JP2007254563A - Thermally expandable putty composition - Google Patents
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本発明は、熱膨張性パテ組成物に関する。より詳しくは、防火用目地材として用いられる熱膨張性パテ組成物に関する。 The present invention relates to a thermally expandable putty composition. More specifically, the present invention relates to a thermally expandable putty composition used as a fireproof joint material.
一般に、建築物等において建築基準法で定められた防火区画等に配管類や電力ケーブルや通信ケーブル等のケーブル類を貫通させる場合では、延焼防止等の観点から前記防火区画等には一定の耐火性能が求められている。そのため、建築物内の配管類・ケーブル類と防火壁等との間には、防火性能を付与した防火用目地材として、液状ポリマーに金属水和物等を配合したパテ状の防火剤等が用いられている（特許文献１参照）。 In general, in the case where piping, power cables, communication cables, and other cables are passed through fire prevention compartments, etc. stipulated by the Building Standards Act for buildings, etc., the fire prevention compartments, etc. have a certain fire resistance from the viewpoint of preventing the spread of fire. Performance is required. Therefore, between the pipes and cables in the building and the fire barrier, etc., there is a putty-like fire retardant containing a liquid polymer and a metal hydrate as a fireproof joint material with fireproof performance. Used (see Patent Document 1).
また、火災時に前記配管類が変形し、あるいはケーブル被覆材が燃焼して生じた隙間をもふさぐことが出来るパテ状防火材として、バーミキュライトや、熱膨張性黒鉛や、マイクロカプセル化したポリリン酸アンモニウムを有機樹脂に混合した樹脂組成物（例えば、特許文献２参照）や、ベース樹脂に熱膨張性黒鉛と共にポリカーボネート樹脂やポリフェニレンサルファイド樹脂等の形崩れ防止用樹脂を配合した熱膨張性の組成物（例えば、特許文献３参照）も提案されている。 In addition, vermiculite, thermally expandable graphite, and microencapsulated ammonium polyphosphate are used as putty-like fire-proofing materials that can close the gaps created by the deformation of the piping or the burning of the cable covering material in the event of a fire. A resin composition in which an organic resin is mixed (for example, see Patent Document 2), or a heat-expandable composition in which a base resin is blended with a heat-expandable graphite and a resin for preventing deformation such as polycarbonate resin and polyphenylene sulfide resin ( For example, see Patent Document 3).
しかし、防火用目地材としては、該防火用目地材自身の不燃性を備えていること（不燃性）や、火災発生時には自己の熱膨張により建築物壁面等の隙間を塞ぐこと（熱膨張性）や、火炎の熱等による防火用目地材自身の型崩れを防止できること（形状安定性）等のそれぞれの効果を十分に併せ持つことがより望ましく、延焼防止等の観点からは重要である。また、現場施工上の観点からは成形や加工が容易であること（現場施工性）も備えることが望ましい。従って、これらの効果を十分に併せ持つパテ組成物を提供することは防災・防火上の観点からも十分に意義がある。
そこで、本発明では、不燃性、熱膨張性、形状安定性を備え、かつ成形や加工が容易であるという優れた現場施工性も備えた熱膨張性パテ組成物を提供することを主目的とする。 Thus, the main object of the present invention is to provide a thermally expandable putty composition that has non-flammability, thermal expansion, and shape stability, and also has excellent on-site workability that is easy to mold and process. To do.
本発明は、まず、熱膨張性黒鉛と亜リン酸アルミニウムとを含む熱膨張性パテ組成物を提供する。これによって、火災等の高温条件下においてパテ組成物自らが熱膨張するとともに、炭化した炭化物等の表面にガラス状の被膜を形成させることができる。次に、本発明は、次の（Ａ）〜（Ｄ）成分を含む熱膨張性パテ組成物を提供する。即ち、（Ａ）液状ゴム４０〜９０質量部、ブチルゴム１０〜６０質量部からなるベースゴム成分１００質量部、（Ｂ）熱膨張性黒鉛を１０〜１００質量部、（Ｃ）亜リン酸アルミニウムを５０〜２００質量部、及び（Ｄ）水酸化アルミニウムを５０〜２００質量部の各成分を含む熱膨張性パテ組成物である。これによって、不燃性、熱膨張性、形状安定性、現場施工性をより一層向上させることができる。 The present invention first provides a thermally expandable putty composition comprising thermally expandable graphite and aluminum phosphite. As a result, the putty composition itself thermally expands under a high temperature condition such as a fire, and a glassy film can be formed on the surface of the carbonized carbide or the like. Next, the present invention provides a thermally expandable putty composition containing the following components (A) to (D). That is, (A) 40 to 90 parts by mass of liquid rubber, 100 parts by mass of a base rubber component composed of 10 to 60 parts by mass of butyl rubber, (B) 10 to 100 parts by mass of thermally expandable graphite, and (C) aluminum phosphite. It is a thermally expandable putty composition containing 50 to 200 parts by mass and (D) 50 to 200 parts by mass of each component of aluminum hydroxide. Thereby, nonflammability, thermal expansibility, shape stability, and on-site workability can be further improved.
