GB2306477A - Flame retardant compositions containing a non-salt ammonia neutralisate of a nitrilotris(alkylenephosphonic acid) - Google Patents

Flame retardant compositions containing a non-salt ammonia neutralisate of a nitrilotris(alkylenephosphonic acid) Download PDF

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GB2306477A
GB2306477A GB9521640A GB9521640A GB2306477A GB 2306477 A GB2306477 A GB 2306477A GB 9521640 A GB9521640 A GB 9521640A GB 9521640 A GB9521640 A GB 9521640A GB 2306477 A GB2306477 A GB 2306477A
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neutralisate
ammonia
use according
fabric
flame retardant
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Rebecca Sally-Jane Day
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Solvay Solutions UK Ltd
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Albright and Wilson Ltd
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Priority to GB9521640A priority Critical patent/GB2306477A/en
Publication of GB9521640D0 publication Critical patent/GB9521640D0/en
Priority to EP96116404A priority patent/EP0769584A3/en
Priority to NO964429A priority patent/NO964429L/en
Publication of GB2306477A publication Critical patent/GB2306477A/en
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/244Treating 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 sulfur or phosphorus
    • D06M13/282Treating 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 sulfur or phosphorus with compounds containing phosphorus
    • D06M13/288Phosphonic or phosphonous acids or derivatives thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322Treating 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
    • D06M13/44Treating 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 containing nitrogen and phosphorus
    • D06M13/447Phosphonates or phosphinates containing nitrogen atoms

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Fireproofing Substances (AREA)

