Classifications

• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
  • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
  • D06M11/68—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
  • 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
  • D06M11/44—Oxides or hydroxides of elements of Groups 2 or 12 of the Periodic Table; Zincates; Cadmates
• • 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
  • D06M11/32—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
  • D06M11/47—Oxides or hydroxides of elements of Groups 5 or 15 of the Periodic Table; Vanadates; Niobates; Tantalates; Arsenates; Antimonates; Bismuthates
• • 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
  • D06M11/71—Salts of phosphoric acids
• • 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
  • D06M13/08—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with halogenated 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
  • D06M13/244—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 sulfur or phosphorus
  • D06M13/282—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 sulfur or phosphorus with compounds containing phosphorus
  • D06M13/292—Mono-, di- or triesters of phosphoric or phosphorous acids; 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
  • D06M13/322—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
• • 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
  • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
  • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
  • D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
  • D06M15/244—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated 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
  • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
  • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
  • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
  • D06M15/667—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing phosphorus in the main chain
  • D06M15/673—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing phosphorus in the main chain containing phosphorus and nitrogen in the main chain
• • 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
  • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
  • Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
  • Y10T442/20—Coated or impregnated woven, knit, or nonwoven fabric which is not [a] associated with another preformed layer or fiber layer or, [b] with respect to woven and knit, characterized, respectively, by a particular or differential weave or knit, wherein the coating or impregnation is neither a foamed material nor a free metal or alloy layer
  • Y10T442/2631—Coating or impregnation provides heat or fire protection
  • Y10T442/2656—Antimony containing
• • 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
  • Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
  • Y10T442/20—Coated or impregnated woven, knit, or nonwoven fabric which is not [a] associated with another preformed layer or fiber layer or, [b] with respect to woven and knit, characterized, respectively, by a particular or differential weave or knit, wherein the coating or impregnation is neither a foamed material nor a free metal or alloy layer
  • Y10T442/2631—Coating or impregnation provides heat or fire protection
  • Y10T442/2672—Phosphorus containing
  • Y10T442/268—Phosphorus and nitrogen containing compound
• • 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
  • Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
  • Y10T442/20—Coated or impregnated woven, knit, or nonwoven fabric which is not [a] associated with another preformed layer or fiber layer or, [b] with respect to woven and knit, characterized, respectively, by a particular or differential weave or knit, wherein the coating or impregnation is neither a foamed material nor a free metal or alloy layer
  • Y10T442/2762—Coated or impregnated natural fiber fabric [e.g., cotton, wool, silk, linen, etc.]
  • Y10T442/277—Coated or impregnated cellulosic fiber fabric

Definitions

• This invention relates to a method of imparting flame resistance to a cellulosic material, more particularly a cellulosic material of the class consisting of natural and regenerated celiuloses and mixtures thereof, and specifically to a textile comprising fibers of such cellulosic materials, as well as compositions used in such treatments and to the flame-resistant cellulosic products thereof.
• Agents or treatments for imparting flame resistance to normally flammable organic materials properly may be classified as 1) temporary, (2) semi-durable and (3) permanent or durable, based on their durability in providing continued resistance of the treated textile or other material to flame during use. See page 6 of the aforementioned book by Little for a more complete description of these classes.
• the present invention is concerned primarily with certain new and useful improvements in the permanent or durable agents or treatments of the kind aforementioned.
• the durable treatments heretofore used or sug gested have been of three general kinds or types:
• the present invention is based on our discovcry that fibrous cellulosic materials including those composed solely Or comprised mainly (that is, preponderan'tly by weight) of fibers of natural cellulose (that is, cellulosic materials of natural origin), regenerated cellulose (more particularly viscose rayons) and mixtures thereof can be rendered substantially permanently resistant to flame by suitably treating them with compositions of the kind hereinafter described.
• our treated fibrous cellulosic textiles in thread, yarn, fabric or other form are unique in that they are characterized not only by their substantially permanent flame resistance but also by their improved hand or feeling to the touch as compared with the hand of textiles that have been given a double-bath precipitation or a metallic oxidechlorinated body type of treatment, thereby increasing the field of utility of flame-resistant textiles. Furthermore, these properties are obtained without excessive tendering or the textile.
• the treated textile in general having a tensile strength (average of the sum of the tensile strength of the warp and filling) of at least of that of the untreated textile when similarly tested for tensile strength, and in many cases a tensile strength which is even higher than that of the untreated textile.
• flame-resistant, fibrous, cellulosic textile materials comprising or composed of fibers of natural cellulose, regenerated cellulose or a mixture thereof and which have a good hand, that is, a hand or feeling to the touch which meets the requirements of the trade, and good tensile strength characteristics are produced by impregnating the normally flammable cellulosic textile with certain materials in particular proportions or ranges of proportions which are critical in carrying the invention into efiect.