更に、前記液状ゴムが、ポリブタジエン、ポリイソプレン、ポリブテンのうちの一種または２種以上の混合物である熱膨張性パテ組成物を提供する。また、酸素指数が４０以上で、同時に針入度が７０〜１５０である熱膨張性パテ組成物を提供する。これによって、少なくとも形状安定性と現場施工性をより一層向上させることができる。 Furthermore, the heat-expandable putty composition in which the liquid rubber is one or a mixture of two or more of polybutadiene, polyisoprene, and polybutene is provided. In addition, a thermally expandable putty composition having an oxygen index of 40 or more and a penetration of 70 to 150 at the same time is provided. Thereby, at least shape stability and on-site workability can be further improved.
本発明の熱膨張性パテ組成物は、少なくとも熱膨張性黒鉛と亜リン酸アルミニウムとを含むことにより、現場施工性に優れた不燃性の熱膨張性パテ組成物であって、火災時の熱で自ら熱膨張し、隙間を塞ぐことができる。 The thermally expandable putty composition of the present invention is a nonflammable thermally expandable putty composition excellent in on-site workability by containing at least thermally expandable graphite and aluminum phosphite. Can expand itself and close the gap.
以下、本発明について説明する。なお、以下は本発明についての例示にすぎず、これにより本発明が狭く解釈されることはない。 The present invention will be described below. In addition, the following is only the illustration about this invention, and this invention is not interpreted narrowly by this.
本発明の熱膨張性パテ組成物は、熱膨張生黒鉛と亜リン酸アルミニウムとを含むことを特徴とする。まず、熱膨張性黒鉛とは、天然グラファイト、熱分解グラファイト等のグラファイト粉末を、硫酸や硝酸等の無機酸と、濃硝酸や過マンガン酸塩等の強酸化剤とを用いて表面処理したものであり、かつグラファイト層状構造を維持した結晶化合物である。これらは常圧下で２００℃程度以上の温度に曝されると、１００倍以上に熱膨張する。なお、前記天然グラファイト、熱分解グラファイト等のグラファイト粉末は、脱酸処理を施したものや、更に中和処理したもの等であってもよい。 The thermally expandable putty composition of the present invention is characterized by containing thermally expanded raw graphite and aluminum phosphite. First, thermally expansive graphite is a surface-treated graphite powder such as natural graphite or pyrolytic graphite using an inorganic acid such as sulfuric acid or nitric acid and a strong oxidizing agent such as concentrated nitric acid or permanganate. And a crystalline compound maintaining a graphite layered structure. When these are exposed to a temperature of about 200 ° C. or higher under normal pressure, they thermally expand 100 times or more. The graphite powder such as natural graphite and pyrolytic graphite may be deoxidized or further neutralized.
熱膨張性黒鉛の粒度は、２０〜４００メッシュ（ＪＩＳ Ｚ ８９０１による測定）であることが望ましい。前記熱膨張性黒鉛の粒度が４００メッシュよりも大きくなると、熱膨張性黒鉛の膨張度が小さくなってしまい、得られた熱膨張性目地材が火災時に十分に熱膨張しない場合があるからである。また、前記熱膨張性黒鉛の粒度が２０メッシュよりも小さくなると、分散性が減少してしまい、得られた熱膨張性目地材の弾性が低下する場合があるからである。なお、本発明では、前記熱膨張性黒鉛を所望の粒度にする手段については特に限定されない。例えば、粉砕機と分級機とを用いて所望の粒度にすることもできる。 The particle size of the thermally expandable graphite is preferably 20 to 400 mesh (measured according to JIS Z 8901). This is because when the particle size of the thermally expandable graphite is larger than 400 mesh, the degree of expansion of the thermally expandable graphite becomes small, and the obtained thermally expandable joint material may not be sufficiently thermally expanded in a fire. . Further, when the particle size of the thermally expandable graphite is smaller than 20 mesh, the dispersibility is decreased, and the elasticity of the obtained thermally expandable joint material may be decreased. In the present invention, the means for making the thermally expandable graphite have a desired particle size is not particularly limited. For example, a desired particle size can be obtained using a pulverizer and a classifier.