Description

PF736 FLAME RETARDANT COMPOSITIONS 2306477 The present invention relates
to the use of non-reactive, non-salt, non- durable ammonia neutralisates of nitrilotris (alkylenephosphonic acids), especially of nitrilotris methylenephosphonic acid, as a flame retardant composition. In particular it relates to the use of said neutralisates as, or in connection with a flame retardant for amongst other applications fabrics, timber, paper, and timber coatings. Fabrics, including natural, man made or synthetic fibres and blends thereof, treated with the aforementioned neutralisates exhibit excellent flame retardant properties, good fabric strength, handle and drape, do not bloom and are of low fogging characteristics even under conditions of high humidity. Such treated fabrics are particularly suitable for use in automotive and aerospace applications (where such low blooming and/or fogging characteristics are required), and are also suitable for use in soft furnishings, clothing and the like.
Flame retardants are incorporated into many products on the grounds of safety in order to control the spread of fire through the product. Flame retardants can, for example, act by causing rapid extinguishing of flames, or by making the product difficult to set alight. Flame retardants have conventionally been used to treat inter alia fabrics and soft furnishings, especially within the home furnishings, automotive, aerospace and construction industries. The use of flame retardants within these and other industries in conventional applications is increasing in response to more stringent fire control and safety legislation, and as a consequence thereof many new applications for flame retardants are now being found.
Non-durable flame retardant compositions are applied to many fabrics, either during the manufacture of the fabric by means of a particular process stage or as a separate treatment after the manufacture of an article prepared from a fabric, eg, the post manufacture treatment of curtains to render them flame retardant. Non-durable flame retardant compositions are not permanent in their application to fabric, and are removed by washing. However, non-durable flame retardants do exhibit same durability to dry cleaning.
-2It is an important feature of flame retardant treated fabrics that the feel or the 'handle' of the fabric is not excessively harsh to the touch, especially if the fabric is to be used for applications such as safety clothing and soft furnishings. Furthermore, such treated fabrics should maintain good flexibility after treatment, ie, show good drape characteristics, especially if the fabric is to be used for applications such as curtains etc.
Some flame retardants, especially salt based flame retardants, may produce or contain volatile components which upon contact with glass, especially cold glass, cause fogging. This is particularly undesirable where the flame retardant is to be used in automative or aerospace applications.
Alternatively, or in the case of some flame retardants, additionally, the flame retardant may under certain conditions bloom' on the fabric to which it has been applied, and is then visible. This blooming is especially problematic in conditions of high humidity. As well as being unsightly on the fabric, blooming can result in poor fabric handle.
The ammonia neutralisate of nitrilotris (methylenephosphonic acid) is a water soluble phosphonate which is known as a scale-inhibitor for use in water treatment and also as a deflocculating and dispersing agent, due to its ability to form calcium and magnesium complexes, and very stable complexes with heavy metals. Said neutralisate has also previously found use in other applications such as cooling water treatment, corrosion control, oil-field water treatment, bottle washing and textile bleaching. However, hitherto said neutralisate has not been used as, or in connection with, flame retardant compositions. The aforementioned ammonia neutralisate has been available commercially as BRIQUEST 301-34N'.
1 MRIQUEST'is a registered trademark of Albright & Wilson UK Limited.
Flame retardants for fabrics should ideally exhibit excellent flame retardancy on natural, man made and synthetic fibres and blends thereof, and not result in unacceptable levels of loss of strength of the treated fabric. The problem of the loss of strength is particularly prevalent with acid sensitive fibres such as cotton, in cases where an acidic flame retardant is used. Such strength loss results in a decreased useful life of the fabric due to its premature wear and tear. Also, the flame retardant treated articles should, if the application requires, exhibit good drape andlor hand characteristics. In particular salt based flame retardants, eg ammonium polyphosphate, are known to be susceptible to precipitation which may cause blooming, and also produce unacceptable fogging levels under conditions of high humidity. For the reasons mentioned hereinabove, blooming and unacceptable fogging levels caused by the use of flame retardants is undesirable.