• a substantial proportion of the impregnant initially applied is fixedly held by the cellulosic textile after subsequent heat treatment and washing; hence the flame-resistant textiles of our invention properly may be designated as being of the "durable" type or kind.
• the "char length" (charred length) ordinarily is not more than about 6 inches, e. g. from 3 to 5% inches, when the textile material (e. g., cotton cloth or viscose rayon fabric) which has been treated and then subjected to 5 washes in neutral soap solution is one weighing 4 ounces about 8 inches e. g., the fabric which stantialiy less than 4 ounces, e. g., per square yard.
• a cellulosic material is impregnated with ingredients comprising (1) a finely divided, oxygen-containing substance of the group consisting of tin, titanium, antimony and bismuth oxides and mixtures thereof and (2) a thermally unstable, halogen-containing thermoplastic substance, more particularly a thermosplastlc substance containing at least by weight of combined halogen and capable of rupturing under heat at carbonhalogen bonds, the ingredients of (l) and (2). which together are designated hereinafter as (A), being employed in a weight ratio of 1 part of the former to from 0.6 to 20 parts, more particularly from 0.8 to 4 parts, of the latter.
• ingredients comprising (1) a finely divided, oxygen-containing substance of the group consisting of tin, titanium, antimony and bismuth oxides and mixtures thereof and (2) a thermally unstable, halogen-containing thermoplastic substance, more particularly a thermosplastlc substance containing at least by weight of combined halogen and capable of rupturing under heat at carbonhalogen bonds, the ingredients of (
• thermoplastic substances of (2) that may be employed, alone or in the form of mixtures thereof, are halogen-containing vinyl resins in which not less than 20% by weight of combined halogen is present, for instance, polyvinyl halides (e. g., polyvinyl chloride, polyvinyl bromide, etc.) polyvinylidene halides (e. g., polyvinylidene chloride, polyvinylidene bromide, etc.) copolymers of a a vinylidene halide (e.
• polyvinyl halides e. g., polyvinyl chloride, polyvinyl bromide, etc.
• polyvinylidene halides e. g., polyvinylidene chloride, polyvinylidene bromide, etc.
• copolymers of a a vinylidene halide e.
• halogenated e. g., chlorinated parailins containing not less than 20% by weight of combined halogen, more particularly from about 30 or 40% up to '70 or 75% by weight of combined chloride, bromine, or other halogen, etc.
• ingredients with which the cellulosic material is impregnated are (3) a water-soluble salt (or mixtures thereof) of an oxygen-containing acid of phosphorus wherein the phosphorus atom has a valence of 5, e. g., a guanidine phosphate, a diguanidine pyrophosphate, diammonium hydrogen phosphate, sodium polyphosphate, ammonium metaphosphate, pyrophosphates, etc., and (4) a water-soluble nitrogenous substance of the group consisting of urea, biuret, ammonium cyanate, ammonium dicyanimide and mixtures thereof.
• ingredients of (3) and (4) which together are designated hereinafter as (B), are employed in a weight ratio of 1 part of the former calculated as phosphoric acid (HJPOO to from i to 20 parts, more particularly of the latter, while the ingreclients of (A) and (B) are employed in a weight ratio of 1 part of the former to from 0.2 to l parts, more particularly from 1 to 3 parts, of the latter.
• the fibrous cellulosic material may be impregnated with the aforementioned ingredients in one or more steps or stages. Thus, it may be impregnated with a dispersion,
• an aqueous dispersion containing the ingredients mentioned in the preceding paragraph within the ranges of proportions therein specified.
• the treated cellulosic material is dried at a suitable temperature, e. g., at 40 or 50 to or 0., and then heated at a higher temperature within the range of C. (about 135 C.) to 200 C. (about 200 0.).
• a suitable temperature e. g., at 40 or 50 to or 0.
• a higher temperature within the range of C. (about 135 C.) to 200 C. (about 200 0.).
• the fibrous cellulosic material may be impregnated first with an aqueous solution containing a guanidine phosphate or other water-soluble salt of an oxygen-containing acid of phosphorus wherein the phosphorus atom has a valence of 5 (or a mixture of such salts) and one or more of the following: urea, biuret. ammonium cyanate and ammonium dicyanimide.
• the water-soluble salt of the acid of phosphorus and the urea or other water-soluble nitrogenous substance, which together are designated herein as (B), are employed in ratios by weight within the ranges mentioned hereinbefore.
