JP7080289B2 - Flame-retardant chemicals, non-combustible wood using them, and methods for adjusting flame-retardant chemicals - Google Patents

Flame-retardant chemicals, non-combustible wood using them, and methods for adjusting flame-retardant chemicals Download PDF

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JP7080289B2
JP7080289B2 JP2020161579A JP2020161579A JP7080289B2 JP 7080289 B2 JP7080289 B2 JP 7080289B2 JP 2020161579 A JP2020161579 A JP 2020161579A JP 2020161579 A JP2020161579 A JP 2020161579A JP 7080289 B2 JP7080289 B2 JP 7080289B2
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JP2021055088A (en
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祥太郎 川村
拓哉 宮村
篤史 渡邊
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Daikin Industries Ltd
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本発明は、難燃化薬液、それを用いた不燃木材及び難燃化薬液の調整方法に関するものである。 The present invention relates to a flame-retardant chemical solution , a non-combustible wood using the same, and a method for adjusting the flame-retardant chemical solution .

近年、国産の木材の利用拡大等を図るために、例えば、天然木等の木質基材に難燃剤が溶解された難燃化薬液を含浸させた不燃木材が注目されている。 In recent years, in order to expand the use of domestically produced wood, for example, non-combustible wood in which a wood base material such as natural wood is impregnated with a flame retardant chemical solution in which a flame retardant is dissolved has attracted attention.

例えば、特許文献1には、ホウ酸及びホウ砂がそれぞれの単独化合物の溶解度を超える量で含有されてなる安定なホウ素化合物の液状組成物が開示されている。 For example, Patent Document 1 discloses a stable liquid composition of a boron compound containing boric acid and borax in an amount exceeding the solubility of each single compound.

特許第5079983号公報Japanese Patent No. 5097983

ところで、特許文献1に開示された安定なホウ素化合物の液状組成物では、100℃の沸騰水にホウ酸及びホウ砂を溶解させ、木材に含浸する含浸処理を高温(例えば、90℃以上)で行う必要があるので、含浸処理の作業性が悪くなってしまう。 By the way, in the liquid composition of a stable boron compound disclosed in Patent Document 1, boric acid and borax are dissolved in boiling water at 100 ° C., and the impregnation treatment of impregnating wood is performed at a high temperature (for example, 90 ° C. or higher). Since it is necessary to perform the impregnation process, the workability of the impregnation process is deteriorated.

本発明は、かかる点に鑑みてなされたものであり、その目的とするところは、可及的に低温で且つ高濃度で含浸処理が可能な難燃化薬液を提供することにある。 The present invention has been made in view of this point, and an object of the present invention is to provide a flame-retardant chemical solution capable of impregnation treatment at a low temperature and a high concentration as much as possible.

上記目的を達成するために、本発明は、ホウ酸及びホウ砂の他に、所定量のホウ酸アンモニウムを含有させるようにしたものである。 In order to achieve the above object, the present invention contains a predetermined amount of ammonium borate in addition to boric acid and borax.

具体的に本発明に係る難燃化薬液は、100質量部の水に対して、5質量部~75質量部のホウ酸、10質量部~80質量部のホウ砂、及び1質量部~50質量部のホウ酸アンモニウムが含有され、リン酸アンモニウム、リン酸水素二アンモニウム、リン酸二水素アンモニウム、炭酸アンモニウム、炭酸水素アンモニウム、炭酸カリウム、エチレングリコール及びポリエチレングリコールが含有されていないことを特徴とする。 Specifically, the flame-retardant chemical solution according to the present invention contains 5 parts by mass to 75 parts by mass of boric acid, 10 parts by mass to 80 parts by mass of boric acid, and 1 part by mass to 50 parts by mass with respect to 100 parts by mass of water. It is characterized by containing parts by weight of ammonium borate and not containing ammonium phosphate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate, ammonium carbonate, ammonium hydrogen carbonate, potassium carbonate, ethylene glycol and polyethylene glycol . do.

上記の構成によれば、100質量部の水に対して、5質量部~75質量部のホウ酸、10質量部~80質量部のホウ砂、及び1質量部~50質量部のホウ酸アンモニウムが含有されている。そのため、例えば、80℃の水にホウ酸、ホウ砂及びホウ酸アンモニウムを高濃度で溶解させた後に、60℃に冷えても固形分が析出し難い難燃化薬液を実現することができる。これにより、木質基材に難燃化薬液を含浸する含浸処理を60℃程度の低い温度で行うことができるので、可及的に低温で且つ高濃度で含浸処理が可能な難燃化薬液を提供することができる。 According to the above configuration, 5 parts by mass to 75 parts by mass of boric acid, 10 parts by mass to 80 parts by mass of borax, and 1 part by mass to 50 parts by mass of ammonium borate with respect to 100 parts by mass of water. Is contained. Therefore, for example, it is possible to realize a flame-retardant chemical solution in which boric acid, borax and ammonium borate are dissolved in water at 80 ° C. at a high concentration and then solids are less likely to precipitate even when cooled to 60 ° C. As a result, the impregnation treatment of impregnating the wood substrate with the flame-retardant chemical solution can be performed at a low temperature of about 60 ° C., so that the flame-retardant chemical solution capable of impregnation treatment at a low temperature and a high concentration can be obtained. Can be provided.

