JP4658567B2 - Sealing material composition suitable for top coating specification, and method for applying sealing material using the same - Google Patents
Sealing material composition suitable for top coating specification, and method for applying sealing material using the same Download PDFInfo
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- JP4658567B2 JP4658567B2 JP2004331594A JP2004331594A JP4658567B2 JP 4658567 B2 JP4658567 B2 JP 4658567B2 JP 2004331594 A JP2004331594 A JP 2004331594A JP 2004331594 A JP2004331594 A JP 2004331594A JP 4658567 B2 JP4658567 B2 JP 4658567B2
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- molecular weight
- sealing material
- plasticizer
- material composition
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- Prior art date
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- 239000003566 sealing material Substances 0.000 title claims description 78
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- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 claims description 43
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- 239000011347 resin Substances 0.000 claims description 31
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- 125000003808 silyl group Chemical group [H][Si]([H])([H])[*] 0.000 claims description 19
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- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 3
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Description
本発明は、大気中などの水分により硬化してゴム状弾性体となる、耐久性及び耐汚染性に優れた常温硬化性樹脂からなる上塗り塗装仕様向けシーリング材組成物、およびこれを使用した上塗り塗装したとき塗膜の亀裂防止性および汚染防止性に優れたシーリング材の施工方法に関する。 The present invention relates to a sealing material composition for topcoat coating specifications comprising a room temperature curable resin excellent in durability and contamination resistance, which is cured by moisture in the air or the like to form a rubber-like elastic body, and a topcoat using the same The present invention relates to a method for applying a sealing material having excellent anti-cracking and anti-contamination properties when applied.
建築構造物の外壁目地や土木構造物の目地などには、防水、意匠等の目的で多くのシーリング材が使用されている。これらのシーリング材は、モルタル板、コンクリート板、ALC板、金属材等の外壁などを構成する部材間の接合部から構造体内部への雨水の侵入を防ぎ、また地震、日射による温度差、風圧などによって生じる外壁材の歪を緩和して外壁材の破壊を防ぎ、更には外壁の美観を損ねないことなどが求められる。 Many sealing materials are used for the purpose of waterproofing, design, and the like on the outer wall joints of building structures and joints of civil engineering structures. These sealing materials prevent the intrusion of rainwater into the structure from the joints between the mortar board, concrete board, ALC board, and the outer wall of metal materials, etc., as well as temperature differences and wind pressure due to earthquakes and solar radiation. Therefore, it is required to alleviate the distortion of the outer wall material caused by the above, to prevent the destruction of the outer wall material, and to not impair the appearance of the outer wall.
また近年は外壁材に対して長期にわたって本来の性能を維持することが求められることが多くなってきている。すなわち、いわゆる高耐久性化・長寿命化の要求が出てきている。この高耐久性化・長寿命化の要求を実現する方法の1つとして、優れた耐久性を持つ塗料を外壁材に上塗り塗装する方法がある。この上塗り塗装は、形成される塗膜によって雨水の侵入を防ぎ、日射による熱劣化、紫外線劣化などから外壁材を保護するという本来の機能を有しなければならないとともに外壁の美観を保つという建築構造物及び土木構造物の良否を左右する意匠上重要な役目を負っている。 In recent years, it has been increasingly required to maintain the original performance over a long period of time for the outer wall material. That is, there is a demand for so-called high durability and long life. One way to achieve this demand for higher durability and longer life is to top-coat the exterior wall with a paint with excellent durability. This top coat must have the original function of preventing rainwater from entering by the coating film that is formed, protecting the outer wall material from heat deterioration due to solar radiation, UV deterioration, etc. and maintaining the aesthetics of the outer wall It plays an important role in the design that affects the quality of objects and civil engineering structures.
