JP2010162727A - Non-combusting chemical liquid for wood material, method of manufacturing non-combusting chemical liquid for wood material, non-cmbusting method of wood material using non-combusting chemical liquid for wood material and non-combustible wood material - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a non-combusting chemical liquid for wood material in which problems of hygroscopicity and the exudation of a non-combustible chemical liquid or the like, which are a long pending issue for a non-combustible wood material is solved. <P>SOLUTION: The non-combustible chemical liquid for wood material is prepared by adding 90 g succinic acid as carboxylic acid into 1,000 cm<SP>3</SP>water while stirring and further adding 480-600 g chemical liquid comprising guanidine and phosphoric acid in weight ratio of 3:2, wherein the succinic acid, guanidine and phosphoric acid are completely dissolved at the room temperature to obtain a transparent solution that is the non-combustible chemical liquid for wood material. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

  The present invention relates to an incombustible agent for a wood material that incombusts a wood material used for interiors and exteriors of houses, stores, and other building structures, a method for producing the incombustible agent for a wood material, and an incombustible agent for the wood material. The present invention relates to a method for incombusting a wood material using a chemical, and an incombustible wood material that has been incombustible by this incombustibility method.

In 1998, the Building Standards Law was amended, and if certain performance was satisfied, wood materials could be certified as non-combustible materials. Since then, research and development on the incombustibility of wooden materials has become active.
As one of the evaluation methods of nonflammability performance, a heat generation test using a corn calorimeter is defined. In order to satisfy the standard of nonflammability, it is necessary to satisfy the following three conditions in a heating test for 20 minutes using the same apparatus.
(1) The total calorific value is 8 MJ / m ² or less.
(2) There should be no cracks or holes penetrating to the reverse side, which is harmful to fire prevention.
(3) The maximum heat generation rate should not exceed 200 kW / m ² for 10 seconds or more.

In order for the wood material to satisfy these three conditions, it is necessary to introduce a considerably large amount of the flame retardant agent for the wood material into the wood material. As in No. 3538194, it is essential to repeat the impregnation and drying of the incombustible agent for wood material a plurality of times.
As a method for obtaining an incombustible chemical for woody materials having a high concentration, a method using a chemical having extremely high solubility such as phosphoric acid or an inorganic compound of phosphoric acid, or heating a treatment solution as disclosed in JP-A-2006-219329. Examples thereof include a method and a method of increasing solubility using a plurality of drugs.

  However, in the above method, the method of repeating the impregnation and drying of the wood material incombustible agent a plurality of times has a fatal disadvantage that the treatment period becomes extremely long and the cost performance is lacking.

  In addition, phosphoric acid and inorganic compounds of phosphoric acid having high solubility have extremely high hygroscopicity, and the wood material treated with the phosphor has a great disadvantage that it absorbs a large amount of moisture in the air and thereby the drug exudes. Furthermore, it has an adverse effect on the surface coating film such as painting performed to suppress it, and there is a problem that peeling and cracking occur in a short time.

  It is not difficult to obtain a high-concentration flame retardant for woody materials by increasing solubility by heating, but heating is also required during treatment such as impregnation, making the work complicated and the equipment complicated. It will be a thing. In particular, in the case of a pressurized infusion canister that seems to be the most effective device for impregnating a wood material with an incombustible chemical for wood material, there is a liquid feed pipe or pump between the chemical storage tank and the pressure infusion canister. Although indispensable, if the incombustible chemical | medical agent for woody materials which remain | survives in such a site | part deposits, it will become very difficult to remove. In order to avoid such troubles, it is necessary to always heat the entire apparatus. Therefore, it is considered that the production cost of the method for obtaining a high-concentration wood material incombustible chemical by increasing the solubility by heating is extremely high even if it is put into practical use.

