US2953480A - Process for producing fire-retardant nylon fabric - Google Patents
Process for producing fire-retardant nylon fabric Download PDFInfo
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- US2953480A US2953480A US392999A US39299953A US2953480A US 2953480 A US2953480 A US 2953480A US 392999 A US392999 A US 392999A US 39299953 A US39299953 A US 39299953A US 2953480 A US2953480 A US 2953480A
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- United States
- Prior art keywords
- fabric
- parts
- flame
- nylon
- ammonium bromide
- Prior art date
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- 239000004744 fabric Substances 0.000 title claims description 43
- 229920001778 nylon Polymers 0.000 title claims description 21
- 239000004677 Nylon Substances 0.000 title claims description 20
- 239000003063 flame retardant Substances 0.000 title claims description 13
- 238000000034 method Methods 0.000 title claims description 11
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 claims description 20
- 239000007864 aqueous solution Substances 0.000 claims description 8
- XOGJBKWFLRETGW-UHFFFAOYSA-N 5-aminotriazine-4-carbaldehyde Chemical compound NC1=CN=NN=C1C=O XOGJBKWFLRETGW-UHFFFAOYSA-N 0.000 claims description 6
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 229920005989 resin Polymers 0.000 description 16
- 239000011347 resin Substances 0.000 description 16
- 239000000463 material Substances 0.000 description 13
- 239000004753 textile Substances 0.000 description 11
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 10
- 238000005108 dry cleaning Methods 0.000 description 10
- 230000002209 hydrophobic effect Effects 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 239000000835 fiber Substances 0.000 description 8
- USDJGQLNFPZEON-UHFFFAOYSA-N [[4,6-bis(hydroxymethylamino)-1,3,5-triazin-2-yl]amino]methanol Chemical class OCNC1=NC(NCO)=NC(NCO)=N1 USDJGQLNFPZEON-UHFFFAOYSA-N 0.000 description 7
- 229920002994 synthetic fiber Polymers 0.000 description 7
- 238000011282 treatment Methods 0.000 description 7
- QQOWHRYOXYEMTL-UHFFFAOYSA-N triazin-4-amine Chemical compound N=C1C=CN=NN1 QQOWHRYOXYEMTL-UHFFFAOYSA-N 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 229920000877 Melamine resin Polymers 0.000 description 5
- 235000019270 ammonium chloride Nutrition 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 4
- 238000007706 flame test Methods 0.000 description 4
- 239000012209 synthetic fiber Substances 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 229920000297 Rayon Polymers 0.000 description 3
- 150000003863 ammonium salts Chemical class 0.000 description 3
- 229920002301 cellulose acetate Polymers 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000002657 fibrous material Substances 0.000 description 3
- 238000004079 fireproofing Methods 0.000 description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 3
- 229920002972 Acrylic fiber Polymers 0.000 description 2
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000004640 Melamine resin Substances 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- MBHRHUJRKGNOKX-UHFFFAOYSA-N [(4,6-diamino-1,3,5-triazin-2-yl)amino]methanol Chemical class NC1=NC(N)=NC(NCO)=N1 MBHRHUJRKGNOKX-UHFFFAOYSA-N 0.000 description 2
- 150000001299 aldehydes Chemical class 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- IVJISJACKSSFGE-UHFFFAOYSA-N formaldehyde;1,3,5-triazine-2,4,6-triamine Chemical compound O=C.NC1=NC(N)=NC(N)=N1 IVJISJACKSSFGE-UHFFFAOYSA-N 0.000 description 2
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 2
- -1 methyl acrylate Chemical class 0.000 description 2
- 229920002239 polyacrylonitrile Polymers 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004758 synthetic textile Substances 0.000 description 2
- 238000009988 textile finishing Methods 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- YZEZMSPGIPTEBA-UHFFFAOYSA-N 2-n-(4,6-diamino-1,3,5-triazin-2-yl)-1,3,5-triazine-2,4,6-triamine Chemical compound NC1=NC(N)=NC(NC=2N=C(N)N=C(N)N=2)=N1 YZEZMSPGIPTEBA-UHFFFAOYSA-N 0.000 description 1