このような目的で使用される優れた耐久性を持つ上塗り塗料は、高耐久性、長寿命の性能を付与するために塗膜樹脂成分の架橋密度を高くすることが多く行なわれているが、その結果塗膜は硬く伸びが少なくなる傾向にある。さらに、同時に美観を良くしたり、またより自然に見せるために塗料に無機系有機系のいろいろな形の粒子やバルーンなどを配合したり、様々な塗装パターンを駆使することが行われていることから、表面の形状や性状が複雑なものとなっている。 Top coatings with excellent durability used for such purposes are often made to increase the crosslink density of the coating resin component in order to impart high durability and long life performance. As a result, the coating film tends to be hard and less stretched. In addition, to improve the appearance at the same time, and to blend more various types of inorganic and organic particles and balloons into the paint to make it look more natural, and to make full use of various paint patterns Therefore, the shape and properties of the surface are complicated.
このように、建築物概観や土木構造物などに対する高耐久性、長寿命化を実現するために高耐久性塗料を用いた塗装仕様は、優れたものであるが、塗膜は硬く伸びが少ないために、このような塗料が目地部分のシーリング材硬化物上に塗装された場合には、塗膜の割れや亀裂を生じるという問題がある。
すなわち、外壁等を構成する部材は硬く、剛性の高い材料であるため、塗膜をこれに適合させるため、上塗り塗料においても高耐久化のため硬く、伸びを小さくする方向に進んでいるが、外壁等の構成部材の接合部にできる目地に充填、施工するシーリング材は、気候に応じた温度差等で生じる部材の膨張や収縮、あるいは風圧や地震等で生じる種々の目地変位を吸収しなければならないことから、硬化後の物性が低モジュラスで伸びの大きな柔らかなものとなるように設計されている。このため、塗布した塗料の硬化後、塗膜が硬く、伸びの小さなものであると、シーリング材上に塗布し形成された塗膜がシーリング材の変位に追従できず、その歪みが塗膜の割れ、亀裂となって現れると考えられている。更には、シーリング材組成物に相溶性の悪い液状物が多く含まれていると、シーリング材硬化後、この液状物が塗膜中に移行(ブリード)して上塗りした塗膜が粘着性となり、空気中を浮遊する砂埃や煤等の塵埃が付着して、塗膜表面に汚染が生じるという問題もある。
In this way, the coating specifications using high-durability paint to achieve high durability and long life for building overviews and civil engineering structures are excellent, but the coating film is hard and has little elongation For this reason, when such a paint is applied onto the cured sealant at the joint, there is a problem that the coating film is cracked or cracked.
That is, the members that make up the outer wall are hard and highly rigid materials, so that the coating film is adapted to this, it is hard for high durability even in the top coating, and it is progressing in the direction of reducing elongation, The sealing material that fills and constructs joints that form the joints of components such as outer walls must absorb various joint displacements caused by expansion and contraction of members caused by temperature differences depending on the climate, wind pressure, earthquakes, etc. Therefore, the properties after curing are designed to be soft with low modulus and large elongation. For this reason, after the applied coating is cured, if the coating film is hard and has a small elongation, the coating film formed on the sealing material cannot follow the displacement of the sealing material, and the distortion of the coating film It is thought that it appears as a crack. Furthermore, if the sealing material composition contains a lot of liquids with poor compatibility, after the sealing material is cured, the liquid material migrates (bleeds) into the coating film, and the coated film becomes sticky, There is also a problem that dust such as dust and soot floating in the air adheres and the surface of the coating film is contaminated.
