SE2151389A1 - Flame retardant composition - Google Patents
Flame retardant compositionInfo
- Publication number
- SE2151389A1 SE2151389A1 SE2151389A SE2151389A SE2151389A1 SE 2151389 A1 SE2151389 A1 SE 2151389A1 SE 2151389 A SE2151389 A SE 2151389A SE 2151389 A SE2151389 A SE 2151389A SE 2151389 A1 SE2151389 A1 SE 2151389A1
- Authority
- SE
- Sweden
- Prior art keywords
- solution
- flame retardant
- amino acids
- inositol polyphosphate
- forming
- Prior art date
Links
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- 235000013601 eggs Nutrition 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000009970 fire resistant effect Effects 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229940045189 glucose-6-phosphate Drugs 0.000 description 1
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- LWFPYLZOVOCBPZ-UHFFFAOYSA-N hydrindantin Chemical compound O=C1C2=CC=CC=C2C(=O)C1(O)C1(O)C(=O)C2=CC=CC=C2C1=O LWFPYLZOVOCBPZ-UHFFFAOYSA-N 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002417 nutraceutical Substances 0.000 description 1
- 235000021436 nutraceutical agent Nutrition 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 230000026731 phosphorylation Effects 0.000 description 1
- 238000006366 phosphorylation reaction Methods 0.000 description 1
- 229920001690 polydopamine Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920001184 polypeptide Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229940083542 sodium Drugs 0.000 description 1
- 235000015424 sodium Nutrition 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical class [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 239000010887 waste solvent Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K21/00—Fireproofing materials
- C09K21/06—Organic materials
- C09K21/12—Organic materials containing phosphorus
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C13/00—Cyclic hydrocarbons containing rings other than, or in addition to, six-membered aromatic rings
- C07C13/02—Monocyclic hydrocarbons or acyclic hydrocarbon derivatives thereof
- C07C13/16—Monocyclic hydrocarbons or acyclic hydrocarbon derivatives thereof with a six-membered ring
- C07C13/18—Monocyclic hydrocarbons or acyclic hydrocarbon derivatives thereof with a six-membered ring with a cyclohexane ring
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C229/00—Compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C229/76—Metal complexes of amino carboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F1/00—Compounds containing elements of Groups 1 or 11 of the Periodic System
- C07F1/04—Sodium compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F3/00—Compounds containing elements of Groups 2 or 12 of the Periodic System
- C07F3/04—Calcium compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic System
- C07F5/06—Aluminium compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F1/00—Compounds containing elements of Groups 1 or 11 of the Periodic System
- C07F1/06—Potassium compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F1/00—Compounds containing elements of Groups 1 or 11 of the Periodic System
- C07F1/08—Copper compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F15/00—Compounds containing elements of Groups 8, 9, 10 or 18 of the Periodic System
- C07F15/02—Iron compounds
- C07F15/025—Iron compounds without a metal-carbon linkage
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F3/00—Compounds containing elements of Groups 2 or 12 of the Periodic System
- C07F3/02—Magnesium compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F3/00—Compounds containing elements of Groups 2 or 12 of the Periodic System
- C07F3/06—Zinc compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/22—Tin compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/28—Titanium compounds
Abstract
A flame retardant composition comprising inositol polyphosphate complexes, comprising: inositol polyphosphate, having 4-6 phosphates, complexed with amino acids and metal ions, and methods of preparing a flame retardant coating on a surface of a material and a flame retardant material.
Description
1 FLAME RETARDANT COMPOSITION TECHNICAL FIELD id="p-1" id="p-1" id="p-1" id="p-1"
id="p-1"
[001] The present disclosure relates to a flame retardant composition, methods of preparing a material comprising such a flame retardant composition or a substrate having a coating with such a flame retardant composition, flame retardant kits, substrates provided with a coating of such flame retardant composition and a material comprising such flame retardant composition.
BACKGROUND ART id="p-2" id="p-2" id="p-2" id="p-2"
id="p-2"
[002] Many flame retardants used today are harmful to the environment and human health, and some have even been banned. During their production, they may give rise to by-products and waste solvents, which can be flammable and toxic. Therefore, there is an increased demand to develop environmentally friendly and non-toxic ways to fire-proof products. One way is to use bio-based substances as flame retardants, such as phosphorus- based flame retardants. Phosphorus-based flame retardants is a broad class of additive or reactive organic or inorganic compounds used to improve the fire safety of flammable materials such as plastics, textiles, wood, paper, and other flammable materials. id="p-3" id="p-3" id="p-3" id="p-3"
id="p-3"
[003] A non-toxic, naturally occurring substance with high phosphorus content is phytic acid (also called inositol hexaphosphate), which is used by plants as the main storage of phosphorus. When phytic acid is heated, it will decompose, simply put, into phosphoric acid and cyclohexane. This decomposition is endothermic (removes heat). Some generally accepted flame retarding mechanisms are summarised by S. L. LeVan (Chemistry of Fire Retardancy, R. Rowell (editor), The Chemistry of Solid Wood, Advances in Chemistry, 1984, 207, 531-574). On cellulosic materials (e.g. wood and cotton), the phosphoric acid will char the surface. Charring will reduce the amount of pyrolysis gases as well as their ignitability (removes fuel). lt is known that many metal ions, e.g. their hydroxides, can inhibit radical reactions [J. W. Hastie, Molecular basis of flame inhibition, Journal of Research ofthe National Bureau of Standards - A. Physics and Chemistry Vol 77A, no 6, 1973]. Phosphoric acid can also inhibit radical reactions, and thus impede the development of fire (removes the chain 2 reaction) [F. Laoutid et al., New prospects in flame retardant polymer materials: From fundamentals to nanocomposites, Materials Science and Engineering R, 2009, 63, 100-125]. [004] lnsoluble phytate complexes can be formed by replacing hydrogen from the phosphate groups in the phytic acid with metal ions [J. Nissar et al., A review phytic acid: As antinutrient or nutraceutical, Journal of Pharmacognosy and Phytochemistry, 2017, 6, 1554-1560]. The insoluble metal phytates can function as a barrier preventing contact between pyrolysis gases and air (removes oxygen) and because of the insolubility, it will not leach in contact with water (e.g. rain). At higher temperatures, the hydrocarbon part ofthe phytic acid molecule (the cyclohexane part) becomes partly charred and partly combusted. id="p-5" id="p-5" id="p-5" id="p-5"
id="p-5"
[005] By combining phytic acid with gas forming species, e.g. ammonia, the gas formation can be onset at a lower temperature, and the amount of gas that forms will be larger. lt is known that an intumescent layer will isolate the fuel source (the cellulose-based material) from the oxygen in the air, and improve the thermal properties ofthe flame retardant so that the fire is impeded [LeVan, Laoutid]. Since ammonia is a gas, it can slowly evaporate from the coating so that the flame retardant effect is inadvertently diminished. With the use of amino acids, this evaporation can be avoided because the gas production will then be onset only after the amino acids are heated to decomposition. Both NH; and C02 gases will form. id="p-6" id="p-6" id="p-6" id="p-6"
id="p-6"
