06M2101/10—Animal fibres
    • D06M2101/12—Keratin fibres or silk
    • 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 relates to a method of treating a material.
  • the invention relates to a method of treating a material to impart flame retardant properties thereto.
  • a material thus treated is durable to laundering and/or dry cleaning.
  • Wool is inherently flame retardant although not enough to be used in certain applications, for example mass transit seating.
  • flame retardant materials are low cost, durable, do not impact on the mechanical properties of the fabric, meet health and safety requirements, are environmentally acceptable, and are able to tolerate traditional dyeing and printing processes for all colour ranges when used on dyed materials.
  • T he ⁇ Z irpro ' treatment s are b a s e d on th e exhau s t i on o f the se negative ly charged s al t s , under acidi c conditi ons , onto pos itively charged s ites in wool .
  • Other flame retardants for wool are based upon halogen donors, which tend to interfere with free radical processes that maintain a flame, although these are environmentally unacceptable.
  • Alternative treatments available are based on phosphate / polyphosphate salts, but these have achieved only limited commercial success, and are not usually durable.
  • the present invention relates in particular to a method of providing wash-durable flame retardant compositions.
  • Each of the known existing wash-durable flame retardant compositions has one or more disadvantages.
  • One existing durable FR composition is the ⁇ Zirpro' system mentioned above, in which a solution containing the relevant salt is applied to wool via an exhaustion method.
  • An ⁇ exhaustion' method refers to a process where the material is soaked in the FR solution for a period of time until the active chemical has been absorbed (or Exhausted') onto the material. This is usually done in a winch machine or other batch machine.
  • Noflan (RTM) supplied by Firestop (UK) which is a phosphorous based chemical that is normally applied using a pad bake system, as is described in US6863846 and US 625947.
  • RTM Noflan
  • UK Firestop
  • This product however contains a large amount ( ⁇ 30%) of ammonium chloride which has the potential to form hydrochloric acid under humid conditions .
  • a method of treating a material to improve its flame retardancy comprising applying to the material a composition having a pH of less than 4 and which comprises urea and an acid selected from phosphorous acid, phosphoric acid, sulfamic acid and mixtures thereof.
  • phosphorous acid we mean to refer to the material having a molecular formula H 3 PO 3 which upon reaction with a base produces phosphite salts.
  • phosphoric acid we mean to refer to the material having a molecular formula H3PO4 which upon reaction with a base produces phosphate salts.
  • sulfamic acid we mean to refer to the material having the formula H 2 N-SO 3 H which upon reaction with a base forms sulfamate salts.
  • the composition is an aqueous composition. It may further comprise other water-mi s proficient solvents. Preferably however water is the only solvent present.
  • the composition consists essentially of water, urea and an acid selected from phosphorous acid, phosphoric acid, sulfamic acid and mixtures thereof.
  • the composition preferably comprises less than 10 wt% further ingredients, preferably less than 5 wt%, more preferably less than 1 wt% .
  • the composition has a pH of less than 3.5, more preferably it has a pH of less than 3.
  • the composition applied to the material has a pH of at least 0.5, for example at least 1 or at least 1.5.
  • the pH of the composition may have a pH of from 1.5 to 2.5, for example about pH 2.
  • the composition applied to the material in the method of the present invention does not comprise a base.
  • the composition is substantially free of a base comprising a monovalent metallic cation.
  • the composition may be applied to the material by any suitable means.
  • suitable means Typically different methods are used depending on the physical form of the material.
  • wool top may typically be treated in a bump machine; fabric may suitably treated in a jet machine or winch machine; garments or other finished articles may typically be treated using a paddle machine; and for yarn a package machine is preferred.
  • the composition may be applied to the material by any suitable means, for example by a padding or foaming technique.
  • the composition is applied to the material using an exhaustion technique. This technique involves immersing the material in the composition for a period sufficient to allow uptake ( ⁇ exhaustion' ) by the material of the active components. Exhaustion may be described as the transfer of a component from a liquor bath to the fibre. The extent of exhaustion is sometimes given as a percentage. For example, a process involving 60% exhaustion of a component would mean that 60% of the total amount of the component in the composition has attached to the fibre, and the remaining 40% remains in solution.
  • Exhaustion techniques are commonl y used in dyeing processes. In some cases reactive dyes and acid dyes may exhaust to the point that the dye liquor becomes nearly colourless. It should be noted that a component which has exhausted on t o a material ha s no t necessarily "permanently" bonded to the material. In some instances a component may form a permanent covalent bond with a material but in other instances a more transient electrostatic interaction may exist.
  • the liquor ratio used in the method of the present invention that is the weight ratio of composition to material treated depends on the application method employed. However selection of an appropriate application method and a suitable liquor ratio for use in such an application method is well within the capabilities of the person skilled in the art.
  • the concentration of each component present in the composition may vary according to the liquor ratio used.
