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
  • D06M13/244—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
  • D06M13/285—Phosphines; Phosphine oxides; Phosphine sulfides; Phosphinic or phosphinous acids or derivatives 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
  • 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
• • 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
  • Y10T442/2672—Phosphorus containing
  • Y10T442/2689—A phosphorus containing compound and a nitrogen containing compound

Definitions

• TETRAKIS (HYDROXYMETHYL) PHOSPHONIUM CHLORIDE Inventors: Robert B. Eggenweiler, West Seneca; James J. Duffy, Buffalo, both of NY.
• ABSTRACT A process for imparting flame-retardant character to cellulosic containing material has been devised in which the cullolosic material is impregnated with an aqueous solution of a tetrakis(hydroxymethyl)phosphonium compound, preferably partially neutralized tetrakis(hydroxymethyl)phosphonium chloride, the impregnated material is at least partially dried, e.g., to about 5 to 25 percent by weight moisture retention, without fixation of the phosphonium compound on the material, the partially dried material is cooled and then treated with dry ammonia gas optionally in the presence of water vapor whereby the phosphonium compound is cured on the material and a fireretardant character is imparted thereto.
• a tetrakis(hydroxymethyl)phosphonium compound preferably partially neutralized tetrakis(hydroxymethyl)phosphonium chloride
• This invention relates to a processof producing flame retardant cellulosic containing materials. More particularly it relates to a process of incorporating a phospho-- rus containing polymer in and on cellulosic containingmaterials.
• U. S. Pat. No. 3,236,676 discloses a process wherein a phosphonium compound is fixed on the cellulosic material prior to curing with an agent such as ammonia.
• the process disclosed therein involves the steps ofimpregnating cellulosic materials with a solution of a tetrakis (hydroxymethyl) phosphonium salt, having a pH in the range of 3 to 9.5, heating the material between 100 C and 180 C., to dry the material and to fix the phosphonium salt on the fiber and thereafter treating the heat treated material with ammonia to cure the phosphonium salt on the material.
• Another object is to devise a simple, economical, and effective process for treating cellulosic containingw materials with aqueous solutions of tetrakis(hydroxymethyl) phosphonium compounds to render such materials fire-retardant.
• cellulosic containing material is impregnated with a solution containing tetrakis(hydroxymethyl )phosphonium chloride, or a partially neutralized derivative thereof, the impregnated material is heated to at least partially dry it, without fixation of the phosphonium compound thereon, and then, after cooling the heated material,
• a preferred mode of carrying out the process of the present invention comprises padding a cotton cloth with an aqueous solution of about 20 to about 40 percent by weight of tetrakis(hydroxymethyl)- phosphonium chloride which has been partially neutralized with about to about percent of the stoichiometric amount of caustic alkali.
• the padded cloth containing about 25 to percent of its weight of the padding liquor, is dried at least partially, preferably to about 5 to about 25 percent moisture retention, without fixation of the phosphonium compound on the cloth, the partially dried cloth, is cooled and then is exposed to gaseous ammonia, preferably in the presence of water vapor to fix the phosphonium compound on the cloth, and thereby to impart thereto fire-retardant properties which are fast to repeated washings.
• the treated cloth is preferably rinsed with an aqueous solution of an oxidizing agent, such as hydrogen peroxide, sodium perborate and the like, which after treatment removes color and odor from the treated material.
• the padding solution used may be merely an aqueous solution of tetrakis(hydroxymethyl)phosphonium chloride. However such solutions have a pH value of about 1 and may be detrimental to the textile material being treated. Preferably the solution is partially neturalized to a pH within the range of about 5 to 6.5. Alkaline materials such as sodium or potassium hydroxides, soda ash, organic amines such as triethanolarnine, triethyl amine and the like can be used to adjust the pH of the padding liquor.
• the impregnated cloth It is preferred to dry the impregnated cloth, to remove at least a portion of the aqueous liquor.
• This drying step can be effected in a drying oven, by moving the padded cloth over heated cans, by hot pressing the cloth, and the like.
• the impregnated material is dried to a 5 to 25 percent by weight moisture retention. It has been found that this partial drying of the impregnated material does not result in the fixation of any noticable amount of the phosphonium compound on the fiber.
