Modifier

Abstract

The present invention relates to a timber or wood treatment composition comprising a flame retardant and a crosslinking or fixing agent, or both, whereby the composition is boron and halogen free.

Description

[Technical Field]

[0001] The present invention relates to the field of modified wood, in particular timber treated with fire retardants. [Background technology]

[0002] Fire resistance plays a vital role in the use of timber and wood products, for example in the construction area, especially in buildings and public places, such as stations and airports. Summary of the Invention [Problem to be solved by the invention]

[0003] While flame retardants are largely known, there is a constant need for new alternative compositions, their uses, and application methods, especially compositions that avoid borates and / or halogens, avoid the use of additional catalysts if possible, and exhibit high resistance to leaching when exposed to the outdoors. [Means for solving the problem]

[0004] This object is solved by the composition according to claim 1 of the present invention.

[0005] Therefore, a) flame retardants containing the moiety -NC(=X)-N-, where X is O, S and substituted or unsubstituted nitrogen; and There is provided a boron- and halogen-free treatment composition for timber and / or wood and / or wood-based composites, comprising at least one of components b) a crosslinking agent, or c) a fixative.

[0006] Surprisingly, it has been found that by using such compositions for the modification of timber and / or wood, one or more of the following advantages can be achieved in most applications within the present invention: the composition can be easily applied to timber and / or wood, meaning solid wood, and, as will be shown later, to wood-based composites; The composition avoids the use of polluting and hazardous materials, The compositions not only increase the fire resistance of the treated timber or wood, but also typically reduce moisture absorption, improve biological durability, dimensional stability, and surface hardness; the compositions can be used in timber products, such as solid wood, fiberboard, particleboard, plywood, as well as veneer-based or lamella-based composites and other composites; The composition is chemically stable and can be applied to wood in one step. [Brief explanation of the drawings]

[0007] [Figure 1] FIG. 1 shows a diagram illustrating the maximum weight loss of two inventive samples and two comparative samples.

[0008] [Figure 2] FIG. 2 shows a diagram illustrating the burning rate of the test specimen of FIG.

[0009] [Figure 3] FIG. 3 shows a diagram illustrating the burn times of the test specimens of FIG.

[0010] [Figure 4] FIG. 4 shows a diagram illustrating the glow time of the test specimen of FIG.

[0011] [Figure 5] FIG. 5 shows a diagram illustrating the maximum swelling ratio of one inventive sample and four comparative samples.

[0012] [Figure 6] FIG. 6 shows a diagram illustrating the anti-swelling efficiency (ASE) of the samples of FIG.

[0013] [Figure 7] FIG. 7 shows a diagram illustrating water vapor absorption (W24100%RH), water vapor release (W240%RH), and liquid absorption (W24submerged) of the sample of FIG.

[0014] [Figure 8] FIG. 8 shows a diagram illustrating the maximum weight loss for three inventive samples and one comparative sample.

[0015] [Figure 9] FIG. 9 shows a diagram illustrating the burning rates of the samples of FIG.

[0016] [Figure 10] FIG. 10 shows a diagram illustrating the burn times of three inventive samples.

[0017] [Figure 11] FIG. 11 shows a diagram illustrating the glow time of the sample of FIG.

[0018] [Figure 12] FIG. 12 shows a diagram showing the WPG of one inventive sample and one comparative sample.

[0019] [Figure 13] FIG. 13 shows a diagram illustrating the maximum weight loss of one inventive sample and two comparative samples.

[0020] [Figure 14] FIG. 14 shows a diagram illustrating the burn rates of one inventive sample and two comparative samples. DETAILED DESCRIPTION OF THE INVENTION

[0021] The term "[X]-free" in the sense of the present invention means and / or includes a content of [X] in the composition of <0.1 wt% (wt / wt of total composition), more preferred <0.01 wt%, and most preferred <0.001 wt%, in particular when applied to timber or wood. It is an advantage of the compositions according to the invention that flame retardancy is provided to wood-containing substrates, even though the compositions according to the invention are halogen- and / or boron-free.