  As a method for increasing the solubility by mixing a plurality of drugs, (1) a method for increasing the concentration of a boron compound by adding sodium hydrogencarbonate as in JP-A-2006-082533, and (2) JP-A-2007- A method of adjusting pH with sodium hydroxide, potassium hydroxide or monoethanolamine as in 090839 and dissolving boric acid at a high concentration, or (3) organic as in JP-A-03-223205 and JP-A-07-088808 A method in which a boron compound is dissolved at a high concentration using an amine, or a method in which the solubility of guanidine phosphate is increased by addition of phosphoric acid as disclosed in JP-A-2007-160570 is known.

  However, since the chemicals added to improve the solubility used in these methods are all highly hygroscopic, the wood materials treated with them are also extremely hygroscopic. For wood materials treated with boric acid chemicals, a phenomenon occurs in which the surface becomes white due to crystals of boric acid. Moreover, in the woody material treated with the flame retardant for phosphorous-based woody material, stickiness unique to phosphoric acid occurs.

  In this way, all of the wood materials treated with the conventionally known incombustible chemicals for wood materials have extremely high hygroscopicity, sucking moisture in the air, which causes exudation and painting of chemicals, etc. Since the surface coating film is peeled off and cracks are generated, the usage environment is significantly restricted. For this reason, if the hygroscopicity of the non-combustible wood material can be suppressed, its use is considered to expand dramatically, and establishment of its treatment technology has been strongly desired.

Japanese Patent No. 3538194 JP 2006-219329 A JP 2006-082533 A JP2007-090839 JP 03-223205 A JP 07-088808 JP2007-160570

Under such circumstances, the inventor has repeatedly studied to develop a technique for suppressing the hygroscopicity of the non-combustible wood material by a method as simple as possible. As is well known, guanidine phosphate (diguanidine phosphate) and guanylurea phosphate are effective chemicals for incombustibility of wood materials, and it should be noted that non-combustibility for wood materials such as ammonium phosphate. Unlike chemicals, it has almost no hygroscopicity.
However, the solubilities of these drugs are 15.5 g / 100 ml (20 ° C.) for diguanidine phosphate and 8.5 g / 100 ml (20 ° C.) for guanylurea phosphate (“Chemical Dictionary Dictionary 11th Edition”). Published on February 5, 1986, Kyoritsu Publishing).
In order to impart incombustibility to wood materials, it is necessary to use an incombustible agent for wood materials of 160 to 170 kg or more per 1 m ³ of wood material. On the other hand, the injection amount of incombustible agent for wood materials per 1 m ³ of wood material Is a maximum of 1000 kg (injection amount of 800 liters, liquid density of 1.25 g / cm ³ ), so that a minimum of 20 g / 100 ml solubility is required to produce non-combustible wood material in a single injection operation. In order to prepare an incombustible agent for a wood material using guanidine phosphate (diguanidine phosphate) or guanylurea phosphate as a main ingredient, it is necessary to devise measures to increase their solubility by some means.

Japanese Patent Application Laid-Open No. 2007-160570 (Patent Document 7) discloses a technique for increasing the solubility of guanidine phosphate to a concentration necessary for incombustibility of woody material by adding a predetermined amount of phosphoric acid.
As estimated from this invention, it was thought that the solubility of guanylurea, which is a derivative of guanidine or guanidine, can be improved by adding an inorganic acid. In addition to phosphoric acid, inorganic acids include sulfuric acid, hydrochloric acid, and nitric acid, all of which are strong acids, and are expected to promote the thermal decomposition of wood materials and suppress the amount of heat generated during combustion. On the other hand, it is necessary to use powerful drugs when formulating incombustible chemicals for wood materials, and the danger that the prepared incombustible chemicals for wood materials will be significantly inclined to acidity and the material quality and quality of wood materials to be processed will deteriorate. High nature.
Carbonic acid is an inorganic acid other than the above-mentioned inorganic acid, but as is well known, carbonic acid is unstable, and when carbonic acid is used as an incombustible agent for wood material, it is removed as carbon dioxide from the incombustible agent for wood material, There is an extremely high risk that guanidine and guanylurea, which are the main ingredients, are deposited during storage or during impregnation.