なお、前記熱膨張性黒鉛を前記無機酸と前記強酸化剤とを用いて表面処理等を行う場合には、所望の粒度範囲を逸脱しないために、所望の処理方法や処理時間を選択することができる。これにより、所望の粒度範囲を逸脱した微細な熱膨張性黒鉛が、本発明に係る熱膨張性パテ組成物に含有されることを防止できる。 In addition, when performing surface treatment or the like on the thermally expandable graphite using the inorganic acid and the strong oxidizing agent, a desired treatment method and treatment time should be selected so as not to depart from the desired particle size range. Can do. Thereby, it can prevent that the fine thermal expansible graphite which deviated from the desired particle size range is contained in the thermal expansible putty composition concerning the present invention.
そして、亜リン酸アルミニウムを熱膨張性パテ組成物に配合することにより、火災時に熱膨張して、炭化した炭化物の表面にガラス状の強固な被膜を形成し、結果として燃焼残渣が容易に型崩れせず、それによって火炎や煙を遮断することができる。亜リン酸アルミニウムは、分散性の観点から、数平均粒径がレーザー回折法の測定値（ＪＩＳ Ｚ ８８２５−１による測定）で１〜１００μｍであることが好ましい。 Then, by blending aluminum phosphite into the thermally expandable putty composition, it thermally expands in the event of a fire, forming a strong glass-like film on the surface of the carbonized carbide, and as a result, the combustion residue can be easily molded. It doesn't collapse, and it can shut out flames and smoke. From the viewpoint of dispersibility, the aluminum phosphite preferably has a number average particle diameter of 1 to 100 μm as measured by a laser diffraction method (measured according to JIS Z 8825-1).
また、本発明に係る熱膨張性パテ組成物は、以下の（Ａ）〜（Ｄ）の成分比率であることが望ましい。（Ａ）液状ゴム４０〜９０質量部、ブチルゴム１０〜６０質量部からなるゴム成分１００質量部。（Ｂ）熱膨張性黒鉛を１０〜１００質量部。（Ｃ）亜リン酸アルミニウムを５０〜２００質量部。（Ｄ）水酸化アルミニウムを５０〜２００質量部。以下、各成分について説明する。 In addition, the thermally expandable putty composition according to the present invention preferably has the following component ratios (A) to (D). (A) 100 mass parts of rubber components consisting of 40-90 mass parts of liquid rubber and 10-60 mass parts of butyl rubber. (B) 10 to 100 parts by mass of thermally expandable graphite. (C) 50-200 mass parts of aluminum phosphite. (D) 50-200 mass parts of aluminum hydroxide. Hereinafter, each component will be described.
まず、ベースゴム成分として使用される前記液状ゴムは、液状のゴムであればよく、特にその化合物等については限定されない。好適には、ポリブタジエン、ポリイソプレン、ポリブテン等であることが好ましい。なお、前記液状ゴムは単独で用いてもよいし、あるいは２種以上組み合わせて用いてもよい。ここで、複数の液状ゴムを組み合わせて用いる場合には、前記ベースゴム成分中の液状ゴムの含有量が、好適には４０〜９０質量部であることが好ましい。前記液状ゴムの含有量が４０質量部未満では、得られた熱膨張性パテ組成物の針入度が小さくなるので、硬くなりすぎるため加工性が低下するからである。一方、前記液状ゴムが９０質量部を超えると、粘着性が大きくなりすぎるため現場施工性が悪くなるからである。 First, the liquid rubber used as the base rubber component may be a liquid rubber, and the compound and the like are not particularly limited. Preferable are polybutadiene, polyisoprene, polybutene and the like. In addition, the said liquid rubber may be used independently or may be used in combination of 2 or more types. Here, when using combining a some liquid rubber, it is preferable that content of the liquid rubber in the said base rubber component is 40-90 mass parts suitably. This is because if the content of the liquid rubber is less than 40 parts by mass, the penetration of the obtained thermally expandable putty composition becomes small, so that it becomes too hard and the workability deteriorates. On the other hand, when the amount of the liquid rubber exceeds 90 parts by mass, the on-site workability deteriorates because the adhesiveness becomes too large.