[0022] Halogen means a halogen-containing compound or halogen or halide. Halogen includes fluorine, chlorine, bromine, and / or iodine. Halide includes fluoride, chloride, bromide, and / or iodide.

[0023] The term "treatment composition" in the sense of the present invention means and / or includes in particular that, after application, the composition penetrates at least part of the timber and, in the best case, completely / sufficiently penetrates the timber and / or wood to be treated; this will be explained in more detail below.

[0024] The term "timber and / or wood" in the sense of the present invention means and / or includes in particular both solid wood and wood-based composite materials, which may be fiber-based, particle-based or veneer-based or lamella-based.

[0025] The term "timber" as used within the context of the present application should be understood to include in particular applications in which the wood has already undergone some kind of physical or chemical treatment, such as a drying procedure, a sawing procedure, a pressing procedure, etc.

[0026] The term "wood" as used within the context of the present application includes and / or encompasses compounds that contain or consist essentially of cellulose and hemicellulose, and lignin, among others. Thus, the term "wood" includes fresh wood, reclaimed wood, etc.

[0027] The compositions according to the invention have the advantage of increasing the durability, dimensional stability and surface hardness of timber and / or wood, and therefore preferred sources of timber and / or wood are selected from the sapwood of Pinus sylvestris L, Pinus radiata D. Don, European beech L, Populus spp. L and Alnus spp. L.

[0028] The term "consisting essentially of" in the sense of the present invention means in particular (whenever applicable wt / wt) >90%, preferably >95%, more preferably >97% and most preferably >99%.

[0029] In the following, the components of the compounds of the invention are described in more detail, whereby the individual combinations and preferred embodiments can be freely combined:

[0030] a) Flame retardants containing the moiety -NC(=X)-N- As is well known in the art, the term "flame retardant" means and / or includes substances used to reduce or stop the ignition, spread of fire, or strength of wood, among other things.

[0031] Preferably, the flame retardant consists essentially of a compound containing the moiety -NC(=X)-N-, where X is O, S, and substituted or unsubstituted nitrogen.

[0032] X can include a substituted nitrogen, preferably nitrogen substituted with hydrogen, C1-C6 linear or branched or cycloalkyl, or C1-C6 linear or branched or cycloaryl.

[0033] Preferably, X denotes O, NH or N(phenyl).

[0034] Preferably, the flame retardant comprises a urea and / or guanidine moiety. If urea or guanidine is not present in the flame retardant as a compound, alkyl- or aryl-substituted urea or guanidine is particularly preferred. The substituents of the substituted urea and / or guanidine moiety are selected from C1-C6 linear, branched, or cycloalkyl, or C1-C6 linear, branched, or cycloaryl. C6-cycloaryl (phenyl) is particularly preferred as a substituent.

[0035] The flame retardant may be present in the composition according to the present invention as a salt. When the flame retardant is designed as a salt, the -NC(=X)-N- moiety carries one or more positive charges, i.e., the -NC(=X)-N- moiety forms a cation. A suitable anion for balancing the positive charge of the -NC(=X)-N- moiety may be selected from carbonate and / or phosphate, with phosphate being most preferred. The term "carbonate" as used within the context of this application refers to a compound having the chemical formula HCO3 - and CO3 2- The term "phosphate" as used within the context of this application refers to the anion of the chemical formula H2PO4 - , HPO4 2- , and PO4 3- where HPO4 2- and H2PO4 3- Particularly preferred flame retardants designed as salts are urea, guanidine and phenylguanidine salts, in particular salts consisting of one or more guanidine and / or phenylguanidine cations and one or more anions selected from carbonates and phosphates.

[0036] Preferred flame retardants are urea, guanidine and phenylguanidine salts, more preferably guanidine and phenylguanidine carbonates and phosphates.

[0037] Particularly preferred are flame retardants according to the following formulae (a) to (c) or mixtures thereof: [ka]

[0038] According to a preferred embodiment of the present invention, the flame retardant may further comprise a phosphate compound.