- KGIGUEBEKRSTEW-UHFFFAOYSA-N 2-vinylpyridine Chemical class C=CC1=CC=CC=N1 KGIGUEBEKRSTEW-UHFFFAOYSA-N 0.000 description 1
- NAMCDLUESQLMOZ-UHFFFAOYSA-N 6-ethyl-1,3,5-triazine-2,4-diamine Chemical compound CCC1=NC(N)=NC(N)=N1 NAMCDLUESQLMOZ-UHFFFAOYSA-N 0.000 description 1
- GEHMBYLTCISYNY-UHFFFAOYSA-N Ammonium sulfamate Chemical compound [NH4+].NS([O-])(=O)=O GEHMBYLTCISYNY-UHFFFAOYSA-N 0.000 description 1
- 238000012935 Averaging Methods 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- NJYZCEFQAIUHSD-UHFFFAOYSA-N acetoguanamine Chemical compound CC1=NC(N)=NC(N)=N1 NJYZCEFQAIUHSD-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 150000005215 alkyl ethers Chemical class 0.000 description 1
- 230000002152 alkylating effect Effects 0.000 description 1
- YSKUZVBSHIWEFK-UHFFFAOYSA-N ammelide Chemical compound NC1=NC(O)=NC(O)=N1 YSKUZVBSHIWEFK-UHFFFAOYSA-N 0.000 description 1
- MASBWURJQFFLOO-UHFFFAOYSA-N ammeline Chemical compound NC1=NC(N)=NC(O)=N1 MASBWURJQFFLOO-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 150000001642 boronic acid derivatives Chemical class 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000007859 condensation product Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical class [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 1
- 235000019838 diammonium phosphate Nutrition 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000009970 fire resistant effect Effects 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- YSRVJVDFHZYRPA-UHFFFAOYSA-N melem Chemical compound NC1=NC(N23)=NC(N)=NC2=NC(N)=NC3=N1 YSRVJVDFHZYRPA-UHFFFAOYSA-N 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000002685 polymerization catalyst Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002964 rayon Substances 0.000 description 1
- 230000000979 retarding effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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
- D06M11/07—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
- D06M11/13—Ammonium halides or halides of elements of Groups 1 or 11 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
- 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
Definitions
- the present invention relates to a fire-retardant treatment for flammable hydrophobic synthetic textile materials and the resulting product.
- An object of the invention is to provide an improved fire-retardant treatment for fibrous materials of nitrogen containing hydrophobic synthetic fibers.
- Another object of the invention is to provide improved flame-res-istant textile materials of nitrogen con-- taining hydrophobic synthetic fibers.
- a further object of the invention is to provide improved flame-resistant stiffened textile materials containing nylon fibers.
- the present invention is concerned with a process of applying an aqueous solution of ammonium bromide and an aminotriazine-aldehyde condensate to a flammable material containing synthetic hydrophobic fibers and curing the condensate to the water-soluble state as well as the resulting fire-resistant product.
- the present treatment is highly effective with flammable, hydrophobic synthetic fibrous materials. Hydrophobic fibers absorb little or no water; hence viscose and cupro-ammonium rayon fibers are outside of the scope of this invention even if they are considered to be synthetic materials. However, it is operative with cellulose acetate and other polyesters including polyethylene glycol terephthalate, whereas prior art compositions do not provide satisfactory flame-resistance.
- the invention is particularly adapted for the treatment of nitrogen-containing syntetics such as the linear polyamides known as.
- nylon and acrylic fibers containing homopolymers of acrylonitrile or copolymers with suitable ethylenic compounds such as methyl acrylate, 2-methyl S-vinyl pyridine,
- the salt In addition to its fire-retardant qualities the salt also functions as a curing agent for the aminotriazinealdehyde condensate; while other and more eflicient accelerators may be added if desired, they are not necessary.
