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
  • D01F1/00—General methods for the manufacture of artificial filaments or the like
  • D01F1/02—Addition of substances to the spinning solution or to the melt
  • D01F1/04—Pigments
• • 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
  • C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
  • C08G73/14—Polyamide-imides
• • 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
  • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
  • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
  • D01F6/74—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polycondensates of cyclic compounds, e.g. polyimides, polybenzimidazoles
• • 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
  • Y10T428/00—Stock material or miscellaneous articles
  • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
  • Y10T428/2913—Rod, strand, filament or fiber
  • Y10T428/2918—Rod, strand, filament or fiber including free carbon or carbide or therewith [not as steel]

Definitions

• the present invention relates to noninflammable yarns and fibers having a base of polyamide-imide, with a high power of adsorption.
• yarns and fibers containing 8 to 35% activated carbon referred to the quantity of dry materials
• an iodine number of 100 to 500 and a specific surface of 90300 m lg.
• the yarns in accordance with the invention are used, for example, in fabrics for protection against harmful gases, in the manufacture of cigarette filters, etc.
• the present invention relates to novel 'noninflammable fibers and yarns having a base of polyamide-imide which comprise substantial quantities of activated carbon, as well as articles obtained from said yarns.
• Noninflammable fibers and yarns are to be understood as yarns which have Successfully passed the test published in the American Association of Textile Chemists and Colourists No. 34, 1966.
• the present invention also concerns the process of.
• the quantity of pigment incorporated is preferably of the order of 1% and not in excess of 3% of the total quantity of the material if it is desired to be able to spin under good conditions and to obtain yarns having sufficiently good qualities to be used as such and not carbonized or graphitized.
• the invention also relates to a process of obtaining noninflammable fibers having a base of polyamideimide which comprises in succession:
• polyamide-imide there are understood polymers having amide-imide linkages of the formula:
• the polyamides-imides of the above formula are obtained by reacting, in a polar organic solvent, in substantially stoichiometric proportions, at least one aromatic diisocyanate and one acid reagent comprising at least one aromatic, aliphatic or cycloaliphatic acid anhydride and possibly a diacid.
• diisocyanates which can be used for the obtaining of these polymers mentioned may be made of monocyclic diisocyanates, such as toluylenediisocyanates, and dicyclic diisocyanates, of preferably symmetrical nature, such as 4,4-diisocyanatodiphenyl-methane, 4,4'-diisocyanato-diphenyl-propane and 4,4'-diisocyanato-diphenyl-ether.
• monocyclic diisocyanates such as toluylenediisocyanates
• dicyclic diisocyanates of preferably symmetrical nature, such as 4,4-diisocyanatodiphenyl-methane, 4,4'-diisocyanato-diphenyl-propane and 4,4'-diisocyanato-diphenyl-ether.
• trimellitic anhydride is preferably employed.
• diacids there are preferably employed terephthalic acid or isophthalic acid, the proportions of the diacid in the acid reagent being generally between 5 and mol and preferably 20807( referred to the mixture of anhydride and diacid.
• the polyamide-imides utilized herein are, of course, a well known class of polymers.
• the activated carbon which can be used in accordance with the present invention is a form of carbon of high specific surface, and of very small particle size, of the order of a few microns, which possesses active centers and which contains other substances such as oxygen.
• an activated carbon of good iodine number and of a specific surface which is generally greater than 1000 m /g in order to obtain the maximum effect.
• the fabrics obtained from the said yarns are very use ful as fabrics for protection against harmful gases and furthermore have the advantage of being noninflammable due to the very nature of the polyamides-imides.
• the yarns of the present invention can also be used in the manufacture of cigarette or antipollution filters.
• the adsorbent power of the yarns containing activated carbon is evaluated by the iodine number" which represents the number of milligrams of iodine fixed per gram of dry substance.
• the specific surface of the yarns is measured by the BET (Brunauer-Emmett-Teller) method which has been described in numerous publications.
• the polymer used must have an inherent viscosity of between 0.8 and 1.6 (and preferably between 0.9 and 1.4). The inherent viscosity is measured at C on a 0.5 wt. solution of polymer per volume ofpolar organic solvent.
• organic solvent N-methylpyrrolidone is preferably employed.
• the spinning solution it is generally preferred first of all to prepare a master mix containing the solvent, the polymer and a high proportion of activated carbon.
• the master mix is crushed so as to obtain good uniformity of the polymer and carbon mix and avoid agglomeration of the particles of carbon'and thus permit easy spinning.
• the spinning is effected by the wet process, which is well known to those skilled in the art, in a coagulating bath composed essentially of water and of solvent for the polymer wherein the proportion of solvent may vary between and 65%, ordinarily at room temperature.
• the filaments are drawn in customary fashion by any means known to those skilled in the art, for instance in air at room temperature, to the extent of generally between 12 X and 2.5 X.
• the drawing contributes to imparting good physical and mechanical properties to the filaments without decreasing the number of active sites of the carbon, which retains its adsorbent power.
• the filaments are then washed with water, generally continuously, at room temperature, for instance by passage through one or more tanks or over rollers to eliminate the solvent, which is then reused.
• the drying can be effected in customary fashion, for instance on rollers. It is generally preferable to dry at a temperature not above 150C in order that the yarns may retain their full activity.
• the filaments may undergo a heat treatment at a temperature which may vary from 200 to 220C in a stove, or preferably a subsequent washing in known manner, for instance with a volatile organic compound such as acetone.
• a solution A of a polyamide-imide is prepared by reaction of 153.6 g of trimellitic anhydride, 250 g of diisocyanato-4,4-diphenylmethane and 33.2 g of terephthalic acid in 1310 g of N-methyl-pyrrolidone.
• the polymer obtained has an inherent viscosity of 1. l l and the I solution has a concentration of 21% by weight of polymer.
• the spinning solution thus obtained is spun into a coagulating bath containing 40% water and 60% N-methylpyrrolidone, maintained at a temperature of 22C.
• the filaments drawn in air by 1.51 X are washed on rollers at a speed of 1 1.7 m/min. before being dried in a known manner and treated in a stove for 2 /2 hours at 240C under a pressure of 5 mm Hg,
• the noninflammable filaments which have been treated in this manner and which contain 35% activated carbon have the following properties.
• a mixture is prepared containing 136 g of the polymer obtained above with 796 g of N-methylpyrrolidone and 68 g of activated carbon, of a specific surface of 1270 m /g and an iodine number of 1100, which was previously crushed.
• This C mixture obtained in this manner was treated, after crushing, with an equivalent quantity of A solution to obtain a spinning solution containing 79.3% N-methyl-pyrrolidone,
• the solution is spun into a coagulating bath composed of 40% water and 60% N-methyl-pyrrolidone at about 22C at a speed of 8 m/min. through a spinneret having apertures of 012 mm diameter, provided with a filter the packing of which is composed successively of longotte, cotton and flannelette.
• the filaments drawn in air at a rate of 2 X are washed on rollers at a speed of 16 m/min. and then dried in customary fashion at about 90C and heat-treated under the same conditions as in Example 1.
• Each of these D solutions is mixed with the A solution in equal proportions.
• the spinning solutions thus obtained are extruded into a coagulating bath composed of 40% water and 60% N-methyl-pyrrolidone, maintained at room temperature, through a spinneret having 32 orifices of 0.2 mm diameter.
• the filaments drawn in air tothe extent of 2 X are washed with water at room temperature, then dried at a temperature of about 90C and washed for 30 minutes with acetone.
• noninflammable filaments the properties of which are set forth in the following table:

Landscapes

• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Engineering & Computer Science (AREA)
• General Chemical & Material Sciences (AREA)
• Textile Engineering (AREA)
• Medicinal Chemistry (AREA)
• Organic Chemistry (AREA)
• Polymers & Plastics (AREA)
• Health & Medical Sciences (AREA)
• Manufacturing & Machinery (AREA)
• Artificial Filaments (AREA)
• Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
• Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
• Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Applications Claiming Priority (1)

Publications (1)

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ID=9081896

Family Applications (1)

Country Status (13)

Cited By (16)

Families Citing this family (2)

Citations (12)

Family Cites Families (1)

• 0
  • BE BE787501D patent/BE787501A/xx not_active IP Right Cessation
• 1971
  • 1971-08-12 FR FR7129800A patent/FR2149021A5/fr not_active Expired
• 1972
  • 1972-07-25 NL NLAANVRAGE7210240,A patent/NL178267C/xx not_active IP Right Cessation
  • 1972-07-31 US US276748A patent/US3904577A/en not_active Expired - Lifetime
  • 1972-08-10 JP JP8034172A patent/JPS5514169B2/ja not_active Expired
  • 1972-08-10 IT IT52093/72A patent/IT965976B/it active
  • 1972-08-10 GB GB3743772A patent/GB1392555A/en not_active Expired
  • 1972-08-10 IE IE1112/72A patent/IE36868B1/xx unknown
  • 1972-08-11 DK DK398472AA patent/DK138400B/da not_active IP Right Cessation
  • 1972-08-11 NO NO2884/72A patent/NO138218C/no unknown
  • 1972-08-11 CA CA149,307A patent/CA985443A/en not_active Expired
  • 1972-08-11 LU LU65893A patent/LU65893A1/xx unknown
  • 1972-08-12 DE DE2239707A patent/DE2239707C3/de not_active Expired

Patent Citations (12)

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