JP2011031405A - Woody material processing composition, method for processing woody material, and woody material processed by the method - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a woody material processing composition which improves the flame retardancy etc., of woody materials such as wood, and prevents the occurrence of the efflorescence problem of the processed woody materials, a method for processing the woody materials using the composition, and the woody materials processed by the method. <P>SOLUTION: The woody material processing composition is prepared by adding a silicic acid compound in an amount of 0.05-0.5 mol in terms of the number of silicon atoms into 1 L of an aqueous solution containing 1.2-3 mol/L of phosphoric acid or phosphate ions, 0.15-0.5 mol/L of alkaline earth metal ions, 0.04-0.4 mol/L of alkaline metal ions, and 1.0-2.0 mol/L of ammonium ions. The method for processing the woody materials includes a process for impregnating the composition. The woody materials are obtained by being processed by the method. <P>COPYRIGHT: (C)2011,JPO&amp;INPIT

Description

The present invention relates to a wood material treatment composition, a wood material treatment method, and a wood material treated thereby.

Woody materials have been widely used as building materials since ancient times, and as a building material with a unique texture regardless of changes in architectural style, it is still widely used not only as structural materials but also as exterior materials and interior materials. It is used. However, wood-based materials have problems such as decay and flammability, and conifers such as Japanese cypress and cedar that are most widely used in Japan have scratches due to low hardness of the early wood parts. There are also problems such as ease, generation of irregularities due to aging shrinkage (so-called “eye loss”), and the like.

As described above, in order to reduce decay and flammability in wood materials, improve hardness and dimensional stability, etc., it is widely performed to apply a treatment agent to the surface or impregnate the inside. A treatment agent and a treatment method have been proposed.
For example, organic or inorganic halogen flame retardants have been used for a long time. Moreover, nitrogen-type flame retardants, such as melamine pyrophosphate, are also used (for example, refer patent document 1).

In Patent Document 2, an insoluble incombustible compound, which is a reaction product of two or more water-soluble compounds impregnated in raw wood, is fixed, and a compound having two or more aldehyde groups is used between the hydroxyl groups of the raw wood. Disclosed is a method for producing modified wood that retains flame retardancy and improves dimensional stability by heating the crosslinked modified wood in a steam atmosphere of formaldehyde derivatives and in the presence of an acid catalyst for formalization. Yes.
In Patent Document 3, a flame-retardant metal salt and an acrylic polymer are impregnated in wood, and the cured acrylic polymer surrounds the flame-retardant material in the wood and has resistance to flame. However, a flame-retardant polymer-impregnated wood that is stable in dimensions and does not adversely affect the living environment is disclosed.

Patent Documents 4 and 5 each disclose a fireproof, fireproof, noncombustible material, and a noncombustible wood board using a borate having an effect of suppressing smoke combustion and red heat combustion of a wood-based material as a fireproofing agent.

JP-A-6-218708 JP-A-6-143209 JP 2000-141318 A JP 2005-112700 A JP 2006-182024 A

However, halogen-based flame retardants and nitrogen-based flame retardants described in Patent Document 1 have problems in that harmful gases are generated during combustion and cause discoloration.
In the method for producing modified wood described in Patent Document 2, formaldehyde remaining in the wood may cause so-called sick house syndrome and adverse environmental effects.
In the flame-retardant polymer-impregnated wood described in Patent Document 3, the polymerization of the impregnated acrylic polymer precursor may not proceed completely, and problems such as a decrease in dimensional stability may occur.
In the fireproof, fireproof, incombustible material described in Patent Document 4, and the incombustible wood board described in Patent Document 5, the water-soluble boric acid compound is leached and precipitated on the surface as the wood is absorbed and desorbed, and the surface becomes white. There is a disadvantage of causing the white flower phenomenon. Alkalis are often added to improve the water solubility of boric acid for the purpose of reducing processing costs, but in such cases, the leaching of boric acid is promoted by the hygroscopicity of alkalis, and Occurrence may be more noticeable.

