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
  • 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
  • D06M15/39—Aldehyde resins; Ketone resins; Polyacetals
  • D06M15/423—Amino-aldehyde resins
  • D06M15/43—Amino-aldehyde resins modified by phosphorus compounds
  • D06M15/431—Amino-aldehyde resins modified by phosphorus compounds by phosphines or phosphine oxides; by oxides or salts of the phosphonium radical
• • 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

Definitions

• Phosphonium salts of the formula (HOCH P C- H OH.X wherein X is an anion are used in flame retardant finishes.
• Tetrakis(hydroxymethyl)phosphonium chloride (THPC) is a component of some flame retardant finishes for textile materials.
• THP tris(hydroxymethyl)phosphine
• the treated textile materials have flame retardant properties which are durable to repeated laundering but the finishes impart a stiff, boardy hand and cause an objectionable and sometimes severe strength loss in the treated fabric. Textile tensile strength, tear strength and abrasion resistance are reduced.
• My invention provides a flame retardant finish for cellulosic textile materials which imparts a soft hand to the material, i.e., it does not make the material stiff; the materials treated with the finish are durable to repeated laundering; and the finish does not reduce the resistance of fabric to wear.
• U.S. Pat. No. 2,937,207 teaches a process for manufacturing tetrakis(hydroxymethyl)phosphonium oxalate.
• the patent suggests that the products obtained according to the process of the invention can be used as flame-proofing agents for textiles and woods.
• my Example 4 below, when tetrakis(hydroxymethyl)phosphonium oxalate is used alone on fabric, the fabric burns even before laundering.
• the invention is a process for imparting durable flame retardant properties and a soft hand to cellulosic textile materials by applying an aqueous finish solution of tetrakis(hydroxymethyl)phosphonium oxalate and at least 1 organic nitrogenous compound having a trivalent nitrogen bearing at least 2 members comprised of hydrogen atoms and methylol groups, for example, urea, a melamine or a water soluble methylolated nitrogenous celluose reactant or mixtures thereof to the textile material and heating the textile material to effect a cure of the finish thereon; the finish compositions and the cel-lulosic textile material produced by my pro- DETAILED DESCRIPTION I have discovered that when an aqueous solution containing tetrakis(hydroxymethyl)phosphonium oxalate (TKS) and a nitrogenous compound having trivalent nitrogen bearing at least 2 hydrogen atoms or methylol groups is applied to cellulosic textile materials, the materials become flame
• aqueous solutions of tetrakis(hydroxymethyl)- phosphonium oxalate can be prepared by reacting in aqueous medium 1 mol of tris(hydroxymethyl)- phosphine with at least 1 mole of formaldehyde and essentially one-half mole of oxalic acid.
• Sufficient oxalic acid is used to provide between 0.3 and 1.0 moles, preferably between 0.4 and 0.6 moles, of real oxalic acid per mole of THP.
• the formaldehyde should be used in an amount sufficient to provide one mole of formaldehyde per mole of THP.
• the formaldehyde can be in the form of an aqueous solution or as paraformaldehyde.
• the temperature of the mixture is held at about 30C. for about 4 hours.
• the reaction temperature should be between 20C. and C., preferably between 25C. and 50C.
• the product is an aqueous solution which can be used in preparing the flame retardant finishes.
• the finish may contain free formaldehyde and oxalic acid.
• the amount of TKS'present in the product depends on the amount of TH? used initially. Each mole of the THP requiries by theory 0.5 moles ,of oxalic acid and one mole of formaldehyde. For each mole of TKS formed, the amount of THF in the product is reduced by two moles.
• the application-solutions are prepared by diluting the aqueous solution of TKS in water to a given concentration of solids and adding urea or a urea formaldehyde condensate in sufficient amount to provide about 1.25 moles prescribed above of urea and/or ureaformaldehyde condensate per mole of phosphonium salts.
• concentration phosphorus and urea in the application solutions will depend, in general, on the method of application, the amount of phosphorus and urea to be applied to the textile material, and on the weight, structure and fiber composition of the textile material.
• the nitrogenous compounds of use in this invention include the organic amido compounds which are conventionally employed in the form of their methylol derivatives as thermosetting aminoplast textile finishes. They include the melamines, urea, cyclic ureas, carbamates, triazinones, etc., and their methylol and alkylated methylol derivatives.