- a combined fire-retardant and resin finish is obtained on the textile which is particularly desirable for stiffening fabrics such as the nylon netting used in making underskirts and veils for women.
- Aminotriazine resins suitable for use in the process described herein include water-soluble condensates of an aldehyde with an aminotriazine of the type disclosed in the Widmer et al. Patent No. 2,197,357 as well as those set forth in Iohnstone et al. Patent Re. 22,566. These materials are commonly applied to cloth in textile finishing as aqueous solutions containing a curing or polymerization catalyst or accelerator; then the fabric is dried and cured at an elevated temperature to convert the resin to the water-insoluble state.
- Widmer et al. disclose a large number of aminotriazines including melamine, acetoguanamine, propioguanamine, melam, melem,
- ammeline, ammelide, and the like which may be condensed with various aliphatic, aromatic and heterocyclic aldehydes.
- Formaldehyde is of course the preferred aldehyde by reason of its cheapness and ready availability.
- Johnstone et a1. teach that desirable textile treating resins can be manufactured from such products by alkylating them to produce the methyl or other alkyl ethers of the aminotriazine-aldehyde condensation product. Methylated trimethylol melamine and diand trimethylol melamines are especially recommended for the present purposes.
- aminotriazine resin aminotriazine-aldehyde condensate
- melamine-formaldehyde condensate are employed herein to denote both the alkylated and unalkylated derivatives disclosed in the aforesaid patents.
- the treated fabrics should contain at least about 12% of the ammonium bromide based on the dry weight of the untreated fabric and it is usually preferred to deposit or more of ammonium bromide on the fabric. Where a relatively stiff fabric is desirable or acceptable, this quantity may be increased to between and 50% and in some instances it may be desirable to deposit the largest quantity obtainable in an aqueous bath; thus, amounts of ammonium bromide running up to 100% or more of the Weight of dry untreated fabric are suggested.
- the Weight of resin deposited should be more than the weight of the ammonium salt; thus, for each 100 parts of ammonium bromide in the treating bath the quantity of aminotriazine resin may range from slightly more than 100 up to 500 parts or more, bearing in mind that excessive amounts of resin may limit the deposition of ammonium salts on the fabric to an extent sufficient to diminish the fire-retardant qualities of the product. In general, between about 105 and about 300 parts of resin are desirable for each 100 parts of ammonium bromide in the pad bath.
- the impregnated fabrics may be cured in conventional equipment operating at temperatures ranging from about 200 to about 500 F. for periods varying inversely with the temperature and ranging from about 10 seconds to about 30 minutes. In practice, there is little need to ever exceed 400 F.
- Example 1 Nylon twill is padded through an aqueous solution of 40 parts of methylated methylolmelamine and 20 parts of ammonium bromide in solution in 40 parts of water. The squeeze rolls are adjusted for a wet pick-up of 100% based on the weight of dry cloth. The impregnated cloth is dried for 3 minutes at 220 F. and then cured for 6 minutes at 290 F. The resulting fabric does not flame when tested with a match flame.
- Example 2 Example 1 is repeated with a more dilute treating bath containing 30 parts of methylated methylolmelamine and 15 parts of ammonium bromide dissolved in 55 parts of water.
- the nylon twill is bearing 30% resin and 15% ammonium bromide based on the weight of dry fabric. Again, the treated fabric does not flame when tested with a match flame.
- Example 3 Nylon net is impregnated and cured in the manner set forth in Example 1.
- the char height is found to be 7.2 inches and no dripping of molten particles of nylon occurs during the test.
- the untreated nylon net material melts and some flaming drops fall off in this test whereas nylon net stiffened with the same quantity of the melamine resin is completely combustible because of its open construction Which affords ready access to air and its relatively great surface area, thus this particular material provides an extremely severe test for a flameretardant composition.