When such white flower phenomenon occurs in wood for inner and outer walls, the value is reduced, and in these materials, deformation such as warping and twisting is likely to occur after processing, and dimensional and shape stability There is also the disadvantage of poor nature. In addition, when the white flower phenomenon occurs, the affinity with the paint decreases, so that a commercially available paint cannot be used, and there is a problem that the coating cost increases.

Furthermore, boric acid used in the fireproof, fireproof, incombustible material described in Patent Document 4 and the incombustible wood board described in Patent Document 5 is toxic. It is said that 10-20g is a lethal dose. Therefore, there is a need for a woody material treatment composition that includes a flame retardant instead of boric acid. Phosphate is mentioned as an inorganic flame retardant widely used with boric acid, but the occurrence of white flower phenomenon is also known in the case of phosphate, improving flame retardancy and suppressing white flower phenomenon In this case, there is a trade-off relationship.

The present invention has been made in view of such circumstances, and improves the flame retardancy and the like of wood materials such as wood, and uses the wood material treatment composition that is less prone to white matter problems after treatment. It is an object of the present invention to provide a method for treating a wood material, and a wood material treated thereby.
The “woody material” in the present invention includes, in addition to so-called “wood” obtained from trees, materials obtained from herbaceous stems, leaves, etc., and materials mainly composed of cellulose and lignin. To do.

The first aspect of the present invention includes 1.2 to 3 mol / L phosphoric acid or phosphate ions, 0.15 to 0.5 mol / L alkaline earth metal ions, and 0.04 to 0.4 mol / L. An aqueous solution containing L alkali metal ions and 1.0 to 2.0 mol / L ammonium ions is added with an amount of 0.05 to 0.5 mol of a silicate compound in terms of the number of silicon atoms per 1 L of the aqueous solution. The above-mentioned problems are solved by providing a woody material treatment composition characterized by being obtained by adding.

Phosphoric acid or phosphate ion contained in the woody material treatment composition forms a so-called charcoal fire layer during the combustion of the woody material impregnated with it, and blocks the supply of oxygen to the inside, thereby preventing the combustion prevention effect. Can demonstrate. Therefore, high flame retardancy can be imparted to the wood material without using boric acid. Alkali metal ions, alkaline earth metal ions, and ammonium ions contained in the woody material treatment composition cause an endothermic reaction at high temperatures and are thermally decomposed, so they have the effect of absorbing combustion heat and inhibiting the progress of combustion. is doing. In addition, the silicate compound contained in the wood material treatment composition is polymerized after penetrating into the wood material to form polysiloxane, thereby leaching the phosphate contained in the wood material treatment composition and the associated white flower. The phenomenon can be suppressed. Moreover, since the woody material treatment composition according to the present embodiment does not contain a synthetic resin, the woody material treated thereby does not cause a problem of disposal at the time of disposal, and since boric acid is not used, excessive hygroscopicity. Does not have.

By making the woody material treatment composition as described above, high flame retardancy can be imparted to the woody material, and the occurrence of the white flower phenomenon and discoloration in the woody material after treatment can be suppressed. Furthermore, since it does not contain halogen-based flame retardants or nitrogen-based flame retardants, no harmful or irritating gases are generated during combustion.

In this case, the alkaline earth metal is preferably calcium, and the alkali metal is preferably potassium.
By using these metal ions, a wood material treatment composition capable of imparting high incombustibility to a wood material can be obtained at low cost.

In the first aspect of the present invention, 0.2 to 0.4 mol of alkaline earth metal dihydrogen phosphate and 0.04 to 0.3 mol of alkali metal dihydrogen phosphate per 1 L of the aqueous solution. Further, a woody material treatment composition may be obtained by dissolving 0.6 to 0.95 mol of ammonium hydrogenphosphate in a phosphoric acid aqueous solution containing a predetermined amount of phosphoric acid.
Alkali metal hydroxides that are strongly basic and require careful handling, alkaline earth metal hydroxides that are difficult to dissolve in water, and alkali metals and alkaline earths that generate carbon dioxide when dissolved in an aqueous phosphoric acid solution and foam Compared to the case of using a metal carbonate or the like, the raw material can be easily managed and handled, and foaming during production and generation of harmful gases can be suppressed.

