Modifier

Abstract

To provide a treatment composition for lumber or wood that contains a flame retardant and a cross-linking agent or fixative, or both.SOLUTION: The composition of the present invention contains no boron or halogen.SELECTED DRAWING: Figure 1

Description

Technical Field

[0001] The present invention relates to the field of modified materials, in particular wood treated with flame retardants.

Background Art

[0002] Fire resistance plays a very important role in the use of wood and wood products, for example in construction areas, especially in buildings and public places such as stations and airports.

Summary of the Invention

Problems to be Solved by the Invention

[0003] Although flame retardants are mainly known, there is always a need for new alternative compositions, their methods of use, and application methods, in particular compositions that avoid borates and / or halogens and, if possible, the use of further catalysts and show high resistance to leaching when exposed outdoors.

Means for Solving the Problems

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

[0005] Therefore, a) a flame retardant containing partial - N - C(=X) - N - (where X is O, S and substituted or unsubstituted nitrogen); and There is provided a boron - and halogen - free treatment composition for wood and / or wood - based composite materials, comprising at least one of component b) a cross - linking agent or c) a fixing agent.

[0006] Surprisingly, it has been found that by using such a composition for the modification of wood 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 wood and / or wood, which means solid wood, and wood - based composite materials, as shown later. - The composition avoids the use of pollutants and hazardous substances. - The composition not only enhances the fire resistance of processed lumber or wood, but also usually reduces the hygroscopicity, improves the biological durability, dimensional stability, and surface hardness, - The composition can be used for wood products, such as solid wood, fiberboard, particleboard, plywood, and further veneer-based or lamella-based composites, and other composites, - The composition is chemically stable and can be applied to wood in one step.

Brief Description of the Drawings

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DETAILED DESCRIPTION OF THE INVENTION

[0021] The term "[X]-free" in the context of the present invention means, in particular when applied to lumber or wood, that the content of [X] in the composition is <0.1 wt% (wt / wt of the total composition), more preferably <0.01 wt%, and most preferably <0.001 wt%, and / or contains. The compositions according to the invention are halogen-free and / or boron-free, and the fact that they provide flame retardancy to wood-containing substrates is an advantage of the compositions according to the invention.

[0022] "Halogen" means a halogen-containing compound, or halogen, or halide. Halogens include fluorine, chlorine, bromine, and / or iodine. Halides include fluorides, chlorides, bromides, and / or iodides.

[0023] The term "treatment composition" in the context of the present invention particularly means that, after application, the composition penetrates at least a part of the sawn timber and, optimally, completely / sufficiently penetrates the sawn timber and / or wood to be treated, and / or contains; this will be explained in detail later.

[0024] The term "sawn timber and / or wood" in the context of the present invention particularly means and / or includes both solid wood and wood-based composite materials that can be fiber-based, particle-based, veneer-based, or lamella-based.

[0025] The term "sawn timber" used within the context of this application should be understood to particularly include applications where the wood has already undergone certain physical or chemical treatments such as drying procedures, sawing procedures, pressing procedures, etc.

[0026] The term "wood" used within the context of this application particularly includes or consists essentially of compounds containing cellulose, hemicellulose, and lignin, and / or encompasses them. Thus, the term "wood" includes fresh wood, recycled wood, etc.

[0027] The composition according to the present invention has the advantage of enhancing the durability, dimensional stability, and surface hardness of sawn timber and / or wood. Thus, preferred sources of sawn 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 context of the present invention means, in particular (whenever applicable, wt / wt) > 90%, preferably > 95%, more preferably > 97%, and most preferably > 99%.