次に、前記熱膨張性黒鉛の含有量については、ベースゴム成分の粘度や、所望の膨張倍率がどの程度か等により、好適な含有量が異なってくるが、ベースゴム成分１００質量部に対して１０〜１００質量部の範囲で適宜設定することが好ましい。そして、より好適には１０〜８０質量部、更に好ましくは２０〜６０質量部であることが望ましい。前記熱膨張性黒鉛の含有量が１０質量部未満であれば、得られた熱膨張性目地材が火災時に十分熱膨張しなくなってしまうからである。一方、前記熱膨張性黒鉛の含有量が１００質量部を超えると、熱膨張率は大きくなるものの、得られる熱膨張性パテ組成物の硬度が上昇し、加工性が低下するからである。 Next, the content of the heat-expandable graphite varies depending on the viscosity of the base rubber component, the desired expansion ratio, and the like. It is preferable to set appropriately in the range of 10 to 100 parts by mass. And it is more preferable that it is 10-80 mass parts, More preferably, it is 20-60 mass parts. This is because if the content of the heat-expandable graphite is less than 10 parts by mass, the obtained heat-expandable joint material will not be sufficiently thermally expanded in a fire. On the other hand, if the content of the heat-expandable graphite exceeds 100 parts by mass, the coefficient of thermal expansion increases, but the hardness of the resulting heat-expandable putty composition increases and the workability decreases.
そして、前記亜リン酸アルミニウムの含有量は、ベースゴム成分１００質量部に対して５０〜２００質量部が好ましく、より好適には８０〜１５０質量部、更に好ましくは１００〜１４０質量部であることが望ましい。前記亜リン酸アルミニウムの含有量が５０質量部未満であれば、得られる熱膨張性パテ組成物の燃焼残渣の形状安定性が不十分なため火災時の防火性能が低下してしまうからである。一方、前記亜リン酸アルミニウムの含有量が２００質量部を超えると、得られる熱膨張性パテ組成物の硬度が上昇しすぎるため、加工性が低下してしまうからである。 And as for content of the said aluminum phosphite, 50-200 mass parts is preferable with respect to 100 mass parts of base rubber components, More preferably, it is 80-150 mass parts, More preferably, it is 100-140 mass parts. Is desirable. This is because, if the content of the aluminum phosphite is less than 50 parts by mass, the shape stability of the combustion residue of the obtained thermally expandable putty composition is insufficient and the fireproof performance at the time of fire is lowered. . On the other hand, when the content of the aluminum phosphite exceeds 200 parts by mass, the hardness of the obtained heat-expandable putty composition is excessively increased, so that workability is deteriorated.
また、本発明では、熱膨張性パテ組成物の難燃性をより向上させるために水酸化アルミニウムを用いることが望ましい。前記熱膨張性パテ剤に水酸化アルミニウムを含有させることで、加熱時の脱水反応によって生成する水によって吸熱反応が起こる。これにより、前記熱膨張性パテ材の温度上昇が控えられるからである。また、前記水酸化アルミニウムの分散性の観点から、その数平均粒径が、レーザー回折法を用いた測定値（ＪＩＳ Ｚ ８９０１による測定）で１〜５０μｍであることが好ましい。なお、前記水酸化アルミニウムは、ベースゴム成分１００質量部に対して５０〜２００質量部の範囲で含有させることが望ましい。前記水酸化アルミニウムの添加量が５０〜２００質量部の範囲を逸脱すると、得られる熱膨張性パテ組成物の硬度が高くなりすぎて、加工性が低下してしまうからである。 In the present invention, it is desirable to use aluminum hydroxide in order to further improve the flame retardancy of the thermally expandable putty composition. By containing aluminum hydroxide in the thermally expandable putty agent, an endothermic reaction occurs due to water generated by a dehydration reaction during heating. Thereby, the temperature rise of the thermally expansible putty material is suppressed. Further, from the viewpoint of the dispersibility of the aluminum hydroxide, the number average particle diameter is preferably 1 to 50 μm as measured by a laser diffraction method (measured according to JIS Z 8901). The aluminum hydroxide is preferably contained in the range of 50 to 200 parts by mass with respect to 100 parts by mass of the base rubber component. This is because when the amount of the aluminum hydroxide added deviates from the range of 50 to 200 parts by mass, the hardness of the resulting heat-expandable putty composition becomes too high and the workability is lowered.
更に、本発明に係る熱膨張性パテ組成物は、酸素指数（ＪＩＳ Ｋ７２０１による測定）が４０以上であることが望ましい。酸素指数４０未満では火災時の難燃性が不十分となるため、前記熱膨張性パテ組成物の型崩れ防止性も低下するからである。その際、膨張性黒鉛及び水酸化アルミニウムの配合量を適宜調整することで、酸素指数の調整を行うことができる。 Furthermore, it is desirable that the heat-expandable putty composition according to the present invention has an oxygen index (measured according to JIS K7201) of 40 or more. This is because if the oxygen index is less than 40, the flame retardancy at the time of fire becomes insufficient, so that the ability of the thermally expandable putty composition to lose its shape is also lowered. At that time, the oxygen index can be adjusted by appropriately adjusting the blending amounts of expansive graphite and aluminum hydroxide.