A second aspect of the present invention solves the above problems by providing a method for treating a wooden material, characterized by impregnating the wooden material with the wooden material treatment composition according to the first aspect of the present invention. Is.

In this case, it is preferable that the wood material left for a predetermined time under reduced pressure is immersed in the wood material treatment composition and the wood material treatment composition is impregnated with the wood material treatment under pressure.

Further, in this case, the change in mass of the wood material before and after the impregnation of the wood material treatment composition is measured for each of the wood materials, and when the amount of impregnation per unit volume is a predetermined value or less, the wood material is again measured. It is preferred to impregnate the treatment composition.

According to a third aspect of the present invention, there is provided a wooden material characterized by being processed by the method for processing a wooden material according to the second aspect of the present invention.
The wood material obtained in this way has improved flame retardancy compared to untreated wood material, and it is less likely to cause problems such as deterioration in design due to the occurrence of white flower phenomenon. It can be used suitably. Further, since deformation and discoloration due to changes with time are less likely to occur, the durability is also excellent.

In this case, the wooden material shall be the quasi-incombustible material of Article 1, Item 5 of the Building Standards Act Enforcement Ordinance (December 16, 1983). It must conform to any of the standards for non-combustible materials in Article 2, Item 9 of the Incombustible Materials and Building Standards Act (Act No. 211 of May 24, 1947) preferable.

In addition, "the quasi-incombustible material of Building Standard Law enforcement order Article 1 item 5" means the following (1) to (3) (10 minutes after the start of heating, when the heat from a normal fire is applied: In thing to use for exterior finishing of building, we say building materials which meet requirements to raise in (1) and (2). The same applies hereafter, and "flame retardant material of the same article sixth" Buildings that meet the requirements listed in (1) to (3) below (Article 108-2 of the Building Standards Law Enforcement Ordinance) for 5 minutes after the start of heating when fire heat from a normal fire is applied The material refers to the “non-combustible material of Article 2-9 of the Building Standards Law”. When fire heat is applied by a normal fire, it is listed in the following (1) to (3) for 20 minutes after the start of heating. A building material that meets the requirements.
(1) It must not burn.
(2) It shall not cause deformation, melting, cracking or other damage harmful to fire prevention.
(3) Do not generate smoke or gas harmful to evacuation.

As described above, according to the present invention, it is possible to obtain a wood material treatment composition that improves the flame retardancy and the like of wood materials and is less prone to white matter problems. Moreover, according to this invention, the processing method of the wooden material using a wooden material processing composition, and the wooden material processed by it are obtained.

It is a graph which shows the relationship between the sticking amount of the woody material processing composition in the cedar material which performed the flame-retardant process in Example 7, and the total calorific value for 10 minutes. It is a graph which shows the relationship between the adhering amount of the woody material processing composition to a cedar material in Example 7, and the total calorific value for 20 minutes. It is the graph which plotted the time change of the total calorific value and combustion rate in the cedar material which performed the flame-retardant process in Example 7. FIG. It is the graph which plotted the time change of the total calorific value and combustion rate in the cedar material which performed the flame-retardant process in Example 7. FIG. It is the graph which plotted the time change of the total calorific value and combustion rate in the cedar material which performed the flame-retardant process in Example 7. FIG. It is the graph which plotted the time change of the total calorific value and combustion rate in the cedar material which performed the flame-retardant process in Example 7. FIG.

The woody material treatment composition according to the first embodiment of the present invention includes 1.2 to 3 mol / L phosphoric acid or phosphate ions, 0.15 to 0.5 mol / L alkaline earth metal ions, In an aqueous solution containing 0.04 to 0.4 mol / L alkali metal ions and 1.0 to 2.0 mol / L ammonium ions, the amount is 0.05 to 0.5 mol in terms of silicon atoms per liter of the aqueous solution. An aqueous composition obtained by adding an amount of a silicic acid compound, and can be impregnated into a woody material by coating or pressure injection.