塗膜表面の汚染の問題を改善するため、シーリング材中に含まれる低分子量の可塑剤成分に代えて、ビニル重合体からなる可塑剤を添加するか、特定量以下の可塑剤とポリオールとを組み合わせて使用するとか、プロセスオイルとひまし油系ポリオールとを組み合わせて使用するなどの方法が提案されている(たとえば、特許文献1、特許文献2および特許文献3、参照)。
しかしながら、未だ上塗り塗装仕様において、上塗り塗装の亀裂、割れがみられ、フリードによる汚染を防止する効果がまだ不十分であったり、汚染防止効果はみられるが使用する化合物や樹脂などそれ自身の粘度が比較的高いため、シーリング材の粘性が高くなり作業性を損なっているなどの課題が残っている。
このように上塗り塗装仕様向けのシーリング材組成物において、上塗りした塗膜に亀裂、割れを起こさない、また塗料へのブリードがなくしたがって耐汚染性に優れ、更には基材である外壁材との接着性が良く、耐久性に優れた低ジュラス、高伸び、高強度な性能を有する上塗り塗装仕様向けのシーリング材組成物は、未だ見出されていない。
In order to improve the problem of coating surface contamination, a plasticizer made of a vinyl polymer is added instead of a low molecular weight plasticizer component contained in the sealing material, or a plasticizer and a polyol of a specific amount or less are added. Methods such as use in combination or use of process oil and castor oil-based polyol in combination have been proposed (see, for example, Patent Document 1, Patent Document 2, and Patent Document 3).
However, in the top coat specifications, cracks and cracks in the top coat are still seen, and the effect of preventing contamination by freed is still insufficient, or the contamination prevention effect is seen, but the viscosity of the compound or resin used itself However, since the viscosity of the sealing material is high, problems such as the loss of workability remain.
In this way, in the sealant composition for the top coat specification, the top coat film does not crack or break, there is no bleed to the paint, therefore it is excellent in stain resistance, and further with the outer wall material which is the base material. No sealant composition has yet been found for topcoat specifications having good adhesion, excellent durability, low dura, high elongation, and high strength.
上述のように上塗り塗装仕様向けのシーリング材組成物において、上塗りした塗膜に亀裂、割れを起こさせないとともに塗膜の耐汚染性に優れ、更には基材である外壁材との接着性が良く、耐久性に優れた低モジュラス、高伸び、高強度な性能を有する上塗り塗装仕様向けのシーリング材組成物が求められている。
そこで、本発明は、上記問題点を解決したシーリング材組成物を提供するとともに、このシーリング材組成物を使用した施工方法を提供することを目的とするものである。
As mentioned above, in the sealing material composition for topcoat coating specifications, it does not cause cracks or cracks in the overcoated film, and is excellent in stain resistance of the coated film, and also has good adhesion to the outer wall material that is the base material. Therefore, there is a need for a sealing material composition for topcoat specifications having excellent durability, low modulus, high elongation, and high strength.
Then, this invention aims at providing the construction method using this sealing material composition while providing the sealing material composition which solved the said problem.
本発明者らは上記問題に鑑み鋭意検討した結果、高耐久性を有する上塗り塗料を使用する外壁材への塗装仕様において、この仕様に用いられるシーリング材組成物に低分子量の可塑剤を少なくとも含有する可塑剤を配合することにより、シーリング材からのブリードが極めて少なくしたがって上塗り塗装仕上げをしても目地汚染がなく、更に塗膜の割れを発生させないことを見出し本発明を完成した。
すなわち、本発明は、常温硬化性樹脂を含有するシーリング材組成物に、低分子量可塑剤を少なくとも含有する可塑剤を、該低分子量可塑剤が、該シーリング材組成物中に2〜12質量%となるように配合することを特徴とする上塗り塗装仕様向けに適したシーリング材組成物に関するものである。
ここで、常温硬化性樹脂を含有するシーリング材組成物としては、常温硬化性樹脂を含むものまたは常温硬化性樹脂からなるものを指し、この常温硬化性樹脂としてはイソシアネート基含有ウレタンプレポリマー、架橋性シリル基含有樹脂などが挙げられる。
さらに、低分子量可塑剤を少なくとも含有する可塑剤としては、低分子量可塑剤を含有する可塑剤、低分子量可塑剤と高分子量可塑剤との混合物よりなる可塑剤が挙げられる。低分子量可塑剤としては、酸エステル類、さらにはジイソノニルフタレートなどが挙げられ、高分子量可塑剤としてはウレタン系高分子可塑剤などが挙げられる。
また、本発明のシーリング材組成物には、そのほかの添加剤、たとえば耐候安定剤、揺変性付与剤、充填剤、接着性付与剤、保存安定性改良剤(脱水剤)、着色剤、硬化促進触媒などが添加されていてもよい。
さらに、本発明の上塗り塗装仕様の塗膜の伸びが100%以下である上塗り塗装仕様向けに適したシーリング材組成物に関するものであり、また本発明のシーリング材組成物よりなるシーリング材を外壁目地に充填施工した後、上塗り塗料を塗装したとき、上塗り塗膜が亀裂防止性かつ汚染防止性に優れていることを特徴とするシーリング材の施工方法に関するものである。
As a result of intensive studies in view of the above problems, the present inventors have at least a low molecular weight plasticizer in the sealing material composition used in this specification in a coating specification for an outer wall material using a highly durable top coating. By blending the plasticizer to be used, the present invention was completed by finding that there is very little bleed from the sealing material, so that there is no joint contamination even when the top coat is finished, and no cracking of the coating film occurs.