[0029] The components of the compounds of the present invention are described in more detail below, such that each combination and preferred embodiment can be freely combined:

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

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

[0032] X is substituted nitrogen, preferably hydrogen, C 1 -C 6 linear or branched or cycloalkyl, or C 1 -C 6 and may contain nitrogen substituted with linear or branched or cycloaryl of C

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

[0034] Preferably, the flame retardant contains a urea and / or guanidine moiety. If urea or guanidine does not exist as a compound in the flame retardant, alkyl or aryl substituted urea or guanidine is particularly preferred. The substituents of the substituted urea and / or guanidine moiety are selected from linear or branched or cycloalkyl of C 1 -C 6 linear or branched or cycloaryl of C 1 -C 6 linear or branched or cycloaryl of C 6 -cycloaryl (phenyl) is particularly preferred as a substituent.

[0035] The flame retardant can be present as a salt in the composition according to the invention. When the flame retardant is designed as a salt, the -N-C(=X)-N- moiety bears one or more positive charges, i.e., the -N-C(=X)-N- moiety forms a cation. Suitable anions for balancing the positive charge of the -N-C(=X)-N- moiety can be selected from carbonates and / or phosphates, with phosphates being most preferred. The term "carbonate" as used within the context of this application refers to the anions of the chemical formulas HCO 3 - and CO 3 2- The term "phosphate" as used within the context of this application refers to the anions of the chemical formulas H 2 PO 4 - HPO 4 2- and PO 4 3- wherein HPO 4 2- and H 2 PO 4 3- are most preferred. Particularly preferred flame retardants designed as salts are salts consisting of urea, guanidine and phenylguanidine salts, in particular 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 carbonates and phosphates of guanidine and phenylguanidine.

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

Chemical formula

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

[0039] The term "phosphate compound" means, in particular, any compound in which there is a phosphorus(V) substance to which four oxygens are bonded and / or which contains them. Thus, the term "phosphate compound" means, in particular, and / or contains phosphate anions, 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] A combination of at least one crosslinking agent and / or fixing agent according to formula (I) and at least one flame retardant for providing flame retardancy to a wood-containing substrate treated with the composition according to the present invention is an advantage of the composition according to the present invention, wherein the flame retardancy is minimally maintained or reduced even after the wood-containing substrate treated with the composition according to the present invention is treated with water.

[0042] b) Crosslinking agent The composition of the present invention may contain a crosslinking agent. The term "crosslinking agent" means, in particular, and / or contains a compound that reacts with the hydroxyl groups from wood and / or the cellulose and hemicellulose of wood treated at high temperature and / or brings about polymerization in wood through the condensation reaction of reactive hydroxymethyl groups.

[0043] According to one embodiment of the present invention, the crosslinking agent contains a 2-imidazolidone moiety, preferably it consists essentially of it. In particular, the following structure (I):

Chemical formula

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

[0045] Preferably, R 1 and R 2 are the same, in particular, it is preferred that R 1 and R 2 are OH. Preferably, R 3 and R 4 are the same.

[0046] The term "alkyl" includes linear alkyl as well as branched alkyl moieties. R 1 means OH, and / or R 2 means OH, and / or R 3 is H, CH 3 , CH 2 OH, CH 2 OMe, CH 2 OC 2 H 4 OC 2 H 4 OH, and / or R 4 is H, CH 3 , CH 2 OH, CH 2 OMe, CH 2 OC 2 H 4 OC 2 H 4 OH, preferably R1 is OH and / or R 2 means OH, and / or R 3 is H, CH 3 , CH 2 OH, CH 2 means OMe, and / or R 4 is H, CH 3 , CH 2 OH, CH 2 means OMe.

[0047] Particularly preferred are crosslinking agents according to the following formulas (II) to (IX) or mixtures thereof:

Chemical formula

[0048] According to a preferred embodiment, the ratio (wt / wt) of the flame retardant to the crosslinking agent (which, when a plurality of crosslinking agents and / or flame retardants are present, relates to the total weight) is preferably ≧0.05:1 to ≦10:1, more preferably ≧0.2:1 to ≦2:1. This has been shown to be advantageous for many applications within the present invention.