The composition of each component can be appropriately adjusted within the above range in order to adjust the pH, the polymerization rate of the silicic acid compound after impregnation, and the like. For example, in order to make the pH of the woody material treatment composition near neutral, the amount of phosphoric acid added is decreased and the amount of ammonium salt added is increased.

As a metal salt containing an alkali metal ion and an alkaline earth metal ion, any metal salt belonging to these genera can be used. That is, lithium, sodium, potassium, rubidium and cesium salts can be used as the alkali metal salt, and magnesium, calcium, strontium and barium salts can be used as the alkaline earth metal salt. Of these, potassium salts are particularly preferably used as alkali metal salts, and calcium salts are particularly preferably used as alkaline earth metal salts. The anions of these metal salts and ammonium salts are hydroxides, halides, carbonate ions (including both bicarbonate ions HCO ₃ ⁻ and carbonate ions CO ₃ ²⁻ ), nitrate ions, sulfate ions (hydrogen sulfate). Ion HSO ₄ ⁻ and sulfate ion SO ₄ ²⁻ ), carboxylate ion, sulfonate ion, phosphate ion (dihydrogen phosphate ion H ₂ PO ₄ ⁻ , hydrogen phosphate ion HPO ₄ ²⁻ and Any one of phosphoric acid ions PO ₄ ³⁻ ) and perchloric acid ions may be used, but phosphate ions are preferred.

As the metal salt containing phosphate ions, any salt that dissolves in water to generate phosphate ions can be used. Specific examples include (ortho) phosphate, hydrogen phosphate, dihydrogen phosphate. Examples thereof include salts, diphosphates, tripolyphosphates, and polyphosphates. Examples of the metal salt and ammonium salt that are preferably used for the production of the woody material treatment composition include potassium dihydrogen phosphate (KH ₂ PO ₄ ), calcium dihydrogen phosphate (Ca (H ₂ PO ₄ ) ₂ ), and diphosphate phosphate. Examples include ammonium hydrogen (NH ₄ H ₂ PO ₄ ), potassium hydrogen phosphate (K ₂ HPO ₄ ), calcium hydrogen phosphate (CaHPO ₄ ), and ammonium hydrogen phosphate ((NH ₄ ) ₂ HPO ₄ ).

The woody material treatment composition contains a silicic acid compound in an amount of 0.05 to 0.5 mol in terms of the number of silicon atoms per liter of the aqueous solution. The silicic acid compound may be dissolved in an aqueous solution, or may be uniformly dispersed in a colloidal state or the like. The silicate compound may be an (ortho) silicate ion (SiO ₄ ⁴⁻ ) or an arbitrary one capable of producing a polysilicate ion or polysiloxane obtained by dehydration condensation of a plurality of silicate ions in an aqueous solution. Examples thereof include orthosilicate, metasilicate, anhydrous silica, colloidal silica, and polyalkoxysilane.

The woody material treatment composition is prepared by mixing alkaline earth metal salt, alkali metal salt, ammonium salt and phosphoric acid, and silicic acid compound in water. The amount of each component is appropriately adjusted so that phosphoric acid or phosphate ions, alkaline earth metal ions, alkali metal ions, ammonium ions, and silicate compounds are in amounts within the above ranges. The woody material treatment composition is, for example, 0.2 to 0.4 mol of alkaline earth metal dihydrogen phosphate, 0.04 to 0.3 mol of alkali metal dihydrogen phosphate, and 1 By dissolving 6 to 0.95 mol of ammonium hydrogenphosphate salt in a phosphoric acid aqueous solution containing a predetermined amount of phosphoric acid, diluting to a predetermined amount with water, and adding a silicate compound to the resulting aqueous solution Can be prepared.

The concentration of phosphoric acid or phosphate ion, alkaline earth metal ion, alkali metal ion, ammonium ion and silicate compound contained in the woody material treatment composition can be measured using any known method. it can. Specific examples of the measurement method include an ion chromatography method, an inductively coupled plasma method (ICP), an emission analysis method such as atomic absorption analysis, and a molybdic acid colorimetric method for silicate ions.

