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
  • D06M15/667—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
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
• • 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
  • D06M13/425—Carbamic or thiocarbamic acids or derivatives thereof, e.g. urethanes
• • 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

• This invention relates to an improved composition and process for treating cellulosic materials and more particularly relates to an improved composition and process for the treating of cellulosic textile materials to render them substantially flame retardant.
• the durability of the flame-retardant finish in such products is generally adversely affected and the cellulosic materials frequently are stiff and/ or boardy and, hence, not desirable.
• the cellulosic textile materials treated in accordance with this procedure do not undergo the reduction in tear strength and tensile strength of materials which have been subjected only to a heat cure and do not have the white surface deposits of resin as do materials which are subjected only to an ammonia cure, in some instances it has been found that the heat cure cycle of the process is dificult to control and the bath of polymeric material with which the textile is treated may become unstable in an undesirably short period of time.
• a further difliculty which has been encountered in the fire processes for preparing flame-retardant cellulosic materials is that, frequently, these processes can only be used on yard goods at the textile mill and are not adaptable for use on consumer goods in a commercial laundry. In many instances, this may be disadvantageous in that it limits the application of flame-retardant finishes to new consumer articles made from yard goods which have previously been given a flame-retardant finish. Moreover, with such processes, it may not be possible to re-treat consumer articles which have previously been flame retardant so as to renew the flame-retardant properties. Accordingly, it is desirable for a process for treating cellulosic materials to render them flame retardant to be adaptable for application in both the mill to yard .goods and in commercial laundries to finished consumer articles.
• an object of the present invention to provide an improved composition and process for treating cellulosic materials to render them substantially flame retardant.
• a further object of the present invention is to provide an improved composition and process for flameproofing cellulosic textiles whereby the resulting textile material is rendered durably flame retardant and undergoes substantially no reduction in tear strength or tensile strength.
• a further object of the present invention is to provide a process and composition for preparing flame-retardant cellulosic textile materials, which process is readily adapted for application in both textile mills and in commercial laundries.
• a still further object of the present invention is to provide a composition and process for preparing flameretardant cellulosic textiles wherein the criticality of the curing portion of the process is substantially reduced and the stability of the impregnated composition used is materiailly increased.
• the process of the present invention includes impregnating a cellulosic material with a polymerizable composition comprising a tetrakis(ahydroxyorgano)phosphonium halide, a water-soluble, cy-
• copolymerizable compound which is a carbamic acid derivative such as urea, .thiourea, biuret, ethylene urea, 01' dicyandiamide, and an alkaline inorganic stabilizer, heating the thus-impregnated material at a temperature and for a period of time sufficient to partially polymerize the polymerizable composition only to the extent that it is substantially insoluble in ammonia-containing solutions, and, thereafter, contacting the material containing the thus-partially polymerized composition with ammonia in an amount and for a period of time suflicient to substantially completely cure the composition and to render it substantially completely water-insoluble.
• a carbamic acid derivative such as urea, .thiourea, biuret, ethylene urea, 01' dicyandiamide, and an alkaline inorganic stabilizer
• the cellulosic materials such ;as cellulosic textiles, treated in accordance with the above process are found to be durably flame retardant, even after repeated launderings and show no evidence of resin spotting on the surface as a result of partial dissolving of the impregnating composition during the ammonia cure. Additionally, the hand of the fabric is essentially unchanged from that of the untreated fabric and the tear strength and tensile strength are comparable to that of the untreated fabric.
• the heat curing portion of the process may be carried out at appreciably higher temperatures than have heretofore been possible, while still obtaining a uniform cure of the polymerizable composition, and there is further found to be a marked increase in the stability of the polymerizable impregnating composition.
• the polymerizable composition with which the cellulosic material is impregnated is preferably an aqueous composition.
• This composition will generally be comprised of the following substituents in the following proportions:
• nitrogen-containing compound 5-15 percent by weight.