[0049] The crosslinking agent according to formula (II) is also called DMeDHEU (1,3-bis-methyl-4,5-dihydroxyimidazolidin-2-one). The crosslinking agent 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 crosslinking agent according to formula (II) (DMDHEU) and monoguanidine phosphate as a flame retardant, or a crosslinking agent according to formula (III) and monoguanidine phosphate as a flame retardant, or a crosslinking agent according to formula (IV) (DMeDHEU) and monoguanidine phosphate as a flame retardant, or a crosslinking agent of formula (V) and monoguanidine phosphate as a flame retardant, or a crosslinking agent according to formula (II) and a phenyl-based guanidine flame retardant of formula (c).

[0051] Flame retardants in the composition according to the invention: The appropriate weight ratio range of the crosslinking agent according to formula (I) is as follows: maximum 1:20, or maximum 1:18, or maximum 1:16, or maximum 1:14, or maximum 1:12, or maximum 1:10, or maximum 1:8, or maximum 1:6, or maximum 1:5, or maximum 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. The appropriate weight ratio range of the flame retardant in the composition according to the invention to the crosslinking agent according to formula (I) is 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) Fixing agent The composition of the present invention may contain a fixing agent.

[0053] The term "fixing agent" as used within the context of the present application particularly preferably means and / or encompasses a compound that can contribute to protecting the flame retardant in a wood-containing substrate treated with the composition according to the invention from leaching by forming a larger complex and / or neutralizing the positive or negative charge of the flame retardant to reduce the water solubility of the flame retardant.

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

[0055] The fixing agent is preferably used in an amount of at least 1% by weight to a maximum of 10% by weight, or at least 3% by weight to a maximum of 8% by weight, or at least 4% by weight to a maximum of 7% by weight, where the weight % is based on the dry weight of the composition according to the present invention.

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

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

[0058] According to one embodiment, the composition further contains a catalyst that can catalyze the crosslinking reaction, thus the interaction between the crosslinking agent and the wood and / or wood, and the condensation reaction of the crosslinking agent itself. This is particularly for the purpose of enhancing the reactivity of the crosslinking agent, so that the crosslinking agent of the wood can be cured at low / medium temperatures (preferably below 130°C).

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

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

[0061] Even more suitable and heretofore 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] Particularly preferred is magnesium nitrate.

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

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

[0065] The composition according to the invention can further comprise a solvent which is capable of dissolving the components of the composition according to the invention, in particular at least one crosslinking agent and / or at least one flame retardant. Particularly preferred as the solvent is water. The term "water" as used within the context of the present 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, i.e. 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 at least one crosslinking agent and at least one flame retardant is as follows: per 100 mL of solvent, in particular per 100 mL of water, 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. Particularly preferred is that the total amount of at least one crosslinking agent and at least one flame retardant is 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 composition of the present invention as a treatment agent for lumber and / or wood.

[0069] The present invention further relates to lumber and / or wood composite materials, whereby at least a part of the lumber and / or wood is impregnated with the composition of the present invention. Preferably, the lumber and / or wood is completely impregnated.

[0070] The present invention further relates to an application method for applying the composition of the present invention to the lumber and / or wood to be treated, wherein the method comprises the following steps: a) Optionally, a step of pre-drying the lumber and / or wood to be treated, b) A step of impregnating the lumber and / or wood to be treated with an aqueous solution of the composition under high pressure, including a step of drying the impregnated lumber and / or wood.

[0071] The steps of this method are described in more detail, whereby the process conditions, in particular the application pressure during impregnation and the temperature during the drying process, are strong and vary depending on the shape and dimensions of the raw materials (solid wood, veneer, particles, fibers) and the type of wood being treated. Each combination and preferred embodiment can be freely combined.

[0072] a) Any preliminary drying step In step a), the sawn timber and / or wood is optionally pre-dried in order to enhance the absorption capacity of the composition of the present invention.

[0073] Preferably, step a) is carried out at a pressure of ≧20 mbar to ≦100 mbar, and 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 at a temperature of 20 °C or higher to 140 °C or lower, preferably 50 °C or higher to 90 °C or lower. This has been shown to be particularly advantageous for large sawn timber and / or wood chips.