In order to adjust pH and improve flame retardancy, other components than the above may be added to the woody material treatment composition. Examples of the component that can be added include carbonates, hydroxides, and aluminum salts of alkali metals and alkaline earth metals.

The wood material which concerns on the 2nd Embodiment of this invention is manufactured using the processing method of the wood material which has the process of making a wood material impregnate the wood material processing composition which concerns on the 1st Embodiment of this invention.
The type of wood material is not particularly limited, and materials obtained from any kind of tree, herbaceous stems, leaves, etc., and mainly composed of cellulose and lignin can be used. Not only plywood and laminated wood can be used. Also, the shape and dimensions are not particularly limited.

The impregnation of the wood material with the wood material treatment composition can be performed using any known method. Examples of the impregnation method include a method of applying and infiltrating the wood material treatment composition onto the surface of the wood material and a method of injecting under pressure, but the latter method is more preferable for thick plate materials, pillar materials, etc. In particular, a pressure injection method based on JIS A9002, which is widely used in insect-proofing treatment of wooden materials, is particularly preferably used. In addition, before dipping in the woody material treatment composition and pressurization, in order to remove gas components such as moisture and air adsorbed on the woody material and increase the amount of impregnation, the woody material is used for a predetermined time under reduced pressure. You may perform the decompression process which leaves a material as it is. As an example of the steaming process, a steaming decompression process in which drying at a reduced pressure is performed after heating with steam at about 120 ° C.

More specifically, the wood material treatment composition is impregnated (pressure injection) by pressurizing the wood material immersed in the wood material treatment composition in a pressure vessel at a predetermined pressure for a predetermined time. The pressure at the time of pressurization and the pressurization time are appropriately adjusted according to the strength, shape and size of the wood material, the amount of the substance to be impregnated, and the like. The pressurization may be performed by increasing the atmospheric pressure in the immersion container, or may be performed by increasing the hydrostatic pressure of the wood material treatment composition injected into the immersion container.

After the treatment, the wood material taken out from the pressure vessel is washed with water and dried to remove the wood material treatment composition adhering to the surface. Drying may be either natural drying or hot air drying. Hot air drying also has the effect of shortening the time required for processing the wood material by speeding up the polymerization of the silicic acid compound impregnated in the wood material. In order to increase the amount of impregnation, the above-described pressure injection treatment may be repeatedly performed on the dried woody material regardless of the measurement result of mass change described later.

The change in mass of the wood material before and after impregnation with the wood material treatment composition is measured for each wood material, and if the amount of impregnation per unit volume is less than a predetermined value, the wood material treatment composition is impregnated again. preferable. For the wood material that has been impregnated again, the mass change before and after the impregnation is measured, and those that do not reach the predetermined amount per unit volume are discarded.

Furthermore, in order to accelerate the polymerization of the silicic acid compound impregnated in the wood material, heat treatment may be performed after washing and air drying.

The concentration of each component impregnated in the woody material can be determined using an arbitrary leaving method such as an X-ray microanalyzer (XPS).

The woody material treatment composition remaining in the impregnation container after the impregnation treatment is analyzed again if necessary, after analysis of the contained components (can be carried out using the above-mentioned method) and / or replenishment of the missing components. It can be used for impregnation treatment. In this case, when the wood material treatment composition is colored, the wood material may be colored by impregnation, and the quality may be deteriorated. However, the activated carbon treatment may remove the colored matter. It was confirmed that the problem of coloring the woody material did not occur even if it was used again for the impregnation treatment.

The wood material obtained in this way is the quasi-incombustible material of Article 1, Item 5 of the Building Standards Law Enforcement Order, the flame-retardant material of Article 6 of the same, or the incombustible material of Article 2, Item 9 of the Building Standards Act. Meets standards. Whether or not these standards are met can be confirmed by any test method that meets the technical standards defined by these standards. Specific examples of test methods are described in ISO-5660. The exothermic test by the corn calorimeter method to which it conforms is mentioned.