There is therefore a need to provide a non salt-based flame retardant, which exhibits excellent flame retardancy on natural, man made and synthetic fabrics and blends thereof but which does not result in excessive loss of strength of the fabric after treatment, and which does not exhibit unacceptable levels of blooming andlor fogging, and which retains or improves handle and drape characteristics of the fabric.
We have now discovered that an ammonia neutralisate of a nitrilotris (alkylenephosphonic acid), in particular a nitrilotris (methylenephosphonic acid) may be used as, or in connection with, a flame retardant composition. Said neutralisates provide excellent flame retardancy on natural man made, and synthetic fabrics and blends thereof, do not result in unacceptable levels of loss of strength of the fabric, impart excellent blooming and fogging control characteristics (even in conditions of high humidity) and fabrics treated with said flame retardant compositions exhibit good handle and drape characteristics. We have further discovered that said neutralisates are suitable in some circumstances for use as, or in connection with, flame retardants iniff alia for timber, paper and timber coatings.
It is believed, although we do not wish to be limited thereto, that the neutralisation by a nitrogen containing base may aid the flame retardancy characteristics of the neutralisate, or provide a synergistic effect.
Accordingly, in a first embodiment, the present invention provides the use of an ammonia neutralisate of nitrilotris (alkylenephosphonic acid) as, or in connection with, a flame retardant compositiow In particular anammonia neutralisate of nitrilotris methylene phosphonic acid is provided.
Preferably, the ammonia neutralisate of nitrilotris (alkylenephosphonic acid), has a pH of from 6.5 to 7.0 at 250C.
in the use of the ammonia neutralisates of the present invention, the flame retardant may be contacted with a fabric either before, during or after the manufacture of said fabric, or applied to an article made from said fabric. The present invention further provides articles rendered flame retardant by the use of the neutralisate described in the two immediately preceding paragraphs.
The ammonia neutralisate of the nitrilotris (alkylenephosphonic acids) are non-reactive, non-durable, non-salt compounds prepared by the neutralisation of nitrilotris (alkylenephosphonic acids) with ammonia. It is preferred that the ammonia neutralisate is prepared by the neutralisation of nitrilotris (methylenephsophonic acid), with the corresponding ethylenephosphonic acids, and propylene phosphonic acids also being suitable.
Typically the nitrilotris (alkylenephosphonic acid) is neutralised by the addition of ammonia to an aqueous solution of said acid. Typically said aqueous solution of said acid is used at an active concentration of 1 to 99% by weight, preferably 10% to 80%, most preferably 25% to 65%, eg, 35% to 55% by weight, such as 50% by weight active concentration. The ammonia may be added as an aqueous solution, at any suitable active concentration, typically as a saturated ammonia solution, (ie, 88% by weight ammonia solution).
The neutralisation of the nitrilotris (alkylenephosphonic acid) may be undertaken according to any suitable method. Typically, the ammonia solution is slowly added to the nitrilotlis (alkylenephosphonic acid) with stirring, for example at a rate of 1 drop of ammonia solution per second, until the requisite pH is obtained and maintained. No further ammonia solution is then required to be added.
The ammonia neutralisate of the nitrilotris (alkylenephosphonic acid) typically has a pH in the range of 6.5 to 7.0, preferably 6.52 to 6.95, most preferably 6.55 to 6.9, when measured at 25C.
Said ammonia neutralisate is typically used in an amount sufficient to render the fabric or article to which it is applied sufficiently flame retardant to meet recognised flammability standards, eg, the British Safety Standards Council's BS5867 Part 2 Types A and B for curtains, BS476 Parts 6 and 7 for wall coverings and BS7175 for mattress tickings.
Typically said ammonia neutralisate is used at a concentration of 0.5% to 20%, expressed as % dry chemical add on (with respect to phosphorus content) to the fabric, preferably 1% to 16%, most preferably 3% to 15%, eg, 3.5% to 13%. The actual amount of said neutralisate required will depend upon the nature, construction and weight of the fabric to be treated, the uniformity of the application and the flame retardant performance required.
The concentration of said ammonia neutralisate when used as a bath composition for treating fabric typically lies within the range of 1 00g11 to 6008/1, preferably 1 50g/1 to 500g11, most preferably 175g11 to 400g11, eg, 204g/1 to 370g/1, dependent upon the factors recited in the immediately preceding paragraph.
The addition of an excessive amount of said ammonia neutralisate may result in a poor handle of the fabric, and should preferably be avoided if an acceptable level of flame retardancy can be achieved with a lower level of said neutralisate. However, in virtually all cases excellent flame retardancy and good fabric handle may be achieved at a low application level of said neutralisate.