Therefore, in the invention described in Patent Document 7, the solubility of guanidine was increased by using phosphoric acid which is a medium acid and has no volatility, and succeeded in preparing an incombustible chemical for woody materials.
However, phosphoric acid is a deliquescent agent, and as described above, the incombustible wood material produced using it is extremely hygroscopic, and it is the moisture that it absorbs when placed under high humidity conditions. Phosphoric acid oozed out onto the surface of the woody material.

In order to increase the solubility of guanidine and guanylurea, it was considered to use an organic acid as the remaining method. Compared to strong inorganic acids such as sulfuric acid and hydrochloric acid, organic acids are relatively mild acids, and safety during work such as preparation of incombustible chemicals for wood materials is ensured. However, using an organic acid as a part of the flame retardant for wood materials brings more organic materials into the wood material. Unlike inorganic acids, organic acids are pyrolyzed to carbon dioxide and water with heating, generating heat, resulting in an increase in the amount of heat generated by pyrolysis of the treated wood material, In the exothermic test, there was a concern that the total calorific value in 20 minutes could not achieve 8 MJ / m ² or less, which is the certified reference value for non-combustible materials.
However, as will be described later, several experiments were conducted thereafter, the manufacturing method was established, and the present invention was completed.

  The flame retardant for woody material according to claim 1 of the present invention is characterized in that a phosphate of a basic nitrogen compound is dissolved at a solubility higher than its solubility using carboxylic acid or its anhydride. is there.

  The incombustible chemical for woody material according to claim 2 of the present invention is characterized in that 200 g or more of the basic nitrogen compound according to claim 1 is dissolved in 1000 ml of water.

  The flame retardant for wood material according to claim 3 of the present invention is such that the basic nitrogen compound in the flame retardant for wood material according to claim 1 is guanidine, guanylurea, or a mixture thereof. It is a feature.

  The wood material incombustible agent according to claim 4 of the present invention is such that the carboxylic acid or anhydride thereof in the wood material incombustible agent according to claim 1, 2 or 3 is a divalent or higher polyvalent carboxylic acid. It is characterized by.

  The flame retardant agent for wood material according to claim 5 of the present invention is a divalent or higher polyvalent carboxylic acid in the flame retardant agent for wood material according to claim 4, wherein oxalic acid, malonic acid, succinic acid, glutaric acid, One of maleic acid, malic acid, tartaric acid, tricarballylic acid, citric acid, and butanetetracarboxylic acid, or a mixture of two or more thereof.

The method for producing an incombustible agent for a woody material according to claim 6 of the present invention is characterized in that a phosphate of a basic nitrogen compound is dissolved to a degree higher than its solubility using a carboxylic acid or an anhydride thereof. Is.
By slightly heating when preparing the flame retardant for woody material, the dissolution rate increases and an aqueous solution can be efficiently prepared. The step of dissolving the carboxylic acid or its anhydride in water and the step of dissolving the phosphate of the basic nitrogen compound do not have to be in that order. There is no problem.

According to a seventh aspect of the present invention, there is provided a method for making a wood material incombustible by impregnating and applying any one of the wood material incombustible agents according to claims 1 to 5 and then drying the wood material. It is a feature.
In addition, although the method of impregnation is not ask | required, the immersion method to the incombustible chemical | medical agent for wood materials, a pressurization type injection method, etc. can be mentioned. In addition, the drying mentioned here is preferably artificial drying, but may be natural drying. The heating means for the artificial drying may be natural energy such as solar heat, direct or indirect heating with a steam boiler, or dielectric heating with high frequency or the like. It is also effective to blow or keep the pressure reduced. The heating temperature is more preferably 35 ° C to 90 ° C.
Further, the woody material referred to here refers to lignocellulosic materials such as wood and bamboo, and products made from these materials, such as laminated wood, fiberboard, and particle board.

  The incombustible wood material according to claim 8 of the present invention is obtained by impregnating and applying any one of the incombustible agents for wood material according to claims 1 to 5 and then drying the wood material. Is.