また、本発明に係る熱膨張性パテ組成物は、針入度（ＪＩＳ Ｋ２２０７による測定）が７０〜１５０であることが好ましい。前記熱膨張性パテ組成物の針入度が７０未満では硬くなりすぎるため、その加工性が低下してしまうからである。一方、前記針入度が１５０を超えると、前記熱膨張性パテ組成物を防火用目地材として実際に使用した際に、火炎の熱等によるダレ現象（熱ダレ現象）が起きてしまうからである。 In addition, the heat-expandable putty composition according to the present invention preferably has a penetration (measured according to JIS K2207) of 70 to 150. This is because if the penetration of the heat-expandable putty composition is less than 70, it becomes too hard and its workability is lowered. On the other hand, if the penetration exceeds 150, when the thermally expandable putty composition is actually used as a fireproof joint material, a sagging phenomenon (thermal sagging phenomenon) due to the heat of the flame or the like occurs. is there.
更に、熱膨張性パテ組成物は、前述のように適宜その柔軟性、熱膨張性、断熱性、耐火性等を調整することで様々な分野で利用することができる。即ち、本発明では、前記熱膨張性パテ組成物をどのように使用するかという工法については特に限定しないが、より好適には、防火膨張性材料として使用する工法に利用することができる。 Furthermore, the heat-expandable putty composition can be used in various fields by appropriately adjusting its flexibility, heat-expandability, heat insulation, fire resistance, etc. as described above. That is, in the present invention, the method for using the thermally expandable putty composition is not particularly limited, but more preferably, the method can be used for a method for use as a fireproof expandable material.
そして、前記熱膨張性パテ組成物は、好適には、防火区画体に設けられた貫通口の隙間の一部もしくは全部を閉塞するために用いられる。具体的には、防火壁、床スラブ等の防火区画体に設けられた貫通口を通る電源ケーブルや通信ケーブル、パイプ等と防火壁の隙間に本発明の熱膨張性パテ組成物を充填して用いることができる。 The heat-expandable putty composition is preferably used to close part or all of the gaps of the through holes provided in the fire prevention compartment. Specifically, the heat-expandable putty composition of the present invention is filled in the gap between the power cable, communication cable, pipe, etc. and the fire wall through the through-hole provided in the fire compartment such as the fire wall and floor slab. Can be used.
また、前記熱膨張性パテ組成物を得る方法についても本発明では限定されない。例えば、市販のミキサー、バンバリーミキサー、ニーダーミキサー、二本ロール等の混練装置を用いて混練する方法によって得ることもできる。また、混練された前記熱膨張性パテ組成物は、プレス成形や押出成形等の手法によって所望の形状に成形することで、現場への携行性を更に向上させることもできる。その際、例えば、前記熱膨張性パテ組成物をゴム用押出機で角柱形状に押出して、所定の長さで裁断することでブロック状の成形体とすることもできる。あるいは、金型に前記熱膨張性パテ組成物を充填してプレスすることで、所望の形状を得ることも出来る。 Further, the method for obtaining the thermally expandable putty composition is not limited in the present invention. For example, it can also be obtained by a kneading method using a kneading apparatus such as a commercially available mixer, Banbury mixer, kneader mixer, or two rolls. Moreover, the knead | mixed said thermally expansible putty composition can further improve the portability to the field by shape | molding in a desired shape by techniques, such as press molding and extrusion molding. At that time, for example, the thermally expandable putty composition can be extruded into a prismatic shape with a rubber extruder and cut into a predetermined length to obtain a block-shaped molded body. Alternatively, a desired shape can be obtained by filling the metal mold with the thermally expandable putty composition and pressing it.
更に、本発明に係る熱膨張性パテ組成物には、その効果を阻害しない範囲で、可塑剤、軟化剤、老化防止剤、加工助剤、滑剤、粘着付与剤等を配合することができる。加えて、前記熱膨張性パテ組成物の成形性の調整に有効な軟化剤や可塑剤の例としては、パラフィン系やナフテン系等のプロセスオイル、流動パラフィンやその他のパラフィン類、ワックス類、フタル酸やアジピン酸系、セバシン酸系やリン酸系等のエステル系可塑剤類、ステアリン酸やそのエステル類や粘着付与剤等が挙げられる。 Furthermore, the heat-expandable putty composition according to the present invention may contain a plasticizer, a softening agent, an anti-aging agent, a processing aid, a lubricant, a tackifier, and the like as long as the effect is not impaired. In addition, examples of softeners and plasticizers effective for adjusting the moldability of the thermally expandable putty composition include paraffinic and naphthenic process oils, liquid paraffin and other paraffins, waxes, phthalates. Examples thereof include ester plasticizers such as acid, adipic acid, sebacic acid and phosphoric acid, stearic acid and esters thereof, and a tackifier.
