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
  • 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
  • D06M15/43—Amino-aldehyde resins modified by phosphorus compounds
  • D06M15/431—Amino-aldehyde resins modified by phosphorus compounds by phosphines or phosphine oxides; by oxides or salts of the phosphonium radical
• • 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
  • Y10T442/2697—Phosphorus and halogen containing compound
• • 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
  • Y10T442/2705—A phosphorus containing compound and a halogen containing compound

Definitions

• the present invention concerns the treatment of cellulose-containing textiles with a tetrakis-(hydroxymethyl)- phosphonium salt, preferably with tetrakis-(hydroxymethyl)-phosphonium chloride, which is abbreviated in what follows as THPC, or with tris-(hydroxymethyl)' phosphine oxide.
• THPC flame-proofing of cellulose textiles. Eight development stages can be dis tinguished. To begin with, it was recommended to impregnate aminated cellulose with THPC as such or in admixture with melamine or methylolmelamine and then to carry out the fixation by heat treatment, cf. US. Patent 2,668,096, patented Feb. 2, 1954, to Wilson A. Reeves and John D. Guthrie, New La, U.S.A. Further development was represented by the proposal to use polymerisable precondensates of THPC with urea, melamine or formaldehyde condensation products of amides such as urea or melamine.
• Patent- 2,772,188 and British Patent 882,993 to Albright & Wilson Limited, Oldbury, Warwickshire, England, published Nov. 22, 1961.
• a further proposal was to treat the cellulose textiles with aqueous emulsions of an aminoplast-THPC-precondensate and dispersions of hardened THPC-precondensates.
• the sixth development stage concerns the proposal to treat the cellulose textiles first of all with an aminoplast with dry hardening and then with a THPC-precondensate.
• the treatment with the aminoplast consists in impregnation with an aqueous solution 3,421,923 Patented Jan. 14, 1969 followed by hardening of the aminoplast, preferably by heat treatment.
• the fixation of the subsequently applied THPC-precondensate was brought about by thermo-fixation, cw. British Patent 884,785 to Bradford Dyers Association Limited, Bradford 1, England, and Albright & Wilson Limited, Oldbury, Birmingham, Warwickshire, England, published Dec. 20, 1961. Further progress was brought about by the seventh development stage which recommended the fixation of the THPC-precondensates applied to the fibres, not with ammonia gas or ammonium hydroxide but with ammonia gas and ammonium hydroxide cf. US.
• the last proposal returns to the treatment of cellulose textiles with THPC alone which is applied in a bath at a pH of 3 to 9.5.
• the THPC is fixed on the fabric by heat treatment after which an after-treatment with gaseous ammonia or with ammonium hydroxide is carried out, cf.
• British Patent 938,990 is
• the process consists in that a cellulose fabric treated with an aminoplast, in which the hardening of the aminoplast is brought about by a special process, is padded with an aqueous solution of THPC, dried and then after-treated with gaseous and/or aqueous ammonia.
• the essential features of the process are that the aminoplast is not hardened by drying and/ or heating but wet in the presence of the impregnation liquid, that THPC as such is used that the latter is not thermo-fixed. It is particularly surprising that no washfast fixation of the THPC is obtained by thermofixation of the aminoplast for 5 minutes at C. and subsequent THPC treatment, but that wash-fast fixation occurs with a fabric on which the aminoplast has been hardened in the presence of the impregnation liquid.
• the object of the present invention is thus a process for the flameproofing of cellulose-containing textiles wherein the textile material is impregnated in a first stage with a water soluble hardenable aminoplast, the hardening of the aminoplast is carried out in the presence of impregnation liquid on the textile material, dried if desired, and the textile material impregnated in a second stage in an aqueous bath which contains a tetrakis-(hydroxymethyl) -phosp'h0nium halide or tris-(hydroxymethyl)-phosphine oxide, dried and after-treated with gaseous and/or aqueous ammonia.
• Example 1 Example 1 application THPC amount (g./l) 250 150 330 230 260 410 300. Squeeze-off eiIect per- 80 85 80 85 76 78....
• thermofixing mofixing.
• the mechanical testing of the treated fabric gave the The amount of the aminoplast to be applied to the fibres following results: amounts to 2 to 10, preferably 4 to 6%, based upon the Material.-(a) Cotton fabric; (b) Cellulose fabric. weight of the fabric.
• the concentration of THPC amounts Tests-(I) Tensile strength in accordance with SNV to 150 to 400, preferably 200 to 350 g. per liter. For neu- Standard of the Schwcizerischer Normcnver) tralisation of the THPC to 70, preferably to g. 98461; (11) Tear strength in accordance with Elmendorf. 40 triethanolamine per liter is added to the bath.
• the fabric After impregnation in the THPC bath the fabric is dried, pref- TABLE erably at the temperatures of 60 to C.
• the fixing of ifgfi lggf gig Eggs the THPC is carried out for instance by padding in a bath containing 50 to 500, preferably 100 to 300 g. 25%
• the fabric After treatment with ammonia the fabric is ad- Eg; g2 tg gig 53:3 28 ⁇ 3 r vantageously left in the air for 1 to 15 minutes and then 00 treated in a boiling bath which contams sodium carbonate BPFBmEh Patent if desired; also a wetting agent and hydrogen peroxide.
• the wet fixing is carried out in such a way that the An ordinary Bunsen burner is used, the l ngth f the fabric, after impregnation in a bath which contains the luminous flame of which is adjusted to 4 cm. water soluble aminoplast as well as a suitable reaction
• Weight of fabric from 200-300 g./rn. 8 The simplest process consists in storing for a lengthy Weight of fabric from 300 500 gjmg 10 P t me the fabr c which has been impregnated with a solu- Weight of fabric from 500750 -g./m. 12 i0 tron or emuls on after squeezing out or centrrf ug ng, 1 .e., Weight of fabric from 750 100O 14 after mechanical removal of the excess bath liquid without drying steps and with avoidance of premature drying In assessing the flame resistan on aft r-fla time 05 out. The time during which the material should be stored 1-2 seconds represents a very good degree of protection. varies between a few minutes and several days. It is dependent on the one hand on the aminoplasts and reaction The fabric must not after-glow.
• the storage can be carried out at normal or raised temperature, e.g., at 80 C. It has proved advantageous to store the impregnated fibre in a closed vessel, since by this means premature drying out is avoided.
• After fixing of the resin the fabric is dried.
• a partial drying in accordance with the process of the invention, can also be carried out before or during the fixing of the resin. In this case care should be taken that no excessive drying of individual parts of the treated textile material occurs and no migration of the unfixed resin during the drying, as otherwise the success of the treatment can be unfavorably affected.
• Uniform drying can, for example, be achieved by storing the impregnated fabric in a drying chamber through which a stream of air, with a controlled relative humidity, is passed. The fabric can then only give up so much moisture until it reaches the degree of humidity of the air passing over it.