-6The aforementioned ammonia neutralisate may be applied to the fabric to be treated by any suitable method. Said fabric should be clean, absorbent, and free from alkali, or otherwise reduced uptake of the flame retardant will occur as a result of the presence of soils, natural waxes or applied finishes. The application of said ammonia neutralisate to the fabric may be effected any suitable method, for example by brushing, dipping, spraying or by a pad dry technique.
The treated fabric may be dried at ambient or at elevated temperatures. If the fabric is heat dried, it is preferred that a temperature of between 70C and 160C is used, preferably between 900C and HO'C. Alternatively the treated fabric may be dried by infit-red heating, as the ammonia neutralisate is not prone to arcing and subsequent scorching, as is commonly encountered with salt type flame retardants.
Where the ammonia neutralisate flame retardant compositions of the present invention are used as an application bath composition for the treatment of fabrics, said reaction bath composition may optionally include minor amounts of other ingredients such as water and/or oil repellent fluorocarbons, fabric softeners, to impart said respective characteristics to the treated fabric or other article. Furthermore, other minor ingredients such as binders, or surfactants may be used with or in connection with, the ammonia neutralisate as required. Suitable binders include acrylics, vinyl chloride and polyvinyl alcohol. Suitable surfactants include anionic, cationic, amphoteric and especially nonionic surfactants. Particularly preferred non-ionic surfactants include fatty acid alkylolamines; ethylene oxide condensates of fatty alcohols, fatty acids and alkylolamides; fatty acid esters; and ethylene oxide/propylene oxide block copolymers. Typically the aforementioned optional ingredients are present in said reaction bath compositions in total amounts of up to 80g11, preferably up to 60g/1, eg, up to 50g11 or up to 25% by weight based on the total weight of the active flame retardant composition, preferably up to 20%, most preferably up to 10% by weight.
The ammonia neutralisate of nitrilotris (alkylenephosphonic acid) may be used as, or in connection with, a flame retardant composition for natural, man made, or synthetic fibres, and blends thereof, for example wool, wool blends, cotton, cotton blends, and polyesters.
The use of the aforementioned neutralisate as, or in connection with a flame retardant, finds particular application in areas where low fogging and blooming characteristics of the treated fabric are required. Such applications include amongst others, the aerospace and automotive industries, in particular for seat and carpet fabrics. Other uses include mattress tickings, wall coverings and other soft furnishings, eg, curtains and settee covers. The excellent drape and handle characteristics imparted to fabrics by treatment with said neutralisate, makes treated fabrics also suitable for non durable safety clothing, etc. Furthermore, said neutralisate may be used in some circumstances as, or in connection with, a flame retardant compositon for timber, paper, timber coatings and the like.
The ammonia neutralisates of the present invention may be used as a flame retardant additive for suitable applications.
The flame retardants of the present invention will be further illustrated by reference to the following examples, although is not to be construed as being limited thereto.
Example 1: Method of preparation of the ammonia neutralisate of nitrilotris (methylene phosphonic acid) To a 50% by weight aqueous solution of nitrilotris (methylenephosphonic acid) (1 litre, 500g of acid, 1.67 moles), an 88% ammonia solution (1 13g, 6.64 moles) was added dropwise at a rate of 1 drop per second with constant stirring. The ammonia addition was maintained until the pH of the solution reached, and stabilised at pH 6.5 (as measured at 25Q Example 2: Level of the flame retardant composition reguired on difFerent fabrics Table 1 below shows the typical concentration of the flame retardant composition required on different fabrics to meet recognised flammability standards. The concentration is expressed as percentage dry chemical add on, with respect to the fabric.
TABLE 1: % dry add on for different fabrics Fabrics % dry add-on Cotton 6-12% parts cotton / 30 parts polyester 6-12% polyester 8-12% ool/polyester 4-10% 1. i1, For each of the above fabrics the amount of the flame retardant composition required'is relatively low, and the loss of strength of the fabric due to the treatment was within acceptable linuts.
Example 3: Typical bath compositions for the treatment of fabrics Table 2 shows the typical bath composition concentration used to treat various fabrics to render them sufficiently flame retardant to meet the relevant flammability standard stated.
TABLE 2: Typical bath composition concentration Ammonia neutralisate $2 Fabric to be Safety Standard of nitrilotris methylene- ENIPILAN treated requirements fulfilled phosphonic acid KI8/65 9/1 9/1 A 370 4 136 USA Standard FMVSS302 g1M2 1 00o/ polyester automotice end use B 204 4 405g/m' 100% EC Standard CAA 8/2 wool aircraft upholstery end use c 320 4 232g/M2 100% UK Standard BS5867 Part 2 cotton, pigment Type B - curtains printed D 360 4 409g/m'42% UK Standard BS5867 Part 2 polyamide, 40% Type B curtains polyester, 18% viscose, colour The above table shows that the flame retardant compositions of the present invention are effective in the treatment of various types of fabrics, and such treated cloth easily fulfils the requirements of recognised flammability standards.