ホウ素の含有量は、5mol/L以上であってもよい。 The boron content may be 5 mol / L or more.

上記の構成によれば、5分間の総発熱量が8MJ/mを超えない、という難燃の要件を満たすことができる。 According to the above configuration, the flame retardant requirement that the total calorific value for 5 minutes does not exceed 8 MJ / m 2 can be satisfied.

ホウ素の含有量は、11mol/L以上であってもよい。 The boron content may be 11 mol / L or more.

上記の構成によれば、20分間の総発熱量が8MJ/mを超えない、という不燃の要件を満たすことができる。 According to the above configuration, the non-combustible requirement that the total calorific value for 20 minutes does not exceed 8 MJ / m 2 can be satisfied.

また、本発明に係る不燃木材は、上述した難燃化薬液が木質基材に含浸されていることを特徴とする。 Further, the non-combustible wood according to the present invention is characterized in that the wood base material is impregnated with the above-mentioned flame-retardant chemical solution.

上記の構成によれば、例えば、難燃化薬液におけるホウ素の含有量が11mol/L以上である場合には、不燃木材の不燃性を確保することができる。 According to the above configuration, for example, when the content of boron in the flame-retardant chemical solution is 11 mol / L or more, the nonflammability of non-combustible wood can be ensured.

また、本発明に係る難燃化薬液の調整方法は、上述した難燃化薬液を調製する方法であって、70℃~80℃に加温した上記水に上記ホウ酸、上記ホウ砂及び上記ホウ酸アンモニウムを加えて溶解させることを特徴とする。 Further, the method for preparing the flame-retardant chemical solution according to the present invention is the method for preparing the flame-retardant chemical solution described above, wherein the boric acid, the borax and the above-mentioned boric acid, the above-mentioned borax and the above-mentioned water in the water heated to 70 ° C. to 80 ° C. It is characterized in that ammonium borate is added and dissolved.

本発明によれば、ホウ酸及びホウ砂の他に、所定量のホウ酸アンモニウムが含有されているので、可及的に低温で且つ高濃度で含浸処理が可能な難燃化薬液を提供することができる。 According to the present invention, since a predetermined amount of ammonium borate is contained in addition to boric acid and borax, a flame-retardant chemical solution capable of impregnation treatment at a low temperature and a high concentration as possible is provided. be able to.

本発明の第1の実施形態に係る難燃化薬液を用いて含浸処理した不燃木材の断面図である。It is sectional drawing of the non-combustible wood impregnated with the flame-retardant chemical liquid which concerns on 1st Embodiment of this invention. 本発明の第1の実施形態に係る難燃化薬液におけるホウ酸/ホウ砂の各配合におけるホウ酸アンモニウムの最大溶解量を示す表である。It is a table which shows the maximum dissolution amount of ammonium borate in each composition of boric acid / borax in the flame retardant chemical solution which concerns on 1st Embodiment of this invention. 本発明の第1の実施形態に係る難燃化薬液におけるホウ酸アンモニウム未添加(0質量部)の場合のホウ酸/ホウ砂の各配合における溶解性を示す表である。It is a table which shows the solubility in each composition of boric acid / borax when ammonium borate is not added (0 part by mass) in the flame retardant chemical solution which concerns on 1st Embodiment of this invention. 本発明の第1の実施形態に係る難燃化薬液におけるホウ酸アンモニウム添加(15質量部)の場合のホウ酸/ホウ砂の各配合における溶解性を示す表である。It is a table which shows the solubility in each composition of boric acid / borax in the case of addition of ammonium borate (15 parts by mass) in the flame retardant chemical solution which concerns on 1st Embodiment of this invention. 本発明の第1の実施形態に係る難燃化薬液におけるホウ酸アンモニウム添加(30質量部)の場合のホウ酸/ホウ砂の各配合における溶解性を示す表である。It is a table which shows the solubility in each composition of boric acid / borax in the case of addition of ammonium borate (30 parts by mass) in the flame retardant chemical solution which concerns on 1st Embodiment of this invention. 本発明の第1の実施形態に係る難燃化薬液におけるホウ酸アンモニウム添加(50質量部)の場合のホウ酸/ホウ砂の各配合における溶解性を示す表である。It is a table which shows the solubility in each composition of boric acid / borax in the case of addition of ammonium borate (50 parts by mass) in the flame retardant chemical solution which concerns on 1st Embodiment of this invention. 本発明の第1の実施形態に係る難燃化薬液における薬液固形分量と発熱性試験の総発熱量との関係を示すグラフである。It is a graph which shows the relationship between the amount of solids of a chemical solution in the flame-retardant chemical solution which concerns on 1st Embodiment of this invention, and the total calorific value of the exothermic test. 本発明の第1の実施形態に係る難燃化薬液におけるホウ素モル濃度と発熱性試験の総発熱量との関係を示す表である。It is a table which shows the relationship between the boron molar concentration in the flame retardant chemical solution which concerns on 1st Embodiment of this invention, and the total calorific value of the exothermic test. 本発明の第1の実施形態に係る難燃化薬液を用いた不燃木材の吸湿性を示すグラフである。It is a graph which shows the hygroscopicity of the non-combustible wood which used the flame-retardant chemical liquid which concerns on 1st Embodiment of this invention.