A cone calorimeter is a device that heats a test piece having a size of 10 cm × 10 cm with a cone heater and measures the oxygen concentration in the generated gas. The test piece is heated at 50 kw / m ² , ignited by an electric spark, and the calorific value and the heat generation rate are calculated from the oxygen concentration decreased by combustion.
The heat generation rate thus obtained is less than 8 MJ / m ^{2 in} total heat generation for a predetermined time (non-combustible material: 20 minutes, semi-incombustible material: 10 minutes, flame-retardant material: 5 minutes), and 200 kW / m ^{When the} heat generation rate exceeding ² does not continue for 10 seconds or more, it is determined that the heat generation test has been passed.

The woody material thus obtained can be used for any application depending on the material, size, shape, noncombustibility, and the like. If necessary, processing such as surface processing (surface grinding, painting, etc. with sandpaper, canna) may be appropriately performed.

Next, examples carried out for confirming the effects of the present invention will be described.
Example 1: Preparation of woody material treatment composition (1)
789.4 g of water having a water temperature of 20 to 25 ° C. was put in a container, 145.1 g of phosphoric acid (85%) was added, and the mixture was stirred and dissolved. To this phosphoric acid aqueous solution, 85.0 g of calcium dihydrogen phosphate monohydrate (Ca (H ₂ PO ₄ ) ₂ .H ₂ O) was added and stirred. When stirring was continued for 4 to 5 minutes, all the solids were dissolved and a transparent solution was obtained. Next, 14.2 g of potassium dihydrogen phosphate (KH ₂ PO ₄ ) was added to this solution and stirred. When stirring was continued for 2 to 3 minutes, all solids were dissolved and a transparent solution was obtained. Next, 122.7 g of diammonium hydrogen phosphate ((NH ₄ ) ₂ HPO ₄ ) was added and stirred. When stirring was continued for 5 to 6 minutes, all the solids were dissolved, and a transparent solution was obtained. Next, 23.6 g of anhydrous silicic acid (30.5%) was added to the resulting solution and stirred, to obtain 1 L (1180 g) of a wood material treatment composition, which is an aqueous solution having a specific gravity of 1.18 and a pH of 2.7.

Example 2: Preparation of woody material treatment composition (2)
15,788 g of water having a water temperature of 20 to 25 ° C. was put in a container, 2241.2 g of phosphoric acid (85%) was added, and the mixture was stirred and dissolved. To this phosphoric acid aqueous solution, 1700 g of calcium dihydrogen phosphate monohydrate (Ca (H ₂ PO ₄ ) ₂ .H ₂ O) was added and stirred. When stirring was continued for 4 to 5 minutes, all the solids were dissolved and a transparent solution was obtained. Next, 284 g of potassium dihydrogen phosphate (KH ₂ PO ₄ ) was added to this solution and stirred. When stirring was continued for 2 to 3 minutes, all solids were dissolved and a transparent solution was obtained. Next, 2454 g of diammonium hydrogen phosphate ((NH ₄ ) ₂ HPO ₄ ) was added and stirred. When stirring was continued for 5 to 6 minutes, all the solids were dissolved, and a transparent solution was obtained. Next, 472 g of silicic acid anhydride (30.5%) was added to the resulting solution and stirred, to obtain a wood material treatment composition 20L (23,600 g) which was an aqueous solution having a specific gravity of 1.18 and pH 2.7.

Example 3: Preparation of flame-retardant treated cedar material Cedar wall material (actually processed product: hereinafter referred to as “cedar material”) (W = 115 mm, L = 2000 mm, T = 15 mm, volume 3.45 × 10 ^{− 3} m ³ , moisture content of 15% or less) and the woody material treatment composition prepared in Example 2 were used for the treatment as follows.
After the cedar material was put in the tank of the pressure impregnation apparatus and the anti-floating treatment was performed, the tank internal pressure was reduced to a negative pressure of -0.1 MPa, and then the pressure reduction treatment was performed for 1 hour. Quickly added the woody material treatment composition into the tank under evacuation (Sugi 1 m ³ per 385L), the tank in a state in which cedar material is immersed pressurized, after 90 minute hold at tank pressure 1 MPa, 45 minutes The pressure was naturally reduced to atmospheric pressure. The cedar wood taken out from the tank was washed with water and then naturally dried for 4 hours. Next, it was dried in a warm air drying room at a room temperature of around 60 ° C. for 47 hours. The moisture content after drying was 15% or less.

