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
  • D06M11/32—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
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
  • C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
  • C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
• • 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
  • D06M11/07—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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
  • D06M11/11—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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
  • D06M11/155—Halides of elements of Groups 2 or 12 of the Periodic Table
• • 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
  • D06M11/07—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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
  • D06M11/11—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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
  • D06M11/22—Halides of elements of Groups 5 or 15 of the Periodic Table
• • 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
  • Y10S260/00—Chemistry of carbon compounds
  • Y10S260/24—Flameproof
• • 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
  • Y10S8/00—Bleaching and dyeing; fluid treatment and chemical modification of textiles and fibers
  • Y10S8/21—Nylon

Definitions

• R represents a divalent hydrocarbon radical of two to 12 carbon atoms, e.g. a straight chain or branched chain saturated or unsaturated aliphatic radical of two to 12 carbon atoms or a cycloaliphatic, araliphatic or aromatic radical of six to 12 carbon atoms have been disclosed in Luxembourg Pat. Specification No. 55,732. These filaments are not flame-resistant although they do possess other desirable properties.
• the object of the present invention is to provide a process for the production of flame-resistant polyacyloxalamidrazone filaments, especially those consisting essentially of polyterephthaloyloxalamidrazone and polyfumaroyloxalamidrazone.
• a flame-resistant polyacyloxalamidrazone filament can be obtained by a process or method which comprises treating said polyacyloxalamidrazone with a solution of at least one solvent-soluble compound of one or more of the metals, zinc, tin, cadmium, barium, strontium, calcium, antimony or tantalum, for a period of time sufficient to render the filament resistant to flame, preferably so as to combine at least about 3 percent by weight of the metal with the polyacyloxalamidrazone filament.
• filament is employed herein as including all types of filamentary or fibrous materials, e.g., continuous filaments, staple fibers, yarns, threads, fabrics, felts or any similar products.
• Especially satisfactory flame-resistant filaments are obtained by treating a polyacyloxalamidrazone in which the recurring acyl units consist predominately of terephthaloyl or fumaroy] radicals.
• those polyacyloxalamidrazone consisting essentially of recurring units of the above-noted formula in which R is one of the divalent radicals:
• Polyterephthaloyloxalamidrazone and polyfumaroyloxalamidrazone filaments can be produced, for example, according to the process described in Luxembourg Pat. No. 55,732, by spinning an aqueous alkaline solution of the polymer into a suitable precipitating or coagulating bath.
• polyterephthaloyland polyfumaroyl-oxalamidrazones The preparation of the initial polymer, e.g., polyterephthaloyland polyfumaroyl-oxalamidrazones has been described in Luxembourg Pat. Specifications Nos. 54,747 and 57,177. These polymers are thus obtained in a conventional manner by the reaction of terephthaloyl or fumaroyl chloride with oxalic acid bisamidrazone. Polyterephthaloyland polyfumaroyl-oxalamidrazones having a reduced viscosity of 0.2 to 5.4 are already known, but filaments of these same polymers of higher molecular weight may also be used in the process according to the invention.
• filaments of pure polyterephthaloyloxalamidrazone or pure polyfumaroyloxalamidrazone are not absolutely necessary.
• filaments of polyacyloxalamidrazones which contain both the terephthaloyl and the fumaroyl radical as recurring acyl components.
• the preparation of such copolyacyloxalamidrazones has also been described in Luxembourg Pat. Specification No. 54,747. They are obtained by reacting terephthaloyl and fumaroyl chloride with oxalic acid bisamidrazone. Filamentary products such as yarns or the like which contain both polymers may also be used.
• the process according to the invention may also be advantageously carried out using filaments of polyterephthaloyloxalamidrazone' or polyfumaroyloxalamidrazone which in addition to the terephthaloyl or fumaroyl acyl units, also contain small quantities of other acyl units, preferably not more than about 5-10 molar percent with reference to the total acyl units.
• Suitable metal compounds include any inorganic or organic salts and also complex compounds of the metals zinc, tin, cadmium, barium, strontium, calcium, antimony and tantalum. Such compounds should be either water-soluble or soluble in organic solvents which are substantially inert to the polyacyloxalamidrazone filaments, i.e. solvents which do not materially affect the desirable physical properties of such filaments. J
• Suitable solvents containing the metal in solution for the treatment of the polyacyloxalamidrazone filaments are such conventional solvents as water, including alkaline or acidic aqueous solutions, and many organic solvents, including for example: alkanols such as methanol or ethanol, dimethyl sulfoxide, hexamethyl phosphoric acid triamide, sulfolane (tetrahydrothiophene-l,l-dioxide), tetramethylurea, dimethyl formamide, pyridine and other organic amines. In some cases, chlorinated hydrocarbons, esters or ketones are also quite suitable. The metal compounds may also be used as solutions in mixtures of different solvents.
• Saturated or highly concentrated solutions of at least one of the metal compounds are preferably used, but dilute solutions may also be used.
• solutions having a concentration of at least about 5 percent by weight of the metal compound or compounds is desirable in order to reduce the total time of treatment, but the concentration can vary over a wide range where a relatively long treatment or repeated treatments are considered to be feasible. It is advantageous to use the solution at approximately room temperature, but solutions at higher temperatures may also be used provided that the filaments are not seriously damaged or decomposed.
• the treatment of the polyacyloxalamidrazone filaments with the solutions of the metal compounds may be carried out, for example, by dipping the filaments or threads into a vat or bath containing the metal in solution. Fibers or filaments may be introduced into the treatment bath, e.g. in a loose form or as yarn in the form of Strands. Polyacyloxalamidrazone filaments wound on a spool may also be exposed to this treatment with the dissolved metal compound in a conventional spool pressure washing process.