  According to the flame-retardant agent for wood material according to the present invention, the phosphate of the basic nitrogen compound has a low hygroscopic agent, and by using it to prepare the flame-retardant wood material, in the flame-retardant wood material Problems such as “Hygroscopicity” and “Bleeding of non-combustible chemicals” that have been a long-standing concern can be solved. However, phosphates of basic nitrogen compounds are less soluble in water than drugs with extremely high hygroscopic properties such as phosphoric acid and ammonium phosphate, so if only those drugs are dissolved, the wood material No incombustibility was achieved. In the present invention, by using an organic acid, the solubility of the phosphate of the basic nitrogen compound is increased, and a chemical solution having a concentration necessary for achieving incombustibility of the wood material by one injection process is prepared. I was able to. By treating the wood material using this, it is expected that a non-combustible wood material having low hygroscopicity and no drug exudation can be created, and its use is expected to expand dramatically.

  Hereinafter, some examples will be introduced, but the contents described here are not all, and the scope of claims of the present patent is not limited by these.

As a carboxylic acid, 90 g of succinic acid was added to 1000 ml of water with stirring, and then 480 to 600 g of a drug composed of guanidine and phosphoric acid at a weight ratio of 3: 2 was added. At this time, all the drugs were dissolved at room temperature to obtain a transparent solution.
As shown in Comparative Example 1 to be described later, when 480 g of guanidine and phosphoric acid consisting of 3: 2 was added to 1000 ml without adding succinic acid, all of the drugs could not be dissolved at room temperature. From the addition of succinic acid as a carboxylic acid, guanidine phosphate, a basic nitrogen compound, dissolves in excess of its solubility (15.5 g / ml, 20 ° C.) and is used for non-combustible treatment of wood materials. It is clear that an incombustible chemical for wood materials has been prepared.

A cedar slab slab plate (thickness 15 mm, plate width 120 mm, fiber direction length 120 mm) with a density of 0.36 g / cm ³ sufficiently dried at 60 ° C. was obtained by using guanidine and phosphoric acid shown in Example 1. Submerged in 550 g of succinic acid and 550 g of succinic acid in 1000 ml of water, in a non-combustible chemical for wood materials, using a pressurized can, reduced pressure of about 50 hPa for 45 minutes, followed by about 1.2 MPa Was impregnated under the condition of 1.5 hours. At that time, the permeability of the same solution (wood material incombustible agent) was good, and an injection amount according to the theoretical maximum value was obtained.
Then, it dried until it became constant weight at 60 degreeC using the ventilation type dryer. This was conditioned at 23 ° C in a constant temperature and humidity chamber with a relative humidity of 50% until equilibrium was reached, then cut so that the plate surface was 100 mm square, and subjected to a heat generation test using a cone calorimeter. did.
As a result, the total calorific value in 20 minutes was 4.70 MJ / m ² , which was a value of 8 MJ / m ² or less, which is the certified reference value for non-combustible materials. Moreover, the standard as an incombustible wood material was satisfy | filled, without the through-cracking and the heat release rate exceeding 200 kw / m < ² > being observed. Furthermore, the equilibrium moisture content at 30 ° C. and 90% relative humidity of this incombustible wood material was 12.6%, which was clearly lower than that of the untreated wood material (19.2%).

Comparative Example 1
480 g of a drug composed of guanidine and phosphoric acid in a weight ratio of 3: 2 was added to 1000 ml of water and stirred well at room temperature, but all the drugs could not be dissolved, and the drugs that could not be dissolved A considerable amount precipitated. The amount was expected to be more than 1/3 of the added drug.
The supernatant of the liquid thus obtained was taken, and the same treatment as in Example 1 and the exothermic test were conducted. As a result, the total calorific value in 20 minutes was 14.6 MJ / m ² , which was based on the incombustible material certification standard. A certain value of 8 MJ / m ² or less could not be satisfied.

