Classifications

• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
  • D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
  • D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
  • D06P1/673—Inorganic compounds
  • D06P1/67333—Salts or hydroxides
  • D06P1/67341—Salts or hydroxides of elements different from the alkaline or alkaline-earth metals or with anions containing those elements
• • 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
  • D06M11/11—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 halogen acids or salts thereof
  • D06M11/22—Halides of elements of Groups 5 or 15 of the Periodic Table
• • 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
  • D06M11/32—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
  • D06M11/36—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
  • D06M11/46—Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic Table; Titanates; Zirconates; Stannates; Plumbates
• • 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
  • D06M11/51—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 sulfur, selenium, tellurium, polonium or compounds thereof
  • D06M11/55—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 sulfur, selenium, tellurium, polonium or compounds thereof with sulfur trioxide; with sulfuric acid or thiosulfuric acid or their salts
  • D06M11/57—Sulfates or thiosulfates of elements of Groups 3 or 13 of the Periodic Table, e.g. alums
• • 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
  • D06M13/192—Polycarboxylic 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
  • D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
  • D06M13/503—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms without bond between a carbon atom and a metal or a boron, silicon, selenium or tellurium atom
• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
  • D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
  • D06P3/02—Material containing basic nitrogen
  • D06P3/04—Material containing basic nitrogen containing amide groups
  • D06P3/14—Wool
  • D06P3/148—Wool using reactive dyes
• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
  • D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
  • D06P3/02—Material containing basic nitrogen
  • D06P3/04—Material containing basic nitrogen containing amide groups
  • D06P3/14—Wool
  • D06P3/20—Wool using mordant dyes using metallisable dyes
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10S428/00—Stock material or miscellaneous articles
  • Y10S428/92—Fire or heat protection feature
  • Y10S428/921—Fire or flameproofing
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10S8/00—Bleaching and dyeing; fluid treatment and chemical modification of textiles and fibers
  • Y10S8/929—Carpet dyeing
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
  • Y10T428/00—Stock material or miscellaneous articles
  • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
  • Y10T428/2913—Rod, strand, filament or fiber
  • Y10T428/2933—Coated or with bond, impregnation or core
  • Y10T428/294—Coated or with bond, impregnation or core including metal or compound thereof [excluding glass, ceramic and asbestos]
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
  • Y10T428/00—Stock material or miscellaneous articles
  • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
  • Y10T428/2913—Rod, strand, filament or fiber
  • Y10T428/2933—Coated or with bond, impregnation or core
  • Y10T428/2964—Artificial fiber or filament
  • Y10T428/2967—Synthetic resin or polymer
  • Y10T428/2969—Polyamide, polyimide or polyester

Definitions

• ABSTRACT The flame-resist properties of natural and synthetic polyamide fibres, especially wool and wool blends, are improved by depositing in the fibres an organic chelate or fluoride complex of titanium, preferably to the extent of 0.2 2.5% calculated as titanium dioxide.
• the complexes may be dissolved as such in an aqueous medium and applied by spraying, padding or by exhaustion from a bath.
• the complexes may be formed in situ in the aqueous medium by adding a complexing agent to a water-soluble titanium compound or on the fibre, as by treating with a fluoride solution fibres already treated with a titanium compound, which may itself be a chelate complex.
• a dye can be applied to the fibres from the same bath, either simultaneously or as a separate step.
• the present invention relates to textile finishing, and more especially to the improvement in the properties of natural and synthetic polyamide fibres.
• Naturally occurring polyamide fibres for example the wool of sheep, display a high degree of natural flame retardancy because of their relatively high nitrogen and moisture content, high ignition temperature (570600C), low heat of combustion, low flame temperature and high limiting oxygen index.
• a horizontal test method is much less severe than a 45 or a vertical test. Most wool fabrics will pass a horizontal test but may not pass some 45 or vertical tests. The influence of fabric construction is also very important, the denser and heavier the fabric the-lower the flammability. For example a conventional wool carpet will pass the American tablet test (DOC FF 1-70, DOC FF 2-70), while an open shag pile or Flokati carpet will not pass the'same test.
• titanium compounds especially titanium tetrachloride, when when applied to textile fibres,
• the present invention provides a process forirnproving the flame-resist properties of natural or synthetic polyamide fibres which comprises applying to the fibres a complexed titanium compound, usually as a solution, wherein the complex is formed with an organic chelating agent or with fluoride ions.