[0039] The term "phosphate compound" means and / or includes in particular any compound in which a phosphorescent substance (V) with four oxygens attached is present. Thus, the term "phosphate compound" means and / or includes in particular phosphate anion, phosphate esters, polyphosphoric acids and their esters, and phosphoric acid.

[0040] In many applications, this has been shown to further enhance the flame retardancy of the compositions of the present invention.

[0041] It is an advantage of the compositions according to the invention that the combination of at least one crosslinking agent and / or fixative according to formula (I) with at least one flame retardant to provide flame retardancy to wood-containing substrates treated with the compositions according to the invention, wherein the flame retardancy is only minimally maintained or reduced even after the wood-containing substrate treated with the compositions according to the invention is treated with water.

[0042] b) Crosslinking agent The compositions of the present invention may contain a crosslinking agent. The term "crosslinking agent" means and / or includes compounds that react with hydroxyl groups from the wood and / or cellulose and hemicellulose of the wood, in particular under high temperature, and / or bring about polymerization in the wood through condensation reactions of reactive hydroxymethyl groups.

[0043] According to one embodiment of the present invention, the crosslinker comprises, and preferably consists essentially of, a 2-imidazolidone moiety, particularly the following structure (I): [ka] [In structure, R 1 and R 2 are independently OH and OR 5 where R 5 (independently for each residue) is C1-C5 alkyl (especially methyl), -CH2O-C n H 2n -OH and -CHO-C n H 2n -OC m H2m OH (wherein n and m are independently 2 or 3, preferably 2); R 3 and R 4 are independently hydrogen, R 5 (independently for all residues), -CH2OR 5 (independently for all residues) and CH2OH] are preferred.

[0044] Preferably, R 1 , R 2 , R 3 or R 4 At least two of are or contain terminal OH moieties.

[0045] Preferably, R 1 and R 2 are identical, and in particular, R 1 and R 2 is preferably OH. Preferably, R 3 and R 4 are identical.

[0046] The term "alkyl" encompasses straight chain alkyl as well as branched alkyl moieties. R 1 means OH and / or R 2 means OH and / or R 3 means H, CH, CHOH, CHOMe, CHOCHOCHOH, and / or R 4 means H, CH, CHOH, CHOMe, CHOCHOCHOH, preferably R 1 OH and / or R 2 means OH and / or R 3 means H, CH, CHOH, CHOMe, and / or R 4 means H, CH3, CH2OH, and CHOMe.

[0047] Particularly preferred are crosslinkers according to the following formulae (II) to (IX) or mixtures thereof: [ka]

[0048] According to a preferred embodiment, the ratio of flame retardant to crosslinker (wt / wt) (whereby, if several crosslinkers and / or flame retardants are present, this relates to the total weight) is ≧0.05:1 to ≦10:1, preferably ≧0.2:1 to ≦2:1, which has been shown to be advantageous for many applications within the present invention.

[0049] The crosslinker according to formula (II) is also called DMeDHEU (1,3-bis-methyl-4,5-dihydroxyimidazolidin-2-one). The crosslinker according to formula (III) is also called DMDHEU (1,3-bis-(hydroxymethyl)-4,5-dihydroxyimidazolidin-2-one).

[0050] Particularly preferred compositions according to the present invention comprise or consist of a crosslinker (DMDHEU) according to formula (II) and a monoguanidine phosphate salt as flame retardant, or a crosslinker (DMeDHEU) according to formula (III) and a monoguanidine phosphate salt as flame retardant, or a crosslinker (DMeDHEU) according to formula (IV) and a monoguanidine phosphate salt as flame retardant, or a crosslinker (DMeDHEU) according to formula (V) and a monoguanidine phosphate salt as flame retardant, or a crosslinker according to formula (II) and a phenyl-based guanidine flame retardant of formula (c).