Using one cedar material, the amount of substance impregnated per unit volume (hereinafter referred to as “fixed amount”) was determined from the difference in mass before and after the treatment, and found to be 135 kg / m ³ . Further, even after being left for a long time after the treatment, none of deformation such as warping, twisting, or discoloration called “wood burn” was observed. It is known that woodburn caused by the reaction of lignin is noticeable particularly when an acidic treatment solution is used, but interestingly, it was not observed in this example.

Example 4: Preparation of flame-retardant treated cedar wood Cedar wood (W = 105 mm, L = 1920 mm, T = 15 mm, volume 3.024 × 10 ⁻³ m ³ ), and wood material treatment composition prepared in Example 2 the use, increasing the injection amount of wood material treatment composition was (Sugi 1 m ³ per 570L) is, after 180 minute hold at tank pressure 1 MPa, 60 minutes over a procedure similar to natural vacuum and then example 3 to atmospheric pressure The cedar wood was impregnated.
Using two cedar, from the difference between before and after the treatment by mass, it was determined the amount of per unit volume impregnated material were respectively 219.3kg / ^{m 3,} and 195 kg / ^{m 3.} Further, even after being left for a long time after the treatment, none of deformation such as warping, twisting, or discoloration called “wood burn” was observed.

Example 5: Preparation of flame-retardant treated cedar wood Cedar wood (W = 100 mm, L = 230 mm, T = 30 mm, volume 0.69 × 10 ⁻³ m ³ ), and wood material treatment composition prepared in Example 2 Using the same method as in Example 3, the cedar wood was processed.
Using two cedar, from the difference between before and after the treatment by mass, was determined the amount of per unit volume impregnated material were respectively 140.5kg / ^{m 3,} and 111 kg / ^{m 3.}

Example 6: Nonflammability performance test The exothermic test was conducted using a cone calorimeter in accordance with ISO-5660 and using a plate material of 100 mm x 100 mm. While supplying radiant heat with a burner having a radiant heat of 50 kw / m ² , ignition was performed with an electric spark, and the total calorific value for 10 minutes and 20 minutes was measured. In this test, if the total calorific value for 10 minutes is 8 MJ / m ² or less but the total calorific value for 20 minutes exceeds 8 MJ / m ² , it is “quasi-incombustible material”, and the total calorific value for 20 minutes is also 8 MJ / m ^2. When it is m ² or less, it is determined as “non-combustible material”. The results were as shown in Table 1 below. In the total calorific value column, “◯” represents 8 MJ / m ² or less, and “X” represents that it exceeds 8 MJ / m ² .

From these results, the cedar materials treated with flame retardant in Example 3 and Example 5 were in conformity with the standards for quasi-incombustible materials in Article 1, Item 5 of the Building Standards Law Enforcement Ordinance. On the other hand, it was confirmed that the cedar materials processed in Example 4 conformed to the standards for non-combustible materials in Article 2, Item 9 of the Building Standard Law.

Example 7: Relationship between the impregnation amount of the wood material treatment composition and the non-combustibility performance Using a cedar wood (W = 110 mm, L = 1700 mm) with a thickness of 17 mm, except that the injection amount of the wood material treatment composition was changed. The impregnation treatment was performed in the same procedure as in Example 3. The cured flame-retardant cedar materials thus obtained (four types with impregnation amounts of 110 kg / m ³ , 130 kg / m ³ , 140 kg / m ³ and 150 kg / m ³ ), respectively, are divided into 15 equal parts in the longitudinal direction. Then, 15 test pieces having a length of 100 mm were cut out (there was a loss of 20 mm per cedar material), and the amount of fixing was determined from the density change before and after the curing flame retardant treatment. Thereafter, the total calorific value and the temporal change of the calorific value for 10 minutes and 20 minutes were measured under the conditions described in Example 6 (ISO-5660). The results were as shown in Table 2 below. In Table 2, the sample number with the branch number “10” is the one cut out from the tenth position counted from one end when the cedar material before cutting is divided into 15 equal parts in the longitudinal direction. The one not represented by the branch number represents one that is cut out from one end when the cedar material before cutting is divided into 15 equal parts in the longitudinal direction.