2 ENPILAN KIS/65 is a CHalcohol 8 mole ethoxylate surfactant. EXPILAN is a registered trade mark of Albright & Wilson UK Limited Examide 4: Waterloil repellent and flame retardant finishe The following typical bath composition provides a flame retardant and water/oil repellent finish to the treated fabric. The composition is particularly effective for treating 100% cotton: Ammonia neutralisate of nitrilotris (methylenephosphonic acid) Water and oil repellant ' Amine oxide surfactant -4 340g/1 44g11 4g/1 Cotton treated with the above composition has an oil repellancy rating of 6, and a spray rating of 80 (BS3702: 1982). 3 available commercially as SCOTCHGARD FC25 1, a dispersion of a fluroalkyl copolymer. 4 available commercially as IMON NRW-3. SCOTCHGARD and MYKON are trade marks.
Example 5: Flame retardant and fabric softening finishes The following typical bath composition provides a flame retardant and fabric softening finish to the treated fabric: Ammonia neutralisate of nitrilotris (methylenephosphonic acid) 340g/1 Fabric Softener ' 44g/1 -10available commercially as Patsoft 1220, a fatty amine/polyolefin blend. PATSOFT is a trade mark Example 6: Comparison of blooming and fogging characteristics The bloom control characteristics of the ammonia neutralisate of the present invention was tested under controlled conditions against two conventional salt based flame retardants (AMGARD TR6 and AMGARD FSD') and a commercially available non-salt flame retardant (FLOVAN CGN').
The flame retardants were applied to various fabrics as listed below in Table 3. The fabrics were stored under conditions which would typically induce blooming by leaving the samples on a draughty windowsill, with the samples being regularily inspected. A small draught from the window was maintained with the temperature of the test varying between -5C to 25C over a 6 month period.
The fogging characteristics of the ammonia neutralisate of the present invention were tested by determining the gravimetric weight gain on aluminium foil from the test material. A Haake fogging apparatus (instrument Nos 00032, 00033, 00034 and 00035) was used- Samples were cut in to 8Omm diameter pieces, with the thickness measured to the nearest 0. 02mm, and kept in a desicator until required. Immediately prior to use the samples were removed from the desicator, placed into beakers and weighted with metal rings. Silicone rubber rings were placed on each of the beakers and covered by 105mm x 105mm pieces of aluminium foil, followed by glass plates, filter papers and condensors. The beakers were placed in the fogging apparatus, and the condensors pushed down to ensure the beakers were level with the top of the oil bath part of the apparatus. The fogging apparatus was heated to 1OWC +/- 0.3Q and the test was run for 16 hours +/- 10 minutes. After this time the condensors, glass plates, aluminium foil were removed and the foil stored in a desicator for 3 1/2 to 4 hours, prior to being weighed to the nearest 0.0 1 mg. The fogging value was recorded as mg/ 1 Omm of foam, taken as an average of five results.
-11A result of greater than 1 mg/ 1 Omm of foam represents unacceptable fogging characteristics, and a result of less than ling/10min of foam represents low fogging characteristics. Obviously the lower the value of mg/ 1 Omm of foam, the more acceptable are the fogging characteristics.
TABLE 3: Fogging Characteristics BLOOM TEST FOGGING TEST Fabric X Fabric Y Fabric Z Fabric X Fabric Y Fabric Z AMGARD TR Slight Bloom Slight Bloom Slight Bloom Unacceptable Unacceptable Unacceptable after 1 month after 1 month after 1 month Fogging Fogging Fogging AMGARD FSD Bloomed Bloomed Bloomed Low Fogging Low Fogging Low Fogging after 9 days after 9 days after 9 days FLOVAN CGN No Bloom No Bloom No Bloom Low Fogging Low Fogging Low Fogging ammonia No Bloom No Bloom No Bloom Low Fogging Low Fogging Low Fogging neutralisate of (methylene phosphonic acid) The handle of the fabrics subjected to the 'bloom' experiment was assessed by simply feeling the fabric. The ammonia neutralisate treated fabric was judged to have the most acceptable hand, followed by the FLOVAN treated fabric which exhibited some degree of stiffening. Both the aforementioned products were judged to provide a superior hand when compared to the AMGARD treated fabrics. Furthermore, the fabric strength loss and the flame retardant performance of the ammonia neutralisate and FLOVAN treated fabric were found to be comparable. The fogging control characteristics of the ammonia neutralisate and the FLOVAN were excellent, whilst the conventional salt based flame retardants exhibit poor control characteristics.
6 Amgard TR is an ammonium polyphosphate and urea mixture, and Amgard FSD is a ammonium polyphosphate, ammonium bromide and urea mixture. Amgard is a trademark of Albright & Wilson UK Limited.
-1207 Flovan CGN is a methylphosphonate, Dicyanamide and triethanolamine based flame retardant. FLOVAN is a trademark.