• the impregnated fibrous material is dried, heated and washed as described in the preceding paragraph with reference to the one-step process. Thereafter it is treated, as by immersion in a bath containing the same, with a liquid dispersion, more particularly an aqueous liquid dispersion. containing a finely divided metallic oxide or mixture of metallic oxides of the kind aforementioned and, also, a thermally unstable, thermoplastic substance containing at least 20%, preferably at least 40%, of combined chlorine or other halogen and which is capable of rupturing under heat at carbon-halogen bonds, e. g., polymers and copolymers of vinyl chloride.
• the metallic oxide or oxides and the halogen-containing thermoplastic substance or substances, which together are designated herein as (A) also be employed in weight ratios within the ranges hereinbefore mentioned.
• the treated cellulosic material is dried, e. g., by allowing it to stand at room temperature or by heating it at an elevated temperature such, for instance, as at a temperature within the range of 40 or 50 C. up to 100 or 105 C.
• ingredients of (A) and (B) may be applied to the cellulosic material in one stage (i. e., a one-bath system) or in two stages (i. e., a twobath system); or, in other words, in the form of at least one and not more than two aqueous liquid compositions containing the same.
• the aqueous composition containing the ingredients of (B) have a pH of from about 3 to about 10, more particularly a pH within the range of about 3 /2 or 4 to about I or 8, since at the lower pH values (below about 3) the tensile strength losses in the treated goods are excessive while at the higher pH values (above about 10) the treated textiles have much poorer fire resistance.
• the ingredients of (A) and (B) be employed in a weight ratio of 1 part of the former to from 0.2 to 8 parts, e. g., from 0.5 to 6 parts, of the latter.
• the total amount of the ingredients of (A) and (B) with which the cellulosic material, e. g., a cotton or viscose rayon textile material, initially is impregnated is sufllcient to impart flame resistance thereto upon heating within the range of 135 C. to 200 C. and thereafter washing to remove any residual water-soluble substances.
• the total amount of the ingredients of (A) and (B) with which the cellulosic material is impregnated advantageously is such that the finished flame-resistant textile contains from about to about 50% by weight (which in some cases may be as high as about 75% by weight when the matter of the hand of the treated material is relatively unimportant), based on the dry weight of the untreated textile, of washfast impregnant.
• a preferred method of applying to fibrous cellulosic materials the ingredients used in practicing our invention is in the form of an aqueous dispersion containing the same.
• the amount or solids in such a dispersion may be varied as desired or as conditions may require, but usually the solids constitute from about 40% to about 70% by weight of the dispersion.
• a dispersion having excellent storage stability and which is dilutable with water to any desired extent, e. g., to about 50 or 55% by weight of solids, may be prepared, for example, as disclosed and claimed in the copending application of Maurice R. Burnell and William J. Van Loo, Jr., Serial No. 64,418, filed concurrently herewith.
• the first bath is prepared by dissolving in water the proper proportions of (l) guanidine phosphate or other water-soluble salt of an oxygen-containing acid of phosphorus in which the phosphorus atom has a valence of 5 and (2) urea or other water-soluble nitrogenous substance of the group previously described.
• This bath should be within a pH range of from about 3 to about 10.
• the bath also may contain a small amount, advantageously not over 7% by weight of the ingredients of (l) and (2), of a polyalkylene polyamine, preferably such a polyamine which is normally a solid or which has a boiling point substantially above 200 C., e.
• ingredients are dissolved in water merely by stirring and heating at a suitable temperature, e. g.. at 40 C. to 70 C. or higher.
• concentration of ingredients in the aqueous bath may be varied as desired or as conditions may require, but usually they constitute from about 30% to about 50% by weight of the aqueous solution.
• the composition of a typical bath is as follows:
• a dispersion of a polyvinyl halide polymerization product more particularly a polyvinyl chloride polymerization product, e. g., polyvinyl chloride itself or a vinyl chloride copolymer comprising mainly vinyl chloride, for instance a copolymer of, by weight, to 99% of vinyl chloride (in the copolymer molecule) and 20 to 1% of vinylidlne chloride.
• a lower alkyl acrylate e. g., methyl, ethyl, etc., acrylates
• vinyl ester of an aliphatic monocarboxylic acid e.
• thermoplastic substance containing at least 20% by weight of combined halogen and capable of rupturing under heat at carbon-halogen bonds.
• the mixture is thoroughly agitated until a homogeneous liquid composition or dispersion is obtained.
• concentration of solids in this dispersion may be varied as desired or as conditions may require. but usually they constitute from about 10% to about 30% by weight thereof.
• any suitable apparatus may be employed in applying the treating composition (used in a. one-bath process) or compositions (used in a two-bath process) to the cellulosic material.