以上より、本発明に係る熱膨張性パテ組成物によれば、現場施工性に優れた不燃性の熱膨張性パテ組成物として使用することができるとともに、火災時の熱で自ら熱膨張し、隙間をふさぐ効果を有しながら、長時間火災に晒されても、その加熱残渣が十分にその形状を保持し、火炎や煙が隙間を通過することを阻止すること等ができる。 From the above, according to the thermally expandable putty composition according to the present invention, it can be used as a non-combustible thermally expandable putty composition excellent in on-site workability, and is thermally expanded by heat at the time of fire, Even if it is exposed to a fire for a long time while having the effect of closing the gap, the heated residue can sufficiently retain its shape and prevent flames and smoke from passing through the gap.
以下、本発明を実施例及び比較例により具体的に説明するが、これらの実施例は本発明を限定するものではない。なお、以下の説明における「部」及び「％」は質量基準に基づくものである。 EXAMPLES Hereinafter, although an Example and a comparative example demonstrate this invention concretely, these Examples do not limit this invention. In the following description, “parts” and “%” are based on mass standards.
表３に示す配合量で、ベースゴム成分、熱膨張性黒鉛、亜リン酸アルミニウム、水酸化アルミニウム及び加工助剤を容量３リットルのニーダーミキサー（（株）モリヤマ製、ＤＳ３−Ｓ型）を用いて回転速度３０ｒｐｍで３分間混練した後、押出機（（株）三葉製作所製、６０Ｋ型ゴム押出し機）で幅７ｃｍ、厚さ３．５ｃｍの板状成形体を押出し、長さ２０ｃｍで裁断し熱膨張性パテ成形体の評価用試料を得た。 Using a kneader mixer (manufactured by Moriyama Co., Ltd., DS3-S type) with a base rubber component, thermally expandable graphite, aluminum phosphite, aluminum hydroxide and processing aid in the compounding amounts shown in Table 3 After kneading for 3 minutes at a rotational speed of 30 rpm, a plate-shaped molded body having a width of 7 cm and a thickness of 3.5 cm is extruded with an extruder (manufactured by Mitsuba Corporation, 60K type rubber extruder) and cut into a length of 20 cm. A sample for evaluating a thermally expandable putty molded body was obtained.
実施例において使用した材料は、それぞれ表１に示したものである。 The materials used in the examples are those shown in Table 1, respectively.
＜実施例・比較例の各成分比率と物性の評価方法＞
まず、実施例として使用したものを説明する。各素材はベースゴム成分として液状ゴム（ポリブタジエン）、液状ゴム（ポリイソプレン）、ブチルゴムを一種類又は複数種類使用した。実施例１は、ポリイソプレンを６０質量部、亜リン酸アルミニウムを２００質量部含有したものである。実施例２は、液状ゴムとしてポリイソプレンを６０質量部含有したものである。実施例３は、液状ゴムとしてポリブタジエン３０質量部とポリイソプレン３０質量部とを含有したものである。実施例４は、液状ゴムとしてポリイソブタンを６０質量部含有したものである。実施例５は、液状ゴムとしてポリイソプレンを３５質量部含有し、ブチルゴムを６５質量部含有したものである。
<Each component ratio and physical property evaluation method in Examples and Comparative Examples>
First, what was used as an Example is demonstrated. Each material used one or more kinds of liquid rubber (polybutadiene), liquid rubber (polyisoprene), and butyl rubber as a base rubber component. Example 1 contains 60 parts by mass of polyisoprene and 200 parts by mass of aluminum phosphite. Example 2 contains 60 parts by mass of polyisoprene as a liquid rubber. Example 3 contains 30 parts by mass of polybutadiene and 30 parts by mass of polyisoprene as a liquid rubber. Example 4 contains 60 parts by mass of polyisobutane as a liquid rubber. Example 5 contains 35 parts by mass of polyisoprene as a liquid rubber and 65 parts by mass of butyl rubber.
次に、比較例として使用したものを説明する。熱膨張黒鉛を含有しないものを比較例１とした。そして、亜リン酸アルミニウムを含有しないものを比較例２とした。これらの実施例１〜５及び比較例１，２として使用した各試料について、表２の方法に基づき特性を評価した。表３に各実施例・比較例の成分比と各物性の結果をまとめた。 Next, what was used as a comparative example is demonstrated. A sample containing no thermally expanded graphite was designated as Comparative Example 1. And the thing which does not contain aluminum phosphite was made into the comparative example 2. About each sample used as these Examples 1-5 and Comparative Examples 1 and 2, the characteristic was evaluated based on the method of Table 2. Table 3 summarizes the component ratios of the examples and comparative examples and the results of physical properties.