  • the concentrations of the components are selected to provide a specific treatment level defined as % omf (% on mass of fibre) . This is the percentage by mass of a component which has been fixed onto the material during the treatment process and is calculated by measuring the dry mass of the material at the start and the end of the process. For example, if lOOg of dry material is treated and after processing has dry weight of 103g, then a treatment level of 3% omf has been achieved.
  • the treatment level of the acid is at least 0.1% omf, more preferably at least 1% omf, more preferably at least 3% omf, and most preferably at least 5% omf.
  • the treatment level of the acid is up to 50% omf acid, for example up to 40% omf, preferably up to 30% omf, more preferably up to 20% omf, and most preferably up to 10% omf.
  • the treatment levels of acid stated above refer to the total amount of acid when a mixture of acids is used.
  • the composition comprises phosphorous acid.
  • at least 50 wt% of the acid component present in the composition is phosphorous acid, preferably at least 75 wt%, more preferably at least 90 wt%, for example at least 95 wt%.
  • the treatment level of urea is at least 0.1% omf, more preferably at least 1% omf, more preferably at least 3% omf, and most preferably at least 5% omf.
  • the treatment level of urea is up to 50% omf, for example up to 40% omf, preferably up to 30% omf, more preferably up to 20% omf, and most preferably up to 10% omf .
  • the weight ratio of urea to acid in the composition used in the present invention is preferably at least 0.2:1, more preferably at least 0.5:1, and most preferably at least 0.8:1.
  • the weight ratio of urea to acid is preferably up to 10:1, for example up to 5:1, preferably up to 3:1, and most preferably up to 2:1.
  • composition used in the method of the present invention may comprise one or more further ingredients.
  • the composition may further comprise a smoke-reducing compound.
  • a smoke-reducing compound Such compounds are well known to those skilled in the art and when present are suitably contained in an amount sufficient to provide a treatment level of from 1 to 25% omf, preferably 15 to 20% omf, more preferably from 7 to 15% omf, for example about 10% omf.
  • Suitable smoke-reducing compounds include halogen- containing materials, fo r example tetrabromophthalic anhydride which is available from Dixon-Chew in West Yorkshire under the trade mark Flameban; along with smoke- reducing materials sold under the trade mark Cetaflam by Avocet Dye & Chemical Co. Ltd.
  • composition applied in the method of the present invention may further comprise a water soluble or water dispersable cationic polymeric resin.
  • a water soluble or water dispersable cationic polymeric resin Preferred ar e cationic cross-linking resins, most preferred are cationic resins which are capable of self cross-linking or cross-linking under a baking or curing regime. Specific selection of the optimum resin can be made according to specific circumstances relating to the end-use by someone skilled in the art.
  • polyaminoamide-epichlorohydrin resins such as Hercosett 125 (Hercules) or Beetle Resin PT765 (BIP)
  • polyquaternary ammonium compounds such as Tinofix FRD (Ciba) or Levogen FL (Bayer) or cyclanon E (BASF)
  • polyamine aliphatic quaternary amines such as Optifix F (Clariant) .
  • a cationic polymeric resin may be advantageous as material which has been treated with an acid may have a high concentration of covalently bonded and also unbound phosphite, phosphate or sulfamate residues on the surface. This leads to an anionic surface which is hydrophilic and thus likely to absorb water. The material therefore often becomes damp and may also be prone to shrinkage.
  • the inclusion of a cationic polymeric resin may help to reduce the anionic nature of an acid treated material and thus helps to prevent dampness and shrinkage. Careful choice of an appropriate cationic polymeric resin by those skilled in the art, can improve the physical handle of the fabric and may also impart hydrophobic properties. This method could thus be used to provide waterproof fabrics.
  • the composition used in the method of the present invention may include a dispersed phase material, for example a pigment, filler or mixtures thereof.
  • a dispersed phase material for example a pigment, filler or mixtures thereof.
  • the composition may include a flame retardant pigment, for example magnesium hydroxide, calcium carbonate, aluminium phosphate, aluminium phosphite, aluminium silicate, magnesium phosphite or magnesium phosphate.
  • Other pigments may be used to impart other properties such as colour, opacity, hydrophobicity, easy iron properties and a soft handle.
  • the range of suitable dispersed phase materials is large. Appropriate selections could however be readily made by the person skilled in the art, according to the precise properties required.
  • compositions used in the method of the present invention may include a dye, thereby introducing fabric colouration at the same time as other properties.
  • the dye may for example be a reactive dye, an acid dye, a premetallised dye, or a mordant dye. If such compounds are present in the compositions used in the present invention the material produced may be dyed a deep colour and the dyed material may be fast to multiple washing .
  • composition used in the method of the present invention may further comprise a wetting agent.
  • Suitable wetting agents are known to the person skilled in the art.
  • the method of the present invention preferably comprises applying to a material an aqueous composition comprising an acid and urea.
  • the composition may suitably be prepared by the addition of urea to an aqueous solution of the acid.
  • composition may be provided in concentrated form, to be diluted by the user.
  • the material treated in the method of the present invention comprises polyamide fibres, for example natural polyamide fibres for example wool, silk, alpaca, angora, leather etc; or synthetic polyamide fibres, for example Nylon 6, Nylon 6, 6 etc.
  • polyamide fibres for example natural polyamide fibres for example wool, silk, alpaca, angora, leather etc.
  • synthetic polyamide fibres for example Nylon 6, Nylon 6, 6 etc.
  • Blends or mixtures including polyamide fibres and non- polyamide fibres are within the scope of the present invention .