Example 7: Flame retardancy The flame retardancy of fabric treated with the ammonia neutralisate of the nitrilotris (methylenephosphonic acid) was tested and compared against conventional flame retardants, on the fabrics given below in Table 4.
TABLE 4: Flame retardancy on different fabric types FABRIC TYPE CONIPOSITION & CONSTRUCTION WEIGHT G1W 1 100% Cotton plain woven fabric 155 2 50/50 Polyester/wool blended woven fabric 223 3 100% polypropylene plain woven fabric 220 4 100% acrylic plain woven fabric 270 100% polyamide plain woven fabric 90 6 100% polyester satin weave fabric 102 The flame retardants used as a comparison to the above ammonia neutralisate are given below in Table 5.
Comparative testing to BS 5867, Part 2 Type B, for flame retardancy was carried out on the finished textiles.
The flame retardancy, of the fabrics of table 4, treated with the various flame retardants is given below in Table 5.
TABLE 5: Flame retardancy results SAAPLE AFTERFLAME AFTERGLOW CHARLENGTH AND FABRIC TYPE (SECONDS) (SECONDS) AMGARD FSD Fabric 1 0.0 0.0 76.0 type 2 0.0 0.0 68.0 3 0.0 0.0 94.0 4)35.0 0.0 TIE 47.8 0.0 T/E 6 0.0 0.0 106.0 AMGARD TR Fabric 1 0.5 0.0 70.0 type 2 1.6 0.0 63.0 3 18.9 0.0 108.0 4)35.0 0.0 T/E 28.5 0.0 T/E 6 0.0 0.0 106.0 FLOVAN CGN Fabric 1 0.3 0.0 76.0 type 2 1.6 0.0 64.0 3 0.0 0,0 101.0 4 > 35.0 0.0 T/E 15.6 0.0 TIE 6 Ammonia neutralisate of nitrilotris (methylenephosphonic acid) Fabric 1 0.0 0.0 58.0 type 2 3.5 0.0 67.0 3 22.5 0.0 T/E 4)35.0 0.0 T/E 48.5 0.0 T/E 6 0.0 0.0 106.0 T/E Top Edge Ignites Results Fabric types 1, 2 and 6 met the requirements of BS 5867 Part 2 Type B when treated with any of the five chemical finishes, whereas fabric types 4 and 5 did not meet said requirements when treated with any of the conventional flame retardants, or the flame retardant of the present invention.
Both the conventional Amgard products produced a salty handle to the fabric, and the Flovan product a stifF or sticky handle. The flame retardant of the present invention was considered to give the best handle of the flame retardant compositions tested, when manually compared.
Example 8: Tensile strengh of the treated fabrics Samples were taken from both the warp and weft directions of fabric types 1, 2, 5 and 6 of Example 7, and were tested to BS 2576 Tensile Strength and BS 4303 Wing Rip Tear. Each result was compared to the result obtained for the untreated fabric, with the difference in Tensile Strength being recorded as a % change in strength and tear strength when compared to the untreated fabric. The ammonia neutralisate used was that of the nitrilotris (methylenephosphonic) acid. The results are given in Table 6.
The results in table 6 show all the treated fabrics exhibit some change in the strength thereof, with the loss of strength for the ammonia neutralisate being within acceptable limits and comparable to the conventional flame retardants.
TABLE 6: Tensile Strength of Treated Fabric SAMPLE TENSILE % CHANGE IN TEAR % CHANGE IN STRENGTH STRENGTH OF STRENGTH TEARSTRENGTH (N) FABRIC (N) WARP WEFT WARP WEFT WARP WEFT WARP WEFT FABRIC 1: 100% COTTON 355.7 336.5 7.84 9.28 AMGARD FSD 377.2 312.8 + 6.0 - 7.0 7.56 7.62 - 4.0 -18.0 AMGARD TR 380.7 292.3 + 7.0 -13.0 8.12 7.64 + 4.0 -18.0 FLOVAN CGN 375.0 330.7 + 5.0 - 2.0 7.24 7.48 - 8.0 -19.0 Ammonia Neutralisate 346.1 344.2 - 3.0 + 2.0 7.20 8.48 - 8.0 - 9.0 FABRIC 2: 50% PE/50% WOOL 826.9 719.2 32.64 33.80 AMGARD FSD 771.1 694.2 -7.2 -3.6 36.12 36.20 +10.6 +7.1 AMGARD TR 788.0 721.1 -3.6 +0.2 37.24 36.36 +14.1 +7.6 FLOVAN CGN 809.6 728.8 -2.1 + 1.3 33.08 32.76 + 1.3 -3.2 Ammonia Neutralisate 807.6 701.9 -2.3 -2.5 36.04 35.60 +10.4 +5.3 FABRIC 5: 100% POLYAMIDE 407.6 625.0 15.88 21.68 AMGARD (R) FSD 363.4 548.0 -12.2 -14.0 17.08 27.40 + 7.6 +26.4 AMGARD (R) TR 386.5 530.7 - 5.5 -17.8 18.76 26.72 + 18.1 +23.2 FLOVAN CGN 376.9 575.0 - 8.1 - 8.6 19.20 28.88 +20.9 +33.2 Ammonia Neutralisate 390.3 578.8 - 4.4 - 7.9 15.32 25.04 - 3.6 + 15.5 FABRIC 6: 100% POLYESTER 759.6 550.0 14.20 11.68 AMGARD FSD 763.4 526.9 + 0.5 -4,4 17.08 14.84 +20.3 +27.1 AMGARD TR 769.2 575.0 + 1.3 +4.5 13.64 11.64 - 4.1 - 0.3 FLOVAN CGN 705.7 563.4 7.6 +2.4 16.52 13.00 +16.3 + 11.3 Ammonia Neutralisate 638.4 532.6 - 18.9 -3.3 18.92 12.96 +33.3 +10.9 1 Ir Example 9: Drape characteristics Each of the samples of Example 6 was tested for the assessment of the drape characteristics according to BS 5058: 1993 after the aforementioned 6 month storage period. The samples were not reconditioned prior to testing. The ammonia neutralisate was of the nitrilotris (methylenephosphonic) acid. The results are given below in Table 7. It should be noted that small samples of fabric were used for the test and therefore the drape co-efficient values obtained are comparative with respect to each other, and represent higher co-efficients than would typically be obtained.
TABLE 7: Drape Characteristics FLAMIFE RETARDANT DRAPE CO-EFFICIENT Amgard FSD 89.3 Amgard TR 89.1 Flovan CGN 88.9 Ammonia Neutralisate 86.8 In each case the smallest test size was carried out. The samples all show comparable drape characteristics. A drape co-efficient of 100.0 shows a stiff fabric.
- i"+ - PF736/GB