[0051] Suitable weight ratio ranges of flame retardant to crosslinker according to formula (I) in the composition according to the invention are: at most 1:20, or at most 1:18, or at most 1:16, or at most 1:14, or at most 1:12, or at most 1:10, or at most 1:8, or at most 1:6, or at most 1:5, or at most 1:4, and / or at least 1:0.1 or at least 1:0.2 or at least 1:0.4 or at least 1:0.5 or at least 1:0.7 or at least 1:0.8 or at least 1:0.9 or at least 1:1 or at least 1:1.2 or at least 1:1.4 or at least 1:1.6 or at least 1:1.8 or at least 1:2 or at least 1:2.2 or at least 1:2.4 or at least 1:2.6 or at least 1:2.8 or at least 1:3. Suitable weight ratio ranges of flame retardant to crosslinker according to formula (I) in the composition according to the invention are 1:20 to 1:0.1, or 1:15 to 1:0.5, or 1:10 to 1:1, or 1:5 to 1:1.5, or 1:4 to 1:2.

[0052] c) Fixative The compositions of the present invention may include a fixative.

[0053] The term "fixative" as used within the context of the present application means and / or includes compounds that can contribute to protecting the flame retardant in wood-containing substrates treated with the composition according to the invention from leaching, in particular by preferably forming larger complexes and / or neutralizing the positive or negative charge of the flame retardant, reducing the water solubility of the flame retardant.

[0054] According to a further embodiment of the present invention, the fixative comprises a polyamine, preferably consisting essentially of a polyamine, and a cyanoguanidine-diethylenetriamine-containing polymer, particularly a cyanoguanidine-diethylenetriamine-epichlorohydrin polymer, is particularly preferred. Without being bound by theory, the inventors believe that the fixative properties of these compounds may result from complex formation, at least when the flame retardant is negatively charged, similar to the complex described by Yu et al., Modern Applied Science, 2009, Vol. 10, No. 3, 9-16.

[0055] The fixative is preferably used in an amount of at least 1% by weight and up to 10% by weight, or at least 3% by weight and up to 8% by weight, or at least 4% by weight and up to 7% by weight, where the weight percentages are based on the dry weight of the composition according to the invention.

[0056] A particularly preferred composition according to the invention comprises or consists of cyanoguanidine-diethylenetriamine-epichlorohydrin as fixative and a mixture of potassium dihydrogen phosphate and urea (in a 1:1 ratio) as flame retardant.

[0057] According to a preferred embodiment of the present invention, the composition comprises all compounds a) to c).

[0058] According to one embodiment, the composition further comprises a catalyst capable of catalyzing the crosslinking reaction and therefore the interaction of the crosslinking agent with the timber and / or wood, and the condensation reaction of the crosslinking agent itself, which is intended in particular to increase the reactivity of the crosslinking agent, so that it is possible to cure the crosslinker in the wood at low / moderate temperatures (preferably below 130°C).

[0059] Preferred catalysts are selected from the group comprising metal salts from the group consisting of metal sulfates, metal nitrates, metal phosphates or mixtures thereof, examples being magnesium nitrate, magnesium sulfate, aluminum sulfate, zinc nitrate, copper nitrate or mixtures thereof.

[0060] Suitable and hitherto preferred catalysts are also ammonium salts from the group consisting of ammonium sulfate, ammonium oxalate, diammonium phosphate or mixtures thereof.

[0061] Further suitable and hitherto preferred catalysts are organic or inorganic acids. Suitable examples are maleic acid, formic acid, citric acid, tartaric acid, oxalic acid, p-toluenesulfonic acid, sulfuric acid, nitric acid or mixtures thereof.

[0062] Magnesium nitrate is particularly preferred.

[0063] The at least one catalyst is present in the composition according to the invention in an amount of at least 2% by weight up to 10% by weight, or at least 2% by weight up to 7% by weight, or at least 2% by weight up to 5% by weight, where the weight percentages are based on the dry weight of the composition according to the invention.

[0064] However, according to another embodiment of the present invention, the composition does not include a catalyst.