• the preferred nitrogenous compound is urea.
• Representative methylol compounds include monomethylol urea, dimethylol urea, tetramethylol urea, dimethylol melamine, partially methylated trimethylol melamine, and the like. Combinations of'two or more nitrogenous compounds may be employed.
• Sufficient flame retardant finish should be applied to cellulosic textile-material to provide between about 1% and 6%, preferably between about 2% and 4% of phosphorus based on the weight of the textilematerial.
• Sufficient nitrogenous compound is used to provide between about 1% and preferablybetween about 2% and 6% of nitrogen based on the weight of the textile material.
• the ratio of nitro derived phosphorus on a parts by weight basis is between 0.5 and 5.0 preferably between 0.7 and 2.0.
• the cellulose textile material ishould contain at least 20% cellulosic fibers.
• cellulosic fibers it is meant such fibers as cotton, regenerated cellulose (rayon), linen, jute, etc.
• the components of the flame retardant compositions temperaturebetween about i67-350F. or higher.
• - drying time'can range from several minutes at the lower temperature to asbriefly as seconds atthe higher tem- I perature. .
• the finish is then cured at a temperature of between about248--392F. preferably between about 300-350F.
• the time required for curing the finish is between I and'5 minutes, depending on the tempera ture and the weight and structure of the textilemate rial.
• compositions and. processes of the present invention are further described and compared with related compositions and process by the following examples. These examplesare not tobe taken'as being limitative of the present invention. In each case, percentages are by weight unless otherwise indicated.
• EXAMPLE 1 EXAMPLE 2 Four pad baths were prepared. Pad Baths A and B contained the product of Example 1, and pad baths C and D contained a 60/40 molar mixture of tetrakis(hydroxymethyl )phosphonium acetate/tetrakis(hydroxy- I treatment.
• each pad bath also contained urea and 0.56% by weight of a surfactant.
• the padbaths were applied to cotton flannelette and the treated fabrics were dried-at 225F. for 3.0miriutesand then heated at 350F. for 3.0 minutes. After curing all fabrics were washed in a solution con-- taining 5% real hydrogen peroxide based on the dry weight of the treated fabric using sufficient sodium silicate to maintain apI-I in the range of-9.0 to 9.5 duringthe washing cycle.
• the compositions of the pad baths and treated fabrics are shown in Table II.
• the TKS-treated fabrics had a softer hand then those treated with TKP.
• the hand of the TKS-treated fabric at the 3.58% phosphorus level (pad bath E) was as soft as the TKP-treated fabric at the 3.04% phosphorus level (pad bath B).
• the durability of the TKS treatment is about the same as that of the TKP treatment at any level of addon under the same washing conditions.
• EXAMPLE 4 A pad bath was prepared containing the product of Example 1 at 32.5% TKS on the weight of the pad bath, the pad bath had a pH of 4.2. The pad bath was applied to 5.5oz/-yd bleached, mercerized cotton at 100% expression, and the treated fabric was dried 4 minutes at 225F. and heated 4 minutes at 325F. to obtain a phos phorus content of 3.5% onthe weight of the fabric. The treated fabric, before process washing, burned completely when subjected to the Dept. of Commerce Test PFF-3-7O using a 3 second flame.
• An aqueous flame retardant finish composition solution for cellulosic textile materials comprising:
• a finish composition according to claim 2 comprising 0.3 to 1.0 mole of tetrakis(hydroxymethyl)- phosphonium oxalate and from 0.5 to 2 moles of urea per liter of solution.

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• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Engineering & Computer Science (AREA)
• Textile Engineering (AREA)
• Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Priority Applications (9)

Applications Claiming Priority (1)

Publications (1)

Family

ID=23236190

Family Applications (1)

Country Status (8)

Cited By (5)

Families Citing this family (3)

Citations (3)

• 1972
  • 1972-12-26 US US317998A patent/US3888779A/en not_active Expired - Lifetime
• 1973
  • 1973-11-22 CA CA186,460A patent/CA1013507A/en not_active Expired
  • 1973-12-18 GB GB5862873A patent/GB1402670A/en not_active Expired
  • 1973-12-21 FR FR7345934A patent/FR2211558B1/fr not_active Expired
  • 1973-12-21 BE BE139243A patent/BE809057A/xx unknown
  • 1973-12-21 IT IT54520/73A patent/IT1000762B/it active
  • 1973-12-24 DE DE2364589A patent/DE2364589A1/de active Pending
  • 1973-12-26 JP JP48144195A patent/JPS4987898A/ja active Pending

Patent Citations (3)

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