• the impregnated material can be dried substantially completely, at a moderate temperature, e.g., about 200 degrees Fahrenheit, without fixation of the phosphonium compound, and thereafter the dried material cooled by rewetting before treating with ammonia to fix the phosphonium compound.
• a moderate temperature e.g., about 200 degrees Fahrenheit
• EXAMPLE l A 40 percent aqueous solution of tetrakis(hydroxymethyl) phosphonium chloride was partially neutralized with about 80 percent of the theoretical amount of sodium hydroxide. The resulting solution was used to pad samples of 4.5 ounce per square yard cotton flannel. The padded cloth was then heated in a 200 oven for times specified in the following table. The partially dried cloth was extracted with water. A sample of the extract was evaporated to dryness and the residue analyzed.
• aqueous solution containing 27.5 percent of tetrakis-(hydroxymethyl)phosphonium chloride was neutralized with about percent of the stoichiometric amount of sodium hydroxide to give 27.5 percent of the partially neutralized species.
• Samples of 4.5 ounce per square yard of cotton flannel were impregnated with this solution to a wet pick up of about -95 percent.
• the impregnated cloth samples were dried for various periods at 200 and then exposed to gaseous ammonia to cure the resin.
• the treated material was then scoured in an aqueous alkaline bath containing sodium perborate and dried. Two of the samples were treated thusly directly from the drier with a relatively short, i.e., about 2 to 3 minutes cooling period.
• One sample was removed from the drier, held in air for at least one minute, passed over a perforated pipe emitting steam and then exposed to gaseous ammonia.
• the partially dried samples were cooled slightly and then exposed to a mixture of gaseous ammonia and wet steam by passing the samples over a perforated pipe emitting the steam-ammonia mixture.
• the cured samples were scoured in an aqueous alkaline bath containing sodium perborate.
• EXAMP E 4 An aqueous solution containing 22.5 percent of partially neutralized (85 percent) tetrakis(hydroxymethyl)phosphonium chloride, was used to impregnate three samples of 4.5 ounce cotton flannel. The wet pick up of the three samples was 92.5, 91.7, and 94.5 percent respectively.
• the other two samples were heated at 200 for 1.5 and 3.0 minutes respectively and the partially dried cloth hung in air at ambient temperature for about 16 hours, and then cured.
• the resin add on of these two samples was 14.6 and 17.3 percent respectively.
• XAMP E5 An aqueous solution containing 22.5 percent of partially neutralized tetrak-is( hydroxymethyl )phosphonium chloride was used to impregnate samples of 4.5 ounce cotton flannel. The samples had an add on of between about 85 and 90 percent.
• the samples (three) were partially dried for one minute at 200, for 1.75 minutes at 200 and for 1.75 minutes at 250.
• the resin add on was determined to be minute at 200.
• the heated cloth was then exposed to a mixture of an ammonia gas and air to cure the resin on the cloth.
• the resin add on in this instance was 15.6 percent.
• the fire retardant characteristic of the treated cloth was substantially the same as that of the above samples. However, after 50 home washes, the fire retardance of this sample was substantially inferior to the above samples, the char increasing to about twice of that of the initial char length (3.94 inch initial; 6.58 inch after 50 home washes).
• a method for producing fire retardant cellulosic containing materials which comprises a. impregnating a cellulosic containing material with an aqueous composition comprising a tetrakis(hydroxymethyl)phosphonium compound or a partially neutralized derivative thereof,
• compound 8 The method of claim 1 wherein the phosphonium compound is tetrakis(hydroxymethyl)phosphonium chloride partially neutralized with from about '70 to about percent of the stoichiometric amount of a caustic alkali.

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

Applications Claiming Priority (1)

Publications (1)

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Family Applications (1)

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Cited By (8)

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Citations (5)

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• 0
  • BE BE790943D patent/BE790943A/xx not_active IP Right Cessation
• 1971
  • 1971-11-04 US US3775155D patent/US3775155A/en not_active Expired - Lifetime
• 1972
  • 1972-10-30 GB GB4998172A patent/GB1388696A/en not_active Expired
  • 1972-11-01 JP JP10984272A patent/JPS4856994A/ja active Pending
  • 1972-11-01 CA CA155,402A patent/CA990909A/en not_active Expired
  • 1972-11-02 FR FR7238788A patent/FR2158453B1/fr not_active Expired
  • 1972-11-03 NL NL7214855A patent/NL174074C/xx not_active IP Right Cessation
  • 1972-11-03 IT IT3128972A patent/IT970213B/it active
  • 1972-11-03 DE DE2253976A patent/DE2253976C2/de not_active Expired

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