As a carboxylic acid, 120 g of succinic acid was added to 1000 ml of water while stirring, and 330 g of a drug composed of guanidine and phosphoric acid in a weight ratio of 3: 2 and guanylurea and phosphoric acid in a weight ratio of 1: 1 were added. 220 grams of drug was added. At this time, all the chemical | medical agents melt | dissolved at room temperature and obtained the transparent solution (incombustible chemical | medical agent for wooden materials).
As shown in Comparative Example 2, which will be described later, without adding succinic acid, 330 g of a drug in which guanidine and phosphoric acid are configured at a weight ratio of 3: 2, and guanylurea and phosphoric acid are configured at a weight ratio of 1: 1. When 220 g of the added drug was added to 1000 ml of water, these drugs could not be completely dissolved at room temperature. Therefore, by adding succinic acid, the phosphates of these basic nitrogen compounds had their solubility (8 It is clear that an incombustible agent for wood material can be prepared which dissolves in excess of 0.5 g / 100 ml) and is used for the incombustibility treatment of wood material.

After the cedar test piece was treated in the same manner as in Example 1 using the wood material incombustible agent prepared in Example 2, it was further subjected to a heat generation test using a corn calorimeter in the same manner as in Example 1.
As a result, the total calorific value in 20 minutes was 4.58 MJ / m ² , which was a value of 8 MJ / m ² or less, which is the certified reference value for incombustible materials. Moreover, the standard as a nonflammable material was satisfy | filled, without the through-cracking and the heat generation rate exceeding 200 kw / m < ² > being observed. Furthermore, the equilibrium moisture content at 30 ° C. and 90% relative humidity of the incombustible wood material was 15.6%, which was clearly lower than that of the untreated wood material (19.2%).

Comparative Example 2
330 g of a drug composed of guanidine and phosphoric acid in a weight ratio of 3: 2 and 220 g of a drug composed of guanylurea and phosphoric acid in a weight ratio of 1: 1 were added. Although it was sufficiently stirred at room temperature, not all of the drug could be dissolved, and a considerable amount of the drug that could not be dissolved was precipitated. The amount was expected to be more than 1/3 of the added drug.

Instead of the succinic acid shown in Example 1, 90 g of butanetetracarboxylic acid was added to 1000 ml of water, and then a drug composed of 350 g of guanidine and 200 g of phosphoric acid was added. At this time, all the chemical | medical agents melt | dissolved at room temperature and obtained the transparent solution (incombustible chemical | medical agent for wooden materials).
As shown in Comparative Example 3 described later, when a drug consisting of 350 g of guanidine and 200 g of phosphoric acid was added to 1000 ml of water without adding butanetetracarboxylic acid, the drug could not be completely dissolved at room temperature. By the addition of butanetetracarboxylic acid as carboxylic acid, the phosphate of guanidine was dissolved beyond its solubility (15.5 g / 100 ml), and an incombustible agent for wood materials used for incombustibility treatment of wood materials could be prepared. It is clear.

After processing the cedar test piece in the same manner as in Example 1 using the wood material incombustible agent obtained in Example 3, a heat generation test using a corn calorimeter was further carried out in the same manner as in Example 1. The total calorific value was 4.55 MJ / m ² , which was a value of 8 MJ / m ² or less, which is the certified reference value for incombustible materials. Moreover, the standard as a nonflammable material was satisfy | filled, without the through-cracking and the heat generation rate exceeding 200 kw / m < ² > being observed. Furthermore, the equilibrium moisture content at 30 ° C. and 90% relative humidity of the incombustible wood material was 22.4%, which was slightly higher than that of the untreated wood (19.2%). No drug oozing was observed as seen with the treatment.

Comparative Example 3
A drug composed of 350 g of guanidine and 200 g of phosphoric acid was added to 1000 ml of water and stirred sufficiently at room temperature. However, all the drugs could not be dissolved, and a considerable amount of the drug that could not be dissolved was precipitated. The amount was expected to be more than 1/3 of the added drug.