- Example 4 Nylon netting is padded through a bath made up of 30 parts of ammonium bromide, 32 parts of methylated trimethylol melamine and 38 parts of water, using two dips and two hips and a pressure of one ton; and the wet pick-up amounts to about 75%. After drying and curing [for 3 minutes at 300 F. the material is subjected to a commercial dry cleaning operation and thereafter found to have a char length averaging 4.2 inches when several samples are tested by the standard test. Other samples 'of the treated fabric are subjected to 3 dry cleanings and then found to have an average char length of 6.5 inches in the standard flame test.
- Additional treated samples are subjected to 5 dry cleanings and then found to have an average char length of 4.8 inches in the flame test. None of the samples shows afterglow or afterfiaming in the A.A.T.C.C. test and none supports combustion upon contact with a match flame.
- Example 5 Example 4 is repeated using a pad bath containing 48% methylated trimethylol melamine, 30% ammonium bromide and 22% water with a 75% Wet pick-up as before.
- the average char length of the impregnated fabric is 6. 6 inches after 1 dry cleaning, 6.5 inches after 3 cleanings and 4.8 inches after 5 dry cleanings.
- Example 7 Example 4 is again repeated with a pad bath containing 56 parts of the same resin, 30 parts of ammonium bromide and 114 parts of water with the usual 75 Wet pick-up. After 1 dry cleaning of the treated fabric the average char length is found to be 3.7 inches. After 3 oommerical dry cleanings, the figures is 5.6 inches, and after 5 dry cleanings the average char-length of the material is found to be 7.1 inches upon application of the standard test.
- Example 5 The bath used in Example 5 is stable for 10 hours without appreciable precipitation. By addition of one, two and three percent of ammonia calculated as NH OH, to samples of this pad bath the stability is increased to 20, 28 and 44 hours respectively. Such stability is ample for practical application of the present process in conventional textile finishing plants.
- Example A The procedure of Example 4 is followed in impregnating nylon net with an aqueous solution of 10 parts of ammonium chloride, 40 parts of methylated trimethylol melamine and 50 parts of water. No dry cleaning operations are employed. After curing the impregnated fabric is found to be combustible.
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Description
Patented Sept. 20, 1960 PROCESS FOR PRODUCING FIRE-RETARDANT NYLON FABRIC Maurice R. Burnell, Darien, Conn., assignor to American Cyanamid Company, New York, N.Y.,' a corporation of Maine No Drawing. Filed Nov. 18, 1953, Ser. No. 392,999
2 Claims. (Cl. 117-137) The present invention relates to a fire-retardant treatment for flammable hydrophobic synthetic textile materials and the resulting product.
A wide variety of substances have been applied to textile fabrics woven from natural fibers and viscose rayon for the purpose of fireproofing the fabrics with varying degrees of success. Phosphates, borates, metal oxides, and ammonium salts including the bromide are among the great number of compounds which have been suggested. Practically all of the fire-retardant agents have been found to be either ineffective or otherwise undesirable for use on the synthetic hydrophobic textiles. These materials pose special problems due to their unusual characteristics as, for instance, their behavior in a flame which differs considerably from that of the natural fibers. A number of the synthetic fibers melt before burning and then drip or fall off the fabric as molten flaming pellets. This phenomenon not only spreads the fire but also resulted in very severe burns to persons wearing apparel made from such textile fibers.
An object of the invention is to provide an improved fire-retardant treatment for fibrous materials of nitrogen containing hydrophobic synthetic fibers.
Another object of the invention is to provide improved flame-res-istant textile materials of nitrogen con-- taining hydrophobic synthetic fibers.
A further object of the invention is to provide improved flame-resistant stiffened textile materials containing nylon fibers.
Other objects of the invention will be apparent to those skilled in the art from the detailed description hereinbelow.