• Carbamic acid derivatives 1-10 percent by weight.
• Alkaline inorganic stabilizer .25.75 equivalent of 'base per mole of phosphonium compound.
• the tetrakis(a-hydroxyorgano)phosphonium halide compound of the subject composition may be further defined as a compound having the formula:
• R is selected from the group consisting of hydrogen, lower alkyls having between about 1 and about 6 carbon atoms, halogenated lower alkyls having between about 1 and about 6 carbon atoms, lower alkenyls having between about 1 and about 6 carbon atoms, halogenated lower alkenyls having between about 1 and about 6 carbon atoms, aryls having between about 5 and about 10 carbon atoms, halogenated aryls having between about 5 and about 10 carbon atoms, cycloalkyls having between about 3 and about 6 carbon atoms, halogenated cycloalkyls having between about 3 and about 6 carbon atoms, and X is a halogen, such as chlorine, bromine, fluorine or iodine.
• the phosphonium compounds may be used in monomer form or in a partially polymerized for, so long as they are still water-soluble.
• tetrakis(hydroxymethyl)phosphonium chloride which is the preferred phosphonium compound, may be heated to effect partial polymerization before dissolving it in the solution.
• Water-soluble cyclic nitrogen-containing compounds suitable for use in the present invention include the tri* azines and the dimethylol cyclic alkylene ureas.
• suitable triazines include the methylol melamines, such as mono-, di-, and trimethylol melamine; modified methylol malamines, such as the trimethyl ether of trimethylol melamine, triazones, such as dimethylol triazone; and mixtures thereof.
• suitable cyclic alkylene ureas include dimethylol ethylene urea, dimethylol propylene urea, and the like. Of these, trimethylol melamine is preferred and for this reason hereinafter primary reference will be made to this compound.
• the carbamic acid derivatives used in the present invention are exempified by urea, thiourea, biuret, ethyleneurea and dicyandiamide. Of these, urea and thiourea are preferred. By the incorporation of these compounds in the present composition, the amount of the more expensive tetrakis (ct-hydroxyorgano)phosphonium halide compound can be reduced, over that required when these compounds are not present. Inasmuch as urea or thiourea are preferred in the practice of the present invention, specific reference to these materials will be made hereinafter.
• the alkaline inorganic stabilizer used in the present process may be any alkaline oxide, hydroxide, or carbonate, including bicarbonates, which has an appreciable solubility in the polymerizable impregnating composition.
• exemplary of such stabilizers which may be used are the alkal metal hydroxides, alkali metal carbonates, alkali metal bicarbonates, as Well as the corresponding alkaline earth metal compounds which have the requisite solubility.
• alkali metal it is intended to include sodium, potassium, lithium, cesium and rubidium. Of these, because of its low cost and ready availability, the preferred alkali metal is so dium, and, for this reason, primary reference hereinafter will be made to sodium compounds.
• alkaline earth metals is intended to include the divalent metals of Group II of the Periodic Table, and particularly calcium, strontium, and barium.
• the preferred inorganic alkaline stabilizers are sodium hydroxide, sodium carbonate, and sodium bicarbonate, with sodium hydroxide being specifically preferred.
• the specifically preferred impregnating composition for use in the method of the present invention may contain the following substituents in the following proportions:
• Trimethylol melamines 6-9 percent by weight.
• the impregnating composition may also contain other substituents, such as fabric softeners,
• the non-aqueous substituents are added to the water, preferably in the order set forth hereinabove. Generally, agitation of the bath is desirable in order to insure that the non-aqueous substituents will be substantially completely dissolved in the aqueous portion of the bath.
• the impregnating bath is preferably maintained at a Q temperature below about 85 degrees Fahrenheit, in order to obtain maximum stability and useful. bath life. Typical operating temperatures for the impregnating bath are about 65 to about 85 degrees Fahrenheit.
• the solution may be applied to the cellulosic material, such as cellulosic textiles, in any convenient manner.