That is, the present invention provides a sealing material composition containing a room temperature curable resin, a plasticizer containing at least a low molecular weight plasticizer, and the low molecular weight plasticizer is 2 to 12% by mass in the sealing material composition. It is related with the sealing material composition suitable for top coat specifications characterized by mix | blending so that it may become.
Here, the room temperature curable resin-containing sealing material composition includes a room temperature curable resin or a room temperature curable resin, and the room temperature curable resin includes an isocyanate group-containing urethane prepolymer, a cross-linked resin. And a functional silyl group-containing resin.
Furthermore, examples of the plasticizer containing at least a low molecular weight plasticizer include a plasticizer containing a low molecular weight plasticizer and a plasticizer comprising a mixture of a low molecular weight plasticizer and a high molecular weight plasticizer. Examples of the low molecular weight plasticizer include acid esters and further diisononyl phthalate, and examples of the high molecular weight plasticizer include urethane polymer plasticizer.
In addition, the sealing material composition of the present invention includes other additives such as a weather resistance stabilizer, a thixotropic agent, a filler, an adhesion promoter, a storage stability improver (dehydrating agent), a colorant, and a curing accelerator. A catalyst or the like may be added.
Furthermore, the present invention relates to a sealing material composition suitable for the top coating specification in which the elongation of the coating film of the top coating specification of the present invention is 100% or less, and the sealing material comprising the sealing material composition of the present invention is applied to the outer wall joint. The present invention relates to a method for applying a sealing material, characterized in that when a top coat is applied after filling, the top coat is excellent in crack prevention and contamination prevention.
本発明の上塗り塗装仕様向けに適したシーリング材組成物とは、建築物外壁等を上塗り塗装することを仕様として採用する物件の目地に好適に使用されるシーリング材組成物のことをいう。 The sealing material composition suitable for the topcoat coating specification of the present invention refers to a sealing material composition that is suitably used for joints of properties that employ a topcoat coating on the exterior wall of a building as a specification.
なお、本発明において、上塗り塗装仕様向けとは、建築物外壁等を上塗り塗装することを仕様として採用するものであれば、どのような外壁を構成する部材であってもまたどのような上塗り塗料でもよいが、好ましくは上塗り塗料の塗膜の伸びが100%以下である高耐久性を有する上塗り塗料を使用した外壁材への塗装をする場合のことをいう。 In the present invention, the term “for top coat specification” means that any top coating material can be used for any member that constitutes the outer wall as long as it is used as a specification for coating the outer wall of a building. However, it preferably refers to the case where coating is applied to the outer wall material using a highly durable top coat whose elongation of the top coat is 100% or less.
本発明のシーリング材組成物で使用する成分について以下に説明する。 The components used in the sealing material composition of the present invention will be described below.