• the dry or substantially dry cellulosic textile to be treated may be immersed in the aqueous composition or compositions and then passed through pressure rolls, mangles or centrii'ugal extractors to secure uniform impregnation and a controlled removal of the excess material.
• the cellulosic textile in fabric or other form also may be impregnated by other methods, e. g., by spraying.
• the wet pick-up of the composition (one-bath process) or compositions (two-bath process) by the textile may range, for example, between about 50% and about 150% by weight of the textile undergoing treatment.
• the pick-up of the treating agent by the celluloslc textile material is adjusted so that the finished textile contains from about 10 to about 75%, usually from 10 to 50% by weight, based on the dry weight of the untreated textile, of washfast impregnant.
• the matter of hand of the finished textile is important, it generally contains not more than about 50%, e. g., from 10 or 15% to 30 or 40%, based on the dry weight of the untreated textile. of washi'ast impregnant.
• the treated material After impregnating the cellulosic textile with an aqueous dispersion containing the ingredients of both (A) and (B) or with a solution containing the ingredients of (B) only, the treated material is dried to remove most or substantially all of the liquid present therein, after which it is heated at a higher temperature of the order of about C. to about 200 C. During this latter heat treatment a substantial loss of solids takes place, which may be as much as one-half to twothirds of the total weight of the ingredients of (B) with which the cellulosic material initially was impregnated.
• the amount of solids in the textile as initially impregnated should be sufficiently high to allow for this weight loss of solids during the heat-treating and washing steps.
• EKMLEI This example illustrates the preparation and use of a single-bath or "pad liqul in carrying the present invention into effect.
• the aqueous dispersion of the vinyl chloride copolymer may be, and preferably is, the product which is available from the B. F. Goodrich Chemical Company, Akron, Ohio, under the trade name of "Goon Latex 1-15."
• the resulting dispersion is added to the solution of the other ingredients, and the mass is well mixed to form a substantially homogeneous liquid composition which constitutes the pad liquor.
• the vinyl chloride oopoiymer used in the above aqueous dispersion and in dispersions referred to in other examples which follow, may be, for example, a copolymer of, by weight, about 80% to about 95%, e. g., about 85 to 90% of vinyl chloride and about 20% to about 5%, e. g., about 15% to of an alkyl acrylate, more particularly a lower alkyl acrylate such, for instance, as methyl, ethyl, propyl or butyl acryiate.
• a cellulcsic fabric such, for example as cotton cloth or a viscose rayon fabric is immersed in the pad liquor and immediately passed through two rubber squeeze rolls, the pressure being adiusted so that the so-called wet pick-up" of pad liquor by the fabric is approximately 120% by weight of the dry, untreated fabric.
• the untreated fabric e. g., by heating at 60-70 C.
• the dried fabric is heated at 160 C. for from 10 to minutes.
• the fabric is rinsed well in water to remove residual waterr 8 soluble substances therefrom, and again is dried (for instance at about 40 C.)
• EXAMPLE 2 This example illustrates the preparation and use of two baths in carryin our invention into effect.
• Both2 Parts Aqueous dispersion containing 55-58% by weight of a vinyl chloride copolymer such as described under Example 1 199
• Finely divided antimony trioxide 58 Dispersing agent more particularly the sodium salt of a condensation product of formaldehyde and a naphthalene sulfonic acid (Tamol P) 2 Water 741
• the dispersing agent is dissolved in one-half of the water and the finely divided antimony trioxide is added thereto under rapid stirring with a turbo-type mixer.
• the resulting dispersion is passed through a colloid mill in order to reduce the particle size to 1 micron or less.
• the aqueous dispersion of the vinyl chloride copolymer is diluted with the remainder of the water, the antimony trioxide dispersion added thereto, and the mass is well mixed to form a substantially homogeneous liquid composition.
• Treatment qf fabrics The same procedure is iollowed in treating a celluloslc fabric with the ingredients of Bath 1 as is described under Example 1.
• the treated. rinsed and dried fabric is their immersed in Bath 2 and immediately passed through rubber squeeze rolls, the pressure of which is adjusted so that the wet pick-up of the disgdrsion by the fabric is approximately by weight of the dry fabric resulting from the initial treatment.
• the wet fabric is dried at a suitable temperature, e. g., by heating at 60-'l0 C.
• the flame resistance of the treated fabric is of the same general order as that of fabrics which have been treated by the onebath process described under Example 1.
• Examples 3 to 16, inclusive, which follow, are illustrative of further variations in the ingredients and proportions thereof that may be used in the preparation of the treating compositions of our invention and of their use in imparting flame-resisting characteristics to cotton fabrics and rayon fabrics (other than cellulose ester rayon fabrics) using both onebath and two-bath processes.