The present invention is concerned with a process of applying an aqueous solution of ammonium bromide and an aminotriazine-aldehyde condensate to a flammable material containing synthetic hydrophobic fibers and curing the condensate to the water-soluble state as well as the resulting fire-resistant product.
The present treatment is highly effective with flammable, hydrophobic synthetic fibrous materials. Hydrophobic fibers absorb little or no water; hence viscose and cupro-ammonium rayon fibers are outside of the scope of this invention even if they are considered to be synthetic materials. However, it is operative with cellulose acetate and other polyesters including polyethylene glycol terephthalate, whereas prior art compositions do not provide satisfactory flame-resistance. The invention is particularly adapted for the treatment of nitrogen-containing syntetics such as the linear polyamides known as.
nylon and acrylic fibers containing homopolymers of acrylonitrile or copolymers with suitable ethylenic compounds such as methyl acrylate, 2-methyl S-vinyl pyridine,
other vinyl pyridines, vinyl acetate, vinyl chloride, etc;
All of these flammable hydrophobic synthetic fibers appear to fall into the samefgroup'in respect to the problem of obtaining flame-resistance."
' Tests on cellulose acetate, nylon and acrylic fabrics have indicated very unsatisfactory fireproofing not only with the commercially-used fire-retardants such as the monomethylol dicyandiamide-phosphoric acid mixture, antimony trioxide and polyvinyl chloride latex, monoand diammonium phosphates and ammonium sulfamate, but also prior art agents including ammonium chloride, phosphoric acid, mixed borax and boric acid, chlorides of calcium, magnesium, zinc, copper, chromium, cobalt and nickel, ammonium sulfate, etc. Based on a lesser but still substantial amount of data, it is apparent that admixture with a melamine resin such as methylated trimethylol melamine will -not procure adequate flame retarding qualities on the synthetic fibrous materials. In addition, some of the known fireproofing treatments produce other undesirable results as exemplifiedby the discoloration of polyacrylonitrile fabrics by alkaline substances. From this it is apparent that the flameproofing of synthetic hydrophobic textile materials with any selected composition, including those employed on natural fibers, cannot be predicted as further evidenced by the fact that ammonium chloride cannot be substituted for ammonium bromide in the compositions set forth herein with equivalent results.
Although it was discovered that good flame-resistance could be obtained by impregnating nylon, cellulose acetate, an acrylic fiber (copolymer of acrylon-itr-ile and 5% methyl acrylate), and the like with an aqueous solution of ammonium bromide alone, the resulting finish was nondurable, somewhat hygroscopic and tended to dust off under severe flexing or manipulation of the textile fiabric. It was found that the addition of an aminotriazine condensate overcame these defects and also provided a resin finish durable to dry cleaning; accordingly, the compositions employed in the novel process comprise ammonium bromide and an aminotriazine resin. In addition to its fire-retardant qualities the salt also functions as a curing agent for the aminotriazinealdehyde condensate; while other and more eflicient accelerators may be added if desired, they are not necessary. Thus, a combined fire-retardant and resin finish is obtained on the textile which is particularly desirable for stiffening fabrics such as the nylon netting used in making underskirts and veils for women.
When the novel treatment is applied to a hydrophobic synthetic textile fabric of a flammable and fusible nature, the behavior of the treated fabric in a flame is quite different from that of the untreated fabric. The fabric will still melt While in the flame, but charred beads are formed which show little or no tendency to separate and drop off the remainder of the fabric. This substantially eliminates injury to persons from exposure to molten flaming drops of the textile material and minimizes spreading the fire. Further, the treated fiabric displays no afterglow or afterflaming when the test flame is removed.
The treatment described herein is particularly applicable to the flameproofing of net materials, upholstery fabrics, draperies, stage scenery, and the like. It also provides effective results on knitted and felted fabrics as well as loose fibers which may be employed as stuffing or padding.