• the amount of titanium compound applied to the wool should preferably be at least 0.2%, especially 0.2 2.5% byweight calculated as titanium dioxide on the weight of fabric(o.w.f.
• the complexed titanium compound is normally applied in aqueous solution.
• the invention may be applied to the treatment of synthetic polyamide fibres, for example nylon, but is especially valuable for the treatment of natural polyamide fibres.
• the fibres are of sheeps wool, but they can also be derived from alpaca, cashmere, mohair, vicuna, guanaco, camel hair, silk, and llama, or of blends of these materials with sheeps wool.
• Fabrics consisting of a blend containing major proportion of wool and a minor proportion, generally 30% or less, of
• synthetic fibres, or natural cellulosic fibres, for example polyamide, polyester or cotton fibres, may also be treated.
• the treatment may be applied to the fibres at erably the material to be treated is scoured to-a residual methylene chloride extract of not more than 0.8% in order to remove spinning additives or natural waxes which can contribute to the flammability of the product.
• the titanium compound may be applied using conventional machinery for treating textiles and garments with liquors including dollies, winches, beam dyeing equipment, package dyeing machinery, hank dyeing machinery, top dyeing equipment, washing and laundering equipment and dry-cleaning machinery for batchwise treatments, and including pad mangles, lick rollers, spray units, continuous cloth washing units, backwashing machines and solvent scouring machines for continuous or semi-continuous treatments.
• conventional machinery for treating textiles and garments with liquors including dollies, winches, beam dyeing equipment, package dyeing machinery, hank dyeing machinery, top dyeing equipment, washing and laundering equipment and dry-cleaning machinery for batchwise treatments, and including pad mangles, lick rollers, spray units, continuous cloth washing units, backwashing machines and solvent scouring machines for continuous or semi-continuous treatments.
• the complexed titanium compound may'be added directly to the treatment liquor or alternatively it may be formed in situ.
• Compounds which may be added directly to the treatment liquor include fluorotitanates oxalates and titanium citrates, or alkali metals or ammonia.
• a complex may be formed in situ by treating a soluble titanium salt, for example titanium tetrachloride with a source of fluoride ions or with an organic chelating agent, for example oxalic, or'preferably citric or tartaric acid.
• a soluble titanium salt for example titanium tetrachloride
• an organic chelating agent for example oxalic, or'preferably citric or tartaric acid.
• Compounds which may be used as sources of fluoride ions include sodium and potassium fluorides or bifluorides and ammonium bifluoride.
• a water soluble fluoroborate e.g. ammonium fluoroborate, may also be used as the source of fluoride ions
• the treatment can be carried out at temperatures in the range 20-l30C and at pH of less than 4 and preferably less than 3.5.
• the pH value can readily be adjusted by adding a strong mineral acid, for example hydrochloric acid, or an acidic substance such as ammonium bifluoride.
• fluoride complexes can be carried out with good results at room temperature, it is preferred in the case of organic chelate complexes to work at an elevated temperature.
• the titanium complex can be applied to the fibres to be treated by any conventional method, i.e. by any method heretofore known or described in the literature for applying water-soluble compounds, for example by the pad-dry, pad-steam," stray-'nip-dry,” dripnip-dry or exhaustion methods.
• pad-dry as used herein means the method of applying a liquor or paste to fibres to be treated either bypassing them -term exhaustion means the method of treating the fibres in a bath with a solution of the active substance until the substance is substantially completely taken up, and subsequently drying the fibres.
• pad-steam means the application of the treating liquor by the previously described padding technique followed by steaming at 100l20C.
• drip-nip-dry means the method of immersing the fibres into the treating bath, passing them through a nip, and subsequently drying them.
• flame-retardant agents previously known or described in the literature may be applied provided that they do not interfere with the titanium treatment.
• antimony trifluoride and antimony potassium tartarate can be applied to the wool by exhaustion. Aluminium compounds may also be applied to the wool.
• the present process may be carried out at the same time as dyeing, provided that the dye is capable of exhausting onto wool with level results at pH values below 5.
• Acid levelling, l:l pre-metallised dyes and certain reactive dyes can be used and there is no need to add additional formic or sulphuric acid as is conventional when using these dyes since the pH of the dyebath is already sufficiently low.
• Glaubers salt should preferably not be added to the solution since it interferes with the exhaustion of the titanium complex, but organic non-ionic levelling agents, for example Avolan SC or Albegal B can be used. Acid milling and 1:2 premetallised dyes cannot be applied satisfactorily at the same time as the titanium treatment.