＜熱膨張倍率と形状安定性＞
熱膨張倍率と形状安定性について検討した。熱膨張黒鉛と亜リン酸アルミニウムとを含む実施例１〜５の全てにおいて、熱膨張倍率が５以上であり、かつ形状安定性も「良」であった。これにより、いずれの実施例でも熱膨張倍率、形状安定性ともに優れているであることが示唆された。その中でも、最も高い熱膨張倍率を示したのは実施例１（８倍；表３参照）であった。その次に高い熱膨張倍率を示したのは、液状ゴムの含有量が６０質量部である実施例２〜４（いずれも７倍；表３参照）であった。これに対して、液状ゴムの含有量を３５質量部に減らし、ブチルゴムを６５質量部に増やした実施例５が実施例区の中では最も低い熱膨張倍率（５倍；表３参照）であった。
<Thermal expansion ratio and shape stability>
The thermal expansion ratio and shape stability were investigated. In all of Examples 1 to 5 including thermally expanded graphite and aluminum phosphite, the coefficient of thermal expansion was 5 or more, and the shape stability was “good”. Thereby, it was suggested that both the thermal expansion magnification and the shape stability are excellent in any of the examples. Among them, Example 1 (8 times; see Table 3) showed the highest thermal expansion ratio. The next highest thermal expansion ratio was shown in Examples 2 to 4 (all 7 times; see Table 3) in which the content of the liquid rubber was 60 parts by mass. On the other hand, Example 5 in which the content of the liquid rubber was reduced to 35 parts by mass and the butyl rubber was increased to 65 parts by mass was the lowest coefficient of thermal expansion (5 times; see Table 3) in the examples. It was.
一方、比較例区では、亜リン酸アルミニウムを含まない比較例１は、形状安定性は良好であったものの、熱膨張が認められなかった。そして、亜リン酸アルミニウムを含まない比較例２は、熱膨張倍率は７倍と良好であったものの、形状安定性が「不可」であった。従って、少なくとも、熱膨張黒鉛と亜リン酸アルミニウムとを含有させることで熱膨張倍率と形状安定性は向上することが示唆された（実施例５、比較例１，２等；表３参照）。 On the other hand, in Comparative Example, Comparative Example 1 not containing aluminum phosphite had good shape stability, but no thermal expansion was observed. And although the comparative example 2 which does not contain aluminum phosphite had the thermal expansion rate as favorable as 7 times, shape stability was "impossible". Therefore, it was suggested that at least thermal expansion graphite and aluminum phosphite are contained, so that the thermal expansion ratio and shape stability are improved (Example 5, Comparative Examples 1 and 2; see Table 3).
＜酸素指数＞
次に、酸素指数について検討した。酸素指数に関しては、実施例区の中で熱膨張黒鉛と水酸化アルミニウムの配合量が最も多い実施例５が、実施例区の中で最も高い酸素指数であった（酸素指数＝６０；表３参照）。そして、実施例区の中で水酸化アルミニウムの配合量が最も少ない実施例１が、実施例区の中で最も低い酸素指数であった（酸素指数＝４０；表３参照）。従って、熱膨張性黒鉛と水酸化アルミニウムの配合量を適宜増やすことで酸素指数をある程度上昇させることが示唆された。
<Oxygen index>
Next, the oxygen index was examined. Regarding the oxygen index, Example 5 having the highest blending amount of thermally expanded graphite and aluminum hydroxide in the Example section was the highest oxygen index in the Example section (oxygen index = 60; Table 3). reference). And Example 1 with the few compounding quantity of aluminum hydroxide in an Example section was the lowest oxygen index in an Example section (oxygen index = 40; refer Table 3). Therefore, it was suggested that the oxygen index is increased to some extent by appropriately increasing the blending amount of the thermally expandable graphite and aluminum hydroxide.
＜針入度＞
更に、針入度について検討した。実施例区の中で液状ゴムの質量部数が最も低い実施例５（液状ゴム＝３５質量部；表３参照）が、最も低い針入度であった（針入度＝４０ｍｍ；表３参照）。また、比較例区では、ゴム成分が液状ゴムのみである比較例２が最も高い針入度であった（針入度＝２４０ｍｍ；表３参照）。これらより、ベースゴム成分中の液状ゴムが少ないと針入度が低下し、液状ゴムの含有量が多すぎると針入度が大きくなることが示唆された。
<Penetration>
Furthermore, the penetration was examined. Example 5 (liquid rubber = 35 parts by mass; see Table 3) in which the number of parts by mass of the liquid rubber was the lowest in the Example section was the lowest penetration (Penetration = 40 mm; see Table 3). . In Comparative Example, Comparative Example 2 in which the rubber component was only liquid rubber had the highest penetration (penetration = 240 mm; see Table 3). From these results, it was suggested that when the amount of the liquid rubber in the base rubber component is small, the penetration is lowered, and when the content of the liquid rubber is too large, the penetration is increased.