Claims (25)

1. The use of a non-salt ammonia neutralisate of nitrilotris (alkylene phosphonic acid) as, or in connection with, a flame retardant.
2.
The use according to Claim 1 of an ammonia neutralisate of nitrilotris (methylene phosphonic acid).
The use according to Claim 1 or 2 of an ammonia neutralisate having a pH of from 6.5 to 7.0 at 250C.
The use according to Claim 3, of an ammonia neutralisate having a pH of from 6.52 to 6.95 at 250C.
5. The use according to Claim 4 of an ammonia neutralisate having a pH of from 6.55 to 6.9 at 250C.
6. The use according to any of Claims 1 to 5 wherein said ammonia neutralisate is contacted with a fabric either before, during or after the manufacture of said fabric.
7. The use according to any one of Claims 1 to 5 wherein said ammonia neutralisate is applied to an article made from a fabric.
8.
The use according to any one of Claims 1 to 7 wherein said ammonia neutralisate is used at a concentration of 0.5% to 20% (expressed as % dry chemical add on with respect to the phosphorus content).
The use according to Claim 8, at a concentration of 1% to 16%.
9.
10.
The use according to Claim 8 or 9, at a concentration of 3% to 15%.
11.
The use according to Claim 8, 9 or 10, at a concentration of 3.5% to 13%.
12.
The use according to any one of Claims 1 to 11 wherein said ammonia neutralisate is applied to the fabric to be treated by brushing, spraying or pad-dry techniques.
13.
The use according to any one of Claims 1 to 12, wherein said ammonia neutialisate is used as a bath composition for treating fabric.
14.
The use according to Claim 13 of said ammonia neutralisate at a concentration of 1 00g11 to 600g/1.
is.
The use according to Claim 14 at a concentration of 150g11 to 500g/1.
16.
The use according to Claim 14 or 15 at a concentration of 175g11 to 400g/1.
17.
The use according to Claim 14, 15 or 16 at a concentration of 204g/1 to 3 70g11,
18.
The use according to any one of Claims 1 to 17 of an ammonia neutralisate wherein the fabric to which said ammonia neutralisate is applied is dried at an ambient or elevated temperature.
19. The use according to Claim 18 wherein said fabric is dried by infirared heating.
20. The use according to any one of Claims 1 to 19 of said ammonia neutralisate, wherein said ammonia neutralisate is used together with one or more further ingredients.
0- j CP The use according to Claim 20, in combination with up to 25% by weight of said one or more further ingredients, based on the total weight of the neutralisate and said further ingredients.
21.
22. The use according to Claim 21, in combination with up to 20% by weight of said one or more further ingredients.
23. The use according to Claim 21 or 22 in combination with up to 100/0 by weight of said one or more further ingredients.
24. The use according to any one of Claims 20 to 23 wherein said one or more further ingredients are selected from water and/or oil repellent fluorocarbons, fabric softeners, binders and surfactants.
25. The use of an ammonia neutralisate substantially as herein before described with reference to anyone of the Examples.
GB9521640A 1995-10-21 1995-10-21 Flame retardant compositions containing a non-salt ammonia neutralisate of a nitrilotris(alkylenephosphonic acid) Withdrawn GB2306477A (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
GB9521640A GB2306477A (en) 1995-10-21 1995-10-21 Flame retardant compositions containing a non-salt ammonia neutralisate of a nitrilotris(alkylenephosphonic acid)
EP96116404A EP0769584A3 (en) 1995-10-21 1996-10-14 Flame retardant compositions
NO964429A NO964429L (en) 1995-10-21 1996-10-18 Flame retardant compositions