• the wet fixing can be brought about simply and quickly if instead of hot air containing more or less water vapor, steam is used as the source of heat.
• steam is used as the source of heat.
• saturated water vapor no danger of local drying-out can arise.
• the fixing time can be considerably reduced so that the whole process, including time for heating up, can be concluded in 1 to 2 hours or even considerably less.
• the present process can be employed with all cellulosecontaining fabrics made from fibers such as cotton, regenerated cellulose, jute, manila hemp, sisal and ramie. It is especially useful for the treatment of cotton fabrics for clothing materials such as well as for tents or awning materials.
• the process of the invention is advantageous in cases where cellulose-containing materials are exposed to the danger of fire and where, besides good flamer resistance, optimum mechanical strength after repeated washing is required.
• a particular advantage of the process of the invention is that the textile material also acquires good resistance to rotting.
• water soluble, hardenable aminoplasts which can be used for the present process there are to be understood primarily hardenable aminotriazine resins that are soluble in water or are of limited solubility in water and which may be etherified; they are obtained by known methods by condensation of formaldehyde with melamine, acetoguanamine, benzoguanamine or formo guanamine. Mixtures of such condensation products are also suitable. Particularly good results are obtained with water-soluble condensation products of 2 to 3 mols of formaldehyde with 1 mol of melamine.
• condensation products of limited water-solubility are to be understood as usually those colloidal intermediate products which are first produced on further condensation beyond the crystalline methylol stage. They are formic acid, are used; alternatively, salts of strong acids with weak bases e.g. ammonium salts of strong inorganic or organic acids, such as ammonium chloride, ammonium sulfate, ammonium nitrate, ammonium oxalate and ammonium lactate, can be employed.
• solutions of aminoplasts to which acids have been added care must be taken that the solutions are freshly prepared as owing to certain changes to the solutions on standing their suitability for the purposes of the present invention are adversely affected.
• oxidising agent dispersible in water, which in aqueous phase possesses neither strong alkali-binding properties nor strong acidbinding properties and which, after application of the impregnating liquid to the fabric, has an accelerating effect on the hardening of the aminoplast owing to the formation of oxidation products.
• hydrogen peroxide is suitable as are addition products of hydrogen peroxide to certain inorganic or organic compound, such as for example perborate NaBO .H O or the addition compound of hydrogen peroxide and urea.
• Another suitable oxidizing agent is chlorine dioxide or its stable addition products especially the addition product of C10 to pyridine.
• the salts of peroxymonosulfuric acid, H 50 and the peroxydisulfuric acid, H S O e.g. its alkali salts, especially H S O are also suitable for use as oxidizing agents.
• the impregnation can be carried out by the usual processes and by mean of the usual equipment. Flame-proofing can also be combined with hydrophobation, e.g. with hydrophobing agents known per se.
• a cotton fabric is padded in a bath which contains:
• the padding is carried out in a bath containing:
• the fabric so finished is padded in a bath containing: G./l. THPC 300 Triethanolamine 60 and then dried at 60 to 70 C.
• the fabric is kept at C. for 5 minutes to fix the hydrophobic finish.
• Example 2(IV) In the same manner as in Example 2(IV) the fabric is washed, rinsed and dried.
• Water-repellency of the fabric treated according to Example 3 The fabric is sprinkled with water and shows the following water'eontent in percent:
• Process for the fiame-proofing of cellulose-containing textile material which comprises in a first stage impregnating the material with a water-soluble hardenable aminoplast and hardening the aminoplast in the presence of the impregnating liquid present on the textile material, and in a second stage impregnating the material in an aqueous bath containing tetrakis-(hydroxymethyl)-phosphonium chloride, drying it and after-treating it with ammonia.
• Process for the flame-proofing of cellulose-containing textile material which comprises in a first stage impregnating the material with a water soluble, hardenable aminoplast and hardening the aminoplast in the presence of the impregnating liquid present on the textile material, and in a second stage impregnating the material in an aqueous bath containing tetrakis-(hydroxymethyl)-phosphonium chloride, drying it and after-treating it with gaseous ammonia.
• Process for the flame-proofing of cellulose-contain ing material which comprises in a first stage impregnating the material with a water soluble, condensation product of melamine and formaldehyde and hardening the melamine-formaldehyde condensation product in the presence of the impregnating liquid present on the textile material, and in a second stage impregnating the material in an aqueous bath containing tetrakis-(hydroxymethyl)-phosphonium chloride, drying it and after-treating it with gaseous ammonia.
• Process for the flame-proofing of cellulose-containing itextile material which comprises in a first stage impregnating the material with a water soluble, condensation product of 1 mol of melamine and 3 mols of formaldehyde and hardening the melamine-formaldehyde condensation product in the presence of the impregnating, liquid present on the textile material, and in a second stage impregnating the material in an aqueous bath containing tetrakis-(hydroxymethyl)-phosph0nium chloride, drying it and after-treating it with gaseous ammonia.
• Process for the flame-proofing of cellulose-containing textile material which comprises in a first stage impregnating the material with a water soluble, condensation product of 1 mol of melamine and 3 mols of formaldehyde and hardening the melamine-formaldehyde condensation product in the presence of the impregnating liquid present on the textile material, and drying the material and in a second stage impregnating the material in an aqueous bath containing tetrakis-(hydroxymethyl)- phosphonium chloride, drying it and after-treating it with gaseous ammonia.
• Process for the flame-proofing of cellulose-containing textile material which comprises in a first stage impregnating the material with a water soluble condensation product of 1 mol of melamine and 3 mols of formaldehyde and hardening the melamine-formaldehyde condensation product in the presence of the impregnating liquid present on the textile material, and hydrogen peroxide and drying the material, and in a second stage impregnating the material in an aqueous bath containing tetrakis-(hydroxymethyl)-phosphonium chloride, drying it and after-treating it with gaseous ammonia.
• Process for the flame-proofing of cellulose-containing textile material which comprises in a first stage impregnating the material with a water soluble condensation product of 1 mol of melamine and 3 mols of formaldehyde, hardening the melamineformaldehyde condensation product in the presence of the impregnating liquid present on the textile material and hydrogen peroxide 9 1O storing the material in the moist state and drying it, 2,772,188 11/1956 Reeves et a1 117-136 and in a second stage impregnating the material in an 2,809,941 10/1957 Reeves et a1.