まず本発明において使用する常温硬化性樹脂について説明する。常温硬化性樹脂は、大気中の水分や酸素あるいは硬化剤を利用して常温で硬化する硬化成分として使用するものであり、イソシアネート基含有ウレタンプレポリマー、架橋性シリル基含有樹脂、ポリサルファイド樹脂などが挙げられる。このうち一液型の湿気硬化性樹脂として使用でき、得られるシーリング材組成物の作業性が良好な点で、イソシアネート基含有ウレタンプレポリマーあるいは架橋性シリル基含有樹脂が好ましい。 First, the room temperature curable resin used in the present invention will be described. A room temperature curable resin is used as a curing component that cures at room temperature using moisture, oxygen in the atmosphere, or a curing agent, such as an isocyanate group-containing urethane prepolymer, a crosslinkable silyl group-containing resin, and a polysulfide resin. Can be mentioned. Of these, an isocyanate group-containing urethane prepolymer or a crosslinkable silyl group-containing resin is preferred because it can be used as a one-component moisture-curable resin and the workability of the resulting sealing material composition is good.
イソシアネート基含有ウレタンプレポリマーは、イソシアネート基が大気中の水分(湿気)と反応し、尿素結合を形成して架橋、硬化するもので、本発明における硬化性組成物に硬化成分として含有させるものであり、有機ポリイソシアネートと活性水素含有化合物とを活性水素(基)に対してイソシアネート基過剰条件で反応させて得られるものである。 The isocyanate group-containing urethane prepolymer is one in which an isocyanate group reacts with moisture (humidity) in the atmosphere to form a urea bond to crosslink and cure, and is contained in the curable composition of the present invention as a curing component. Yes, it is obtained by reacting an organic polyisocyanate and an active hydrogen-containing compound with active hydrogen (group) under an excess of isocyanate groups.
有機ポリイソシアネートとしては、具体的には例えば、フェニレンジイソシアネート、ジフエニルジイソシアネート、ナフタレンジイソシアネート、4,4’−ジフエニルメタンジイソシアネート、2,4’−ジフエニルメタンジイソシアネート等のジフエニルメタンジイソシアネート(MDI)類、2,4−トルエンジイソシアネート、2,6−トルエンジイソシアネート等のトルエンジイソシアネート(TDI)類、ジフェニルエーテルジイソシアネート等の芳香族ジイソシアネート、キシリレンジイソシアネート等の芳香脂肪族ジイソシアネート、ヘキサメチレンジイソシアネート、ペンタメチレンジイソシアネート、プロピレンジイソシアネート、ブチレンジイソシアネート等の脂肪族ジイソシアネート、シクロヘキサンジイソシアネート、メチレンビス(シクロヘキシルイソシアネート)、イソホロンジイソシアネート等の脂環族ジイソシアネート、およびこれらジイソシアネートのカルボジイミド変性体、ビウレット変性体、アロファネート変性体、二量体、三量体、または、ポリメチレンポリフェニルポリイソシアネート(クルードMDI、ポリメリックMDI)などが挙げられ、これらは単独または2種以上を組合わせて用いることができる。
これらのうち、硬化後の引張り接着性や耐水性などが優れている点で、有機ポリイソシアネートのなかで芳香族ジイソシアネート、芳香脂肪族ジイソシアネートが好ましく、よりさらにMDI類が好ましく、特に4,4′−ジフェニルメタンジイソシアネートが好ましい。
Specific examples of the organic polyisocyanate include diphenylmethane diisocyanate (MDI) such as phenylene diisocyanate, diphenyl diisocyanate, naphthalene diisocyanate, 4,4′-diphenylmethane diisocyanate, and 2,4′-diphenylmethane diisocyanate. , Toluene diisocyanates (TDI) such as 2,4-toluene diisocyanate, 2,6-toluene diisocyanate, aromatic diisocyanates such as diphenyl ether diisocyanate, araliphatic diisocyanates such as xylylene diisocyanate, hexamethylene diisocyanate, pentamethylene diisocyanate, Aliphatic diisocyanates such as propylene diisocyanate and butylene diisocyanate, cyclohexane diisocyanate , Alicyclic diisocyanates such as methylenebis (cyclohexyl isocyanate) and isophorone diisocyanate, and carbodiimide-modified, biuret-modified, allophanate-modified, dimer, trimer or polymethylene polyphenyl polyisocyanate (crude) of these diisocyanates MDI, polymeric MDI) and the like, and these can be used alone or in combination of two or more.