[0065] The composition according to the present invention may further comprise a solvent, which is capable of dissolving the components of the composition according to the present invention, in particular at least one crosslinking agent and / or at least one flame retardant. A particularly preferred solvent is water. The term "water" as used in the context of this application refers to tap water as well as deionized water.

[0066] It is particularly preferred that the composition according to the invention is designed as an aqueous solution, ie at least one crosslinking agent and at least one flame retardant are dissolved in water, thus forming the composition according to the invention.

[0067] When the composition according to the invention is designed as a solution, the total amount of the at least one crosslinking agent and the at least one flame retardant is at least 0.5 g, or at least 5 g, or at least 8 g, or at least 10 g, or at least 12 g, or at least 15 g, or at least 18 g, or at least 20 g, or at least 25 g, and / or at most 30 g, or at most 35 g, or at most 40 g, or at most 45 g, or at most 50 g, or at most 55 g, or at most 60 g, or at most 65 g, or at most 70 g, or at most 75 g, or at most 80 g per 100 ml of solvent, in particular per 100 ml of water. Particularly preferred is a total amount of the at least one crosslinking agent and the at least one flame retardant of 0.5 g to 80 g, or 5 g to 70 g, or 10 g to 60 g, or 15 g to 45 g, or 20 g to 40 g per 100 ml of solvent, in particular per 100 ml of water.

[0068] The present invention further relates to the use of the compositions of the present invention as timber and / or wood treatment agents.

[0069] The present invention further relates to timber and / or wood composites, whereby the timber and / or wood is at least partially impregnated with the composition of the present invention. Preferably, the timber and / or wood is completely impregnated.

[0070] The present invention further relates to a method for applying the composition of the present invention to timber and / or wood to be treated, said method comprising the following steps: a) optionally pre-drying the timber and / or wood to be treated; b) impregnating the timber and / or wood to be treated with an aqueous solution of the composition at high pressure; and drying the impregnated timber and / or wood.

[0071] The steps of this method are described in further detail, whereby the process conditions, in particular the applied pressure during impregnation and the temperature during the drying step, vary greatly depending on the shape and dimensions of the raw material (solid wood, veneer, particles, fibers) and the type of wood being treated. The individual combinations and preferred embodiments can be freely combined.

[0072] a) Optional Pre-drying Step In step a) the timber and / or wood is optionally pre-dried to enhance its absorption capacity for the composition of the invention.

[0073] Preferably, step a) is carried out at a pressure of ≧20 mbar to ≦100 mbar, preferably step a) is carried out at room temperature or at a temperature of ≧20°C to ≦140°C.

[0074] Alternatively, step a) is carried out at atmospheric pressure and at a temperature of from 20° C. to 140° C., preferably from 50° C. to 90° C. This has been shown to be advantageous especially for large timber and / or wood chips.

[0075] Preferably, step a) is carried out when the moisture content of the wood is in the range of ≧0% to ≦25%.

[0076] b) Impregnation process When step a) is carried out, step b) preferably follows step a) immediately, whereby "immediately" in particular means and / or includes a delay of not more than 30 minutes, preferably not more than 10 minutes.

[0077] If the timber and / or wood has a temperature higher than ambient temperature after undergoing the pre-drying step a), the timber and / or wood can be cooled to ambient temperature before being subjected to the treatment step b).

[0078] In step b), an aqueous solution of the composition of the present invention is used. Preferably, the content of the composition of the present invention (in grams per 100 ml of water before addition) is ≧0.5 g to ≦80 g, more preferably ≧15 g to ≦45 g, and most preferably ≧20 g to ≦40 g.

[0079] Step b) is preferably carried out at a pressure of ≧6 bar to ≦20 bar, preferably ≧8 bar to ≦14 bar, and most preferably ≧10 bar to ≦12 bar.

[0080] c) Drying process Step c) preferably follows step b), preferably immediately after step b), during which curing of the crosslinking agent, if present, preferably also takes place simultaneously.

