US3563793A - Fireproofed cellulosic material - Google Patents

Fireproofed cellulosic material Download PDF

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Publication number
US3563793A
US3563793A US742182A US3563793DA US3563793A US 3563793 A US3563793 A US 3563793A US 742182 A US742182 A US 742182A US 3563793D A US3563793D A US 3563793DA US 3563793 A US3563793 A US 3563793A
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US
United States
Prior art keywords
compound
fireproofing
value
fibrous material
fireproofed
Prior art date
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Expired - Lifetime
Application number
US742182A
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English (en)
Inventor
Hans Brandeis
Klaus Pfleger
Heinz Bille
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BASF SE
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BASF SE
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Publication of US3563793A publication Critical patent/US3563793A/en
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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
    • 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
    • D06M13/487—Aziridinylphosphines; Aziridinylphosphine-oxides or sulfides; Carbonylaziridinyl or carbonylbisaziridinyl compounds; Sulfonylaziridinyl or sulfonylbisaziridinyl compounds
    • 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
    • Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
    • Y10T442/20—Coated or impregnated woven, knit, or nonwoven fabric which is not [a] associated with another preformed layer or fiber layer or, [b] with respect to woven and knit, characterized, respectively, by a particular or differential weave or knit, wherein the coating or impregnation is neither a foamed material nor a free metal or alloy layer
    • Y10T442/2631—Coating or impregnation provides heat or fire protection
    • Y10T442/2672—Phosphorus containing
    • Y10T442/268—Phosphorus and nitrogen containing compound

Definitions

  • a denotes a value from 0.1 to 2.6
  • b a value from 0.3 to 2
  • c a value from 0.1 to 1.0 the total of a, b and 0 being 3, and cellulosic material fireproofed therewith.
  • the present invention relates to a process for the fireproofing of cellulosic fibrous material using certain phosphorus amides.
  • the amides, particularly the dialkylamides and the 1,2- alkylenamides of phosphoric acid are generally known as fireproofing agents for cellulosic fibrous material.
  • the object of the present invention is to provide new and highly effective fireproofing agents for cellulosic fibrous materials which give optimum and wash-resistant fireproofing effects with a minimum of deleterious secondary effects.
  • cellulosic fibrous materials can be given a wash-resistant fireproof finish by means of phosphoric amides by applying to the fibrous material ice a composition containing or consisting of a mixture of compounds which is defined by the general Formula I:
  • a may have any value from 0.1 to 2.6, b any value from 0.3 to 2.0 and c any value from 0.1 to 1.0, the total of a, b and c being 3 and the indices corresponding to the average frequency of the methylamido, ethylenamido and amido groups in weighable amounts of the trivalent compound (I).
  • the mixtures of compounds (I), which are referred to hereinafter as compounds for simplicity, are obtained by conventional methods, preferably by reaction of 1 mole each of phosphorous oxychloride with a moles of methylamide, b moles of ethylenimine and c moles of ammonia in an inert organic solvent at temperatures of from about 40 C. to +40 C. It is recommended that the solvent (for example methylene chloride, benzene, dioxane, tetrahydrofuran or ether) be placed in a reactor and the reactants be passed into the same simultaneously at the same rate in proportion to the molar composition of the product.
  • solvent for example methylene chloride, benzene, dioxane, tetrahydrofuran or ether
  • a tertiary amine such as trimethylamine or triethylamine should be used to bind hydrogen chloride liberated in the reaction.
  • the hydrochlorides of the tertiary amines are insoluble in the said solvents and can be filtered off therefrom.
  • the solution is then evaporated, advantageously at subatmospheric pressure, after which the product remains as a colorless syrupy liquid. So that it should remain stable for long periods it is advisable to dilute it, for example with dioxane, dimethylformamide or low molecular weight water-soluble alcohols.
  • the mixtures of molecules formed have statistical distribution of the amine radicals on the phosphorus.
  • the new agents are advantageously used in 5 to 50% aqueous solution (percentage here and hereinafter being by weight) for finishing cellulosic fibrous materials, the amount being such that the fibrous material absorbs from about 5 to 50%, preferably from 10 to 30%, of the dry weight of (1) depending on the desired intensity of the fireproofing effect.
  • Application may be for example by dipping, spraying or padding.
  • the agent is fixed thereon by heating for from about two to twenty minutes at about to 200 0, preferably from to C.
  • the fibrous material thus finished is given a conventional after-treatment for removal of unfixed agent; for example it may be washed with hot dilute aqueous alkali metal hydroxide solution or alkali metal carbonate solution.
  • agents (I) are compatible with all other agents for textile finishing, particularly with a great variety of aminoplast-formin-g monomeric, oligomeric and polymeric compounds and may be used together with them.
  • the method according to this invention may be carried out by all procedures and in all apparatus which would otherwise be used for finishing fibrous materials.
  • Cellulosic fibrous materials may include cotton, linen, sisal, hemp, regenerated cellulose and wood-wool in the form of filaments, threads, fibers, wadding, nonwoven fabrics or sheet materials, such as textiles and papers of all types. These materials may be mixed with others, for example wool, silk, polyester, polyamide or polyacrylonitrile, the total fireproofing effect then corresponding more or less to that of the cellulose fraction.
  • the compound (1 is prepared as described in Example 1, like the compound (I but at a mol ratio of one mol of phosphorus oxychloride, 1.5 mols of methylamine, one mole of ethylenimine, and 0.5 mol ammonia.
  • the tear length T of the fabric thus finished is 7 to 8 cm. (according to DIN 53,906) after washing three times at the boil (according to DIN 54,011), the burning time 0 sec.
  • the compound (I is prepared as described in Example 1, like compound (I but at a mol ratio of one mol of phosphorus oxychloride, one mol of methylamine, one mol of ethylenimine, and one mol ammonia.
  • Fibrous material consisting of or containing cellulose which has been finished with 10 to 30% by weight, based on the cellulose, of a mixture of compounds having the Formula I (NH-CH3);

Landscapes

  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Fireproofing Substances (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
US742182A 1967-07-05 1968-07-03 Fireproofed cellulosic material Expired - Lifetime US3563793A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEB0093325 1967-07-05

Publications (1)

Publication Number Publication Date
US3563793A true US3563793A (en) 1971-02-16

Family

ID=6986900

Family Applications (1)

Application Number Title Priority Date Filing Date
US742182A Expired - Lifetime US3563793A (en) 1967-07-05 1968-07-03 Fireproofed cellulosic material

Country Status (9)

Country Link
US (1) US3563793A (instruction)
AT (1) AT283267B (instruction)
BE (1) BE717595A (instruction)
CH (2) CH958368A4 (instruction)
DE (1) DE1594937A1 (instruction)
FR (1) FR1575975A (instruction)
GB (1) GB1221849A (instruction)
NL (1) NL6809569A (instruction)
SE (1) SE333350B (instruction)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3640823A (en) * 1970-03-09 1972-02-08 Cpc International Inc Flame-retardant composition

Also Published As

Publication number Publication date
GB1221849A (en) 1971-02-10
SE333350B (instruction) 1971-03-15
NL6809569A (instruction) 1969-01-07
BE717595A (instruction) 1969-01-06
DE1594937A1 (de) 1971-01-28
CH488851A (de) 1969-12-15
AT283267B (de) 1970-07-27
CH958368A4 (instruction) 1969-12-15
FR1575975A (instruction) 1969-07-25

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