• the procedure, in general, was as follows in the case of Examples 3 to 11, inclusive, 15 and 16, wherein the cellnloslc material treated was 80 x 80 cotton cloth.
• the dispersing agent was dissolved in the water, and the finely divided metallic oxide was incorporated slowly therein under high-speed stirring. After all the metallic oxide had been dispersed, the dispersion was passed through a colloid mill (clearance: 0.002 inch). The particle size of the dispersed solid was, for the most part. one micron or less. Aggregates having a particle size up to 3 microns may be present in the dispersion.
• the water-soluble salt of the oxygen-containing acid of phosphorus and the water-soluble nitrogenous substance which ingredients are more specifically identified in the various tables which follow, were dissolved in water. using heat if necessary to effect solution.
• the above dispersion of the finely divided metallic oxide and the dispersion of a thermally unstable, thermoplastic substance containing at least 20% of combined halogen and capable of rupturing under heat at carbon-halogen bonds e. g., a vinyl chloride polymerization product. more particularly a vinyl chloride copoiymer of the kind described under Example 1, were then added to the solution of the other two ingredients, and the resulting mixture was thoroughly agitated to obtain a substantially homogeneous aqueous dispersion.
• the first bath comprises an aqueous solution of the water-soluble nitrogenous substance and the water-soluble salt of the oxygen-containing acid of phosporus.
• the second bath contains the dispersion of finely divided metallic oxide and of the halogen-containing thermoplastic substance.
• the pad liquor of the second bath was applied to the fabric ,(pretreated as described above), using a wet pick-up of IOU-% unless otherwise specifled and dryin at 60-80 C.
• Washing procedure A small oscillating washing machine was used to wash the flame-resistant fabrics unless otherwise specifled. A one-pound load was used for each wash and the fabrics were washed for 15- minute intervals using 12 liters of 0.5% neutral soap solution at 6545 C. They were spun and rinsed for from 3 to 5 minutes in lukewarm water, spun and then rinsed further by hand. Flame tests were made after washing once and five times unless otherwise indicated.
• the burner had previously been regulated to a luminous flame 1 /2 inches high, and was placed under the suspended sample so that the end of the sample extended inch into the flame. The flame was held under the sample for 12 seconds and then extinguished. The duration of after-flaming or the sample was measured by means of a sto watch. Any tendency of the sample to after-glow or smoke was noted and timed if possible. The total length of char in inches was measured by the tear length produced with a tearing weight equal to approximately 10% of the tearing strength of the unburned fabric.
• the pH of the bath of pad liquor (pH of Bath 1 in the case of a two-bath process) as well as the pH of rinsings from the treated fabric after having been heated at between C. and 200 C. (that is, the so-calied "cured" fabric) were determined electrometrically with glass and calomel electrodes.
• the rinsings were prepared by soaking the cured fabric in a small volume of distilled water and squeezing out the excess liquid. This liquid was used in testing for pH. The fabric was then rinsed again in a large volume of running water.
• the tensile strength of the treated fabrics was measured with a pendulum tester, following the strip methods of Federal Specification CCC-T-lilla. Ravelled strips (one-inch wide) as well as one-inch treated cotton tape were tested.
• tic substance was a as that described under Exa lai'ly an about 85% alkyl acrylate plied by both a oneo n in 3 mu 1.
• the water-soluble salt 0! an oxygen-containing acid of phosphorus was mono.- guanidine phosphate the same as in Example 3. oxide and the vinyl chloride copolymer were use 70 in varying amounts and ratios of the one to the other. of a buffering agent, more particularly a polyalkylene polyamine and specifically hexamethylene tetramin taining the water- 78 two-bath application methods were used.
• ammonium cyanate and biuret were used either wholly in place of urea or in comg tg am 5 bination with urea in the case of biuret, the other i zi Se T bl ingredients being monoguanidine phosphate, antigfi z gt sgg ag; a 11 mom trioxide and a vinyl chloride copolymer water Remainder such as was employed in the prior examples.
• Table IV shows the ratios of ammonium dicy- Further information on the treatment and on o animide, ammonium cyanate and o! biuret plus the results obtained are given in Table II. urea to monoguanidine phosphate as such and Table I! Flame Test Vertical Per Cost Per Cent Total Dry A Per Time After Glow, Wei in mm For om Vinyl Add-On pH pH ent if i g Soc.
• ratio of urea to hexamethylene tetramine was EXAM-E '7 5 e ea. o fl d e Phosphate and In this example a diil'erent halogen-containing hexamethylene tetramine together are designated th rmoplastic substance, more particularly a as B."