以下、本発明の実施形態を詳細に説明する。なお、本発明は、以下の各実施形態に限定されるものではない。 Hereinafter, embodiments of the present invention will be described in detail. The present invention is not limited to the following embodiments.

《第1の実施形態》
図1~図3は、本発明に係る難燃化薬液及びそれを用いた不燃木材の第1の実施形態を示している。ここで、図1は、本実施形態の難燃化薬液を用いて含浸処理した不燃木材10の断面図である。
<< First Embodiment >>
1 to 3 show a first embodiment of a flame-retardant chemical solution according to the present invention and non-combustible wood using the same. Here, FIG. 1 is a cross-sectional view of the non-combustible wood 10 impregnated with the flame-retardant chemical solution of the present embodiment.

不燃木材10は、図1に示すように、木質基材5と、木質基材5の内部に含浸された難燃剤6とを備えている。 As shown in FIG. 1, the non-combustible wood 10 includes a wood base material 5 and a flame retardant 6 impregnated inside the wood base material 5.

木質基材5は、例えば、無垢材、集成材、合板、LVL(Laminated Veneer Lumber)、パーティクルボード等である。また、木質基材5を構成する樹種には、限定されないが、例えば、オーク、バーチ、ビーチ、チェリー等の硬い樹種や、スギ、ツガ、ヒノキ、サワグルミ等の軟らかい樹種等が用いられる。 The wood base material 5 is, for example, solid wood, laminated wood, plywood, LVL (Laminated Veneer Lumber), particle board, or the like. Further, the tree species constituting the wood base material 5 are not limited, and for example, hard tree species such as oak, birch, beach, and cherry, and soft tree species such as sugi, hemlock, cypress, and pterocarya rhois are used.

難燃剤6は、本実施形態の難燃化薬液に溶解された溶質である。ここで、本実施形態の難燃化薬液は、後述する実験の結果に基づいて、100質量部の水に対して、5質量部~75質量部のホウ酸(B(OH))、10質量部~80質量部のホウ砂(Na・10HO)、及び1質量部~50質量部のホウ酸アンモニウム((NHO・5B・8HO)が含有されている。また、本実施形態の難燃化薬液では、ホウ素の含有量が5mol/L以上であり、好ましくは11mol/L以上である。なお、本実施形態の難燃化薬液に用いる水は、特に、制限されるものではないが、イオン交換水、蒸留水、水道水、工業用水等である。 The flame retardant 6 is a solute dissolved in the flame retardant chemical solution of the present embodiment. Here, the flame-retardant chemical solution of the present embodiment has 5 parts by mass to 75 parts by mass of boric acid (B (OH) 3 ) 10 with respect to 100 parts by mass of water, based on the results of experiments described later. From 1 part by mass to 80 parts by mass of boric acid (Na 2 B 4 O 7.10H 2 O) and 1 part to 50 parts by mass of ammonium borate ((NH 4 ) 2 O ・ 5B 2 O 3.8H 2 O) ) Is contained. Further, in the flame-retardant chemical solution of the present embodiment, the boron content is 5 mol / L or more, preferably 11 mol / L or more. The water used for the flame-retardant chemical solution of the present embodiment is not particularly limited, but is ion-exchanged water, distilled water, tap water, industrial water, and the like.

上記構成の不燃木材10は、例えば、80℃程度に加温した水に、所定量のホウ酸、ホウ砂及びホウ酸アンモニウムを撹拌しながら加えることにより、難燃化薬液を調製した後に、木質基材に難燃化薬液を含浸する含浸処理を60℃程度で行って、乾燥することにより、製造することができる。ここで、含浸処理では、容器内の減圧及び加圧が可能な圧力容器(チャンバ)内に木質基材5を収容し、所定の圧力(例えば、-0.7atm(-0.709MPa)程度)まで減圧して木質基材5内の導管等に含まれる空気を除去した後に、チャンバ内に難燃化薬液を注入し、所定の圧力(例えば、10atm(1.013MPa)程度)まで加圧して木質基材5の空隙に難燃化薬液を含浸する。 The non-combustible wood 10 having the above constitution is made of wood after preparing a flame-retardant chemical solution by adding a predetermined amount of boric acid, borax and ammonium borate to water heated to about 80 ° C. with stirring. It can be produced by impregnating the base material with a flame-retardant chemical solution at about 60 ° C. and drying it. Here, in the impregnation treatment, the wood substrate 5 is housed in a pressure vessel (chamber) capable of depressurizing and pressurizing the inside of the container, and a predetermined pressure (for example, about −0.7 atm (−0.709 MPa)). After removing the air contained in the conduit or the like in the wood substrate 5, the flame-retardant chemical solution is injected into the chamber and pressurized to a predetermined pressure (for example, about 10 atm (1.013 MPa)). The voids of the wood substrate 5 are impregnated with a flame-retardant chemical solution.