[006] ln CN110646314A is discussed an epoxy composite bio-based flame retardant material, combining the thermal decomposition, flame retardant and smoke suppression characteristics of phytic acid with arginine as a natural gas source which can dilute oxygen. id="p-7" id="p-7" id="p-7" id="p-7"
id="p-7"
[007] US2015073071A shows a flame retardant coating composition comprising poly(dopamine) and tris(hydroxymethyl)aminimethande) or gaseous ammonia. The coating composition can further cc-rnprise phytic acid that cah ha partiaiiy iiautraiizad twith an anime:- acid. [008] CN105085983A relates to a synergistic flame retardant iivhich is a phytic acid anatal precäpitate that obtained by taking phytic: attitl, nfietal salta aiid iiydroxifjes or oxidas as ravv rnateršaâs tiimugia crypractipitatâora. The cornptisite flame retardant førrned by the syawergistic flarne retardant and cornpoiierats containing phoaphorus can aarve as a liaiogafvfree fiame retardant arifi be used for fiarria-riatardant iificifiifiatatior: of polyamifía polyriier materials. [009] CN10569635OA shows a functional cotton fabric by complexing phytic acid through divalent calcium ions. 3 id="p-10" id="p-10" id="p-10" id="p-10"
id="p-10"
[0010] ln Journal of Cleaner Production, Volume 243, 118641, Xiaohui Liu et al., January 10, 2020, Flame retardant cellulosic fabrics via layer-by-layer self-assembly double coating with egg white protein and phytic acid, is discussed Ernpartlrfg flarne retardârlg property en ceiiulfasic fabrics by generatšng pnosnhorus-»rfâtrcwgeal fis-arne retardant systern forrnecl by lntense electrosteatlc attraction of egg v-.fhâte protein and phytic acicl (FA) xfvltlf special hexapnosplfieatfa- suåastltlated cyclâc structure. id="p-11" id="p-11" id="p-11" id="p-11"
id="p-11"
[0011] ln International Journal of Biological I\/lacromolecules, Volume 140, Pages 303-310, Xiaohui Liu et al., November 1, 2019, Eco-friendly flame retardant coating deposited on cotton fabrics from bio-based chitosan, phytic acid and divalent metal ions, is shown :ghštosan and phytlt: acid as intumescent flafne retardant syfstefn and rnetal len as a syfnergist tfaat »vare built on cotton fabritts to achieve efficient 'flaane retardancy. id="p-12" id="p-12" id="p-12" id="p-12"
id="p-12"
[0012] An optimal flame retardant is a flame retardant that is environmentally friendly, that does not leach by rain, and that can remove all necessary requirements for a fire (fuel, heat, oxygen, radical reaction). This can be done by endothermal decomposition (removes heat), charring and reduction of flammable pyrolysis gases (removes fuel), formation of non- flammable gases which dilute the oxygen in air (removes oxygen), and termination ofthe chain reaction (removes radicals). The additional formation of an intumescent layer can also remove the necessary components of a fire mentioned above. [LeVan, Laoutid]. However, the optimal mixture that can balance all ofthe above-mentioned properties in the most efficient way, is yet to be found.
SUMMARY OF THE INVENTION id="p-13" id="p-13" id="p-13" id="p-13"
id="p-13"
[0013] lt is an object of the present invention to provide an environmentally friendly flame retardant composition composed of non-hazardous components, and which further is resistant to leaching. Further objects are to provide methods of preparing a material comprising such flame retardant composition or a substrate having a coating with such flame retardant composition, flame retardant kits, substrates provided with a coating of such flame retardant composition and a material comprising such a flame retardant composition. 4 id="p-14" id="p-14" id="p-14" id="p-14"
id="p-14"
[0014] According to a first aspect there is provided a flame retardant composition comprising: inositol polyphosphate complexes, comprising inositol polyphosphate, having 4-6 phosphates, complexed with amino acids and metal ions. id="p-15" id="p-15" id="p-15" id="p-15"
id="p-15"
[0015] The metal ions may be monovalent, divalent, trivalent, and/or tetravalent metal ions. [0016] The flame retardant composition may for example be arranged as a coating on a surface on a substrate of any type of material, i.e. any combustible material, such as a surface of a cellulosic material, such as cotton, rayon, linen, wood or wood-based material. The material may be of plastics or wool. The substrate may be a soft substrate such as a cloth or a harder substrate such as a piece of wood. The composition may also be applied on materials being a mixture of a cellulosic material and for example polyester. The composition may be a component in a material mixed with other components such as cellulosic fibres or it may be mixed with plastics. The composition may be used on/in/mixed with any material that need fire protection. id="p-17" id="p-17" id="p-17" id="p-17"
id="p-17"
[0017] lt is believed that the inositol polyphosphate reacts with the glucose units in the cellulose (or with the monomeric units of other polymers) and forms covalent ester bonds with the surface. Amino acids can also form covalent amide bonds with PA. I\/|etal ions may form ionic bonds with amino acids and with the inositol polyphosphate and may form a surface coating of ionic nature. id="p-18" id="p-18" id="p-18" id="p-18"
id="p-18"
[0018] The inositol polyphosphate having 4-6 phosphates may be inositol hexaphosphate, inositol pentaphosphate (inositol pentakisphosphate, |nsP5) or inositol tetraphosphate (inositol tetrakisphosphate, lnsP4). ln developing seeds, inositol hexaphosphate (phytic acid), a major phosphorus storage compound in plant seeds, is mainly synthesized from glucose 6- phosphate and 1D-myo-inositol 3-phosphate synthase catalyzes the first step of this pathway. |nositol tetraphosphate and inositol pentaphosphate are generated by subsequent series of phosphorylation and dephosphorylation in this phytic acid pathway. id="p-19" id="p-19" id="p-19" id="p-19"
id="p-19"
[0019] The present flame retardant composition is environmentally friendly and composed of natural, non-hazardous and edible components. lt is further resistant to leaching. None ofthe components of the composition (when dried) leaches to any great extent into solution if the composition is put in a solution or subjected to for example rain. id="p-20" id="p-20" id="p-20" id="p-20"
id="p-20"
[0020] Multivalent metal ions can make the fire resistant composition insoluble (in aqueous solution) and resistant to leaching. |nositol phosphates form stable and insoluble complexes 4 with the metal ions, which can function as a barrier preventing contact between pyrolysis gases and air (removes oxygen), and because of the insolubility, it will not leach in contact with water (e.g. rain). id="p-21" id="p-21" id="p-21" id="p-21"
id="p-21"
[0021] When the present flame retardant composition is heated, the inosito| polyphosphate removes fuel by causing charring when it decomposes to phosphoric acid. This decomposition and charring takes place at a lower temperature than the ignition temperature ofthe fuel, which means that there will be less fuel available at the temperature of ignition. Charring at a low temperature leads to the production of pyrolysis gases (fuel) of less combustible nature [known from literature, LeVan] and the charring efficiently prevents production of more fuel so any fire will self-extinguish with the use of the present flame retardant composition on/in/mixed with a material. id="p-22" id="p-22" id="p-22" id="p-22"
id="p-22"
