Classifications

• • D—TEXTILES; PAPER
  • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
  • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
  • D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
  • D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
  • D01F2/08—Composition of the spinning solution or the bath
  • D01F2/10—Addition to the spinning solution or spinning bath of substances which exert their effect equally well in either
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
  • C08K5/00—Use of organic ingredients
  • C08K5/49—Phosphorus-containing compounds
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
  • C08K5/00—Use of organic ingredients
  • C08K5/49—Phosphorus-containing compounds
  • C08K5/5399—Phosphorus bound to nitrogen

Definitions

• R and R are the same or different alkyl or alkenyl radicals having from one to six carbon atoms and n in an integer of at least three.
• R and R include methyl, ethyl, propyl, isopropyl, butyl, isobutyl, amyl, isoamyl, hexyl, allyl, and crotyl radicals.
• R and R are npropyl, isopropyl or allyl radicals since polymers wherein both R and R have fewer carbon atoms tend to be more water-soluble, whereas the presence of more carbon atoms provide products having a lower phosphorous content thereby reducing their effectiveness as flame retardants. This can be overcome, of course, by using polymers wherein R contains fewer carbons and R contains more.
• R is methyl or ethyl and R is butyl, amyl, isoamyl, or hexyl.
• the liquid phosphonitrilate polymer is a cyclic trimer, tetramer or higher cyclic polymer, or a linear polymer and is preferably employed as a mixture of these isomers for economic reasons. It has been found, however, that the pure polymeric isomer is just as effective as the mixture for the purposes of this invention.
• the amount of phosphonitrilate flame-retardant dispersed in the regenerated cellulose filament varies from about 1 to about 30% and preferably from 2 to 20%, based on the weight of the filament.
• the method of this invention comprises incorporating the above described liquid phosphonitrilate in a viscose solution and spinning the viscose in the shape of one or more filaments into a coagulating and regenerating medium.
• the formed filaments are aftertreated using techniques well-known in the rayon field to provide continuous filaments, fibers and yarn, as well as staple fibers. These may then be used to prepare any known textile article in which the flame-retardant property is desirable.
• the flame-retardant phosphonitrilate of this invention is a liquid of pumpable consistency which is preferably used as a crude reaction product, prepared, for example, in a known manner by the conversion of the corresponding polymeric phosphonitrilic chlorides to the specified esters;
• suitable solutions of the phosphonitrilate may also be prepared and used for incorporation in viscose.
• a controlled amount of the flame-retardant phosphonitrilate is injected into the viscose just prior to its extrusion through the spinnerets.
• the viscose is extruded into an acid bath and processed in a conventional manner.
• EXAMPLE Excellent flame-retardant rayon yarn with no after-glow was produced from viscose comprising 8.2% cellulose, 6.2% sodium hydroxide and 34.0% carbon disulfide, based on the weight of the cellulose, having a common salt test range of 3.5 to 7.3 and a Ball-Fall range of 52 to seconds at 18 C.
• a metered amount based on the weight of the cellulose in the viscose of a liquid mixture of di-n-propyl phosphonitrilate polymers, as defined for this invention, comprising about 65% trimer, about 15% tetramer, between about 15 and 20% of higher cyclic polymers and less than about 5% of linear polymers, was pumped into the viscose line supplying the spinnerets.
• the flame-retardant containing viscose was spun into 3 a bath comprising 9.0% sulfuric acid, 2.0% zinc sulfate and 15.0% sodium sulfate at 55 C. and then further processed by a series of baths including water wash, desulfurization, bleaching, bleach acid, anti-chlorine, and soft finish.
• the yarn was dried and collected.
• the 20 clcles penihloroethylene u number of passes to induce flaming of the sample is Commerclal launderlngi 3 Percent 10582 determined.
• a control yarn bundle (yarn contains no 20 20 cycles flameretardant) mfiames P 1 or 2 Passes f 1 Retention of amount of flame-retardant injected in viscose retardant yarns are classified for mflammabillty as based on phosphorous analysis. follows: 2 Loss from completely processed yarn based on phosphorous prepared from completely processed yarn washed Passes P0913 in automatic washer with 1A cup of sodium oleate per cycle.
• the filaments of this invention in the form of yarns, problems. were tested for strength characteristics before and after The initial retention of the flame-retardant on spinning complete processing.
• Complete processing involves treatinto cellulose filaments and fibers is excellent in contrast ing the wet spun yarn in a series of baths as follows: to many hydrolyzable or water-soluble fire-retardants. Water wash, desulfurization, water wash, bleaching, water Surprisingly, there is little or no hydrolysis of this flamewash, bleach acid, water wash, antichlorine, water wash, retardant even when mixed with viscose and allowed to and soft finish. Yarns tested before complete processing stand for up to 18 hours. were merely subjected to one water wash after spinning.
• the retention is excellent after many launderings and dry cleanings.
• the fire-retardancy of the product of this invention is excellent despite the absence of halogens which often cause ultra-violet light degradation.
• liquid phosphonitrilate polymer of this invention has no tendency to pick up chlorine from bleaching solutions which might lead to yellowing and fiber degradation.
• the phosphonitrilate polymer is dispersed readily and evenly throughout the fiber because of its liquid nature, and therefore, has little effect on the fiber tensile strength. Such small losses in strength that do occur generally result only from displacement of a certain amount of cellulose.
• the appearance and general physical properties of the flame-retardant rayon of this invention differ only slightly from ordinary rayon. Hence, the fibers can be processed in the normal fashion.
• Regenerated cellulose filaments and filamentary articles said filaments having dispersed therein a flameretardant amount of a substantially water-insoluble, liquid phosphonitrilate polymer having the following general formula Lei wherein R and R are alkyl or alkenyl radicals having from 1 to 6 carbon atoms and n is an integer of at least 3.
• the regenerated cellulose filaments of claim 1 containing from about 1 to about 30%, based on the Weight of the cellulose, of the liquid phosphonitrilate polymer.
• a method of preparing a permanently flame-retardant regenerated cellulose filament which comprises mixing viscose and a flame-retardant amount of a substantially water-insoluble, liquid phosphonitrilate polymer having the following general formula:
• R and R are alkyl or alkenyl radicals having from 1 to 6 carbon atoms and n is an integer of at least 3, shaping the mixture into a filament, and coagulating and regenerating said filament.

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• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Health & Medical Sciences (AREA)
• Medicinal Chemistry (AREA)
• Polymers & Plastics (AREA)
• Organic Chemistry (AREA)
• General Chemical & Material Sciences (AREA)
• Engineering & Computer Science (AREA)
• Textile Engineering (AREA)
• Artificial Filaments (AREA)

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Cited By (20)

Citations (3)

• 1966
  • 1966-07-21 US US566757A patent/US3455713A/en not_active Expired - Lifetime
• 1967
  • 1967-04-07 GB GB06031/67A patent/GB1153955A/en not_active Expired
  • 1967-07-19 DE DE19671669427 patent/DE1669427B1/de not_active Withdrawn
  • 1967-07-21 BR BR191382/67A patent/BR6791382D0/pt unknown

Patent Citations (3)

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