• the mode of application of the polymerizable solution to the textile will depend upon the formof the textile being treated.
• the composition and process of the present invention may be utilized:
• the polymerizable solution maybe formulated in a padding box and the cellulosic material to be treated immersed in the solution. Thereafter, impregnationof the material is effected by feeding the goods through a pad or squeeze roll or other suitable means for removing the excess solution.
• impregnationof the material is effected by feeding the goods through a pad or squeeze roll or other suitable means for removing the excess solution.
• the process of the present invention may be carried out in commercial laundry-type equipment.
• the polymerizable impregnating solution may be formulated in any desired container and, thereafter, the goods to be treated may be brought into contact with the solution.
• his contact may be effected in any desired manner as, for example, by dipping the goods in the solution by hand, by wetting out the goods in a Wash wheel, or by impregnating the goods in an extractor. Generally, this latter method of impregnation is preferred in that by its use the amount of solution lost can be reduced to an insignificant amount. 7
• an important factor in the present method is the amount of resin add-on in the cellulosic materials which have been treated. Obviously, a-resin add-on which is too low may result in a product which has poor flame retardancy and/or a product in which the durability of the flame retardancy after repeated launderings is reduced. Moreover, it has been found that a resin add-on which is too great may result in a product which has an unsatisfactory hand, i.e., a product which is stiff and/or boardy.
• the cellulosic material treated is given a resin add-on which provides both satisfactory flame retardancy and durability, without adversely effecting the hand of the material, i.e., a flame-retardant amount.
• resin add-ons within the range of about 16 to 24 percent by weight of the material treated give satisfactory results. It will be appreciated, however, that resin add-ons which are greater or lesser than these preferred amounts may be used in some instances, depending upon the type and weight of the cellulosic material being treated.
• the amount of wet pick-up in the material may be controlled by varying the amount of pressure on the pad or squeeze roll.
• the wet pick-up of the impregnating solution in the textile may be controlled by effecting removal of the excess impregnating solution in any convenient manner.
• the impregnated cellulosic textile may be run in an extractor or similar centrifuge-type of apparatus to remove suflicient of the impregnating solution to give the desired wet pick-up.
• the amount of wet pick-up in the impregnated articles is within the range of about 70 to about 75 percent by weight, so as to give a resin add-on of about 19 to about 21 percent by weight.
• the preferred amount of wet pick-up is within the range of about 60 to about percent by weight, so as to give a resin add-on within the range of about 18 to about 24 percent by weight.
• the wet pick-up is within the range of about 70 to about 75 percent by weight, so as to give a resin add-on within the range of about 19 to about 21 percent by weight.
• the material is subjected to heat at a temperature and for a period of time sufficient to partially polymerize the polymerizable impregnant only to the extent that it is substantially insoluble in ammonia-containing solution.
• this heating will be such that aldehyde groups, generated during the polymerization of the composition will undergo substantially no reaction with the cellulose molecules of the treated material.
• the extent of the polymerization will be such that there is a substantial insolubilization of the composition in ammonia-containing solutions.
• temperatures of from about 200 to about 320 degrees Fahrenheit and curing times from about 0.5 minute to about one hour may be used, the longer curing time being used at the lower temperatures. It will be appreciated, however, that other curing temperatures and times, outside the above ranges, may also be used Where they result in a similar partial polymerization of the impregnating composition only to the extent that there is a substantial insolubilization of the composition in ammonia-containing solutions, without detrimentally affecting the cellulosic material or the composition with which it is impregnated.
• the above heating of the impregnated cellulosic material may be carried out in any convenient equipment, either of the mill type or of the type found in commercial laundries.
• the heat curing operation may be carried out in a loop oven or in a conventional roller type oven, or it may be carried out in a tumble type dryer or other similar drying equipment.
• the combined operation be carried out at low temperatures and long times, generally within the ranges which have been set forth hereinabove.