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
GB9521640A GB2306477A (en) 1995-10-21 1995-10-21 Flame retardant compositions containing a non-salt ammonia neutralisate of a nitrilotris(alkylenephosphonic acid)

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GB9521640D0 GB9521640D0 (en) 1996-01-03
GB2306477A true GB2306477A (en) 1997-05-07

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EP (1) EP0769584A3 (en)
GB (1) GB2306477A (en)
NO (1) NO964429L (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DK1418178T3 (en) * 2001-07-16 2008-06-02 Isle Firestop Ltd Flame retardant for polymeric materials
CN107353437A (en) * 2017-08-08 2017-11-17 青岛长荣化工科技有限公司 A kind of expansion type flame retardant and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1991016402A1 (en) * 1990-04-18 1991-10-31 Contra-Flame Limited Flame-proofing compositions

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2860311B2 (en) * 1990-05-21 1999-02-24 株式会社ジー・ティ・エル Cold-resistant fire extinguisher
JP2941078B2 (en) * 1991-03-30 1999-08-25 城北化学工業株式会社 Flame retardant for plastic
FR2707308B1 (en) * 1993-07-09 1995-09-29 Protex Manuf Prod Chimiq Process for the non-permanent flame retardancy of textiles using solutions of salts of alkylaminomethylenephosphonic acids.

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1991016402A1 (en) * 1990-04-18 1991-10-31 Contra-Flame Limited Flame-proofing compositions

Also Published As

Publication number Publication date
NO964429D0 (en) 1996-10-18
NO964429L (en) 1997-04-22
GB9521640D0 (en) 1996-01-03
EP0769584A2 (en) 1997-04-23
EP0769584A3 (en) 1997-07-30

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