Of these, aromatic diisocyanates and araliphatic diisocyanates are preferred among organic polyisocyanates, and MDIs are more preferred, particularly 4,4 ', in terms of excellent tensile adhesion after curing and water resistance. -Diphenylmethane diisocyanate is preferred.
また、イソシアネート基含有ウレタンプレポリマーの変性用として、n−ブチルモノイソシアネート、n−ヘキシルモノイソシアネート、n−テトラデシルモノイソシアネート、n−オクタデシルモノイソシアネート、p−イソプロピルフェニルモノイソシアネート等の有機モノイソシアネートも使用できる。 In addition, organic monoisocyanates such as n-butyl monoisocyanate, n-hexyl monoisocyanate, n-tetradecyl monoisocyanate, n-octadecyl monoisocyanate, p-isopropylphenyl monoisocyanate are also used for modification of the isocyanate group-containing urethane prepolymer. Can be used.
前記活性水素含有化合物としては、高分子ポリオールや高分子ポリアミンの他、場合により使用する鎖延長剤としての、低分子ポリオール、低分子アミノアルコール、低分子ポリアミン、或いはイソシアネート基含有ウレタンプレポリマーの変性用として用いる高分子や低分子のモノオールなどが挙げられる。 As the active hydrogen-containing compound, in addition to a polymer polyol or polymer polyamine, a low molecular polyol, a low molecular amino alcohol, a low molecular polyamine, or a modification of an isocyanate group-containing urethane prepolymer as a chain extender used in some cases. Examples thereof include a high molecular weight polymer and a low molecular weight monool.
高分子ポリオールとしては、例えば、ポリエステルポリオール、ポリカーボネートポリオール、ポリオキシアルキレン系ポリオール、炭化水素系ポリオール、ポリ(メタ)アクリレート系ポリオール、動植物系ポリオール、これらのコポリオール、またはこれらの2種以上の混合物などが挙げられる。
高分子ポリオールの数平均分子量は、500以上、さらに1,000〜100,000、よりさらに1、000〜30,000、特に1,000〜20,000が好ましい。数平均分子量が500未満では、得られる硬化性組成物の硬化後の伸びなどのゴム弾性物性が悪化し、100,000を超えると、得られるイソシアネート基含有ウレタンプレポリマーの粘度が高くなり過ぎ、作業性が悪くなるため好ましくない。
Examples of the polymer polyol include polyester polyol, polycarbonate polyol, polyoxyalkylene polyol, hydrocarbon polyol, poly (meth) acrylate polyol, animal and plant polyol, these copolyols, or a mixture of two or more of these. Etc.
The number average molecular weight of the polymer polyol is 500 or more, preferably 1,000 to 100,000, more preferably 1,000 to 30,000, and particularly preferably 1,000 to 20,000. If the number average molecular weight is less than 500, rubber elastic properties such as elongation after curing of the resulting curable composition deteriorate, and if it exceeds 100,000, the viscosity of the resulting isocyanate group-containing urethane prepolymer becomes too high, Since workability deteriorates, it is not preferable.