Aminotriazine resins suitable for use in the process described herein include water-soluble condensates of an aldehyde with an aminotriazine of the type disclosed in the Widmer et al. Patent No. 2,197,357 as well as those set forth in Iohnstone et al. Patent Re. 22,566. These materials are commonly applied to cloth in textile finishing as aqueous solutions containing a curing or polymerization catalyst or accelerator; then the fabric is dried and cured at an elevated temperature to convert the resin to the water-insoluble state. Widmer et al. disclose a large number of aminotriazines including melamine, acetoguanamine, propioguanamine, melam, melem,
ammeline, ammelide, and the like, which may be condensed with various aliphatic, aromatic and heterocyclic aldehydes. Formaldehyde is of course the preferred aldehyde by reason of its cheapness and ready availability. Johnstone et a1. teach that desirable textile treating resins can be manufactured from such products by alkylating them to produce the methyl or other alkyl ethers of the aminotriazine-aldehyde condensation product. Methylated trimethylol melamine and diand trimethylol melamines are especially recommended for the present purposes. The expressions aminotriazine resin, aminotriazine-aldehyde condensate and melamine-formaldehyde condensate are employed herein to denote both the alkylated and unalkylated derivatives disclosed in the aforesaid patents.
To provide adequate flame-resistance, the treated fabrics should contain at least about 12% of the ammonium bromide based on the dry weight of the untreated fabric and it is usually preferred to deposit or more of ammonium bromide on the fabric. Where a relatively stiff fabric is desirable or acceptable, this quantity may be increased to between and 50% and in some instances it may be desirable to deposit the largest quantity obtainable in an aqueous bath; thus, amounts of ammonium bromide running up to 100% or more of the Weight of dry untreated fabric are suggested. The Weight of resin deposited should be more than the weight of the ammonium salt; thus, for each 100 parts of ammonium bromide in the treating bath the quantity of aminotriazine resin may range from slightly more than 100 up to 500 parts or more, bearing in mind that excessive amounts of resin may limit the deposition of ammonium salts on the fabric to an extent sufficient to diminish the fire-retardant qualities of the product. In general, between about 105 and about 300 parts of resin are desirable for each 100 parts of ammonium bromide in the pad bath.
The impregnated fabrics may be cured in conventional equipment operating at temperatures ranging from about 200 to about 500 F. for periods varying inversely with the temperature and ranging from about 10 seconds to about 30 minutes. In practice, there is little need to ever exceed 400 F.
For better understanding of the nature and objects of the present invention reference should be had to the following examples in which proportions are expressed in terms of weight unless otherwise indicated.
Example 1 Nylon twill is padded through an aqueous solution of 40 parts of methylated methylolmelamine and 20 parts of ammonium bromide in solution in 40 parts of water. The squeeze rolls are adjusted for a wet pick-up of 100% based on the weight of dry cloth. The impregnated cloth is dried for 3 minutes at 220 F. and then cured for 6 minutes at 290 F. The resulting fabric does not flame when tested with a match flame.
Example 2 Example 1 is repeated with a more dilute treating bath containing 30 parts of methylated methylolmelamine and 15 parts of ammonium bromide dissolved in 55 parts of water. Here the nylon twill is bearing 30% resin and 15% ammonium bromide based on the weight of dry fabric. Again, the treated fabric does not flame when tested with a match flame.
Example 3 Nylon net is impregnated and cured in the manner set forth in Example 1. Upon applying the standard A.A.T.-C.C. flame test, the char height is found to be 7.2 inches and no dripping of molten particles of nylon occurs during the test. The untreated nylon net material melts and some flaming drops fall off in this test whereas nylon net stiffened with the same quantity of the melamine resin is completely combustible because of its open construction Which affords ready access to air and its relatively great surface area, thus this particular material provides an extremely severe test for a flameretardant composition.