• the heat curing operation will generally be carried out at somewhat lower temperatures than those which are used when the drying is carried out in mill apparatus.
• dryer stack temperatures within the range of about 200 to about 250 degrees Fahrenheit and drying times Within the range of about 20 to about 60 minutes are preferred.
• the preferred curing temperatures used are within the range of about 270 to about 320 degrees Fahrenheit With cure times within the range of about 1 to about 5 minutes.
• the treated cellulosic material is subjected to a chemical curing operation, using a source of ammonia.
• the ammonia may be supplied for the curing operation as ammonia gas, aqueous ammonia, including ammonium hydroxide, solutions of amino compounds containing at least two reactive hydrogen atoms per molecule, such as amines containing a primary amino group, hydrazine, alkyl-substituted hydrazine and the like, ammonium carbonate, or other readily dissociated weak acid salts of ammonia such as ammonium acetate, ammonium formate, and the like.
• ammonia gas aqueous ammonia, including ammonium hydroxide
• solutions of amino compounds containing at least two reactive hydrogen atoms per molecule such as amines containing a primary amino group, hydrazine, alkyl-substituted hydrazine and the like, ammonium carbonate, or other readily dissociated weak acid salts of ammonia such as ammonium acetate, ammonium formate, and the like.
• the chemical cure of the impregnated cellulosic material may be effected using a composition comprising a mixture of the ammonium salt of a strong acid, such as ammonium sulfate, an alkali metal carbonate, and an alkali metal bicarbonate, such as sodium carbonate, and sodium bicarbonate.
• a composition comprising a mixture of the ammonium salt of a strong acid, such as ammonium sulfate, an alkali metal carbonate, and an alkali metal bicarbonate, such as sodium carbonate, and sodium bicarbonate.
• the chemical cure of the polymerizable impregnating composition with an aqueous solution of ammonia, such as ammonium hydroxide or the aforementioned aqueous solution of the mixture of ammonium sulfate, sodium carbonate and sodium bicarbonate.
• ammonia such as ammonium hydroxide or the aforementioned aqueous solution of the mixture of ammonium sulfate, sodium carbonate and sodium bicarbonate.
• the chemicalcure is carried out for a period of time sufiicient to upon the amount of resin add-on to be obtained in the treated material, as Well as the nature of the cellulosic material itself, chemical curing times of about 1 to about 5 minutes have been found to be typical.
• the ammonia concentration used in the chemical curing operation may also vary although concentrations of about 3 to about 10 percent by weight have been found to give satisfactory results.
• the chemical curing operation may also be carried out in either mill apparatus or commercial laundry apparatus, depending upon the form of the cellulosic textile material being treated.
• the chemical curing operation may be accomplished in a padder or on a jig, utilizing the curing composition as described hereinabove.
• the chemical curing step may be carried out continuously.
• the finishing operations on the treated fabric are to include scouring in a jig
• the ammonia cure may be more conveniently carried out in a jig during the first end.
• Exemplary of a specific cur ing composition which may be used with such mill apparatus is one containing the following components in the following amounts:
• the chemical curing step may conveniently be effected utilizing a wash wheel.
• curing step will constitute the first cycle of the after- Washing operation.
• a curing solution comprising about 100 gallons of Water, to which has been added 2 gallons of 28 percent ammonia, is added to the Wash wheel, and the cellulosic textile materials agitated in this composition for about 3 minutes.
• a curing composition similar to that used in the mill apparatus, may be added to the wash wheel.
• Such composition may contain the following components in the following amounts:
• the concentration of the ammonia curing solution used in commercial laundry apparatus may be less than that used in mill-type apparatus.
• the reason for this is that in the commercial laundry-type apparatus, a more complete saturation of the cellulosic material with the ammonia curing solution is generally obtained than in mill-type apparatus. Accordingly, a more effective utilization of the ammonia content of the curing solution is possible and hence lower concentrations of ammonia in the solution can be used.