Comparative Example 4
After 120 g of phosphoric acid was dissolved in 1000 ml of water, a drug containing 330 g of guanidine and 270 g of phosphoric acid was added. At this time, all the drugs were dissolved at room temperature to obtain a transparent solution. When the same treatment as in Example 2 was performed and the same exothermic test as in Example 2 was performed, the total calorific value in 20 minutes was 5.12 MJ / m ² , etc. Satisfied.
However, the equilibrium moisture content of the treated wood at 30 ° C. and 90% relative humidity is 56%, much higher than that of the untreated wood (19.2%), and the bound water taken into the cell wall. In addition, free water was clearly present in the intracellular pores, and stickiness due to the exudation of the drug was observed from the wood surface, and the filter paper placed under the test piece during humidity conditioning was contaminated.

  Instead of the succinic acid shown in Example 1, 76 g of succinic anhydride was added to 1000 ml of water, and then a drug composed of 350 g of guanidine and 200 g of phosphoric acid was added. At this time, all the chemical | medical agents melt | dissolved at room temperature, and obtained the transparent solution (incombustible chemical | medical agent for woody materials).

After the cedar test piece was treated in the same manner as in Example 1 using the solution obtained in Example 4, a heat generation test using a cone calorimeter was further conducted in the same manner as in Example 1, and the total calorific value in 20 minutes. It became the 5.02MJ / m ^2, and the a 8 MJ / m ² or less of the value is certified reference value of the noncombustible material. Moreover, the standard as a nonflammable material was satisfy | filled, without the through-cracking and the heat generation rate exceeding 200 kw / m < ² > being observed. Furthermore, the equilibrium moisture content at 30 ° C. and 90% relative humidity of the treated wood was 16.4%, which was lower than that of untreated wood (19.2%).

  Instead of the succinic acid shown in Example 1, 90 g of oxalic acid was added to 1000 ml of water, and then a drug composed of 350 g of guanidine and 200 g of phosphoric acid was added. At this time, all the chemical | medical agents melt | dissolved at room temperature, and obtained the transparent solution (incombustible chemical | medical agent for woody materials).

After the cedar test piece was treated in the same manner as in Example 1 using the solution obtained in Example 5, a exothermal test using a cone calorimeter was further conducted in the same manner as in Example 1, and the total calorific value in 20 minutes. Was 6.22 MJ / m ² , which was a value of 8 MJ / m ² or less, which is a certified reference value for incombustible materials. Moreover, the standard as a nonflammable material was satisfy | filled, without the through-cracking and the heat generation rate exceeding 200 kw / m < ² > being observed. Furthermore, the equilibrium moisture content at 30 ° C. and 90% relative humidity of the treated wood was 21.5%, which was slightly higher than that of untreated wood (19.2%). No drug oozing as seen with the treatment was observed.

  Instead of succinic acid shown in Example 1, 90 g of malonic acid was added to 1000 ml of water, and then a drug composed of 350 g of guanidine and 200 g of phosphoric acid was added. At this time, all the chemical | medical agents melt | dissolved at room temperature, and obtained the transparent solution (incombustible chemical | medical agent for woody materials).

After the cedar test piece was treated in the same manner as in Example 1 using the solution obtained in Example 6, a heat generation test with a cone calorimeter was further conducted in the same manner as in Example 1, and the total calorific value in 20 minutes. It became the 6.08MJ / m ^2, and the a 8 MJ / m ² or less of the value is certified reference value of the noncombustible material. Moreover, the standard as a nonflammable material was satisfy | filled, without the through-cracking and the heat generation rate exceeding 200 kw / m < ² > being observed. Furthermore, the equilibrium moisture content at 30 ° C. and 90% relative humidity of the treated wood was 20.8%, which was slightly higher than that of untreated wood (19.2%). No drug oozing as seen with the treatment was observed.

  Instead of succinic acid shown in Example 1, 90 g of glutaric acid was added to 1000 ml of water, and then a drug composed of 350 g of guanidine and 200 g of phosphoric acid was added. At this time, all the chemical | medical agents melt | dissolved at room temperature, and obtained the transparent solution (incombustible chemical | medical agent for woody materials).