次に、本実施形態の難燃化薬液において、100質量部の水に対するホウ酸アンモニウムの含有量を1質量部~50質量部となる理由について、具体的に行った実験に基づいて説明する。ここで、図2は、本実施形態の難燃化薬液におけるホウ酸/ホウ砂の各配合におけるホウ酸アンモニウムの最大溶解量を示す表である。 Next, in the flame-retardant chemical solution of the present embodiment, the reason why the content of ammonium borate with respect to 100 parts by mass of water is 1 part by mass to 50 parts by mass will be described based on a specific experiment. Here, FIG. 2 is a table showing the maximum dissolution amount of ammonium borate in each formulation of boric acid / borax in the flame-retardant chemical solution of the present embodiment.

まず、図2の表に示すように、100質量部の80℃の水に、所定量(0質量部、5質量部、15質量部、30質量部)のホウ酸、及び所定量(0質量部、20質量部、35質量部、50質量部)のホウ砂を溶解させた各水溶液に溶解可能で且つ60℃でも固形分が析出しないホウ酸アンモニウムの含有量(最大溶解量)を求めた。ここで、実験結果としては、図2の表に示すように、100質量部の80℃の水に対して、5質量部のホウ酸、及び20質量部のホウ砂を溶解させたとき、60℃で析出することなく、50質量部のホウ酸アンモニウムを最大で溶解させることができることが分かった。 First, as shown in the table of FIG. 2, a predetermined amount (0 parts by mass, 5 parts by mass, 15 parts by mass, 30 parts by mass) of boric acid and a predetermined amount (0 parts by mass) are added to 100 parts by mass of water at 80 ° C. The content (maximum dissolution amount) of ammonium borate, which can be dissolved in each aqueous solution in which borosand (parts, 20 parts by mass, 35 parts by mass, and 50 parts by mass) is dissolved and solid content does not precipitate even at 60 ° C., was determined. .. Here, as an experimental result, as shown in the table of FIG. 2, when 5 parts by mass of boric acid and 20 parts by mass of borax are dissolved in 100 parts by mass of water at 80 ° C., 60 parts are dissolved. It was found that 50 parts by mass of ammonium borate can be dissolved at the maximum without precipitation at ° C.

また、100質量部の80℃の水に、9質量部のホウ酸、及び15質量部のホウ砂を溶解させた水溶液(ホウ素のモル濃度:3.0mol/L)では、水溶液を5℃に冷却すると、固形分が析出した。しかしながら、100質量部の80℃の水に、9質量部のホウ酸、13質量部のホウ砂、及び1質量部のホウ酸アンモニウムを溶解させた水溶液(ホウ素のモル濃度:3.0mol/L)では、水溶液を5℃に冷却しても、固形分が析出しなかった。これにより、同じホウ素のモル濃度の難燃化薬液においては、ホウ酸及びホウ砂の2種のみで調整するよりも、1質量以上のホウ酸アンモニウムを添加して、ホウ酸、ホウ砂及びホウ酸アンモニウムの3種で調整した方がより低温でも析出し難いことが分かった。 Further, in an aqueous solution (boron molar concentration: 3.0 mol / L) in which 9 parts by mass of boric acid and 15 parts by mass of borax are dissolved in 100 parts by mass of water at 80 ° C., the aqueous solution is adjusted to 5 ° C. Upon cooling, solids were deposited. However, an aqueous solution in which 9 parts by mass of boric acid, 13 parts by mass of hosand, and 1 part by mass of ammonium borate are dissolved in 100 parts by mass of water at 80 ° C. (molar concentration of boron: 3.0 mol / L). ), The solid content did not precipitate even when the aqueous solution was cooled to 5 ° C. As a result, in a flame-retardant chemical solution having the same molar concentration of boron, boric acid, borax and borax are added by adding 1 mass or more of ammonium borate, rather than adjusting with only two types of boric acid and borax. It was found that it was more difficult to precipitate even at lower temperatures when adjusted with three types of ammonium acid.

したがって、100質量部の水に対するホウ酸アンモニウムの含有量は、1質量部~50質量部となる。 Therefore, the content of ammonium borate with respect to 100 parts by mass of water is 1 part by mass to 50 parts by mass.