• the polymer such as the polyterephthaloylor pulyfumaroyloxalamidrazone which has been or is being formed as a filament reacts chemically with the metal compound and the polyacyloxalamidrazone actually binds the metal in complex form, for example as an enolate.
• the exact nature of this complex combination of the metal with the polymer cannot'be fully established, but it can be assumed that complexing takes place through the oxygen atoms and/or other active sites on the polymer molecule.
• the reaction rate and the quantity of metal taken up depend upon several factors.
• the rate at which metal is absorbed and bound to the polymer depends in part on the type of polyacyloxalamidrazone being used, the particular metal or metal compound, its concentration in the solution, the particular solvent or solvent mixture, the temperature and the pH of the solution.
• substantial amounts of the metal are taken up under a very wide range of conditions so that the determination and maintenance of these conditions offers no problems.
• the filaments continue to take up metal from the solution in the course of the treatment until a saturation limit of the particular polyacyloxalamidrazone hasbeen reached.
• the most suitable method for preparing a polyterephthaloylor polyfumaroyloxalamidrazone of a given metal content, and especially the determination of the necessary reaction time, can easily be obtained from a simple series of preliminary tests.
• the flame-resistant filaments obtained by the process of the invention may also be produced by an alternative but somewhat less advantageous procedure.
• This procedure does not involve a treatment of the finished threads, filaments or fibers but with an alkaline solution of the polyacyloxalamidrazone.
• alkaline solutions can be spun into a precipitating bath which, in addition to the acid and/or salts required for forming the thread, also contains the desired metal compound in solution.
• treatment of the polyacyloxalamidrazone filaments actually starts while they are in the process of being formed in the so-called spinning bath.
• the metal-containing filaments produced by the process of the invention have an increasing flame-resistance with increasing amounts of the metal.
• Filaments of this type which have a characteristic minimum metal content for each metal can be classed as non-inflammable according to DIN 53 906 (German Industrial Standards).
• DIN 53 906 German Industrial Standards
• this minimum metal content is in the approximate range of 4 to 8 percent by weight.
• the minimum zinc content, for example, is approximately 5 percent by weight while the minimum tin content is approximately 3.5 percent by weight and the minimum calcium content is approximately 4 percent by weight.
• the minimum metal contents in polyfumaroyloxalamidrazone filaments are similar to those of polyterephthaloyloxalamidrazone.
• Filaments whose minimum metal content lies between about 3.5 to 8 percent by weight and whose content then extends up to the saturation limit of the polymer are not only non-inflammable according to DIN 53 906, but will also withstand prolonged action of the flames unharmed.
• the process according to the invention is therefore preferably used for producing filaments and fibers which have a metal content of about 3.5 percent to said saturation limit.
• the flame-resistant or non-inflammable filaments produced by the process according to the invention have good textile properties. They can be easily worked up into yarns, mixed staple fiber yarns, woven fabrics, knitted fabrics, fleeces or the like.
• the strength and elongation values of filaments which have a metal content of about to 50 percent by weight are generally only about 10 to percent lower than the values of the corresponding metal-free polyacyloxalamidrazone filaments. Where the metal content is less than about 15 percent by weight, the filaments are only slightly inferior in strength and elongation to the corresponding metal-free polyacyloxalamidrazone filaments.
• the process according to the invention may be used, for example, for producing a polyterephthaloyloxalamidrazone thread with a zinc content of 15 percent by weight which then exhibits a dry strength of 17 Rkm, dry elongation of 15 percent, a wet strength of 6 Rkm, a wet elongation of 8 to 16 percent and a relative loop strength of 75 percent. (Note: Rkm 9 X grams/denier).
• the filaments, threads or fibers produced by the process of the invention are intensely colored, the color depending on the metal bound to the polymer, a property which makes additional coloring unnecessary.
• the filaments and fibers can also be colored with the usual dyes such as disperse dyes, metal complex dyes, substantive dyes, basic or acid dyes. Other conventional additives such as pigments, fillers and the like may also be used. Filaments which contain the metal zinc, tin, cadmium, barium, calcium and strontium are orange to brown in color. Those which contain antimony compounds are red while those which contain tantalum are yellow-orange.
• the spinning composition was spun into a 20 percent aqueous ammonium chloride solution maintained at a temperature of 30 C.
• the polyterephthaloyloxalamidrazone filaments obtained in this manner had the following textile properties:
• the polyfumaroyloxalamidrazone thread used in Examples 15 and 16 was obtained by spinning a solution of 8 parts by weight of polyfumaroyloxalamidrazone, 6 parts by weight of potassium hydroxide and 86 parts by weight of water into a 20 percent by weight aqueous ammonium chloride solution at 30 C.
• the resulting polyfumaroyloxalamidrazone filaments had the following textile properties:
• Dry strength 4.5 Rkm. Dry elongation: 1.5 Absolute loop strength: 3.4 Rkm. Swelling: 67
• suitable solvent-soluble metal compounds include neutral-reacting and also basic or acid-reacting substances and can be listed as follows:
• Inorganic compounds halides and especially chlorides as well as bromides or iodides, sulfates, hydroxides, oxides nitrates, phosphates, etc.
• Organic compounds alcoholates, acetylacetonates, acetoacetates, carboxylates (tartrates, acetates, diamminotetraacetates), etc.
• a process for the production of a flame-resistant polyacyloxalamidrazone filament which comprises treating a polyacyloxalamidrazone filament with a solution of at least one solvent-soluble compound of a metal selected from the class consisting of zinc, tin, cadmium, barium, strontium, calcium, antimony and tantalum for a period of time sufficient to combine at least about 3 percent by weight of said metal in complex form with said polyacyloxalamidrazone filament.
• polyacyloxalamidrazone consists essentially of polyterephthaloyloxalamidrazone.
• polyacyloxalamidrazone consists essentially of polyfumaroyloxalamidrazone.
• a flame-resistant polyacyloxalamidrazone filament as claimed in claim 8 in which the polyacyloxalamidrazone consists essentially of recurring units of the formula consisting of and -OH OH 10.