• the material is preferably scoured or washed to remove unpolymerized materials and the like.
• this scouring operation may be effected using any of In such operation, the
• the conventional scouring processes such as rope scouring, continuous open width scouring, and jig scouring.
• the scouring may conveniently be carried out using, as, e.g., an aqueous soak solution containing small amounts of sodium carbonate and perborate.
• the washing may be carried out in a wash wheel, immediately following the chemical curing operation.
• the scouring or washing operation is then preferably followed by a drying operation wherein the treated fabric is dried in a conventional manner and may then be subjected to any normal finishing operation such as sanforizing, calendering, and the like.
• the cellulosic materials such as cellu'los'ic textile materials, treated in accordance With the procedure set forth hereinabove, whether utilizing mill-type apparatus or commercial laundry-type apparatus, have been found 'to be durably flame retardant, even after numerous launderings. Additionally, such materials are found to have a tear strength, tensile strength and hand which are substantially unchanged from those of untreated materials.
• the thustreated cellulosic tetxiles are further found to be characterized by the absence of .deposits of resinous materials on the surface thereof which deposits have characterized textile materials which have been processed by prior art methods which utilize only a chemical curing operation. Moreover, the criticality of the conditions under which the heat curing portion of the present process is carried out have been found to be measurably reduced and the stability of the polymerizable impregnating composition has been substantially increased.
• Example 1 The following aqueous composition was formulated:
• Cotton sheeting fabric was impregnated with this formulation by immersing the fabric in the solution and, thereafter, subjecting the fabric to squeezing so as .to obtain a 10 0 percent wet pick-up on the fabric.
• the thus-impregnated fabric was thondried for 1.5 minutes at 250 degrees Fahrenheit and cured for 1 minutes at 280 degrees
• the thus-cured material was given an .am-
• This example may be repeated using other carbamic acid derivatives such as thiourea, biuret, ethylene urea or dicyanodiamide instead of urea and/ or using solutions of amino compounds such as ethylamine or hydrazine to effect the ammonia cure, to obtain similar results.
• carbamic acid derivatives such as thiourea, biuret, ethylene urea or dicyanodiamide
• solutions of amino compounds such as ethylamine or hydrazine to effect the ammonia cure
• Example 3 v A polymerizable impregnating composition was formulated containing the following components in the following amounts:
• the total weight of the impregnating solution was 800 pounds.
• An eight-ounce herring bone twill cotten fabric was then impregnated with the above composition by passing it through a padder utilizing a pressure of 6 tons on the pad rolls.
• the thus-impregnated fabric had a wet pick-up of 75 percent.
• the fabric was then dried in a conventional tenter frame at 280 degrees Fahrenheit for 20 seconds, and cured in aroller-type oven for 2 minutes at a temperature of 300 to 310 degrees Fahrenheit.
• the hand of the fabric was soft, comparable to that of the untretaed fabric, and the shrinkage of the treated fabric, warp X fill, was (3.0) X (+2.0) as compared to that of the untreated fabric of (--16) x (+4).
• Example 4 An impregnating composition was formulated containing the following components in the following amounts:
• Example 5 A polymerizable impregnating composition is formulated using the following substituents in the following proportions 250 yards of broadcloth (136 X 64) was impregnated with this composition by passing it through a padder at 1.5 tons pad pressure. The resulting material had a wet pick-up 76 percent. The fabric was then passed through a tenter frame for drying at 180 degrees Fahrenheit; Retention time was 1.25 minutes. The drying conditions were adjusted so that the dried material had a moisture content of 5 to 10 percent. The fabric was then cut into three sections and cured as follows:
• Example 6 A polymerizable impregnating composition is prepared using the following components in the following proportions:
• the cellulosic material treated in accordance with the present invention may be in the form of fibers, yarns, fabrics, films, pulp, paper, fiber board, wood, or the like. Additionally, for purposes of the'present invention, it is intended that wool also be included in those materials which may be treated, even though it is not classified as a cellulosic material.