次に、図3~図6の表に示すように、100質量部の80℃の水に、所定量のホウ酸、所定量のホウ砂、及び所定量のホウ酸アンモニウムを溶解させ、60℃で固形分が析出する(表中の×)/析出しない(表中の〇)を調べた。 Next, as shown in the tables of FIGS. 3 to 6, a predetermined amount of boric acid, a predetermined amount of borax, and a predetermined amount of ammonium borate are dissolved in 100 parts by mass of water at 80 ° C. to 60 ° C. It was examined that the solid content was precipitated (x in the table) / not precipitated (◯ in the table).

実験結果としては、図3~図6の各表中の〇の領域(ハッチング部)がホウ酸アンモニウムの添加量の増加するにつれて、表中の上側にシフトするので、ホウ酸アンモニウムを添加することにより、特にホウ砂を高濃度で溶解させることができ、ホウ酸アンモニウムとホウ砂との間に相乗効果があることが分かった。具体的には、ホウ酸が5質量部~15質量部であり、ホウ砂が40質量部~60質量部である範囲では、ホウ酸アンモニウムが未添加である場合、60℃で固形分が析出したものの、50質量部のホウ酸アンモニウムを添加することにより、60℃で固形分が析出しないようになった。 As an experimental result, as the amount of ammonium borate added increases, the region ◯ (hatching part) in each table of FIGS. 3 to 6 shifts to the upper side in the table, so ammonium borate should be added. It was found that, in particular, borax can be dissolved at a high concentration, and there is a synergistic effect between ammonium borate and borax. Specifically, in the range where boric acid is 5 parts by mass to 15 parts by mass and borax is 40 parts by mass to 60 parts by mass, solid content is precipitated at 60 ° C. when ammonium borate is not added. However, by adding 50 parts by mass of ammonium borate, the solid content did not precipitate at 60 ° C.

次に、本実施形態の難燃化薬液において、ホウ素の含有量が11mol/L以上となる理由について、具体的に行った実験に基づいて説明する。ここで、図7は、本実施形態の難燃化薬液における薬液固形分量と発熱性試験の総発熱量との関係を示すグラフである。 Next, the reason why the boron content of the flame-retardant chemical solution of the present embodiment is 11 mol / L or more will be described based on a specific experiment. Here, FIG. 7 is a graph showing the relationship between the solid content of the chemical solution in the flame-retardant chemical solution of the present embodiment and the total calorific value of the exothermic test.

まず、100質量部の80℃の水に、45質量部のホウ酸、及び35質量部のホウ砂を溶解させた難燃化薬液を調整し、その難燃化薬液を厚さ22mm及び30mmのLVLに含浸させて、不燃木材を作製した。なお、本実験例において、厚さ22mmの不燃木材は、図7のグラフにおける白抜きの四角印であり、厚さ30mmの不燃木材は、図7のグラフにおける白抜きの丸印である。 First, a flame-retardant chemical solution prepared by dissolving 45 parts by mass of boric acid and 35 parts by mass of borax in 100 parts by mass of water at 80 ° C. was prepared, and the flame-retardant chemical solution was prepared to have thicknesses of 22 mm and 30 mm. Incombustible wood was produced by impregnating LVL. In this experimental example, the non-combustible wood having a thickness of 22 mm is a white square mark in the graph of FIG. 7, and the non-combustible wood having a thickness of 30 mm is a white circle mark in the graph of FIG.

また、100質量部の80℃の水に、45質量部のホウ酸、35質量部のホウ砂、及び15質量部のホウ酸アンモニウムを溶解させた難燃化薬液を調整し、その難燃化薬液を厚さ22mm及び30mmのLVLに含浸させて、不燃木材を作製した。なお、本実験例において、厚さ22mmの不燃木材は、図7のグラフにおける塗り潰しの四角印であり、厚さ30mmの不燃木材は、図7のグラフにおける塗り潰しの丸印である。 Further, a flame-retardant chemical solution prepared by dissolving 45 parts by mass of boric acid, 35 parts by mass of borax, and 15 parts by mass of ammonium borate in 100 parts by mass of water at 80 ° C. was prepared to make the flame-retardant. Non-combustible wood was prepared by impregnating LVL having a thickness of 22 mm and 30 mm with a chemical solution. In this experimental example, the non-combustible wood having a thickness of 22 mm is a filled square mark in the graph of FIG. 7, and the non-combustible wood having a thickness of 30 mm is a filled circle mark in the graph of FIG.

上述したように作製した不燃木材(縦100mm×横100mm)について、ISO5660-1に準拠したコーンカロリーメーター試験機を用いて、20分間の総発熱量を測定した。 For the non-combustible wood (length 100 mm × width 100 mm) produced as described above, the total calorific value for 20 minutes was measured using a cone calorimeter tester compliant with ISO5660-1.