• the weight ratios 01' A to B were varied U chlorinated paraflln containing about by 8 Shown in Table which 8180 gives further weight of combined chlorine, was used in place 01' information on the treatment and on the results a vinyl chl ride copolymer. Further details on obtained. weight percentages of ingredients ar given below:
• washing of the treated fabrics was done in pint Jars, each of which contained a 6-inch square sample of fabric, 20 steel balls and 200 m1. 0! a 0.5% neutral soap solution heated to 180 F. The jars were revolved for minutes.
• EXAMPLE 9 This example illustrates the use of other oxide and stannic oxide, instead of antimony trioxide in the treating compositions.
• the vinyl chloride copolymer (used in the form of an aqueous dispersion) was the same Geon copolymer treatment and the results obtained.
• MM llli 55!: a an .1 m mmm m m 3: e wmm Ga c r E I .7 H mm; 53% 7 m e emw m m wm iege u m w mi m m W W 2. s 0 a E4 tut 8 e n 22 e E fl mu m .u m 552m me H m rlna .ehe o m T 870 .6 m m mm m fiamfia n.
• v o t 5 s ma mm ma w n as i. can 232:8 h m em x m c m. um e W .boaeQsEneEoE .afissefiez m m hwm v. 52 5 m wwm a as m mm m ewemm mm w b e s im sfl o ode o ea-poem nm m m m m w naazocnsomom define: e e evv.
• ammonium dicyanimide or ammonium cyanate was used as the water-soluble nitrogeneous substance and monosodium or disheeting and rayon suiting, and the results of flame tests on both kinds of treated goods after being rinsed and after the aforementioned sodium phosphate as the water-soluble oxygenwashes.
• the rinsed and washed samples were containing acid of phosphorus.
• the halogencontaining thermoplastic substance was a vinyl chloride oopolymer such as was employed in prior examples.
• the ingredients were applied by a two-bath process, the second bath being an aqueous dispersion containing, by weight, 5.8% of $1120: and 11% of the aforementioned eopolymer. Further information on the treatment and the results obtained appears in Table Di.
• This example illustrates the results obtained with various concentrations (57%, 42.6% and 28.5% solids) oi the same treating ingredients in the same proportions used in the treating comosition of the prior example in imparting flame resistance to diflerent fabrics, more particularly to 100 x 60 untreated cotton cloth. cotton marquisette, rayon challis and rayon netting.
• the wet pick-up was approximately 80% by weight From Table arr it It will be noted in Table XII that the treatment of the rayon netting resulted, in all cases, in a substantial increase in the tensile strength of the treated fabric as compared with the untreated netting, the percentage increase being more than 21%. This was quite surprising and unexpected. and in no way could have been predicted.
• EXAMPLE 14 The treating composition used in this example was essentially the same as that employed in Examples 1 and 12.
• the aqueous dispersion was applied to various cotton fabrics by a one-bath process. Dryingand curing of the treated fabrics of the dry fabric. in the case of the cotton goods, were carried out under essentially the same conabout 100% by weight of the dry-fabric, in the case ditions described in the prior example.
• the of the rayon ehallis and about 150%, by weight of treated fabrics were given washes of 1 hour each the dry fabric, in the case of the rayon netting. in a 0.1% soap solution at 160 F.
• the results are The time of curing was 5 minutes at 160 C. shown in Table XIII.
• Antimony trioxide introduced in the form of an aqueous dispersion prepared as de- Essentially the same procedure was followed in applying the composition to 80 x 80 cotton cloth as that described under Example 1.
• a dispersing agent more particularly a sodium salt of a condensation product of formaldehyde and a naphthalene sulionic acid (Tamol P) 68.0
• Calcium carbonate in the form of a 40% aqueous dispersion using 0.5% of the aforementioned dispersing agent and water from the 160 parts mentioned in the formula.
• Additional examples include the halogenated diphenyls (e. g., p ntachlorodiphenyl, pentabromodiphenyl, etc.) and the halogenated (e. g., chlorinated, brominated, etc.) naphthalenes, which compounds contain at least by weight of combined chlorine, bromine or other halogen.
• halogenated diphenyls e. g., p ntachlorodiphenyl, pentabromodiphenyl, etc.
• naphthalenes which compounds contain at least by weight of combined chlorine, bromine or other halogen.
• vinyl chloride more particularly a copolymer of, by weight, from chloride and from about 20% to about 1% of an acrylic ester, specifically an alkyl acrylate such, for instance, as methyl, ethyl, propyl or butyl acryiate.