[0081] Preferably, step c) comprises at least two drying steps carried out at different temperatures with the temperature increasing from each step to the other.

[0082] Preferably, step c) comprises a first drying step c1) in which drying is carried out at room temperature or at a temperature between 20° C. and 140° C. for a period of 12 to 504 hours, preferably between 24 and 272 hours, and most preferably between 72 and 168 hours. This step preferably follows step b) immediately.

[0083] Preferably, step c) comprises a second drying step c2) in which drying is carried out at a temperature of 100°C to 180°C, preferably 140°C or less, for 24 to 216 hours, preferably 48 to 168 hours. In many applications of the present application, this drying step c2) also indicates that curing of the crosslinker and reactive moieties in the flame retardant solution occurs simultaneously. Preferably, step c2) follows, preferably immediately after step c1).

[0084] Preferably, the temperature in drying step c2) is higher than the temperature in drying step c1).

[0085] According to one embodiment of the present invention, step c) may comprise a series of drying steps, whereby each drying step has an independent duration of 6 hours to 24 hours and the temperature increase from each drying step to the next is independently 10°C to 30°C.

[0086] The components described above, as well as the components claimed and used in accordance with the present invention in the described embodiments, are free from special exceptions with respect to size, shape, material selection, and technical concept, so that selection criteria known in the relevant field can be applied without limitation.

[0087] Additional details, features, and advantages of the subject matter of the present invention are disclosed in the subclaims, and the following description of the respective figures shows, in an exemplary manner, preferred embodiments according to the present invention. However, such embodiments do not necessarily represent the full scope of the invention, and therefore, reference is made to the claims and the present specification to interpret the scope of the invention. It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are intended to provide further explanation of the invention as claimed. [Example]

[0088] The present invention is further illustrated by the following examples, which are illustrative only and non-binding.

[0089] Example I: In Example I, an impregnation solution containing 20 g of DMDHEU and 10 g of monoguanidine phosphate per 100 ml of water was used. Oven-dried (0% MC) samples of Scots pine sapwood (Pinus sylvestris L.) were impregnated with the impregnation solution using a vacuum pressure impregnation process with 50 mbar vacuum for 1 hour followed by 12 bar overpressure for 1 hour. The fully impregnated samples were first dried at 25°C for 110 hours and then dried and cured in a drying oven at 120°C for 48 hours.

[0090] Example II: In Example II, an impregnation solution containing 9 g of a 1:1 mixture of potassium dihydrogen phosphate and urea and 19 g of cyanoguanidine-diethylenetriamine-epichlorohydrin polymer was used. Oven-dried (0% MC) samples of Scots pine sapwood (Pinus sylvestris L.) were impregnated with the impregnation solution using a vacuum pressure impregnation process with 50 mbar vacuum for 1 hour followed by 12 bar overpressure for 1 hour. The fully impregnated samples were pre-dried at 25°C for 12 hours. The samples were then dried at increasing temperatures (12-hour intervals) at 40°C, 60°C, 80°C, and 103°C, followed by curing in a drying oven at 130°C for 5 hours.

[0091] Example III: In Example III, an impregnation solution containing 20 g DMDHEU and 5 g monoguanidine phosphate per 100 ml water was used. The treatment method was the same as in Example I.

[0092] Example IV: In Example IV, an impregnation solution containing 20 g of methylolated DMDHEU and 5 g of monoguanidine phosphate per 100 ml of water was used. The treatment method was the same as in Example I.

[0093] Example V: In Example V, an impregnation solution containing 20 g of DMeDHEU and 5 g of monoguanidine phosphate per 100 ml of water was used. The treatment method was the same as in Example I.

[0094] Comparative Example: The following were used as comparative examples: -Untreated timber -Sodium polyborate impregnated timber - Timber impregnated with monoguanidinium phosphate - Timber impregnated with DMDHEU crosslinking agent Wood impregnated with an impregnation solution containing 20 g of DMDHEU and 5 g of diammonium phosphate (as flame retardant) per 100 ml of water (Comparative Example I). Impregnation and drying, if applicable, were carried out in the same manner as in Example I.