実験結果としては、図7のグラフに示すように、LVLの厚さを問わず、ホウ酸/ホウ砂系の難燃剤、及びホウ酸/ホウ砂/ホウ酸アンモニウム系の難燃剤を総括して見ると、総発熱量が8MJ/mを超えないようにするには、難燃化薬液の固形分量が280kg/m以上必要であることが分かった。ここで、280kg/m以上の難燃化薬液の固形分量は、ホウ素のモル濃度に換算すると、10.9mol/L以上に相当するので、不燃木材の不燃性を確保するには、ホウ素の含有量が11mol/L以上あればよい。 As the experimental results, as shown in the graph of FIG. 7, boric acid / borax-based flame retardants and boric acid / borax / ammonium borate flame retardants are summarized regardless of the thickness of LVL. It was found that the solid content of the flame retardant chemical solution must be 280 kg / m 3 or more in order to prevent the total calorific value from exceeding 8 MJ / m 2 . Here, the solid content of the flame-retardant chemical solution of 280 kg / m 3 or more corresponds to 10.9 mol / L or more in terms of the molar concentration of boron. The content may be 11 mol / L or more.

次に、本実施形態の難燃化薬液において、ホウ素の含有量が5mol/L以上となる理由について、具体的に行った実験に基づいて説明する。ここで、図8は、本実施形態の難燃化薬液におけるホウ素モル濃度と発熱性試験の総発熱量との関係を示す表である。 Next, the reason why the boron content of the flame-retardant chemical solution of the present embodiment is 5 mol / L or more will be described based on a specific experiment. Here, FIG. 8 is a table showing the relationship between the molar concentration of boron in the flame-retardant chemical solution of the present embodiment and the total calorific value of the exothermic test.

具体的には、図8の表に示すように、100質量部の70℃の水に、所定量のホウ酸、ホウ砂及びホウ酸アンモニウムを溶解させた難燃化薬液(計5種類)を調整し、それらの難燃化薬液を厚さ22mmのLVLにそれぞれ含浸させて、5種類の不燃木材を作製した。その後、作製した5種類の不燃木材(縦100mm×横100mm)について、ISO5660-1に準拠したコーンカロリーメーター試験機を用いて、5分間の総発熱量を測定した。 Specifically, as shown in the table of FIG. 8, a flame-retardant chemical solution (5 types in total) in which a predetermined amount of boric acid, borax and ammonium borate are dissolved in 100 parts by mass of water at 70 ° C. After adjustment, these flame-retardant chemicals were impregnated into LVL having a thickness of 22 mm, respectively, to prepare five kinds of non-combustible wood. Then, the total calorific value for 5 minutes was measured for the five types of non-combustible wood (length 100 mm × width 100 mm) produced using a cone calorimeter tester compliant with ISO5660-1.

実験結果としては、図8の表に示すように、難燃の要件、すなわち、5分間の総発熱量が8MJ/mを超えないようにするには、ホウ素モル濃度が5mol/L以上必要であることが分かった。ここで、ホウ素モル濃度が3mol/Lであれば、図8の表に示すように、5分間の総発熱量が8MJ/mを超える場合があり、難燃の要件を満たさないことがある。 As a result of the experiment, as shown in the table of FIG. 8, the molar concentration of boron must be 5 mol / L or more in order to prevent the flame retardant requirement, that is, the total calorific value for 5 minutes does not exceed 8 MJ / m 2 . It turned out to be. Here, if the molar concentration of boron is 3 mol / L, the total calorific value for 5 minutes may exceed 8 MJ / m 2 as shown in the table of FIG. 8, and the flame-retardant requirement may not be satisfied. ..

次に、本実施形態の難燃化薬液を用いた不燃木材の吸湿性を評価した。ここで、図9は、本実施形態の難燃化薬液を用いた不燃木材の吸湿性を示すグラフである。 Next, the hygroscopicity of non-combustible wood using the flame-retardant chemical solution of the present embodiment was evaluated. Here, FIG. 9 is a graph showing the hygroscopicity of non-combustible wood using the flame-retardant chemical solution of the present embodiment.

まず、100質量部の80℃の水に、45質量部のホウ酸、及び35質量部のホウ砂を溶解させた難燃化薬液を調整し、その難燃化薬液(ホウ酸アンモニウム未添加)を厚さ30mmのLVLに含浸させて、不燃木材を作製した。 First, a flame-retardant chemical solution prepared by dissolving 45 parts by mass of boric acid and 35 parts by mass of borax in 100 parts by mass of water at 80 ° C. was prepared, and the flame-retardant chemical solution (without ammonium borate added) was prepared. Was impregnated into LVL having a thickness of 30 mm to prepare non-combustible wood.

また、100質量部の80℃の水に、45質量部のホウ酸、35質量部のホウ砂、及び15質量部のホウ酸アンモニウムを溶解させた難燃化薬液(ホウ酸アンモニウム添加)を調整し、その難燃化薬液を厚さ30mmのLVLに含浸させて、不燃木材を作製した。 Further, a flame-retardant chemical solution (added with ammonium borate) prepared by dissolving 45 parts by mass of boric acid, 35 parts by mass of borax, and 15 parts by mass of ammonium borate in 100 parts by mass of water at 80 ° C. Then, the flame-retardant chemical solution was impregnated into LVL having a thickness of 30 mm to prepare non-combustible wood.