  • the material treated by the present invention comprises wool. It may be pure wool or it may be a mixture or blend comprising wool and one or more other materials. In embodiments in which the material is a mixture or blend, it preferably comprises at least 20wt% wool, preferably at least 30wt%, for example at least 40wt%, more preferably at least 50wt% . Such blends or mixtures may suitably comprise one or more further materials selected from nylon, viscose, lycra, acrylics and polyester.
  • the wool material may comprise wool in any suitable form, for example wool yarn, wool top, wool fabric, wool carpet, or loose wool; and may include cashmere or non-sheep origin animal fibres. Alternatively, the wool material may be in the form of a garment or other finished article containing wool or a woven fabric containing wool or non- sheep origin fibres.
  • the material may be a fabric including a knitted or woven fabric or a non-woven material.
  • the method the present invention may comprise the steps of:
  • composition comprising urea and an acid selected from phosphorous acid, phosphoric acid, sulfamic acid and mixtures thereof;
  • step (a) comprises preparing a composition comprising an acid and urea in an appropriate ratio to provide the preferred treatment levels of each as detailed above.
  • the material is contacted with a heated composition.
  • the composition may be heated prior to contact with the material or during contact with the material.
  • It may suitably be heated to a temperature of at least 30 0 C, more preferably at least 40 0 C, for example at least 50 0 C, or at least 55°C. It may be heated to a temperature of up to 100 0 C, for example up to 90 0 C, preferably up to 80 0 C, more preferably up to 75°C. In a preferred embodiment a temperature of 60 to 70 0 C is used.
  • step (b ) comprises immersing the material in the composition
  • the composition is suitably heated after immersion of the material.
  • step (b) the material is contacted with the composition for a period of at least one minute, preferably at least five minutes, for example at least 10 minutes, suitably at least 15 minutes, at least 30 minutes or at least 45 minutes.
  • step (c) the material may be contacted with the composition for a period of up to two hours, for example up to 240 minutes, preferably up to 180 minutes, for example up to 150 minutes, preferably up to 120 minutes, for example up to 100 minutes.
  • Step (c) may in some embodiments comprise physical removal of the material from contact with the composition. For example if the material is immersed in the composition, the material may simply be lifted from the composition or the composition drained from the container comprising the material.
  • step (c) may also include rinsing the composition from the material. Such a rinsing step may suitably comprise applying water to the material.
  • step (c) may comprise applying an aqueous alkali solution to the material in order to raise the final pH of the material. Preferably the water or aqueous alkali will be at ambient temperature.
  • the material may suitably be dried. It may optionally be sp i n dried. Alternatively and/or additionally it may be dried at an elevated temperature by passing through or into an oven.
  • the material is first spin dried to remove excess liquor and then dried in an oven.
  • the material is dried at a temperature of from 30 to 180 0 C, for example 40 to 140 0 C, preferably 60 to 100 0 C. It is suitably dried for a period of at least one minute, preferably at least five minutes, for example at least ten minutes, suitably at least fifteen minutes. It may be dried for a period of up to 6 hours, preferably up to two hours, more preferably up to one hour, suitably up to 45 minutes, for example up to 30 minutes .
  • the method may comprise of one or more additional further rinsing and/or drying steps.
  • a material treated by the method of the present invention is suitably provided with wash-durable flame retardant properties.
  • the material is flame retardant after multiple cleaning treatments.
  • Materials treated with a flame retardant composition for use in transportation fabrics must meet various international standards for flame testing / type of wash testing / smoke production / toxicity of smoke evaluation and the like. The standard (s) required depends on the intended use of the material.
  • the British standard requires that the length of the observed char must not exceed the size of the test frame (approximately 15cm) . Afterglow supporting a flame front and a hole in the charred region of the fabric are also observations which result in a test fail.
  • a small Bunsen burner or a kitchen butane torch may be used to assess the flammability characteristics of a material.
  • the flame can be applied at a 45° angle on the bottom edge of the fabric for 15 seconds. For a test pass, after removal of the flame there must be no more than 5 seconds of afterflame on the fabric .
  • phosphorous acid can esterify serine residues under acidic conditions, especially on drying, to form covalent bonds with the material as shown in Scheme 4:
  • the urea present in the system may help improve accessibility through swelling of the wool fibres .
  • the method of the present invention may be carried out as a batch process or a continuous process.
  • a batch process is preferred.
  • the method of the present invention suitably provides a wash-durable flame retardant finish for wool containing materials .
  • composition comprising urea and an acid selected from phosphorous acid, phosphoric acid, sulfamic acid and mixtures thereof to impart flame retardant properties to a material, preferably a material comprising wool.
  • a liquor ratio of 15:1 was used (150 Litres: 10Kg fabric)
  • a liquor ratio of 15:1 was used (150 Litres: 10Kg fabric)
  • a fabric comprising 100% wool in a flat woven state was treated according to the present invention using a wool top dyeing vessel.
  • a liquor ratio of 15:1 was used (150 Litres: 10Kg fabric)
  • the method was carried out according to the following instructions : • Place fabric into dyeing vessel.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