[0022] Amino acids improve the flame retarding properties ofthe composition, as the gases formed during decomposition will dilute the oxygen so that the mixture of oxygen and pyrolysis gases will no longer be ignitable. The amino acid make a bridge between inosito| polyphosphate and metal ions. |nstead of having a strong network of metal-phosphate bonds, there will be a weaker network of bonds between phosphate groups, metal ions and amino acids. The incorporation of amino acids in the composition makes the composition a bit softer and easier to thermally degrade, while at the same time keeping it substantially insoluble. [0023] Heat is first removed through endothermic decomposition ofthe flame retardant composition. After the charring the phosphoric acid residues will polymerize in a second endothermic process. lf no hydrogen ions are present on the phosphate groups, highly insoluble metal phosphates (e.g. calcium phosphates) will form instead of polymerization, and this formation is exothermic and has to be avoided. The inosito| phosphates decompose not only to phosphoric acid, but the hydrocarbon ring will form a polyaromatic graphite-like layer which will swell from the gases formed during the decomposition and heating. This layer has the ability to remove heat by conduction and high heat capacity and can also function as a barrier preventing contact between pyrolysis gases and air (oxygen). The intumescent coating will consist of char, polymerised phosphates, and some metal phosphate. id="p-24" id="p-24" id="p-24" id="p-24"
id="p-24"
[0024] When the flame retardant composition contains inosito| phosphate, amino acids and metal ions, the flame retarding ability improves when it comes to heat release, self- extinguishment and mass loss compared to compositions with only two of the components. 5 6 When multivalent metal ions are used none of the flame retardant components leach to a great extent in contact with water. id="p-25" id="p-25" id="p-25" id="p-25"
id="p-25"
[0025] By combining inositol polyphosphate, amino acids and metal ions in a flame retardant, fire can be prevented by using several mechanisms that attack the four components needed for a fire. Endothermic decomposition ofthe coating will remove heat from the fire. The decomposition of the coating into phosphoric acid leads to charring. The charring reduces the amount of pyrolysis gases formed and since the charring takes place at a low temperature, relative to the normal pyrolysis temperature ofthe combustible material, the composition of the pyrolysis gases formed will be less combustible. ln this way the fuel is removed. The decomposition ofthe coating also gives rise to noncombustible gases which dilute the oxygen and pyrolysis gases so that ignition cannot take place. The gases formed also leads to intumescence. The hydrocarbon part of the inositol polyphosphate forms a polyaromatic graphite-like structure which is expanded by the gases formed from the amino acid part ofthe flame retardant coating. The intumescence alters the heat conducting properties and further decreases the flame retardant efficiency. The intumescent coating further prevents the production and diffusion of pyrolysis gases. ln addition, at a slightly elevated temperature, the phosphoric acid will polymerise into polymeric structures and release water vapor. This formation is endothermic and removes heat. Furthermore, it serves as a barrier preventing pyrolysis gases and oxygen to come into contact with each other in a combustible mixture. Alkali metals and phosphorus containing species have the ability to terminate radical reactions, which will further prevent a fire from developing [Hastie, Laoutid]. ln addition to all of these mechanisms, the flame retardant will also be resistant to water due to the insoluble nature of the coating. id="p-26" id="p-26" id="p-26" id="p-26"
id="p-26"
[0026] Hence, the present flame retardant composition, when used on/in/mixed with any material that need fire protection, decomposes endothermically (removes heat), hinders the release of pyrolysis gases, dilutes the oxygen in air, terminates the radical reactions, and forms an intumescent layer or matrix. Such a flame retardant composition therefore has the ability to remove all necessary requirements for a fire (fuel, heat, oxygen, radical reaction). id="p-27" id="p-27" id="p-27" id="p-27"
id="p-27"
[0027] The amino acid may be selected from one or more of alanine, arginine, asparagine, aspartic acid, cysteine, glutamine, glutamic acid, glycine, histidine, isoleucine, leucine, lysine, methionine, phenylalanine, proline, serine, threonine, tryptophan, tyrosine, and valine. 6 7 id="p-28" id="p-28" id="p-28" id="p-28"
id="p-28"
[0028] The amino acids may be used in the composition as monomers, peptides, polypeptides, or proteins. With the use of individual amino acids, the composition can be optimized to maximize the flame retardant efficiency. E.g., for arginine, which contains the largest amount of gas forming groups, only a small amount is required to reach maximum flame retardancy effect. id="p-29" id="p-29" id="p-29" id="p-29"
id="p-29"
[0029] The metal ion may be a monovalent, divalent, trivalent and/or tetravalent metal ion. [0030] I\/|onovalent ions provide water-soluble compositions. For use in a flame retardant composition, monovalent metal ions work well in dry applications that are not exposed to moisture. id="p-31" id="p-31" id="p-31" id="p-31"
id="p-31"
[0031] ln some embodiments and for some applications, the inositol polyphosphate needs to be neutralized (inositol polyhosphate may be too acidic for the underlying material). This can be done by adding for example NaOH, Ca(OH)2 or AI(OH)3. Thereafter, the amino acids can be added and then a polyvalent metal ion. Hence, the flame retardant composition may comprise both monovalent and multivalent metal ions. id="p-32" id="p-32" id="p-32" id="p-32"
id="p-32"
[0032] The metal ion may be selected from one or more of K+, Na+, Cu+, Cu2+, Ca2+, Zn2+, Fe2+, Fe3+, I\/|g2+, Al3+, Ti4+ and Sn4+. id="p-33" id="p-33" id="p-33" id="p-33"
id="p-33"
[0033] The metal ion may be selected from any non-hazardous metal ion or combination of such ions in the periodic table. id="p-34" id="p-34" id="p-34" id="p-34"
id="p-34"
[0034] The inositol polyphosphate may be phytic acid. id="p-35" id="p-35" id="p-35" id="p-35"
id="p-35"
[0035] According to a second aspect there is provided a flame retardant kit comprising, a first powder or solution comprising an inositol polyphosphate complex of inositol polyphosphate, having 4-6 phosphates, and amino acids, and a second powder or solution comprising metal ions. id="p-36" id="p-36" id="p-36" id="p-36"
id="p-36"
[0036] The solution may be water. id="p-37" id="p-37" id="p-37" id="p-37"
id="p-37"
[0037] ln the first (aqueous) solution, inositol polyphosphate in a concentration ranging from 1% to 50% (w/w), and amino acids in a concentration ranging from 10 mM to saturation limit are mixed. The second (aqueous) solution comprises metal ions in a concentration of 0.1 M to saturation limit. id="p-38" id="p-38" id="p-38" id="p-38"
id="p-38"
[0038] The concentration of inositol polyphosphate may be 1-50%, 1-40%, 1-30%, 1-20%, 1- 10%, 1-5%, 1-2%, 2-50%, 5-50%, 10-50%, 20-50%, 30-50%, 40-50%, 5-10%, 10-20%, 20-30%, 30-40% or 40-50% (w/w). 8 id="p-39" id="p-39" id="p-39" id="p-39"
id="p-39"
[0039] ln some embodiments and for some applications, the inositol polyphosphate may need to be neutralized, fully or partially (inositol polyhosphate may be too acidic for the underlying material), why the first solution also may comprise NaOH, Ca(OH)2 or AI(OH)3. The molar ratio ofe.g. NaOH relative the inositol polyphosphate may be 1-12, 1-10, 1-8, 1-6, 1-4, 1-2, 2-12, 4- 12, 6-12, 8-12, 10-12, 2-4, 4-6, 6-8, 8-10, or 3-9. id="p-40" id="p-40" id="p-40" id="p-40"
id="p-40"
[0040] The concentration of amino acids in the first solution may be 10 mM to saturation, 10 mM-1 M, 10 mM-100 mM, 100 mM to saturation, or 1 M to saturation. The saturation level depends on the amino acid(s) used, pH, temperature etc. id="p-41" id="p-41" id="p-41" id="p-41"
id="p-41"
[0041] The concentration of metal ions in the second solution may be 0.1 M to saturation, 1 M to saturation, 2 M to saturation, 0.1 M-2 M, 1-2 M. The saturation level depends on the metal ions used, pH, temperature etc. id="p-42" id="p-42" id="p-42" id="p-42"
id="p-42"