上述したように作製した不燃木材(縦100mm×横100mm)について、60℃で恒量に達するまで乾燥した後に、温度40℃及び相対湿度90%に設定された恒温恒湿槽内に入れ、所定時間経過後の重量を測定することにより、吸湿率を測定した。ここで、図9のグラフにおいて、ホウ酸アンモニウム添加の難燃化薬液を用いた不燃木材は、塗り潰しの丸印であり、ホウ酸アンモニウム未添加の難燃化薬液を用いた不燃木材は、白抜きの丸印である。 The non-combustible wood (length 100 mm x width 100 mm) produced as described above is dried at 60 ° C. until it reaches a constant weight, and then placed in a constant temperature and humidity chamber set at a temperature of 40 ° C. and a relative humidity of 90% for a predetermined time. The hygroscopicity was measured by measuring the weight after the lapse. Here, in the graph of FIG. 9, the non-combustible wood using the flame-retardant chemical solution containing ammonium borate is a filled circle, and the non-combustible wood using the flame-retardant chemical solution not added ammonium borate is white. It is a circle without a circle.

実験結果としては、図9のグラフに示すように、100質量部の80℃の水に、45質量部のホウ酸、及び35質量部のホウ砂を溶解させた難燃化薬液に、15質量部のホウ砂ホウ酸アンモニウムを添加することにより、200時間後の吸湿率が2%程度低くなることが分かった。ここで、一般的な不燃木材は、吸湿性が高いと、吸放湿によって難燃化薬液が表面に染み出してくる白華や溶脱という問題が発生する。これらの問題は、難燃化薬液を用いた不燃木材の吸湿性が少しでも低いほど、起こり難くなる。そのため、ホウ酸アンモニウムを添加して、吸湿性を低くすることは、白華や溶脱の発生の抑制に有利に働く。 As a result of the experiment, as shown in the graph of FIG. 9, 15 parts by mass of a flame-retardant chemical solution prepared by dissolving 45 parts by mass of boric acid and 35 parts by mass of borax in 100 parts by mass of water at 80 ° C. It was found that the moisture absorption rate after 200 hours was reduced by about 2% by adding the borax ammonium borate. Here, when general non-combustible wood has high hygroscopicity, problems such as whitening and leaching occur in which the flame-retardant chemical liquid exudes to the surface due to moisture absorption and desorption. These problems are less likely to occur as the hygroscopicity of non-combustible wood using flame-retardant chemicals is as low as possible. Therefore, adding ammonium borate to lower the hygroscopicity is advantageous in suppressing the occurrence of white flowers and efflorescence.

以上説明したように、本実施形態の難燃化薬液によれば、100質量部の水に対して、5質量部~75質量部のホウ酸、10質量部~80質量部のホウ砂、及び1質量部~50質量部のホウ酸アンモニウムが含有されている。そのため、例えば、80℃の水にホウ酸、ホウ砂及びホウ酸アンモニウムを高濃度で溶解させた後に、60℃に冷えても固形分が析出し難い難燃化薬液を実現することができる。これにより、木質基材5に難燃化薬液を含浸する含浸処理を60℃程度の低い温度で行うことができるので、可及的に低温で且つ高濃度で含浸処理が可能な難燃化薬液を提供することができる。 As described above, according to the flame-retardant chemical solution of the present embodiment, 5 parts by mass to 75 parts by mass of boric acid, 10 parts by mass to 80 parts by mass of borax, and 10 parts by mass of borax with respect to 100 parts by mass of water. It contains 1 part by mass to 50 parts by mass of ammonium borate. Therefore, for example, it is possible to realize a flame-retardant chemical solution in which boric acid, borax and ammonium borate are dissolved in water at 80 ° C. at a high concentration and then solids are less likely to precipitate even when cooled to 60 ° C. As a result, the impregnation treatment of impregnating the wood substrate 5 with the flame-retardant chemical solution can be performed at a low temperature of about 60 ° C., so that the flame-retardant chemical solution can be impregnated at a low temperature and a high concentration as much as possible. Can be provided.

また、本実施形態の難燃化薬液によれば、ホウ素の含有量が5mol/L以上である場合には、5分間の総発熱量が8MJ/mを超えない、という難燃の要件を満たすことができる。 Further, according to the flame-retardant chemical solution of the present embodiment, when the boron content is 5 mol / L or more, the flame-retardant requirement that the total calorific value for 5 minutes does not exceed 8 MJ / m 2 is satisfied. Can be met.