• the dye When using an acid milling dye, the dye can first be exhausted preferably at the boil from the dyebath, the temperature of the dyebath is then reduced to, for example 70C, the complexed titanium compound is then added, and the bath is then further heated until the titanium complex has exhausted onto the wool.
• the dyeing operation must be carried out after the titanium treatment, otherwise complex formation between titanium in solution and the dye can give rise to ts laleew
• the acid dyes which can be used are water-soluble compounds of, for example, the monazo type or a triphenylmethane or anthraquinone derivative.
• Acid milling dyes form a class of dyestuffs which have greater molecular weight and fewer solubilizing groups than the acid levelling dyes. There is no rigid distinction between the milling class ofdyes and the levelling class, and many dyes have intermediate properties. Milling dyes are generally applied at a pH of 4-5.
• the premetallised dyes comprise a class of dyes having 0,0'-dihydroxy azo, O-amino-Ohydroxy azo or O-carboxyl-Ohydroxy azo groups which are coordinated to a metal atom, for example chromium or cobalt.
• the dyes may be used as 1:1 complexes.
• the dyes that may be employed include reactive dyes, e.g. those that react with the fibres and become covalently bonded to them, and such dyes give a high degree of fixation on the fibres.
• Dyestuffs falling within this class can incorporate the following groups:
• the treatment according to the invention has the further advantage that it is compatible with fluorocarbon oil-and-water repellent treatments for upholstery fabrics for use, for example, on aircraft seats.
• Fluorocarbon resins for example FC-2l4, FC 208, FC 218, all available from the 3M Company can be applied preferably in the presence of an extender, for example Phobotex FTN (CIBA).
• the titanium and fluorocarbon can be applied simultaneously by padding followed by drying at a temperature of at least C, further heating for a period and at a temperature sufficient to cure the resin, washing and drying.
• the titanium treatment can be also applied before or after the water and oilrepellent treatment.
• Undyed wool which has been treated in accordance with the invention exhibits apale yellow color. Such a discolouration is a disadvantage when it is desired to produce a natural-wool-colored or pastel-colored product, and can be reduced or prevented according to the invention by after-treatment of titanium treated fibres with a fluoride solution, a solution containing, for example, alkali metal or ammonium fluoride or bifluoride.
• the fibres are first treated with a titanium complex which can be titanium citrate, potassium titanium oxalate or a complex formed in situ between titanium tetrachloride and a chelating agent, especially oxalic, citric or tartaric acid.
• the fibre is conveniently applied to the fibre in a liquor ratio of 1:20 and preferably not more than 1 :30 by exhaustion at a pH of less than 4, preferably less than 3.5.
• the citric acid is preferably at a concentration of 4%.
• Exhaustion of the titanium compound is normally complete after boiling for a period of 5-30 minutes, generally about minutes.
• a dyestuff can be applied to the fibre in admixture with the titanium compound provided that it exhausts at a pH of less than 4 with level results, otherwise the titanium treatment should be carried out as a pretreatment before dyeing.
• Chrome dyestuffs in particular should always be applied after flame-resist treatment since they complex in solution with the titanium compounds and may then give rise to a color change.
• the fibre is then treated with a solution ofa fluoride preferably ammonium bifluoride.
• the treatment is preferably carried out in acid solution, conveniently at a pH of about 4.
• acid solution conveniently at a pH of about 4.
• the concentration of the ammonium bifluoride is preferably 0.2 to g/litre and the solution is left in contact with the fibre for 5-30 minutes.
• the treated fibre is then rinsed with water, hydroextracted by passing it through a nip and dried.
• a suitable aqueous fluoride solution contains 4% w/v ammonium bifluoride and 4% w/v sodium metabisulphite or 4% sodium formaldehydesulphoxylate and can provide substantially complete removal of the yellow colour.
• Table 1 illustrates the effect of treating carpet yarns firstly by exhaustion with a solution containing potassium titanium oxalate or titanium tetrachloride and oxalic, citric or tartaric acids and subsequently with a solution containing ammonium bifluoride.
• the results show that with increasing titanium concentration the yellowness index increases, the increase being most marked when using oxalic acid and least marked when using citric acid.
• TEST METHODS freed from the dyestuff is treated with 3' ml of 3% hydrogen peroxide. A yellow color develops which indicates the amountof titanium present in the solution.