After the cedar test piece was treated in the same manner as in Example 1 using the solution obtained in Example 7, the exothermic test with a cone calorimeter was further conducted in the same manner as in Example 1, and the total calorific value in 20 minutes. Was 5.88 MJ / m ² , which was a value of 8 MJ / m ² or less, which is the certified reference value for non-combustible materials. Moreover, the standard as a nonflammable material was satisfy | filled, without the through-cracking and the heat generation rate exceeding 200 kw / m < ² > being observed. Further, the equilibrium moisture content at 30 ° C. and 90% relative humidity of the treated wood was 23.2%, which was slightly higher than that of untreated wood (19.2%). No drug oozing as seen with the treatment was observed.

  Instead of the succinic acid shown in Example 1, 78 g of glutaric anhydride was added to 1000 ml of water, and then a drug composed of 350 g of guanidine and 200 g of phosphoric acid was added. At this time, all the chemical | medical agents melt | dissolved at room temperature, and obtained the transparent solution (incombustible chemical | medical agent for woody materials).

After the cedar test piece was treated in the same manner as in Example 1 using the solution obtained in Example 8, a exothermal test with a cone calorimeter was further conducted in the same manner as in Example 1, and the total calorific value in 20 minutes. It became the 5.46MJ / m ^2, and the a 8 MJ / m ² or less of the value is certified reference value of the noncombustible material. Moreover, the standard as a nonflammable material was satisfy | filled, without the through-cracking and the heat generation rate exceeding 200 kw / m < ² > being observed. Furthermore, the equilibrium moisture content at 30 ° C. and 90% relative humidity of the treated wood was 22.3%, which was slightly higher than that of untreated wood (19.2%). No drug oozing as seen with the treatment was observed.

  Instead of succinic acid shown in Example 1, 90 g of maleic acid was added to 1000 ml of water, and then a drug composed of 350 g of guanidine and 200 g of phosphoric acid was added. At this time, all the chemical | medical agents melt | dissolved at room temperature, and obtained the transparent solution (incombustible chemical | medical agent for woody materials).

After the cedar test piece was treated in the same manner as in Example 1 using the solution obtained in Example 9, a exothermal test with a cone calorimeter was further conducted in the same manner as in Example 1 to find the total calorific value in 20 minutes. It became the 5.33MJ / m ^2, and the a 8 MJ / m ² or less of the value is certified reference value of the noncombustible material. Moreover, the standard as a nonflammable material was satisfy | filled, without the through-cracking and the heat generation rate exceeding 200 kw / m < ² > being observed. Furthermore, the equilibrium moisture content at 30 ° C. and 90% relative humidity of the treated wood was 19.2%, which was the same moisture content as that of the untreated wood (19.2%).

  Instead of succinic acid shown in Example 1, 90 g of malic acid was added to 1000 ml of water, and then a drug composed of 350 g of guanidine and 200 g of phosphoric acid was added. At this time, all the chemical | medical agents melt | dissolved at room temperature, and obtained the transparent solution (incombustible chemical | medical agent for woody materials).

After the cedar test piece was treated in the same manner as in Example 1 using the solution obtained in Example 10, a exothermal test with a cone calorimeter was further conducted in the same manner as in Example 1 to find the total calorific value in 20 minutes. It became the 4.47MJ / m ^2, and the a 8 MJ / m ² or less of the value is certified reference value of the noncombustible material. Moreover, the standard as a nonflammable material was satisfy | filled, without the through-cracking and the heat generation rate exceeding 200 kw / m < ² > being observed. Further, the equilibrium moisture content at 30 ° C. and 90% relative humidity of the treated wood was 22.8%, which was slightly higher than that of untreated wood (19.2%). No drug oozing as seen with the treatment was observed.

  Instead of succinic acid shown in Example 1, 90 g of tartaric acid was added to 1000 ml of water, and then a drug composed of 350 g of guanidine and 200 g of phosphoric acid was added. At this time, all the chemical | medical agents melt | dissolved at room temperature, and obtained the transparent solution (incombustible chemical | medical agent for woody materials).