また、本実施形態の難燃化薬液によれば、ホウ素の含有量が11mol/L以上である場合には、20分間の総発熱量が8MJ/mを超えない、という不燃の要件を満たすことができる。 Further, according to the flame-retardant chemical solution of the present embodiment, when the boron content is 11 mol / L or more, the non-combustible requirement that the total calorific value for 20 minutes does not exceed 8 MJ / m 2 is satisfied. be able to.

また、本実施形態の難燃化薬液を用いた不燃木材によれば、ホウ酸及びホウ砂の他に、所定量のホウ酸アンモニウムが主成分として溶解された難燃化薬液を用いているので、ホウ酸及びホウ砂が主成分として溶解された難燃化薬液を用いた不燃木材よりも吸湿率を低下させることができ、白華や溶脱の発生を抑制することができる。
《その他の実施形態》
上記第1の実施形態では、ホウ酸、ホウ砂及びホウ酸アンモニウムが水に溶解された難燃化薬液、並びにそれを用いた不燃木材を例示したが、本発明は、ホウ酸、ホウ砂及びホウ酸アンモニウム以外に他の助剤が水に溶解された難燃化薬液、並びにそれを用いた不燃木材にも適用することができる。
Further, according to the non-combustible wood using the flame-retardant chemical solution of the present embodiment, in addition to boric acid and borax, a flame-retardant chemical solution in which a predetermined amount of ammonium borate is dissolved as a main component is used. It is possible to lower the moisture absorption rate as compared with non-combustible wood using a flame-retardant chemical solution in which boric acid and borax are dissolved as main components, and it is possible to suppress the occurrence of efflorescence and leaching.
<< Other Embodiments >>
In the first embodiment described above, a flame-retardant chemical solution in which boric acid, borax and ammonium borate are dissolved in water, and non-combustible wood using the same are exemplified. In addition to ammonium borate, it can also be applied to flame-retardant chemicals in which other auxiliaries are dissolved in water, and non-combustible wood using it.

上記第1の実施形態では、難燃化薬液を用いた不燃木材を例示したが、本発明の難燃化薬液は、紙や衣類等にも適用することができる。 In the first embodiment, the non-combustible wood using the flame-retardant chemical solution is exemplified, but the flame-retardant chemical solution of the present invention can also be applied to paper, clothing and the like.

以上説明したように、本発明は、不燃木材の製造するための含浸処理を可及的に低温で行うことができるので、極めて有用である。 As described above, the present invention is extremely useful because the impregnation treatment for producing non-combustible wood can be performed at a temperature as low as possible.

Claims (5)

100質量部の水に対して、5質量部~75質量部のホウ酸、10質量部~80質量部のホウ砂、及び1質量部~50質量部のホウ酸アンモニウムが含有され、リン酸アンモニウム、リン酸水素二アンモニウム、リン酸二水素アンモニウム、炭酸アンモニウム、炭酸水素アンモニウム、炭酸カリウム、エチレングリコール及びポリエチレングリコールが含有されていないことを特徴とする難燃化薬液。 With respect to 100 parts by mass of water, 5 parts by mass to 75 parts by mass of boric acid, 10 parts by mass to 80 parts by mass of boric acid, and 1 part by mass to 50 parts by mass of ammonium borate are contained, and ammonium phosphate is contained. , Diammonium dihydrogen phosphate, ammonium dihydrogen phosphate, ammonium carbonate, ammonium hydrogen carbonate, potassium carbonate, ethylene glycol and polyethylene glycol are not contained in the flame-retardant chemical solution. 請求項1に記載された難燃化薬液において、
ホウ素の含有量は、5mol/L以上であることを特徴とする難燃化薬液。
In the flame-retardant chemical solution according to claim 1,
A flame-retardant chemical solution characterized by having a boron content of 5 mol / L or more.
請求項1に記載された難燃化薬液において、
ホウ素の含有量は、11mol/L以上であることを特徴とする難燃化薬液。
In the flame-retardant chemical solution according to claim 1,
A flame-retardant chemical solution characterized by having a boron content of 11 mol / L or more.
請求項1~3の何れか1つに記載された難燃化薬液が木質基材に含浸されていることを特徴とする不燃木材。 A non-combustible wood, wherein the wood substrate is impregnated with the flame-retardant chemical solution according to any one of claims 1 to 3. 請求項1~3の何れか1つに記載された難燃化薬液を調製する方法であって、The method for preparing a flame-retardant chemical solution according to any one of claims 1 to 3.
70℃~80℃に加温した上記水に上記ホウ酸、上記ホウ砂及び上記ホウ酸アンモニウムを加えて溶解させることを特徴とする難燃化薬液の調製方法。A method for preparing a flame-retardant chemical solution, which comprises adding the boric acid, borax and ammonium borate to the water heated to 70 ° C. to 80 ° C. and dissolving them.
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JP2019137805A (en) 2018-02-14 2019-08-22 信越化学工業株式会社 Flame-retardant agent, flame-retardant material including the same and method for producing flame-retardant material using the same

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