• the degree of exhaustion was estimated using quantitive colorimetric estimation at a wavelength of 410 m.
• the amount of titanium and aluminium exhausted on wool during the flame-resist treatment can be estimated as ash content (metal oxides).
• ash content metal oxides
• the ash content of the untreated wool should always be estimated and the difference between the ash content of flame-resist treated and untreated wool indicates the total amount of metal oxides exhausted on wool during the treatment. This method is especially useful when the flame-resist treatment is performed simultaneously with dyeing and the dyestuff can interfere with the titanium hydrogen peroxide reaction.
• the flame-resistance of textile fabrics can be measured by the Vertical Flame Test (A.A.T.C. Test Method 34-1969, Fire Resistance of Textile Fabrics) which involves suspending a conditioned (65% relative humidity) strip of the fabric to be tested in a flame of a Bunsen burner for twelve seconds and determining the length of the charred portion of the fabric and the burning time.
• the flame-resistance of carpets can be measured by the Tablet Test (U.S.
• Titanium tetrachloride (50%) 3.0% o.w.f.
• Citric acid 4.0%
• Aluminium chloride 4.0% o.w.f.
• EXAMPLE ll This Example illustrates the simultaneous treatment of loose wool stock with a flame-resist agent and also the application of dye.
• a loose wool stock was boiled for 45 minutes in a package dyeing machine with a solution containing:
• Neopolar Yellow 4GL is an acid levelling dye.
• the loose stock was then rinsed, dried, spun to a yarn and converted into a carpet having a 2-inch pile and a weight of 36 oz/sq.yd.
• the carpet was then tested for flame-resistance according to the Tablet Test previously referred to, both after dyeing and after it had been cleaned times according to the procedure described in DOC FF 1-70.
• the carpet was found to have excellent resistance both before and after cleaning, thus showing that the effect of the treatment has considerable resistance to removal by the cleaning step.
• EXAMPLE Ill This example illustrates the application of a flameresist treatment to a previously manufactured carpet.
• the pile ofa carpet having a 2-inch pile and a weight of 36 oz/sq.yd. was sprayed with'a solution containing potassium titanium oxalate g/litre), tartaric acid (10 g/litre), antimony trifluoride (20 g/litre). and Tergitol Speedwet (Union Carbide; 1 g/litre), until the pile increased 50% by weight.
• the pile was then pressed lightly to ensure-penetration of the yarns by the solution, after which it was dried.
• the treated carpet was then found to pass the Tablet test described above.
• EXAMPLE IV The following composition was applied to a woollen fabric as an aqueous solution by means of a pad mangle:
• Titanium tetrachloride (50% aqueous solution) .1) on the weight of ool (o.w.w.) Ammonium bifluoridc I 5/1 U. ⁇ '. ⁇ V. Formic acid (80% aqueous solution) 2; o.w.w.
• the fabric was dried. It was subsequently rinsed for 15 minutes in water at 30C at a liquor ratio of 1:20, hydroextracted and dried.
• the fabric was tested for flame-resistance by means of the Vertical flame. test (A.A.T.C. Test Method 34-1969, Fire Resistance of Textile Fabrics) and exhibited a satisfactory flameresistance.
• the test involves suspending a conditioned (65% relative humidity, 20C) strip of the fabric to be tested in the flame of a Bunsen burner for 12. seconds and determining the length of the charred portion of the fabric and the burning time.
• the treatment was found to be fast to at least 10 washings (45C. 15 minutes, Philips automatic washing machine, Woolmark programme), and at least 10 dry cleanings (28C, 15 minutes, liquor ratio 1:20, Perklone, launderometer).
• EXAMPLE V The following composition was applied to a woollen textile fabric as an aqueous solution by means of a pad mangle:
• Titanium tetrachloride (50% aqueous 1.5% o.w.w. solution) Ammonium bifluoride 1.0% o.w.w. Formic acid aqueous solution) 2.0% o.w.w.
• EXAMPLE V1 The following composition was applied to a woollen textile fabric as an aqueous solution by means of a pad mangle:
• Titanium tetrachloride (50% aqueous solution)
• Antimony trichloride 1.5% o.w.w.
• Ammonium bifluoride 1.5% o.w.w.
• Formic acid 85% aqueous solution
• Example V The fabric was subsequently treated as in Example V. In the Vertical Flame test it exhibited a char length 20% less than the fabric of Example V.