Example 4 Nylon netting is padded through a bath made up of 30 parts of ammonium bromide, 32 parts of methylated trimethylol melamine and 38 parts of water, using two dips and two hips and a pressure of one ton; and the wet pick-up amounts to about 75%. After drying and curing [for 3 minutes at 300 F. the material is subjected to a commercial dry cleaning operation and thereafter found to have a char length averaging 4.2 inches when several samples are tested by the standard test. Other samples 'of the treated fabric are subjected to 3 dry cleanings and then found to have an average char length of 6.5 inches in the standard flame test. Additional treated samples are subjected to 5 dry cleanings and then found to have an average char length of 4.8 inches in the flame test. None of the samples shows afterglow or afterfiaming in the A.A.T.C.C. test and none supports combustion upon contact with a match flame.
Example 5 Example 4 is repeated using a pad bath containing 48% methylated trimethylol melamine, 30% ammonium bromide and 22% water with a 75% Wet pick-up as before. The average char length of the impregnated fabric is 6. 6 inches after 1 dry cleaning, 6.5 inches after 3 cleanings and 4.8 inches after 5 dry cleanings.
Example 7 Example 4 is again repeated with a pad bath containing 56 parts of the same resin, 30 parts of ammonium bromide and 114 parts of water with the usual 75 Wet pick-up. After 1 dry cleaning of the treated fabric the average char length is found to be 3.7 inches. After 3 oommerical dry cleanings, the figures is 5.6 inches, and after 5 dry cleanings the average char-length of the material is found to be 7.1 inches upon application of the standard test.
No afterglow or afterfiaming is present during any of the flame tests run in Examples 5 through 7 inclusive and none of those treated samples supports combustion when tested with a burning match.
The bath used in Example 5 is stable for 10 hours without appreciable precipitation. By addition of one, two and three percent of ammonia calculated as NH OH, to samples of this pad bath the stability is increased to 20, 28 and 44 hours respectively. Such stability is ample for practical application of the present process in conventional textile finishing plants.
Example A The procedure of Example 4 is followed in impregnating nylon net with an aqueous solution of 10 parts of ammonium chloride, 40 parts of methylated trimethylol melamine and 50 parts of water. No dry cleaning operations are employed. After curing the impregnated fabric is found to be combustible.
Example B A treating bath containing 30 parts of ammonium chloride, 40 parts of the same resin and 30 parts of water is made up in an eflfort to duplicate Example 5, but the resin precipitates immediately and hence cannot be applied to a textile fabric.
Example C Upon preparing a bath from 20 parts of ammonium chloride, 40 parts of methylated trimethylol melamine and 40 parts of water, the resin again precipitates.
Since certain changes may be made in carrying out the above process and in the product without departing from the scope of the invention, it is intended that all matter contained in the above description and examples shall be interpreted as illustrative and not in a limiting sense.
I claim:
1. A process for producing a fireretardant nylon fabric which comprises applying an aqueous solution of 100 parts by weight of ammonium bromide and between about 100 and about 500 parts of an aminotriazine-formaldehyde condensate to said nylon fabric in suflicient quantity to deposit thereon at least about 12 percent of ammonium bromide based on the dry Weight of the fabric and curing the condensate to the water-insoluble state by heating the treated fabric to an elevated temperature.
2. A process for producing a fire-retardant nylon fabric which comprises applying an aqueous solution of 100 parts by weight of ammonium bromide and between about and about 500 parts of "a melamine-formaldehyde condensate to said nylon fabric in suflicient quantity to deposit thereon at least about il5 percent of ammonium bromide based on the dry weight of the fabric and curing the condensate on the fabric at a temperature between about 200 and about 400 degrees Fahrenheit for a period suificient to convert the condensate to the water-insoluble state.