Landscapes

• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Engineering & Computer Science (AREA)
• Textile Engineering (AREA)
• Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
• Chemical Or Physical Treatment Of Fibers (AREA)

Applications Claiming Priority (1)

Publications (1)

Family

ID=4347930

Family Applications (1)

Country Status (10)

Cited By (17)

Families Citing this family (3)

Citations (7)

• 1964
  • 1964-07-10 CH CH906464A patent/CH418289A/de unknown
• 1965
  • 1965-06-22 US US466117A patent/US3421923A/en not_active Expired - Lifetime
  • 1965-06-23 IL IL23788A patent/IL23788A/xx unknown
  • 1965-06-24 GB GB26883/65A patent/GB1061134A/en not_active Expired
  • 1965-07-07 DE DE1469307A patent/DE1469307C3/de not_active Expired
  • 1965-07-09 AT AT627765A patent/AT256774B/de active
  • 1965-07-09 ES ES0315172A patent/ES315172A1/es not_active Expired
  • 1965-07-09 SE SE9112/65A patent/SE307930B/xx unknown
  • 1965-07-09 NL NL656508901A patent/NL147204B/xx unknown
  • 1965-07-09 BE BE666694A patent/BE666694A/xx unknown

Patent Citations (7)

Also Published As

Similar Documents