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

[0076] b) Impregnation step When step a) is carried out, step b) preferably follows immediately after step a), whereby "immediately" particularly means a delay of 30 minutes or less, preferably 10 minutes or less, and / or includes such a delay.

[0077] If the sawn timber and / or wood has a temperature higher than the ambient temperature after undergoing the preliminary drying step a), the sawn timber and / or wood can be cooled to the 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 g per 100 ml of water before addition) is ≧0.5 g to ≦80 g, 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 step Step c) preferably follows step b), preferably immediately after step b). When a crosslinking agent is present, during this step, preferably, the curing of the crosslinking agent is also carried out simultaneously.

[0081] Preferably, step c) includes at least two drying steps carried out at different temperatures with a temperature rising from each step to the next step.

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

[0083] Preferably, step c) includes 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 hours to 216 hours, preferably 48 hours to 168 hours. In many applications of the present application, it has been shown that in this drying step c2), the curing of the crosslinking agent and the reactive moiety in the flame retardant solution also occurs simultaneously. Preferably, step c2) follows, preferably immediately after step c1).

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

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

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

[0087] Additional details, features, and advantages of the objects of the present invention are disclosed in the subclaims, and the following description of each figure shows, in an illustrative manner, preferred embodiments according to the present invention. However, such embodiments do not necessarily represent the entire scope of the present invention, and thus, for the purpose of interpreting the scope of the present invention, reference is made to the claims and this specification. It should be understood that both the foregoing general description and the following detailed description are merely illustrative and explanatory and are intended to provide a further description of the claimed present invention.

Examples

[0088] The present invention is merely illustrative and is further described by the following examples without binding force.

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

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

[0092] Example IV: In Example IV, an impregnating 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 impregnating 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 - Timber impregnated with sodium polyborate - Timber impregnated with monoguanidinium phosphate - Timber impregnated with a DMDHEU crosslinking agent Wood impregnated with an impregnating solution containing 20 g of DMDHEU and 5 g of diammonium phosphate (as a flame retardant) per 100 ml of water (Comparative Example I). Impregnation and drying were carried out in the same manner as in Example I, where applicable.

[0095] Leaching test The attribute of "with leaching" indicates all samples that were subjected to a 14-day cold water leaching procedure according to European Norm EN 84 (1997) before testing each material property.

[0096] Combustion test All samples were subjected to the "benzene burner combustion test". After treatment with the impregnating solution as described above, dried and cured samples of 13 x 4 x 125 (ax.) mm 3 were conditioned at 20 °C and 65% RH before testing. One end of the test specimen was fixed to the holder at an angle of 45°. The test specimen plus holder were placed on a balance such that the test specimen hung next to the balance. Before fixing the test specimen, the balance was zeroed, and the mass of the conditioned sample was measured in 10 -3 g units. Based on the starting weight of this test specimen, the moisture content was calculated based on the original oven-dry weight of the wood before treatment. The tip of the test specimen was ignited by the benzene burner while being exposed to the flame for 30 seconds. The intensity and height of the flame of the benzene burner were always the same for all test specimens. The weight of the test specimen was recorded at 10-second intervals, and at the same time, it was evaluated whether the test specimen was burning or glowing. The mass loss of the test 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 the maximum mass loss, the maximum mass loss per 10-second interval (burning rate), the burning time, and the glowing time. The test was carried out with n = 10 test specimens for each treatment group.

[0097] Swelling and shrinkage test (dimensional stability) 25 x 25 x 10 (ax.) mm 3The specimens were oven-dried at 103 °C to constant mass (0% MC) after treatment with crosslinkers and / or flame retardants. The oven-dried weight and dimensions were measured, and the samples were subsequently water-saturated with demineralized water by applying a vacuum of 100 mbar for 30 min, followed by storage in demineralized water for 24 h. The dimensions were then measured at maximum swelling and the anti-swelling efficiency [ASE, %] was calculated by comparing the swelling rate of the modified wood with that of the untreated wood, based on the maximum swelling rate. To take into account the long-term effect of the respective treatment on the swelling and shrinkage of the wood, the specimens were re-dried to oven-dried conditions and the described ASE cycle was repeated four times. The decrease in ASE value with increasing number of cycles indicates the effect of chemical leaching due to slight fixation.