[0042] According to a third aspect there is provided a method of preparing a flame retardant material, the method comprising: providing a material; mixing inositol polyphosphate, having 4-6 phosphates, and amino acids in an aqueous solution, wherein a concentration of inositol polyphosphate in the solution is 1% to 50% (w/w) and a concentration of amino acids in the solution is 10 mM to saturation limit, forming a first solution comprising an inositol polyphosphate-amino acid complex; applying the first solution onto at least a surface of said material forming an intermediate coating; or mixing the material with the first solution, forming an intermediate mixture; providing a second solution comprising metal ions in a concentration of 0.1 M to saturation limit, and applying the second solution onto the intermediate coating forming a flame retardant coating on the at least one surface of the material, or mixing the intermediate mixture with the second solution, forming a flame retardant material mixture. id="p-43" id="p-43" id="p-43" id="p-43"
id="p-43"
[0043] The second solution may be obtained by dissolving in an aqueous solution any salt or salts comprising the desired metal ion/ions. id="p-44" id="p-44" id="p-44" id="p-44"
id="p-44"
[0044] As metal-inositol polyphosphate complexes are difficult to dissolve, the metal ions and the inositol polyphosphate-amino acid complexes are provided in different solutions, because the metal-inositol polyphosphate-amino acid complexes otherwise would precipitate from the solution. The aqueous solution may be water. id="p-45" id="p-45" id="p-45" id="p-45"
id="p-45"
[0045] The flame retardant composition may be used as a coating on a surface on a substrate of any type of material, i.e. any combustible material, such as a surface of a cellulosic material, 8 9 such as cotton, rayon, linen, wood or wood-based material. The substrate may also be a soft substrate such as a cloth or a harder substrate such as a piece of wood. The surface coating may also be applied on materials being a mixture of a cellulosic material and for example polyester. The material may be of plastics, such as PVC. The material may be wool. id="p-46" id="p-46" id="p-46" id="p-46"
id="p-46"
[0046] The first and second solutions may be mixed with a material, such as cellulose fibres or a plastic material, forming an intermediate mixture and a flame retardant mixture, respectively. id="p-47" id="p-47" id="p-47" id="p-47"
id="p-47"
[0047] The metal ions enter the inositol polyphosphate complex, which then goes from a two- component complex to a three-component complex. lt is to be understood that the metal ion component in the here-component complex may comprise one or more different metal ions and that the amino acid component in the three-component complex may comprise one or more different amino acids. id="p-48" id="p-48" id="p-48" id="p-48"
id="p-48"
[0048] A drying step may be applied between application ofthe first and second solution to the surface of the substrate. Drying may be performed at ambient conditions. id="p-49" id="p-49" id="p-49" id="p-49"
id="p-49"
[0049] A drying step may be applied after having mixed the material with the first solution, before mixing the material with the second material. Drying may be performed at ambient conditions. id="p-50" id="p-50" id="p-50" id="p-50"
id="p-50"
[0050] The formed flame retardant material or mixture may me dried. id="p-51" id="p-51" id="p-51" id="p-51"
id="p-51"
[0051] The application ofthe first and second solutions may be repeated one or more times (preferably after a drying step) to create a thicker flame retardant coating on the surface. A thicker coating may improve the flame retardancy, but may make substrates such as cloths stiffer. id="p-52" id="p-52" id="p-52" id="p-52"
id="p-52"
[0052] The method may performed in opposite order, i.e. applying/mixing with the second solution, the metal ions, and thereafter the first solution, inositol polyphosphate complexed with amino acids. id="p-53" id="p-53" id="p-53" id="p-53"
id="p-53"
[0053] According to a fourth aspect there is provided a method of preparing a flame retardant material. The method comprising: providing a material; providing an aqueous solution of inositol polyphosphate, having 4-6 phosphates, wherein a concentration of inositol polyphosphate in the solution is 1%-50% (w/w); providing an aqueous solution of amino acids, wherein a concentration of amino acids in the solution is 10 mM to saturation limit; applying the inositol polyphosphate solution onto at least a surface ofthe material forming a first 9 intermediate coating, or mixing the material with the solution comprising inositol polyphosphate, forming a first intermediate mixture; applying the amino acid solution onto at least a surface ofthe material forming a second intermediate coating, or mixing the first intermediate mixture with the solution comprising amino acids, forming a second intermediate mixture; providing a solution comprising metal ions in a concentration of 0.1 M to saturation limit, and applying the solution comprising metal ions onto the second intermediate coating, forming a flame retardant coating on the at least one surface ofthe material, or mixing the second intermediate mixture with the solution comprising metal ions, forming a flame retardant material mixture. id="p-54" id="p-54" id="p-54" id="p-54"
id="p-54"
[0054] ln this method inositol polyphosphate-amino acid complex is formed on the surface of the material instead of being preformed in the solution as discussed for the method of aspect three. The material may be any of the materials described above. id="p-55" id="p-55" id="p-55" id="p-55"
id="p-55"
[0055] According to a fifth aspect there is provided a method of preparing a flame retardant material, the method comprising: providing a material; mixing inositol polyphosphate, having 4-6 phosphates, amino acids and a metal hydroxide in an aqueous solution, wherein a concentration of inositol polyphosphate in the solution is 1%-50% (w/w), a concentration of amino acids is 10 mM to saturation limit, the metal of the metal hydroxide is a bivalent, trivalent or tetravalent metal ion and a concentration of the metal ion is 0.1 M to saturation limit, forming a reaction mixture; applying the reaction mixture onto at least a surface of the material forming an intermediate coating, or mixing the material with the reaction mixture forming an intermediate mixture, and applying NaOH or NazCOg onto the intermediate coating, forming a flame retardant coating on the at least one surface of the material, or mixing the intermediate mixture with NaOH or NazCOg forming a flame retardant mixture. [0056] For the methods above the following applies: id="p-57" id="p-57" id="p-57" id="p-57"
id="p-57"
[0057] The concentration of inositol polyphosphate may be 1-50%, 1-40%, 1-30%, 1-20%, 1- 10%, 1-5%, 1-2%, 2-50%, 5-50%, 10-50%, 20-50%, 30-50%, 40-50%, 5-10%, 10-20%, 20-30%, 30-40% or 40-50% (w/w). id="p-58" id="p-58" id="p-58" id="p-58"
id="p-58"
[0058] ln some embodiments and for some applications, the inositol polyphosphate may need to be neutralized before adding the amino acids (inositol polyhosphate is too acidic), why the first solution also may comprise NaOH, Ca(OH)2 or AI(OH)3. The molar ratio of e.g. NaOH 11 relative the inositol polyphosphate may be 1-12, 1-10, 1-8, 1-6, 1-4, 1-2, 2-12, 4-12, 6-12, 8-12, 10-12, 2-4, 4-6, 6-8, or 8-10. id="p-59" id="p-59" id="p-59" id="p-59"
id="p-59"
[0059] The concentration of amino acids in the first solution may be 10 mM to saturation, 10 mM-1 M, 10 mM-100 mM, 100 mM to saturation, or 1 M to saturation. The saturation level depends on the amino acid(s) used, pH, temperature etc. id="p-60" id="p-60" id="p-60" id="p-60"
id="p-60"
[0060] The concentration of metal ions may be 0.1 M to saturation, 1 M to saturation, 2 M to saturation, 0.1 M-2 M, 1-2 M. The saturation level depends on the metal ions used, pH, temperature etc. id="p-61" id="p-61" id="p-61" id="p-61"
id="p-61"
[0061] The material may be any of the materials described above. id="p-62" id="p-62" id="p-62" id="p-62"
id="p-62"
[0062] The composition may be a component in a material mixed with other components such as cellulosic fibres or it may be mixed with plastics. The composition may be used on/in/mixed with any material that need fire protection. ln a mixture with for example cellulosic fibre the amount of inositol polyphosphate to cellulosic fibre may be 1-50 wt.%, 1-45 wt.%, 1-40 wt.%, 1-35 wt.%, 1-30 wt.%, 1-25 wt.%, 1-20 wt.%, 1-15 wt.%, 1-10 wt.%, 1-5 wt.%, 5-50 wt.%, 10-50 wt.%, 15-50 wt.%, 20-50 wt.%, 25-50 wt.%, 30-50 wt.%, 35-50 wt.%, 40-50 wt.%, 45-50 wt.%, 5-10wt.%, or 10-20wt%. id="p-63" id="p-63" id="p-63" id="p-63"