[0095] Leaching test The attribute "leached" indicates all samples that were subjected to a 14 day cold water leaching procedure according to European Norm EN 84 (1997) before being tested for their respective material properties.

[0096] Combustion test All samples were subjected to the "Bunsen burner combustion test". After treatment with the impregnation solution as described above, the samples were 13x4x125 (ax.) mm 3 The dried and cured samples were conditioned at 20°C and 65% RH before testing. One end of the specimen was clamped in a holder at a 45° angle. The specimen plus holder was placed on a balance so that the specimen was hanging next to it. Before clamping the specimen, the balance was broken and the mass of the conditioned sample was reduced to 10 -3 The moisture content was measured in grams. Based on this starting weight of the specimen, the moisture content was calculated based on the original dry weight of the wood before treatment. The tip of the specimen was ignited by a Bunsen burner while it was exposed to a flame for 30 seconds. The intensity and height of the Bunsen burner flame were always the same for all specimens. The weight of the specimen was recorded at 10-second intervals and simultaneously evaluated as to whether the specimen was burning or glowing. The mass loss of the specimen was related to the original oven-dry weight (pure wood substrate without chemicals) before treatment. The parameters calculated to evaluate the fire resistance of each treated wood were maximum mass loss, maximum mass loss per 10-second interval (burn rate), burn time, and glow time. Tests were performed on n = 10 specimens per treatment group.

[0097] Swelling and shrinkage test (dimensional stability) 25x25x10(ax.)mm 3After treatment with crosslinkers and / or flame retardants, specimens were oven-dried at 103°C to a constant mass (0% MC). The oven-dried weight and dimensions were measured. The samples were then saturated with demineralized water by applying a vacuum of 100 mbar for 30 minutes and then stored in demineralized water for 24 hours. The dimensions were then measured at maximum swelling. Based on the maximum swelling rate, the anti-swelling efficiency (ASE, %) was calculated by comparing the swelling rate of the modified wood with that of untreated wood. To consider the long-term effects of each treatment on wood swelling and shrinkage, specimens were re-dried to oven-dried conditions and the described ASE cycle was repeated four times. The decrease in ASE value with increasing cycles indicates the effect of chemical leaching due to minor fixation.

[0098] Water vapor uptake and release Short-term water absorption and release tests were carried out on 5x10x100(ax.)mm 3 The test was carried out over a 24-hour period using 10 test pieces. Each test piece was dried in an oven and -3 The samples were weighed in grams and stored at 25°C and 100% RH for 24 hours. 100%RH The water vapor release (W24 [%)) during the 24-hour exposure was calculated. The samples were stored for an additional 14 days at 100% RH and reweighed at near fiber saturation. The specimens were then directly exposed to freshly activated silica gel and reweighed after 24 hours. 0%RH The specimens were again oven-dried at 103°C until a constant mass was reached, and the tensile strength (%) was calculated. -3 The samples were weighed in grams and immersed in demineralized water at 25°C and 65% ambient atmosphere. After 24 hours, the samples in water were reweighed and the liquid water uptake [W24 submered ] was calculated.

[0099] result Figure 1 shows a diagram illustrating the maximum weight loss of two inventive and two comparative samples tested both before and after leaching according to EN84 (1997), and Figures 2-4 show the burn rate, burn time, and glow time of the samples in Figure 1. As can be seen, the inventive samples exhibit increased flame retardant behavior.

[0100] Figure 5 shows the maximum swelling ratio of one inventive sample and four comparative samples, based on which the anti-swelling efficiency (ASE) of the samples previously leached according to EN 87 (1997) shown in Figure 6 was calculated. Figure 7 shows the water vapor uptake (W24) of the specimens of Figure 5 tested without leaching according to EN 84 (1997). 100%RH ), water vapor release (W24 0%RH ), and liquid water uptake (W24 submerged ) The improved effect of the sample of the present invention can be clearly observed.