• the water-soluble nitrogenous substance, the water-soluble salt of an oxygen-containing acid oi. phosphorus, the metallic oxide and the halogen-containing thermoplastic substance be used in proportions within the ranges given in the eighth paragraph oi this specification. As shown by the numerous examples, especially in the tables, the proportions may be considerably varied within these broader ranges and still obtain a finished textile which is resistant to time even after numerous laundering or dry-cleaning operations and without excessive tendering (in many cases without any tendering) oi the textile. Furthermore, by using the ingredients within the proportions stated hereinbeiore, a flame-resistant textile having a good band or feeling to the touch is obtained. As will be readily appreciated by those skilled in the textile art, the matter of hand or feeling to the touch is, for most applications, oi considerable importance irom both saleability and utility standpoints.
• compositions of this invention may be modified by incorporating therein various modifying agents which aid in further improving the flame-resistant characteristics of the treated cellulcsic material or which facilitate the technique of application.
• the compositions may also contain minor amounts (e. g., from 1 to by weight of the total solids content) of such glow retardants as the glow-retarding borates, phosphates, pyrophosphates, etc., e. g., zinc borate, zinc phosphate, sinc ammonium phosphate, stannic phosphate, phenyl diamido phosphate, melamine pyrophosphate, etc.
• Agents which have a buifering eifect on the composition after being applied to the fabric or other textile e. g., calcium carbonate, magnesium oxide, hexamethylene tetramine and other polyalkylene polyamines, etc., may be incorporated into the treating compositions as desired or as conditions may require.
• the pH of the bath containing the ingredients of (B) in a two-bath process or the bath containing all of the ingredients in a one-bath procees should be adjusted to a pH (glass electrode pH) within the rail of item about 8 to about 10, e. g., a pH of from about 8% or 4 to about I or B, ii the pH of the aqueous composition contalning these ingredients (water-soluble salt of the oxygen-containing acid of phosphorus and water-soluble nitrogenous substance) is not initially within a pH range of from about 3 to about 10.
• the pH of the aqueous composition containing the ingredients of (B) is between 4 and 'l, e. g., about 6.
• the present invention is applicable to the production of a wide variety of flame-resistant cellulosic materials, e. g., wearing apparel or all kinds, especially children's clothes and clothing used by the armed forces, curtains, draperies, sheeting, furniture coverings, linings for electric blankets, net fabrics, non-woven fabrics, cbenilles, etc., and which are made of cellulosic materials such as are described in the first paragraph of this specification and elsewhere herein.
• Other applications of the flame-resistant products of our invention include those described in Chapters VII and VIII of the aforementioned book, edited by Little, entitled Flameproofing Textile Fabrics.
• flame resistance and flame-resistant as used herein and in the appended claims with reference to cellulcsic materials, specifically cellulcsic textiles, are used generically to include within their meanings treated cellulosic materials (e. g., treated fabrics) which, after ignition, will continue to burn at a relatively slow rate as well as those which, after ignition, will burn over only a limited area beyond that directly exposed to the source of ignition and which may be specifically designated as fireresistant" cellulosic materials. It will be apparent from the examples herein given that most of the products of our invention properly fall within the specific classification of fire-resistant cellulosic materials.
• textile and textile material as used generically herein and in the appended claims include within their meaning filaments. fibers, rovings, slivers, threads, yarns, twisted yarns, etc, as such or in woven, ielted or otherwise iormed fabrics, sheets, cloths and the like.
• a method of imparting flame-resistance to a cellulcsic textile material of the class consistin; or natural celluloses, regenerated celluloses and mixtures thereof comprising impregnating said material with an association of (1) an aqueous liquid composition having a pH of from about 3 to about 10 and containing (0) ingredients initially in the iorm of a water-soluhle salt of an oxygen-containing acid of phosphorus wherein the phosphorus atom has a valence of 5 and a water-soluble nitrogenous substance selected irom the group consisting of urea, biuret, ammonium cyanate, ammonium dicyanimide and mixtures thereof, said salt of an oxygen-containing acid of phosphorus and said nitrogenous substance being employed in a weight ratio of 1 part or the former calculated as HrPOe to from i to 20 parts of the latter, and (2) an aqueous liquid composition containing (0) ingredients comprising a finely divided, oxygen-containing substance of titanium, antimony and bismuth
• thermoplastic substance being employed in a weight ratio of 1 part oi the former to from 0.6 to 20 parts of the latter, and the said ingredients of (a) and (b) being employed in a weight ratio of 1 part of the latter to from 0.2 to 8 parts oi the former: heating the textile material after it has been impregnated with a composition comprising the aqueous liquid composition of (1) at a temperature within the range of about 135" C.