Based on the result of Table 2, the graph which plotted the relationship between the fixed amount and the total calorific value for 10 minutes and 20 minutes is shown in FIG. 1 and FIG. 2, respectively. Moreover, the graph which plotted the time change of the total calorific value and combustion rate of each sample (F11, F24, F35, F37) is shown to FIG.

In this test, if the total calorific value for 10 minutes is 8 MJ / m ² or less but the total calorific value for 20 minutes exceeds 8 MJ / m ² , it is “quasi-incombustible material”, and the total calorific value for 20 minutes is also 8 MJ / m ^2. When m ² or less, it is determined that the material is “non-combustible material”. As is apparent from the results in Table 2, FIG. 1 and FIG. 2, the “quasi-incombustible material” criterion is achieved in all samples. It can also be seen that the standard of “non-combustible material” is achieved for the samples of sample numbers F37 and F11 with an impregnation amount of 0.15 g / cm ³ . Moreover, it can be seen from the comparison results between F24 and F24-10, and F35 and F35-10 that there is no significant difference in the total calorific value and the burning rate depending on the position of the cedar material. This suggests that the woody material treatment composition is substantially uniformly impregnated along the longitudinal direction of the cedar wood.

Furthermore, from FIGS. 1 to 6, the heating rate was always significantly lower than 200 kW / m ² for any sample. From these results, it was confirmed that all the samples satisfied the standards of the quasi-incombustible material and the incombustible material.

Claims (9)

1.2 to 3 mol / L of phosphoric acid or phosphate ions;
0.15 to 0.5 mol / L alkaline earth metal ions;
0.04 to 0.4 mol / L of alkali metal ions;
In an aqueous solution containing 1.0 to 2.0 mol / L of ammonium ions,
A woody material treatment composition obtained by adding a silicic acid compound in an amount of 0.05 to 0.5 mol in terms of the number of silicon atoms per liter of the aqueous solution. The woody material treatment composition according to claim 1, wherein the alkaline earth metal is calcium. The woody material treatment composition according to any one of claims 1 and 2, wherein the alkali metal is potassium. Per liter of the aqueous solution,
0.2 to 0.4 mol of alkaline earth metal dihydrogen phosphate,
0.04 to 0.3 mol of alkali metal dihydrogen phosphate,
0.6 to 0.95 mol of ammonium hydrogenphosphate salt,
The woody material treatment composition according to any one of claims 1 to 3, wherein the composition is obtained by dissolving in a phosphoric acid aqueous solution containing a predetermined amount of phosphoric acid. A method for treating a wood material, comprising impregnating the wood material with the wood material treatment composition according to any one of claims 1 to 4. 6. The method for treating a wood material according to claim 5, wherein the wood material left for a predetermined time under reduced pressure is immersed in the wood material treatment composition, and the wood material treatment composition is impregnated with the wood material treatment under pressure. The change in the mass of the wood material before and after impregnation with the wood material treatment composition is measured for each of the wood materials, and if the amount of impregnation per unit volume is a predetermined value or less, the wood material treatment composition is impregnated again. The method for treating a woody material according to any one of claims 5 and 6, wherein the method is performed. A wood material which is treated by the wood material treatment method according to any one of claims 5 to 7. It conforms to any of the standards for quasi-incombustible materials in Article 1, Item 5 of the Building Standards Law Enforcement Ordinance, flame-retardant materials in Article 6 of the Article 6, and incombustible materials in Article 2, Item 9 of the Building Standards Act The woody material according to claim 8.

Images