• the treatment EXAMPLE vn The following composition was sprayed onto a readymade shag-pile carpet:
• Titanium tetrachloride (50% aqueous 3% o.w.w. solution)
• Ammonium bifluoride 1.5% o.w.w.
• Formic acid 85% aqueous solution
• the treated carpet was passed through a nip and then dried.
• the flammability measured by the Tablet test (U.S. Federal Specification DOC FF 1-70) was satisfactory.
• the Tablet test for carpets involves conditioning a specimen of the carpet at 105C for 2 hours, igniting a time-burning Methenamine (hexamethylene tetramine) tablet on the surface of the carpet, and observing the spread of flame over the surface of the carpet). The carpet pile did not burn away and no spread of flame over the surface fuzz of the unworn treated carpet was observed.
• the treatment was fast to washings (each min., 60C, liquor ratio 1:20, Hotpoint washing machine).
• the composition imparts a soil-repellency which is believed to be due to the presence of titanium compounds on the fibre surface.
• Sodium or potassium bifluorides can be used in place of the ammonium bifluoride, and can be applied to the carpet as described herein.
• EXAMPLE V111 Wool top (100 lbs) was treated by exhaustion with TiCl (50%) 3% o.w.w. and citric acid (4% o.w.w.) simultaneously withdyeing [Xylene light yellow 29 (Sandoz acid levelling dyestuff)].
• TiCl 50% 3% o.w.w.
• citric acid 4% o.w.w.
• the titanium tetrachloride and the dyestuffs were completely exhausted after 30 min. boiling.
• the dyestuff exhaustion was approximately 510% higher than with the same dye; without the addition of TiCL, and the dyeing was level.
• the wool top was spun into a yarn.
• a very open shag pile carpet made from the treated and dyed yarn easily passed the Tablet test. Color fastness to light, water, perspiration and washing (40C) is the same as with the dyed but untreated yarn.
• EXAMPLE IX EXAMPLE X This example illustrates the simultaneous application to wool of a flame-resist treatment and a waterand oilresist treatment.
• composition was applied to a wool fabric by a pad mangle to wet pick up:
• lsopropanol (wetting agent) F0214 (Fluorocarhon resin made by the 3M Company) 0.5% o.w.w. 2.0% o.w.w.
• Phobotext FTN (ClBA) 0.5% o.w.w. Titanium tetrachloride 5.0% o.w.w. Ammonium bifluoride 2.5% o.w.w. Formic acid (85% aqueous solution) 2.0% o.w.w.
• the fabric was then dried at C for a period of 3 minutes and then maintained at 165C for 4 minutes to cure the fluorocarbon resin.
• the fabric was then rinsed on a winch at 20C with water at a liquor ratio of 1:30 for a period of 15 minutes, and then dried at 120C for 3 minutes.
• the dried fabric was tested by the Vertical test and had a char length of 2.6 ins. and a burn time of 5 seconds. It exhibited satisfactory resistance to water and oils as tested by the spray and oil-rating test.
• EXAMPLE X1 This example illustrates the application of a flameresist treatment by the pad-steam technique to a previously manufactured shag pile carpet.
• the carpet was impregnated with the following solution to a pick-up of 400%.
• EXAMPLE XII This example illustrates the application of a'flameresist treatment by the drip-nip-dry technique of a wool sheep-skin used floor-covering and car seat cover.
• the sheep-skin was impregnated with the following solution:
• the sheep-skin was squeezed to a wet pick-up of between rollers and dried at 50C in order to not damage and harden the skin. After dyeing the sheep-skin was rinsed with water at 25C for 15 minutes in order to remove the residual chemicals, which could impair the soft wool handle. After rinsing, the sheep-skin was hydroextracted and dried at 50C.
• the treated sheep-skin passed the Tablet test.
• the difference between the flammability properties of the treated and untreated sheep-skins was very significant, because of the very open pile construction and loose fibre being readily available.
• With the untreated sheepskin no single fibre remained after the Tablet test, while with the treated sheep-skin only a surface flash of 2 ins. in diameter appeared followed by immediate selfextinguishing of the flame-resist treated wool fibre.
• EXAMPLE XIII This example describes the application of the dipnip-dry technique for the continuous flame-resist treatment of loose wool stock in the last bowl of the raw wool scouring machine (leviathan).
• the Tablet test showed a significant degree of flameresistance when compared with the same untreated wool fibres.