References Cited in the file of this patent UNITED STATES PATENTS 2,322,888 Schwartz et a1 June 29, 1943 2,415,113 Seymour et a1. Feb. 4, 1947 2,452,054 Jones et a1 .Oct. 26, 1948 2,462,803 Campbell et a1. Feb. 22, 1949 2,5 82,961 Burnell et al I an. 22, 1952 2,628,946 Juda et al Feb. 17, 1953 2,658,880 Landau Nov. '10, 1953 2,684,953 Stilbert et a1 July 27, 11954 FOREIGN PATENTS 202,302 Great Britain Nov. 3, 1924 476,043 Great Britain Nov. 29, 1937
Claims (1)
1. A PROCESS FOR PRODUCING A FIRE-RETARDANT NYLON FABRIC WHICH COMPRISES APPLYING AN AQUEOUS SOLUTION OF 100 PARTS BY WEIGHT OF AMMONIUM BROMIDE AND BETWEEN ABOUT 100 AND ABOUT 500 PARTS OF AN AMINOTRIAZINE-FORMALDEHYDE CONDENSATE TO SAID NYLON FABRIC IN SUFFICIENT QUANITY TO DEPOSIT THEREON ON THE DRY WEIGHT OF THE FABRIC AND CURING BROMIDE BASED ON THE DRY WEIGHT OF THE FABRIC AND CURING THE CONDENSATE TO THE WATER-SOLUBLE STATE BY HEATING THE TREATED FABRIC TO AN ELEVATED TEMPERATURE.
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US392999A US2953480A (en) | 1953-11-18 | 1953-11-18 | Process for producing fire-retardant nylon fabric |
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US392999A US2953480A (en) | 1953-11-18 | 1953-11-18 | Process for producing fire-retardant nylon fabric |
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Cited By (11)
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US3047425A (en) * | 1959-07-16 | 1962-07-31 | Monsanto Chemicals | Method for producing flame and soil resistant acrylic polymer fibers containing carpet fabric |
US3383240A (en) * | 1964-06-19 | 1968-05-14 | Monsanto Co | Flame resistant composition and method of treating acrylic containing textile fibers therewith and the resulting product |
US3471318A (en) * | 1960-11-28 | 1969-10-07 | Nelson Silk Ltd | Finished flame-resistant textile materials |
DE1694254A1 (en) * | 1968-03-16 | 1971-06-16 | Bayer Ag | Self-extinguishing polyamide molding compounds |
US3620818A (en) * | 1968-10-09 | 1971-11-16 | Monsanto Co | Method of imparting flame resistant properties to nylon and the treated product |
DE2314214A1 (en) * | 1972-03-23 | 1973-10-04 | Toray Industries | METHOD FOR MANUFACTURING MELT RESISTANT SYNTHETIC FIBERS |
US3816212A (en) * | 1970-11-13 | 1974-06-11 | American Cyanamid Co | Process for bonding and flame proofing webs of synthetic fibers |
US3916044A (en) * | 1970-12-21 | 1975-10-28 | Collins & Aikman Corp | Method for improving the flame retardancy of synthetic linear polyesters |
US4600606A (en) * | 1979-04-18 | 1986-07-15 | White Chemical Corporation | Process for rendering non-thermoplastic fibrous materials flame resistant to molten materials by application thereto of a flame resistant composition, and related articles and compositions |
US4623583A (en) * | 1979-04-18 | 1986-11-18 | White Chemical Corporation | Flame retardant textile fabrics |
US20060202175A1 (en) * | 2005-03-10 | 2006-09-14 | Yang Charles Q | Flame retarding system for nylon fabrics |
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Publication number | Priority date | Publication date | Assignee | Title |
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US3047425A (en) * | 1959-07-16 | 1962-07-31 | Monsanto Chemicals | Method for producing flame and soil resistant acrylic polymer fibers containing carpet fabric |
US3471318A (en) * | 1960-11-28 | 1969-10-07 | Nelson Silk Ltd | Finished flame-resistant textile materials |
US3383240A (en) * | 1964-06-19 | 1968-05-14 | Monsanto Co | Flame resistant composition and method of treating acrylic containing textile fibers therewith and the resulting product |
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US20060202175A1 (en) * | 2005-03-10 | 2006-09-14 | Yang Charles Q | Flame retarding system for nylon fabrics |
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