[0098] Water vapor intake and release Short-term water absorption and release tests were performed on 5x10x100(ax.)mm 3 The test was carried out for 24 hours 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 during the 24-hour exposure (W24) was calculated. The samples were stored for an additional 14 days at 100% RH and reweighed at near fiber saturation. The specimens were then exposed directly 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 mass was then calculated. -3 The samples were weighed in grams and immersed in demineralized water at 25°C and 65% ambient. 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 of the maximum weight loss of two invention samples and two comparative samples tested both before and after leaching according to EN84 (1997). Figures 2 - 4 show the combustion rate, combustion time, and glowing time of the samples in Figure 1. As can be seen, the samples of the present invention show increased flame retardant behavior.

[0100] Figure 5 is a diagram showing the maximum swelling ratio of one invention sample and four comparative samples. Based on this, the anti - swelling efficiency (ASE) of the previously leached samples according to EN87 (1997) shown in Figure 6 was calculated. Figure 7 shows the water vapor uptake (W24 100%RH ), water vapor release (W24 0%RH ), and liquid moisture uptake (W24 submerged ) of the test pieces in Figure 5 tested without leaching according to EN84 (1997). The improved effect of the samples of the present invention can be clearly observed.

[0101] Figure 8 shows the maximum weight loss. Figure 9 shows the combustion rate of three invention samples and one comparative sample tested without leaching according to EN84 (1997). Figure 10 shows the combustion time, and Figure 11 shows the glowing time of three invention samples without leaching. Again, in Figures 8 - 11, the improved fire resistance can be clearly seen.

[0102] Figures 12 - 14 show the WPG (weight percent gain), maximum weight loss, and combustion rate for Example III of the invention, Comparative Example I, and the untreated control. Again, in Figures 12 - 14, the improved fire resistance can be clearly seen.

[0103] The specific combinations of elements and features in the above detailed embodiments are merely illustrative; the exchange and substitution of these teachings with other teachings herein, as well as patents / applications incorporated by reference, are also clearly contemplated. As will be recognized by those skilled in the art, 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 claimed invention. Accordingly, the foregoing description is merely exemplary and not intended to be limiting. In the claims, the word "comprising" does not exclude other elements or steps, and the indefinite article "a" or "an" does not exclude a plurality. The mere fact that certain measured values are recited in mutually different dependent claims does not indicate that a combination of these measured values cannot be used advantageously. The scope of the present invention is defined by the following claims and equivalents thereof. Further, the reference signs used in the description and claims do not limit the scope of the invention as claimed herein.

Claims

1. A boron and halogen-free treatment composition for timber and / or wood, comprising: a) flame retardants containing the moiety -N-C(=X)-N-, where X is O, S and substituted or unsubstituted nitrogen; and A composition comprising at least one of components b) a crosslinking agent, or c) a fixative.

2. The composition of claim 1, wherein the crosslinker comprises a 2-imidazolidone moiety.

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

4. The composition of any one of claims 1 to 3, wherein the fixative comprises a cyanoguanidine-diethylenetriamine-epichlorohydrin-polymer.

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

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

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

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

1.

9. The composition of any one of claims 1 to 8, further comprising a catalyst.

10. The composition according to any one of claims 1 to 8, which does not contain a catalyst.

11. Use of a composition according to any one of claims 1 to 10 as a treatment for timber and / or wood and / or wood-based products.

12. A timber and / or wood composite material, at least a part of which is impregnated with a composition according to any one of claims 1 to 10.

13. A method for applying a composition according to any one of claims 1 to 10 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.

14. The method according to claim 13, wherein the content of the composition in step b) (in g per 100 ml of water before addition) is 0.5 g to 80 g.

15. 15. The method according to claim 13 or 14, 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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