L'invention porte sur un procédé de traitement d'un matériau pour améliorer son ignifugation, le procédé comprenant l'application sur le matériau d'une composition ayant un pH inférieur à 4, et qui comprend de l'urée et un acide choisi parmi l'acide phosphoreux, l'acide phosphorique, l'acide sulfamique et des mélanges de ceux-ci.
PCT/GB2010/050060 2009-01-15 2010-01-15 Procédé de traitement de la laine WO2010082063A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB0900624.8 2009-01-15
GB0900624A GB0900624D0 (en) 2009-01-15 2009-01-15 Method of treating wool

Publications (1)

Publication Number Publication Date
WO2010082063A1 true WO2010082063A1 (fr) 2010-07-22

Family

ID=40433343

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/GB2010/050060 WO2010082063A1 (fr) 2009-01-15 2010-01-15 Procédé de traitement de la laine

Country Status (2)

Country Link
GB (1) GB0900624D0 (fr)
WO (1) WO2010082063A1 (fr)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US625947A (en) 1899-05-30 berduist
US2482755A (en) * 1945-05-29 1949-09-27 Bancroft & Sons Co J Flameproofing of fibrous material
ZA9610587B (en) * 1995-10-17 1997-03-04 Futuratec Cc Fire retardant composition and process.
AU747024B2 (en) * 1997-11-26 2002-05-09 Futuratec Cc A preservative and fire retardant composition and combination and process
US6863846B1 (en) 1998-09-08 2005-03-08 Isle Firestop Limited Combustion retardant for polymeric materials

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US625947A (en) 1899-05-30 berduist
US2482755A (en) * 1945-05-29 1949-09-27 Bancroft & Sons Co J Flameproofing of fibrous material
ZA9610587B (en) * 1995-10-17 1997-03-04 Futuratec Cc Fire retardant composition and process.
AU747024B2 (en) * 1997-11-26 2002-05-09 Futuratec Cc A preservative and fire retardant composition and combination and process
US6863846B1 (en) 1998-09-08 2005-03-08 Isle Firestop Limited Combustion retardant for polymeric materials

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