id="p-63"
[0063] The pH of the solution comprising amino acids may be adjusted to pH 1-12 before use. [0064] The pH may adjusted to pH 1-10, 1-8, 1-6, 1-4, 1-2, 2-12, 4-12, 6-12, 8-12, 10-12, 2-4, 4- 6, 6-8, or 8-10. id="p-65" id="p-65" id="p-65" id="p-65"
id="p-65"
[0065] ln some embodiments and for some applications, the inositol polyphosphate may need to be neutralized before adding the amino acids (inositol polyhosphate is too acidic). This can be done by adding for example NaOH, Ca(OH)2 or AI(OH)3. Thereafter, the amino acids can be added and then a polyvalent metal ion. id="p-66" id="p-66" id="p-66" id="p-66"
id="p-66"
[0066] A solution may be allowed to react with the material for at least 10 seconds before being removed and/or adding a next solution. id="p-67" id="p-67" id="p-67" id="p-67"
id="p-67"
[0067] Thicker material may need longer reaction times. id="p-68" id="p-68" id="p-68" id="p-68"
id="p-68"
[0068] At least one ofthe solutions may be applied on the surface of the material by dipping the at least one surface ofthe material in the solution. id="p-69" id="p-69" id="p-69" id="p-69"
id="p-69"
[0069] The material may for example be dipped in a first solution. Thereafter, the material is taken out ofthis solution and is either (i) dipped in a second solution and thereafter put to dry 11 12 or the material may be mounted on a stance and a second solution may be sprayed on the treated surface and thereafter the material is put to dry. id="p-70" id="p-70" id="p-70" id="p-70"
id="p-70"
[0070] A least one ofthe solutions may be applied on the surface ofthe material by spraying the solution onto the surface ofthe material. id="p-71" id="p-71" id="p-71" id="p-71"
id="p-71"
[0071] The method may further comprise a drying step after applying one or more ofthe solutions on the surface. id="p-72" id="p-72" id="p-72" id="p-72"
id="p-72"
[0072] |fthe metal ion solution is applied before the material/substrate has dried after application of inositol polyphosphate and amino acids, there is a risk that the solution runs down along the piece of fabric instead of being distributed more homogeneously on the material/substrate. Drying may take place under ambient conditions, alternatively, at an increased temperature. id="p-73" id="p-73" id="p-73" id="p-73"
id="p-73"
[0073] According to a sixth aspect, there is provided a method of preparing a flame retardant material, comprising mixing the flame retardant composition described above with a material. id="p-74" id="p-74" id="p-74" id="p-74"
id="p-74"
[0074] The material may be any of the materials described above. id="p-75" id="p-75" id="p-75" id="p-75"
id="p-75"
[0075] According to a seventh aspect, there is provided a substrate provided with a flame retardant surface coating on at least a surface thereof, wherein the flame retardant surface coating comprises inositol polyphosphate, having 4-6 phosphates, complexed with amino acids and metal ions. id="p-76" id="p-76" id="p-76" id="p-76"
id="p-76"
[0076] The material may be a soft cellulosic material such as cotton or a harder cellulosic material such as wood. The material may be in the form of a cloth, a plank, wood, chips. The material may comprise cellulosic material mixed with other materials such as mixture cotton and for example polyester. The material may be wool or plastic. id="p-77" id="p-77" id="p-77" id="p-77"
id="p-77"
[0077] According to an eighth aspect, there is provided a flame retardant material comprising a material mixed with a flame retardant composition comprising inositol polyphosphate, having 4-6 phosphates, complexed with amino acids and metal ions. id="p-78" id="p-78" id="p-78" id="p-78"
id="p-78"
[0078] The material may be cellulosic material in the form of fibres or a plastic material such as PVC. 12 13 BRIEF DESCRIPTION OF THE DRAWINGS id="p-79" id="p-79" id="p-79" id="p-79"
id="p-79"
[0079] Fig. 1 shows a schematic composition of a flame retardant composition applied in a surface, the composition comprising phytate complexes, where the complexes comprise phytic acid complexed with amino acids and metal ions. id="p-80" id="p-80" id="p-80" id="p-80"
id="p-80"
[0080] Fig. 2a shows a graph from a thermal gravimetric analysis, % weight remaining, vs temperature, of reference materials (cotton) coated with different flame retardant compositions comprising phytic acid and metal ions. id="p-81" id="p-81" id="p-81" id="p-81"
id="p-81"
[0081] Fig. 2b shows a derivative graph from a thermal gravimetric analysis, change in % weight remaining, vs temperature, of reference materials coated with different flame retardant compositions comprising phytic acid and metal ions. id="p-82" id="p-82" id="p-82" id="p-82"
id="p-82"
[0082] Fig. 2c shows results from cone calorimetry measurements: heat release rate (HRR) vs time of reference materials coated with different flame retardant compositions comprising phytic acid and metal ions. id="p-83" id="p-83" id="p-83" id="p-83"
id="p-83"
[0083] Fig. 2d shows results from cone calorimetry measurements: total heat release (THR) vs time of reference materials coated with different flame retardant compositions comprising phytic acid and metal ions. id="p-84" id="p-84" id="p-84" id="p-84"
id="p-84"
[0084] Fig. 3a shows a graph from a thermal gravimetric analysis, % weight remaining, vs temperature, of reference materials (cotton) coated with different flame retardant compositions comprising phytic acid and amino acids. id="p-85" id="p-85" id="p-85" id="p-85"
id="p-85"
[0085] Fig. 3b shows a derivative graph from a thermal gravimetric analysis, change in % weight remaining, vs temperature, of reference materials coated with different flame retardant compositions comprising phytic acid and amino acids. id="p-86" id="p-86" id="p-86" id="p-86"
id="p-86"
[0086] Fig. 3c shows results from cone calorimetry measurements: heat release rate (HRR) vs time of reference materials coated with different flame retardant compositions comprising phytic acid and amino acids. id="p-87" id="p-87" id="p-87" id="p-87"
id="p-87"
[0087] Fig. 3d shows results from cone calorimetry measurements: total heat release rate (THR) vs time of reference materials coated with different flame retardant compositions comprising phytic acid and amino acids. id="p-88" id="p-88" id="p-88" id="p-88"
id="p-88"
[0088] Fig. 4a shows a graph from a thermal gravimetric analysis, % weight remaining, vs temperature, of test materials coated with different flame retardant compositions comprising phytic acid, amino acids and metal ions. 13 14 id="p-89" id="p-89" id="p-89" id="p-89"
id="p-89"
[0089] Fig. 4b shows a derivative graph from a thermal gravimetric analysis, charge in % weight remaining, vs temperature, of test materials coated with different flame retardant compositions comprising phytic acid, amino acids and metal ions. id="p-90" id="p-90" id="p-90" id="p-90"
id="p-90"
[0090] Fig. 4c shows results from cone calorimetry measurements: heat release rate (HRR) vs time of test materials coated with different flame retardant compositions comprising phytic acid, amino acids and metal ions. id="p-91" id="p-91" id="p-91" id="p-91"
id="p-91"
[0091] Fig. 4d shows results from cone calorimetry measurements: total heat release (THR) vs time of test materials coated with different flame retardant compositions comprising phytic acid, amino acids and metal ions. id="p-92" id="p-92" id="p-92" id="p-92"
id="p-92"
[0092] Fig. 4e shows results from cone calorimetry measurements: heat release rate (HRR) vs time of test materials coated with different flame retardant compositions comprising phytic acids, amino acids and metal ions. id="p-93" id="p-93" id="p-93" id="p-93"
id="p-93"
[0093] Fig. 4f shows results from cone calorimetry measurements: total heat release (THR) vs time of test materials coated with different flame retardant compositions comprising phytic acids, amino acids and metal ions.