[0101] Figure 8 shows the maximum weight loss and Figure 9 shows the burn rate of three inventive samples and one comparative sample tested without leaching according to EN84 (1997). Figure 10 shows the burn time and Figure 11 shows the glow time of three inventive samples without leaching. Again, the improved fire resistance is clearly visible in Figures 8-11.

[0102] Figures 12-14 show the WPG (weight percent gain), maximum weight loss, and burn rate for Inventive Example III, Comparative Example I, and the untreated control. Again, the improved fire resistance is clearly visible in Figures 12-14.

[0103] The particular combinations of elements and features in the above detailed embodiments are merely exemplary; interchangeability and substitution of these teachings with other teachings therein, and patents / applications incorporated by reference, are also expressly contemplated. As those skilled in the art will recognize, variations, modifications, and other implementations of what is described herein may occur to those skilled in the art without departing from the spirit and scope of the invention as claimed. Accordingly, the foregoing description is merely exemplary and is not intended to be limiting. In the claims, the word "comprising" does not exclude other elements or steps, and the indefinite articles "a" or "an" do not exclude a plurality. The mere fact that certain measures are recited in mutually different dependent claims does not indicate that a combination of these measures cannot be advantageously used. The scope of the invention is defined in the following claims and their equivalents. Furthermore, reference signs used in the description and claims do not limit the scope of the invention as claimed.

Claims

1. 1. A boron- and halogen-free and catalyst-free treatment composition for timber and / or wood, comprising: a) a flame retardant comprising the moiety -N-C(=X)-N-, where X is O, S, or substituted or unsubstituted nitrogen, wherein said flame retardant is a salt, said moiety -N-C(=X)-N- carries one or more positive charges, and anions to balance the positive charges of said moiety -N-C(=X)-N- are selected from carbonate and / or phosphate; and b) a crosslinker containing a 2-imidazolidone moiety; A composition comprising:

2. The crosslinker may have the following structure: 【Chemical 1】 [In structure, R １ and R ２ are each independently OH or OR ５ where R ５ (independently for all residues) is C １ -C ５ Alkyl, —CH ２ O-C ｎ H ２ｎ -OH or -CH ２ O-C ｎ H ２ｎ -O-C ｍ H ２ｍ OH (wherein n and m are independently 2 or 3); R ３ and R ４ are each independently hydrogen, R ５ (independently for every residue), —CH ２ OR ５ (independently for all residues) or CH ２ The composition of claim 1, comprising a compound represented by the formula:

3. The composition of claim 2, wherein R 5 is methyl and n is 2.

4. The composition of any one of claims 1 to 3, wherein the flame retardant comprises a urea and / or a guanidine moiety.

5. The composition according to any one of claims 1 to 4, wherein the flame retardant is selected from the group consisting of urea, guanidine, and phenylguanidine salts.

6. The composition of any one of claims 1 to 5, wherein the flame retardant comprises a phosphate.

7. 7. The composition according to any one of claims 1 to 6, wherein the ratio of flame retardant to crosslinker (wt / wt) (which relates to the total weight if several crosslinkers and / or flame retardants are present) is ≧0.05:1 to ≦10:

1.

8. Use of a composition according to any one of claims 1 to 7 as a treatment agent for timber and / or wood and / or wood-based products.

9. A timber and / or wood composite material, at least a portion of which is impregnated with a composition according to any one of claims 1 to 7.

10. 10. A method for applying a composition according to any one of claims 1 to 7 to timber and / or wood and / or wood-based products to be treated, comprising the following steps: a) optionally pre-drying the timber and / or wood to be treated; b) impregnating the timber and / or wood to be treated with an aqueous solution of the composition at high pressure; c) drying the impregnated timber and / or wood.

11. The method according to claim 10, wherein the content of the composition in step b) (g per 100 ml of water before addition) is 0.5 g to 80 g.

12. 12. The method according to claim 10 or 11, wherein step c) comprises at least two drying steps carried out at different temperatures, the temperature increasing from each step to the other.

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