以上より、本実施例に係る熱膨張性パテ組成物が、防火用目地材としての不燃性を備えていること（不燃性）や、火災発生時には自己の熱膨張により建築物壁面等の隙間を十分に塞ぐこと（熱膨張性）や、火炎の熱等による防火用目地材自身の型崩れを十分に防止できること（形状安定性）等の効果を併せ持つことが示された。また、現場施工上の観点からは成形や加工が容易であること（現場施工性）も示された。そして、本発明に係る熱膨張性パテ組成物では、前述のように材料の配合比を適宜調整することで、前記熱膨張倍率、形状安定性、針入度、酸素指数等の物性を調整できることも示唆された。 From the above, the thermally expandable putty composition according to this example has nonflammability as a joint material for fire prevention (nonflammability), and in the event of a fire, gaps such as building wall surfaces are created by its own thermal expansion. It has been shown that it has effects such as sufficient sealing (thermal expansibility) and sufficient prevention of shape loss of the fireproof joint material itself due to the heat of the flame (shape stability). In addition, from the viewpoint of on-site construction, it was also shown that molding and processing are easy (on-site workability). And, in the thermally expandable putty composition according to the present invention, the physical properties such as the thermal expansion ratio, shape stability, penetration, oxygen index, etc. can be adjusted by appropriately adjusting the blending ratio of the materials as described above. Also suggested.
本発明は、熱膨張性パテ組成物に関する。より詳しくは、防火用目地材に用いられる熱膨張性パテ組成物等として利用することができる。
The present invention relates to a thermally expandable putty composition. More specifically, it can be used as a heat-expandable putty composition used for a fireproof joint material.
Claims (4)
（Ａ）液状ゴム４０〜９０質量部と、ブチルゴム１０〜６０質量部と、からなるゴム成分１００質量部。
（Ｂ）熱膨張性黒鉛１０〜１００質量部。
（Ｃ）亜リン酸アルミニウム５０〜２００質量部。
（Ｄ）水酸化アルミニウム５０〜２００質量部。 The thermally expandable putty composition according to claim 1, comprising the following components (A) to (D):
(A) 100 mass parts of rubber components consisting of 40-90 mass parts of liquid rubber and 10-60 mass parts of butyl rubber.
(B) 10 to 100 parts by mass of thermally expandable graphite.
(C) 50 to 200 parts by mass of aluminum phosphite.
(D) 50 to 200 parts by mass of aluminum hydroxide.
The heat-expandable putty composition according to any one of claims 1 to 3, wherein the oxygen index is 40 or more and the penetration is 70 to 150.
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| WO2017126654A1 (en) * | 2016-01-20 | 2017-07-27 | 積水化学工業株式会社 | Fire-resistant resin composition |
| JP2017128712A (en) * | 2016-01-20 | 2017-07-27 | 積水化学工業株式会社 | Fire-resistant resin composition |
| JP7095985B2 (en) | 2016-12-21 | 2022-07-05 | 積水化学工業株式会社 | Refractory resin composition |
| JP2018100410A (en) * | 2016-12-21 | 2018-06-28 | 積水化学工業株式会社 | Fire-resistant resin composition |
| JP2019116606A (en) * | 2017-12-26 | 2019-07-18 | 清典 藏田 | Heat expansion fireproof heat insulation coating, fireproof heat insulation sheet for cable using the same |
| JP6467692B1 (en) * | 2017-12-26 | 2019-02-13 | 清典 藏田 | Thermally expandable fireproof insulation coating and fireproof insulation sheet for cables using the same |
| JP6896134B1 (en) * | 2020-11-20 | 2021-06-30 | デンカ株式会社 | Thermally expandable putty composition |
| JP2022082191A (en) * | 2020-11-20 | 2022-06-01 | デンカ株式会社 | Thermally-expandable putty composition |
| JP7506203B1 (en) | 2023-01-27 | 2024-06-25 | デンカ株式会社 | Putty-like fireproof composition |
| JP7511041B1 (en) | 2023-02-28 | 2024-07-04 | デンカ株式会社 | Putty-like fireproof composition |
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