• part of the treated loose stock was rinsed in a separate bowl with water for 15 minutes at 25C and dried.
• the treated and rinsed loose wool stock passed the Tablet test.
• EXAMPLE XIV This example illustrates the exhaustion treatment of a wool-nylon (80/20) blend knitted garment.
• the garment was treated in a side-paddle dyeing machine with the following chemicals for 45 minutes at the boil:
• the Vertical Flame Test showed a burning time of 1 sec. and char length of 3.5 ins., values easily meeting the specification (Max. burn time sec., max. char length 8 ins.).
• EXAMPLE XV A wool blanket containing 15% of cotton in warp direction was treated by the exhaustion treatment on a winch with the following chemicals:
• the temperature of the bath was brought to the boil at a rate of 40C/min. and boiled for 45 minutes. After checking the exhaustion of the titanium citrate complex the blanket was rinsed and dried.
• the citric acid was dissolved in warm water in bucket and the titanium tetrachloride solution was added to the dissolved citric acid in the bucket while stirring.
• the titanium citrate complex prepared in situ was added to the bath, which was brought to the boil and kept at the boil for 45 minutes. After rinsing and drying a knitted fabric was prepared from the treated yarn and tested by the Vertical Flame Test. The burning time (1 sec.) and char length (2.5 ins.) indicated a sufficiently effective flame-resist effect.
• Titanium tetrachloride (50%) Citric acid 43 cm. 15 cm.
• Example XIX The procedure of Example XVIII was repeated with a sample of undyed wool and in the absence of a dyestuff in admixture the titanium. After the titanium treatment the yarn was treated with 4% ammonium bifluoride o.w.w. for 15 min. at 50C. The aftertreatment completely removed the slight yellow color. A shag pile carpet made from the fluoride after-treated yarn easily passed the Tablet test. A conventional carpet test by the Air Registration Board Specification 8 had a char width of 2 ins. (untreated 3 ins.). The same carpet without any backing tested by the Vertical Test had a char length of 1 in. and burning time 0 sec. (untreated char length 2.7 ins., burning time 23 sec.).
• the solution was then boiled for 45 minutes and the treated yarn was rinsed twice, hydroextracted and dried. It was fabricated into a very open shag pile carpet which easily passed the Tablet test.
• a process for improving the flame resistance of natural and synthetic polyamide fibres which comprises wetting the fibres with an aqueous solution of a complex compound of titanium consisting essentially of titanium complexed with fluoride ions, a dior polycarboxylic acid organic chelating agent or hydroxycarboxylic acid organic chelating agent having a pH less than about 4 until the fibres have taken up at least 0.2% by weight of the complex compound of titanium,-

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

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• 1971
  • 1971-01-29 GB GB351671*[A patent/GB1372694A/en not_active Expired
  • 1971-10-13 IE IE1282/71A patent/IE35724B1/xx unknown
  • 1971-10-14 DK DK497871AA patent/DK139481B/da unknown
  • 1971-10-18 IL IL37954A patent/IL37954A/xx unknown
  • 1971-10-18 CA CA125,342A patent/CA987858A/en not_active Expired
  • 1971-10-19 US US00190665A patent/US3857727A/en not_active Expired - Lifetime
  • 1971-10-20 AU AU34833/71A patent/AU452528B2/en not_active Expired
  • 1971-10-20 SE SE7113302A patent/SE385598B/xx unknown
  • 1971-10-21 SU SU7101707883A patent/SU576971A3/ru active
  • 1971-10-21 FI FI2976/71A patent/FI55059C/fi active
  • 1971-10-21 CH CH1542071A patent/CH557918A/xx unknown
  • 1971-10-21 CH CH1542071D patent/CH1542071A4/xx unknown
  • 1971-10-21 BE BE774257A patent/BE774257A/xx not_active IP Right Cessation
  • 1971-10-21 NO NO3907/71A patent/NO138700C/no unknown
  • 1971-10-22 FR FR7138001A patent/FR2111773B1/fr not_active Expired
  • 1971-10-22 NL NL7114569.A patent/NL163579C/xx not_active IP Right Cessation
  • 1971-10-22 JP JP46083428A patent/JPS5017596B1/ja active Pending
  • 1971-10-22 ES ES396678A patent/ES396678A1/es not_active Expired
  • 1971-10-22 AT AT918771A patent/AT317826B/de not_active IP Right Cessation

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