• the total amount of the compositions of (1) and (2) with which the cellulosic material initially is impregnated being such that the finished flame-resistant textile contains from about to about 75% by weight, based on the dry weight of the untreated textile, of washfast impregnant.
• cellulosic textile material is a viscose rayon textile material.
• An aqueous dispersion suitable for use in imparting flame-resistance to cellulosic textile materials selected from the group consisting of natural celluloses, regenerated celluloses and mixtures thereof, having a pH of from about 3 to about 10 and comprising (i) a finely divided, oxygen-containing substance of the group consisting of tin, titanium, antimony and bismuth oxides and mixtures thereof and (2) a thermoplastic halogen-ccntaining organic substance containing at least 20% by weight of combined halogen and capable of rupturing under heat at carbon-halogen bonds, the ingredients 01' (l) and (2), which together are designated hereinafter as (A), being employed in a weight ratio of 1 part of the former to from 0.6 to 20 parts of the latter and being dispersed in water containing ingredients initially in the form of (3) a water-soluble salt of an oxygen-containing acid of phosphorus wherein the phosphorus atom has a valence of 5 and (4) a water-soluble nitrogenous substance of the
• the aqueous dispersion of claim 6 wherein the finely divided oxygen-containing substance is antimony trioxide, the thermoplastic halogencontaining organic substance is a vinyl chloride polymerization product, the water-soluble salt of an oxygen-containing acid of phosphorus is monoguanidine phosphate and the water-soluble nitrogenous substance is urea.
• a method of imparting flame-resistance to a textile material comprising fibers of a cellulosic material of a class consisting of natural celluloses, regenerated celluloses and mixtures thereof, said method comprising impregnating said textile material with the composition of claim 6, drying the impregnated material, heating the dried material at a temperature within the range of 135 C. to 200 C. and washing the resulting material to remove any residual water-soluble substances therefrom, the total amount 01 said ingredients or (A) and (B) with which the cellulosic textile material initially is impregnated being such that the finished flame-resistant textile contains from about 10% to about 50% by weight, based on the dry weight 01 the untreated textile, of washfast impregnant.
• a method 01' imparting flame-resistance to a textile comprising fibers oi a cellulosic material oi the class consisting of natural celluloses, regenerated celluloses and mixtures thereof, said method comprising impregnating said textile with an aqueous dispersion having a pH within the range of 3 to 10 and comprising (1) a finely divided oxide of antimony and (2) a thermoplastic vinyl chloride polymerization product containing at least 40% by weight of combined chlorine, the ingredients 01 (1) and (2), which together are designated hereinafter as (A), being employed in a weight ratio oi 1 part of the former to from 0.6 to 20 parts of the latter and being dispersed in water containing ingredients initially in the form of (3) a water-soluble guanidine phosphate and (4) urea, the ingredients oi (3) and (4), which together are designated hereinafter as (B), being employed in a weight ratio 0!
• a method as in claim 9 wherein the watersoluble guanidine phosphate of (3) is monoguanidine phosphate.
• aqueous dispersion also contains a small amount, not exceeding about 7% by weight of the ingredients 01' (B), of a polyalkylene polyamine having a boiling point substantially above 200 C.
• a method of imparting flame-resistance to a textile comprising fibers of a cellulosic material oi the class consisting oi natural celluloses, regenerated celluloses and mixtures thereof, said method comprising impregnating said textile with an aqueous solution having a pH within the range of from 3 to 10 and containing ingredients initially in the form of (l) a water-soluble salt of an oxygen-containing acid of phosphorus wherein the phosphorus atom has a valence of 5 and 2) a water-soluble nitrogenous substance of the group consisting of urea, biuret, ammonium cyanate, ammonium dicyanimide and mixtures thereof, the ingredients of (l) and (2), which together are designated hereinafter (B), being employed in a weight ratio 01 1 part 01 the former calculated as 311904 to from 1 to 20.
• thermoplastic halogen-containing organic substance containing at least 20% by weight of combined halogen and capable oi rupturing under heat at carbon-halogen bonds
• the ingredients 01' (8) and (4) which together are designated hereinafter as (A), being employed in a weight ratio 1 part 01 the former to from 0.6 to 20 parts of the latter, the ingredients of (A) and (B) being employed in a weight ratio of 1 part of the iormer to from 0.2 to 8 parts of the latter, and the total amount of the ingradients of (A) and (B) with which the said textile is impregnated being such that the flnished flame-resistant textile contains from about 10% to about 75% by weight, based on the dry weight of the untreated textile, o! washi'ast impregnant.
• a method as in claim 15 wherein the watersoluble guanidine phosphate is monoguanldine phosphate.

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