DETAILED DESCRIPTION id="p-94" id="p-94" id="p-94" id="p-94"
id="p-94"
[0094] Below is described an environmentally friendly flame retardant composition composed of non-hazardous components, and which further is resistant to leaching. Such a flame retardant composition comprises inositol polyphosphate complexes, comprising inositol polyphosphate, having 4-6 phosphates, complexed with amino acids and metal ions. id="p-95" id="p-95" id="p-95" id="p-95"
id="p-95"
[0095] ln Fig. 1 is an example of such a flame retardant composition applied on a surface of a substrate illustrated. ln Fig. 1 the inositol polyphosphate is phytic acid, the metal ions are Na+, Caz* and Al3+. The amino acids, here lysine, make a bridge between the phytic acid and the (multivalent) metal ions. |nstead of having a strong network of direct metal-phosphate bonds, there is a weaker network with metal-phosphate and metal-carbonate bonds. The composition is insoluble in aqueous solutions, and the hydrocarbon chain of the amino acid will facilitate the onset of thermal degradation when exhibited to fire. The incorporation of amino acids in the composition makes the composition a bit softer and more easy to thermally degrade as compared to complexes with direct metal-phytic acid bonds, while at the same time keeping the insolubility of the complex. 14 id="p-96" id="p-96" id="p-96" id="p-96"
id="p-96"
[0096] A flame retardant coating on a surface of a material may be prepared by mixing inositol polyphosphate, having 4-6 phosphates, and amino acids in an aqueous solution, wherein a concentration of inositol polyphosphate in the solution is 1-50% (w/w) and a concentration of amino acids in the solution is 10 mM to saturation limit, forming a first solution comprising an inositol polyphosphate-amino acid complex. Thereafter, the first solution is applied onto the surface of the material (for example by spraying or dipping the surface in the first solution). The surface may then, optionally, be dried. Thereafter, a second solution comprising metal ions in a concentration of 0.1 M to saturation limit, is applied onto the surface of the material treated with the first solution (for example by spraying or dipping the surface in the second solution). The metal ions enter the inositol polyphosphate complex, which then goes from a two-component complex to a three-component complex. When dried, the formed coating forms a protection against fire. The coating is resistant to leaching. id="p-97" id="p-97" id="p-97" id="p-97"
id="p-97"
[0097] The material may be any combustible material in need of fire protection, such as a cellulosic material, such as cotton, rayon, linen, wood or wood-based material. The material may be of plastics or wool. The substrate may be a soft substrate such as a cloth or a harder substrate such as a piece of wood. The composition may also be applied on materials being a mixture of a cellulosic material and for example polyester. id="p-98" id="p-98" id="p-98" id="p-98"
id="p-98"
[0098] A flame retardant material may be prepared by mixing inositol polyphosphate, having 4-6 phosphates, and amino acids in an aqueous solution, wherein a concentration of inositol polyphosphate in the solution is 1-50% (w/w) and a concentration of amino acids is 10 mM to saturation limit, forming a first solution comprising an inositol polyphosphate-amino acid complex. The first solution is mixed with a material, such as cellulose fibres or a plastic material, forming an intermediate mixture. A second solution comprising metal ions in a concentration of 0.1 M to saturation limit is then mixed with the intermediate mixture to form the flame retardant material. Alternatively, the material, such as molten plastics or sawdust and glue, may be mixed with a preformed flame retardant composition precipitate (described above) to form a flame retardant material. id="p-99" id="p-99" id="p-99" id="p-99"
id="p-99"
[0099] Below is described non-limiting examples of different samples treated with a flame retardant composition comprising inositol polyphosphate complexes, comprising inositol polyphosphate, having 4-6 phosphates, complexed with amino acids and metal ions. 16 Experimental Treatment of cotton samples [00100] Cotton samples of 100% cotton, 138 mg/mz, were used in the experiments.
Test material -flame retardant composition comprising phytic acid, amino acids and metal ions [00101] A 10% aqueous solution of phytic acid (PA) was prepared by taking 20 g of 50% (w/w) aqueous solution of PA into a plastic bottle. Then milliQ water was added to it to make the total weight 100 g. pH at this stage was equal to or below zero. To this solution, 1.82 g solid NaOH was added (to give a molar ratio of 3:1 between Na* and PA), and the solution was shaken for an hour to dissolve it. pH was now 2.5. After that, 2.64 g arginine (Arg) was added to it (to give a molar ratio of 1:1 between Arg and PA). lt was shaken for an hour to dissolve it. pH ofthe solution was now 4.5. This procedure formed NagArgPA. id="p-102" id="p-102" id="p-102" id="p-102"
id="p-102"
[00102] The cotton material to be treated was dipped in the solution above (taken in a beaker) for 60 seconds. Thereafter the material was taken out of the solution and mounted on a stance for drying at ambient temperature for 6 days. After that an aqueous solution containing 0.1 M CaClz was sprayed on the dried cloth pre-treated with the solution comprising NagArgPA forming CazïNagArgPA. The material treated with the metal ion containing solution was thereafter put to dry at ambient temperature. id="p-103" id="p-103" id="p-103" id="p-103"
id="p-103"
[00103] NagArgPA was prepared as described above. After that an aqueous solution containing 1.0 M AlClg was sprayed on the dried cloth pre-treated with the solution comprising NagArgPA forming Al3+-Na3ArgPA. The material treated with the metal ion containing solution was thereafter put to dry at ambient temperature. id="p-93" id="p-93" id="p-93" id="p-93"
id="p-93"
[0093] A 10% aqueous solution of phytic acid was prepared by taking 20 g of 50% (w/w) aqueous solution of PA into a plastic bottle. Then milliQ water was added to it to make the total weight 100 g. pH at this stage was equal to or below zero. To this solution, 1.82 g solid NaOH was added (to give a molar ratio of 3:1 between Na* and PA), and the solution was shaken for an hour to dissolve it. pH was now 2.5. After that, 1.59 g glycine (Gly) was added to it (to give a molar ratio of 1:1 between Gly and PA). lt was shaken for an hour to dissolve it. pH of the solution was still 2.5. This procedure formed NagGlyPA id="p-94" id="p-94" id="p-94" id="p-94"
id="p-94"
[0094] A 10% aqueous solution of phytic acid was prepared by taking 20 g of 50% (w/w) aqueous solution of PA into a plastic bottle. Then milliQ water was added to it to make the 16 17 total weight 100 g. pH at this stage was equal to or below zero. To this solution, 1.82 g solid NaOH was added (to give a molar ratio of 3:1 between Na* and PA), and the solution was shaken for an hour to dissolve it. pH was now 2.5. After that, 1.14 g serine (Ser) was added to it (to give a molar ratio of 1:1 between Ser and PA). lt was shaken for an hour to dissolve it. pH of the solution was still 2.5. This procedure formed NagSerPA Reference material 1 -flame retardant composition comprising phytic acid and metal ions id="p-104" id="p-104" id="p-104" id="p-104"
id="p-104"
[00104] NagPA, NagPA, Ca4PA NagPA was formed by forming a 10% aqueous solution of phytic acid by taking 20 g of 50% (w/w) aqueous solution of PA into a plastic bottle. Then milliQ water was added to it to make the total weight 100 g. pH at this stage was equal to or below zero. To this solution, 1.82 g solid NaOH was added (to give a molar ratio of 3:1 between Na* and PA), and the solution was shaken for an hour to dissolve it. pH was now 2.5. id="p-105" id="p-105" id="p-105" id="p-105"
id="p-105"
[00105] A 10% aqueous solution of phytic acid was prepared by taking 20 g of 50% (w/w) aqueous solution of PA into a plastic bottle. Then milliQ water was added to it to make the total weight 100 g. pH at this stage was equal to or below zero. To this solution, 5.46 g solid NaOH was added (to give a molar ratio of 9:1 between Na* and PA). pH was now 8.0. This procedure formed NagPA. id="p-106" id="p-106" id="p-106" id="p-106"
id="p-106"
[00106] A 10% aqueous solution of phytic acid was prepared by taking 20 g of 50% (w/w) aqueous solution of PA into a plastic bottle. Then milliQ water was added to it to make the total weight 100 g. pH at this stage was equal to or below zero. To this solution, 3.64 g solid NaOH was added (to give a molar ratio of 6:1 between Na* and PA). pH was now 4.0. To this solution, 8.91 g solid CaCl2'2H2O was added (to give a molar ratio of4:1 between Caz* and PA). The solution became warm and it was allowed to stand until it was cooled to room temperature. pH was now close to zero. This procedure formed Ca4PA.