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• Chemical & Material Sciences (AREA)
• Engineering & Computer Science (AREA)
• Textile Engineering (AREA)
• Health & Medical Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Medicinal Chemistry (AREA)
• Polymers & Plastics (AREA)
• Organic Chemistry (AREA)
• Artificial Filaments (AREA)
• Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
• Compositions Of Macromolecular Compounds (AREA)

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Cited By (2)

Citations (2)

• 1970
  • 1970-03-23 ZA ZA701993A patent/ZA701993B/xx unknown
  • 1970-03-24 GB GB1252385D patent/GB1252385A/en not_active Expired
  • 1970-04-02 CS CS7000002179A patent/CS184307B2/cs unknown
  • 1970-04-02 BE BE748358D patent/BE748358A/xx unknown
  • 1970-04-07 RO RO63018A patent/RO57974A/ro unknown
  • 1970-04-13 ES ES378502A patent/ES378502A1/es not_active Expired
  • 1970-04-15 BG BG014496A patent/BG17638A3/xx not_active Expired
  • 1970-04-16 AT AT347970A patent/AT301740B/de not_active IP Right Cessation
  • 1970-04-17 CH CH573970A patent/CH515378A/de not_active IP Right Cessation
  • 1970-04-17 CH CH573970D patent/CH573970A4/xx unknown
  • 1970-04-27 US US32394A patent/US3661502A/en not_active Expired - Lifetime
  • 1970-04-28 HU HUGA1006A patent/HU168216B/hu unknown
  • 1970-04-29 SE SE05946/70A patent/SE351870B/xx unknown
  • 1970-04-29 LU LU60826D patent/LU60826A1/xx unknown
  • 1970-04-29 NL NL7006292A patent/NL7006292A/xx unknown
  • 1970-04-30 FR FR7016047A patent/FR2047206A5/fr not_active Expired
• 1994
  • 1994-02-28 BG BG098605A patent/BG98605A/bg unknown

Patent Citations (2)

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