• the present invention has been found to be particularly suitable for the treatment of textile materials which are porous in nature, and, therefore, are readily capable of absorbing resinous impregnating compositions. Included in such materials are cotton, rayon, wool, jute, and ramie textiles. This is not, however, to be taken as a limitation on the materials which may be treated by the process of the present invention, but merely as being exemplary of these materials.
• a process for preparing flame-retardant cellulosic materials which comprises impregnating a cellulosic material with a polymerizable composition consisting essentially of a tetrakis(a-hydroxyorgano)phosphonium halide, a water-soluble cyclic copolymerizable nitrogen-containing compound, a copolymerizable compound which is a carbamic acid derivative, and an alkaline inorganic stabilizer, heating the thus-impregnated material at a temperature and for a period of time sufficient to partially polymerize the polymerizable composition only to the extent that it is substantially insoluble in ammonia-containing solutions, and thereafter, contacting the material containing the thus-partially polymerized composition with ammonia, in an amount and for a period of time sutficient to substantially completely cure the composition and render it substantially completely water-insoluble.
• a polymerizable composition consisting essentially of a tetrakis(a-hydroxyorgano)phosphonium halide,
• a process for preparing a flame-retardant cellulosic material which comprises impregnating the cellulosic material with a polymerizable composition consisting es- 14 sentially of a water-soluble .cyclic copolymerizable nitrogen-containing compound, a copolymerizable compound selected from the group consisting of urea and thiourea, an alkaline inorganic stabilizer, and a tetrakis(a-hydroxyorgano)phosphonium halide .having the formula:
• R is selected from the group consisting of hydrogen, lower alkyls having between -1 and about 6 carbon atoms, halogenated lower alkyls having between about 1 and about 6 carbon atoms, lower alkenyls having between about 1 and about 6 carbon atoms, halogenated lower alkenyls having between about 1 and about 6 carbon atoms, aryls having between about 5 and about 10 car-bon atoms, halogenated aryls having between about 5 and about 10 car-bon atoms, cycloalkyls having between about 3 and about 6 carbon atoms, and halogenated cycloalkyls having between about 3 and about 6 carbon atoms, and halogenated cycloalkyls having between about 3 and about 6 carbon atoms, and halogenated cycloalkyls having between about 3 and about 6 carbon atoms, and X is halogen, heating the thus-impregnated material at a temperature and for a period of time sufficiently to partially polymerize
• a process for preparing a flame-retardant cellulosic textile material which comprises impregnating the cellulosic textile material with a polymerizable composition consisting essentially of tetrakis(hydroxymethyl)phosphonium chloride, trimethylolmelamine, a copolymerizable compound selected from the group consisting of urea and thiourea, and an alkaline inorganic stabilizer selected from the group consisting of alkali metal hydroxides, carbonates, and bicarbonates, heating the thus-impregnated material at a temperature and for a period of time sufficient to partially polymerize the polymerizable composition only to the extent that it is substantially insoluble in ammonia-containing solutions, and thereafter, contacting the material containing the thus-partially polymerized composition with an aqueous solution containing ammonia in an amount and for a period of time sufficient to substantially completely cure the composition and render it substantially completely water-insoluble.
• a polymerizable composition consisting essentially of te

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• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Engineering & Computer Science (AREA)
• Textile Engineering (AREA)
• Health & Medical Sciences (AREA)
• Medicinal Chemistry (AREA)
• Polymers & Plastics (AREA)
• Organic Chemistry (AREA)
• Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
• Chemical Or Physical Treatment Of Fibers (AREA)
• Compositions Of Macromolecular Compounds (AREA)
• Fireproofing Substances (AREA)

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• 1963
  • 1963-04-16 US US273272A patent/US3310419A/en not_active Expired - Lifetime
• 1964
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  • 1964-04-16 NL NL6404149A patent/NL6404149A/xx unknown
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• 1966
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