Reference material 2 -flame retardant composition comprising phytic acid and amino acids id="p-107" id="p-107" id="p-107" id="p-107"
id="p-107"
[00107] A 10% aqueous solution of phytic acid was prepared by taking 20 g of 50% (w/w) aqueous solution of PA into a plastic bottle. Then milliQ water was added to it to make the total weight 100 g. pH at this stage is equal to or below zero. After that, 10.6 g arginine (Arg) was added to it (to give a molar ratio of4:1 between Arg and PA). lt was shaken for an hour to dissolve it. pH of the solution was now 2.5. This procedure formed Arg4PA. 17 18 [00108] A 10% aqueous solution of phytic acid was prepared by taking 20 g of 50% (w/w) aqueous solution of PA into a plastic bottle. Then milliQ water was added to it to make the total weight 100 g. pH at this stage is equal to or below zero. After that, 2.65 g arginine (Arg) and 2.0 g aspartic acid (Asp) were added to it (to give a molar ratio of 1:1:1 between Arg, Asp and PA). lt was shaken for an hour to dissolve it. pH of the solution was now 1.5. This procedure formed ArgAspPA. Cone calorimetry [00109] A cone calorimeter was used to measure heat release rate (HRR) and total heat release (THR). Samples (10x10 cm) of the test material and the different reference materials 1 and 2 were placed horisontally in the sample device. The samples were exposed to a heat flux of 14.9 kW/m2 (reference material 1) and 20 kW/mz (reference material 2 and test material). With this heat exposure, the temperature of the samples increases and flammable gases start to evolve when they degrade. The cone calorimeter generate sparks at regular intervals, which can start a fire if the amount of flammable gases released from the samples are large enough. An untreated cotton sample was used as a reference, a blank. Thermal Gravimetric Analysis (TGA) [00110] TGA was performed on small pieces of the samples (1-2 mg) (test material, reference materials 1 and 2, and non-treated reference material, blank) in a temperature range from 30°C to 800°C and with a heating rate of 20°C/minute. The atmosphere was either nitrogen (to study the thermal degradation, not illustrated in the figures) or air (to study also oxidising processes like combustion). A sample was placed on a balance inside the device and the weight of the samples were recorded as the temperature increased. The remaining mass (%) was plotted as a function of temperature. lt can be seen that untreated cotton loses almost all of its mass (changes into gaseous species) at around 370°C which is the normal self- ignition temperature of cellulose-based materials. At this temperature, the cellulose has degraded into flammable gases which can self-ignite in the air atmosphere. The remaining mass oxidises at around 500°C. Cotton treated with FR (flame retardant) with different composition of metal ions, amino acids and PA loses some of its mass at a lower temperature than untreated cotton, but 50% or more of the mass still remains at 370°C. As has been shown in the literature, charring reduces the amount of pyrolysis gases and charring at low 18 19 temperature forms a mixture of pyrolysis gases with lower flammability. Therefore, the test material and reference material 1 and 2 retain more of their mass at higher temperature. Leaching tests [00111] Leaching tests were performed to investigate how water resistant various flame retardant compositions are. Cotton pieces (1x1 cmz) treated with flame retardant solutions were placed in 100 ml freshly collected I\/|illiQ water (pH 7) in a beaker. At regular intervals, 0.5 ml (for PA) and 1.0 ml (for amino acids) aliquots of the leachate were withdrawn for chemical analysis by standard methods (see below) to determine the amounts of PA and amino acids, respectively, that had dissolved. id="p-112" id="p-112" id="p-112" id="p-112"
id="p-112"
[00112] To check the effect of rainwater on the leaching behaviour of cloths treated with flame retardant mixtures, water saturated with C02 was also tested in parallel. Rainwater can be considered a form of distilled water, but with pH 5.5 due to dissolution of aerial C02. No significant difference in behaviour were observed for water at pH 5.5 compared to 7.0. [00113] The amount of flame retardants that leach from a material can be determined by UV-Vis spectroscopy on the leachate. The absorbance of light is proportional to the amount of substance that absorbs the radiation so first calibration curves with known concentrations of amino acids and PA have to be made.Determination of amount PA leached: PA itself has very low absorbance so direct measurements of the UV-Vis signal requires very large amounts of PA to be detectable. ln order to detect small concentrations of PA, the indirect method of using iron(|||) thiocyanate was used instead by first making a calibration curve based on the absorbance of Fe(SCN)3. PA binds strongly to iron(|||), so the absorbance of Fe(SCN)3 will decrease the larger the amount of PA is present in the solution. id="p-114" id="p-114" id="p-114" id="p-114"
id="p-114"
[00114] Determination of amount amino acids leached: A ninhydrin solution was prepared by taking 400 mg ninhydrin, 60 mg hydrindantin, 15 ml DI\/ISO and 5 ml 4 M lithium acetate buffer in a coloured 100-mL volumetric flask. The suspension was stirred until all solid particles were dissolved. A stock solution of arginine at 50 pIVI concentration in 0.05% glacial acetic acid was prepared.
Five test/tubes were prepared as follows (volumes in ml): Tube 1 2 3 4 5 Standard 0.0 0.5 1.0 1.5 2.0 Water 2.0 1.5 1.0 0.5 0.0 19 Ninhydrin reagent 1.0 1.0 1.0 1.0 1.0 Total volume 3.0 3.0 3.0 3.0 3.0 Standards: The test-tubes were placed in a circular wire rack inside a boiling water bath, covered with aluminum foil, and boiled for 10 min. They were then removed and placed in an ice-water bath for 5 min. To each tube, 5 ml ethanol was added. The tubes were vortexed and covered with Parafilm for 5 min. The absorbance at 570 nm were measured, using the solution in tube 1 as a reference. That will give the standard curve. id="p-115" id="p-115" id="p-115" id="p-115"
id="p-115"
[00115] Determination ofamino acid concentration: in 20 ml milliQ water in a capped glass bottle. 1 mL ofthe leaching solution was withdrawn, and used in place of standard; 1 mL water and 1 mL ninhydrin solution were added (like tube 3). Amino acid concentration is determined, following a similar method as used for standard solution, and then comparison of the absorbance at 570 nm readings to the standard curve. id="p-116" id="p-116" id="p-116" id="p-116"
id="p-116"
[00116] When a highly soluble version of the flame retardant composition, containing sodium ions, is analysed, the results show that 43% of the coating has leached when equilibrium is reached while for insoluble versions with multivalent metal ions, e.g. calcium, no measurable amount has leached.