After the cedar test piece was treated in the same manner as in Example 1 using the solution obtained in Example 11, a heat generation test using a cone calorimeter was further conducted in the same manner as in Example 1, and the total calorific value in 20 minutes. Was 4.98 MJ / m ² , which was a value of 8 MJ / m ² or less, which is the certified reference value for non-combustible materials. Moreover, the standard as a nonflammable material was satisfy | filled, without the through-cracking and the heat generation rate exceeding 200 kw / m < ² > being observed. Further, the equilibrium moisture content at 30 ° C. and 90% relative humidity of the treated wood was 22.1%, which was slightly higher than that of untreated wood (19.2%). No drug oozing as seen with the treatment was observed.

  Instead of succinic acid shown in Example 1, 90 g of tricarballylic acid was added to 1000 ml of water, and then a drug composed of 350 g of guanidine and 200 g of phosphoric acid was added. At this time, all the chemical | medical agents melt | dissolved at room temperature, and obtained the transparent solution (incombustible chemical | medical agent for woody materials).

After the cedar test piece was treated in the same manner as in Example 1 using the solution obtained in Example 12, a exothermal test using a cone calorimeter was further conducted in the same manner as in Example 1, and the total calorific value in 20 minutes. It became the 5.26MJ / m ^2, and the a 8 MJ / m ² or less of the value is certified reference value of the noncombustible material. Moreover, the standard as a nonflammable material was satisfy | filled, without the through-cracking and the heat generation rate exceeding 200 kw / m < ² > being observed. Furthermore, the equilibrium moisture content at 30 ° C. and 90% relative humidity of the treated wood was 21.1%, which was slightly higher than that of untreated wood (19.2%). No drug oozing as seen with the treatment was observed.

  In place of the succinic acid shown in Example 1, 90 g of citric acid was added to 1000 ml of water, and then guanidine. A drug composed of 350 g and phosphoric acid 200 g was added. At this time, all the chemical | medical agents melt | dissolved at room temperature, and obtained the transparent solution (incombustible chemical | medical agent for woody materials).

After the cedar test piece was treated in the same manner as in Example 1 using the solution obtained in Example 13, a heat generation test with a cone calorimeter was further carried out in the same manner as in Example 1. As a result, the total calorific value in 20 minutes was obtained. It became the 5.22MJ / m ^2, and the a 8 MJ / m ² or less of the value is certified reference value of the noncombustible material. Moreover, the standard as a nonflammable material was satisfy | filled, without the through-cracking and the heat generation rate exceeding 200 kw / m < ² > being observed. Furthermore, the equilibrium moisture content at 30 ° C. and 90% relative humidity of the treated wood was 20.4%, which was slightly higher than that of untreated wood (19.2%). No drug oozing as seen with the treatment was observed.

Claims (8)

  A fireproofing agent for woody materials, characterized in that a carboxylic acid or an anhydride thereof is dissolved in water and a phosphate of a basic nitrogen compound is dissolved at a solubility higher than that.   2. The incombustible agent for woody material according to claim 1, wherein the basic nitrogen compound phosphate is dissolved together with carboxylic acid in an amount of 200 g or more per 1000 ml of water.   The flame retardant agent for woody materials according to claim 1 or 2, wherein the basic nitrogen compound is guanidine, guanylurea, or a mixture thereof.   The incombustible chemical for woody material according to claim 1, 2 or 3, wherein the carboxylic acid or its anhydride is a polyvalent carboxylic acid.   The polyvalent carboxylic acid is oxalic acid, malonic acid, succinic acid, glutaric acid, maleic acid, malic acid, tartaric acid, tricarballylic acid, citric acid, butanetetracarboxylic acid, or two or more of them The flame retardant agent for woody materials according to claim 4, which is a mixture.   Incombustibility for woody materials characterized by dissolving phosphate of basic nitrogen compound more than solubility by dissolving carboxylic acid or its anhydride and phosphate of basic nitrogen compound in water A method for producing a drug.   A method for incombustibility of a wood material, comprising: a step of impregnating the wood material with the flame retardant for wood material according to claim 1; and a step of drying the wood.   An incombustible wood material which has been incombustible by the method for incombusting wood material according to claim 7.