RESULTS Reference material 1 -flame retardant composition comprising phytic acid and metal ions id="p-117" id="p-117" id="p-117" id="p-117"
id="p-117"
[00117] TGA curves and derivative curves, shown in Figs 2a and 2b, show that the treated samples start to thermally degrade and lose mass at a lower temperature than the blank with untreated reference. This early thermal degradation cause charring and less pyrolysis so that more sample mass remains. Cone calorimetry with 14.9 kW/mz heat flux shows that the treated samples start to release heat (HRR), Fig. 2c, at an earlier time than the untreated sample, but the total heat released (THR), Fig. 2d, is only slightly lower than for the untreated blank.
Reference material 2 -flame retardant composition comprising phytic acid and amino acids id="p-118" id="p-118" id="p-118" id="p-118"
id="p-118"
[00118] TGA curves and derivative curves, shown in Figs 3a and 3b, show that the treated samples start to thermally degrade and lose mass at a lower temperature than the blank with untreated reference. This early thermal degradation cause charring and less pyrolysis so that more sample mass remains. Cone calorimetry with 20 kW/mz heat flux (Figs 3c and 3d) showed that the treated samples have almost zero heat release heat (HRR) and 21 total heat released (THR). However, the flame retardant solutions were too acidic so the cotton material was damaged from charring already before heat exposure.
Test material -flame retardant composition comprising phytic acid, amino acids and metal ii [00119] Especially with the addition of multivalent metal ions is more mass remaining in TGA, see Figs 4a and 4b. Heat flux in the cone calorimetry had to be increased to 20 kW/mz in order to see any heat release. The measurements of HRR and THR for the blank sample were stopped before the sample had burnt completely, so the curve for THR is expected to continue growing. The treated samples show almost no heat release at this power and the samples self- extinguish and leave residual masses, see Figs 4c and 4d. id="p-120" id="p-120" id="p-120" id="p-120"
id="p-120"
[00120] lllustrated in Fig. 4e is a comparison of a HRR for material treated with a composition comprising the amino acids arginine, glycine and serine. The HRR for glycine and serine is higher than for arginine, but still much lower than for the reference material (max HRR is above 200 kW/mz as can be seen in Fig. 4c). id="p-121" id="p-121" id="p-121" id="p-121"
id="p-121"
[00121] ln Fig. 4f is shown that the THR of the samples are also slightly higher for glycine and serine compared to arginine, but still much lower than for the reference material (see Fig 4d). [00122] The need of higher heat flux in order to see any heat release shows that mixtures of metal, amino acid and phytic acid can withstand heat much better than mixtures with only metal and phytic acid (Figs 2a-2d). Sodium, amino acids and phytic acid shows slightly better flame retarding performance (lower HRR and THR) compared to versions with Al3+ or Caz* added. However, the multivalent ions are needed in order to form insoluble compounds and the performance is still very good. The large mass remaining after heating indicates that the combination of low temperature charring and gas evolution which dilutes the oxygen is very efficient at stopping a fire.
Claims (17)
1. A flame retardant composition comprising: inositol polyphosphate complexes, comprising: inositol polyphosphate, having 4-6 phosphates, complexed with amino acids and metal ions.
2. The flame retardant composition of claim 1, wherein the amino acid is selected from one or more of alanine, arginine, asparagine, aspartic acid, cysteine, glutamine, glutamic acid, glycine, histidine, isoleucine, leucine, lysine, methionine, phenylalanine, proline, serine, threonine, tryptophan, tyrosine, and valine.
3. The flame retardant composition of claim 1 or 2, wherein the metal ion is a monovalent, divalent, trivalent and/or tetravalent metal ion.
4. The flame retardant composition of claim 3, wherein the metal ion is selected from one or more of K+, Na+, Cu+, Cu2+, Ca2+, Zn2+, Fe2+, Fe3+, I\/|g2+, Al3+, Ti4+ and Sn4+.
5. The flame retardant composition of any of claims 1-4, wherein the inositol polyphosphate is phytic acid.
6. A flame retardant kit comprising, a first powder or solution comprising an inositol polyphosphate complex of inositol polyphosphate, having 4-6 phosphates, and amino acids, and a second powder or solution comprising metal ions.
7. I\/|ethod of preparing a flame retardant material, the method comprising: - providing a material, - mixing inositol polyphosphate, having 4-6 phosphates, and amino acids in an aqueous solution, wherein a concentration of inositol polyphosphate in the solution is 1%-50% (w/w)23 and a concentration of amino acids in the solution is 10 mM to saturation limit, forming a first solution comprising an inositol polyphosphate-amino acid complex, - applying the first solution onto at least a surface of said material forming an intermediate coating, or mixing the material with the first solution, forming an intermediate mixture, - providing a second solution comprising metal ions in a concentration of 0.1 M to saturation limit, and - applying the second solution onto the intermediate coating forming a flame retardant coating on said at least one surface of the material, or mixing the intermediate mixture with the second solution forming a flame retardant material mixture.
8. I\/|ethod of preparing a flame retardant material, the method comprising: - providing a material, - providing an aqueous solution of inositol polyphosphate, having 4-6 phosphates, wherein a concentration of inositol polyphosphate in the solution is 1%-50% (w/w), - providing an aqueous solution of amino acids, wherein a concentration of amino acids in the solution is 10 mM to saturation limit, - applying the inositol polyphosphate solution onto at least a surface of said material forming a first intermediate coating, or mixing the material with the solution comprising inositol polyphosphate, forming a first intermediate mixture, - applying the amino acids solution onto said first intermediate coating forming a second intermediate coating, or mixing the first intermediate mixture with the solution comprising amino acids, forming a second intermediate mixture, - providing a solution comprising metal ions in a concentration of 0.1 M to saturation limit, and - applying the solution comprising metal ions onto said second intermediate coating forming a flame retardant coating on said at least one surface of the material, or mixing the second intermediate mixture with the solution comprising metal ions, forming a flame retardant material mixture.9. Method of preparing a flame retardant material, the method comprising: - providing a material, - mixing inositol polyphosphate, having 4-6 phosphates, amino acids and a metal hydroxide in an aqueous solution, wherein a concentration of inositol polyphosphate in the solution is 1%-50% (w/w), a concentration of amino acids is 10 mM to saturation limit, the metal of the metal hydroxide is a bivalent, trivalent or tetravalent metal ion and a concentration of the metal ion is 0.1 M to saturation limit, forming a reaction mixture, - applying the reaction mixture onto at least a surface ofthe material forming an intermediate coating, or mixing the material with the reaction mixture forming an intermediate mixture, and - applying NaOH or NazCOg onto the intermediate coating, forming a flame retardant coating on said at least one surface of the material, or mixing the intermediate mixture with
9.NaOH or NazCOg forming a flame retardant material mixture.
10. The method of any of claims claim 7-9, wherein pH of a solution comprising amino acids is adjusted to pH 1-12 before use.
11. The method of any of claims 7 to 10, wherein a solution is allowed to react with the material for at least 10 seconds before being removed and/or a next solution is added.
12. The method of any of claims 7-11, wherein at least one of the solutions is applied on the surface of the material by dipping said at least one surface of the material in said solution.
13. The method of any of claims 7-12, wherein at least one of the solutions is applied on the surface of the material by spraying said solution onto said surface of the material.
14. The method of any of claims 7-13, further comprising a drying step after applying one or more ofthe solutions on the surface.
15. Method of preparing a flame retardant material, comprising mixing the flame retardant composition of any of claims 1-5 with a material.
16. A substrate provided with a flame retardant surface coating on at least a surface thereof, wherein the flame retardant surface coating comprises inositol polyphosphate, having 4-6 phosphates, complexed with amino acids and metal ions.
17. A flame retardant material comprising a material mixed with a flame retardant composition comprising inositol polyphosphate, having 4-6 phosphates, complexed with amino acids and metal ions.
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