ポリエステルポリオールとしては、例えば、コハク酸、アジピン酸、セバシン酸、アゼライン酸、テレフタル酸、イソフタル酸、オルソフタル酸、ヘキサヒドロテレフタル酸、ヘキサヒドロイソフタル酸、へキサヒドロオルソフタル酸、ナフタレンジカルボン酸、トリメリット酸等のポリカルボン酸、酸エステル、または酸無水物等の1種以上と、エチレングリコール、1,2−プロパンジオール、1,3−プロパンジオール、1,2−ブタンジオール、1,3−ブタンジオール、1,4−ブタンジオール、1,5−ペンタンジオール、1,6−ヘキサンジオール、3−メチル−1,5−ペンタンジオール、ネオペンチルグリコール、1,8−オクタンジオール、1,9−ノナンジオール、ジエチレングリコール、ジプロピレングリコール、1,4−シクロへキサンジメタノール、ビスフェノールAのエチレンオキサイドあるいはプロピレンオキサイド付加物、トリメチロールプロパン、グリセリン、ペンタエリスリトール等の低分子ポリオール類、ブチレンジアミン、ヘキサメチレンジアミン、キシリレンジアミン、イソホロンジアミン等の低分子ポリアミン類、モノエタノールアミン、ジエタノールアミン等の低分子アミノアルコール類の1種以上との脱水縮合反応で得られる、ポリエステルポリオールまたはポリエステルアミドポリオールが挙げられる。
また、例えば、低分子ポリオール類、低分子ポリアミン類、低分子アミノアルコール類を開始剤として、ε-カプロラクトン、γ−バレロラクトン等の環状エステル(ラクトン)モノマーの開環重合で得られるラクトン系ポリエステルポリオールが挙げられる。
Examples of polyester polyols include succinic acid, adipic acid, sebacic acid, azelaic acid, terephthalic acid, isophthalic acid, orthophthalic acid, hexahydroterephthalic acid, hexahydroisophthalic acid, hexahydroorthophthalic acid, naphthalenedicarboxylic acid, triphthalic acid, and the like. One or more of polycarboxylic acids such as merit acid, acid esters, or acid anhydrides, ethylene glycol, 1,2-propanediol, 1,3-propanediol, 1,2-butanediol, 1,3- Butanediol, 1,4-butanediol, 1,5-pentanediol, 1,6-hexanediol, 3-methyl-1,5-pentanediol, neopentyl glycol, 1,8-octanediol, 1,9- Nonanediol, diethylene glycol, dipropylene glycol, 1 , 4-cyclohexanedimethanol, ethylene oxide or propylene oxide adduct of bisphenol A, low molecular polyols such as trimethylolpropane, glycerin, pentaerythritol, butylenediamine, hexamethylenediamine, xylylenediamine, isophoronediamine, etc. Examples thereof include polyester polyols or polyester amide polyols obtained by a dehydration condensation reaction with one or more low molecular amino alcohols such as low molecular polyamines, monoethanolamine, and diethanolamine.
Also, for example, lactone polyesters obtained by ring-opening polymerization of cyclic ester (lactone) monomers such as ε-caprolactone and γ-valerolactone using low molecular polyols, low molecular polyamines, and low molecular amino alcohols as initiators. A polyol is mentioned.
ポリカーボネートポリオールとしては、例えば、前述のポリエステルポリオールの合成に用いられる低分子ポリオール類とホスゲンとの脱塩酸反応、あるいは前記低分子ポリオール類とジエチレンカーボネート、ジメチルカーボネート、ジエチルカーボネート、ジフェニルカーボネート等とのエステル交換反応で得られるものが挙げられる。 Examples of the polycarbonate polyol include dehydrochlorination reaction of low molecular polyols and phosgene used in the synthesis of the polyester polyol described above, or esters of the low molecular polyols with diethylene carbonate, dimethyl carbonate, diethyl carbonate, diphenyl carbonate, and the like. What is obtained by an exchange reaction is mentioned.
ポリオキシアルキレン系ポリオールとしては、例えば、前述のポリエステルポリオールの合成に用いられる低分子ポリオール類、低分子ポリアミン類、低分子アミノアルコール類、ポリカルボン酸の他、ソルビトール、マンニトール、ショ糖(スクロース)、グルコース等の糖類系低分子多価アルコール類、ビスフェノールA、ビスフェノールF等の低分子多価フェノール類の一種以上を開始剤として、エチレンオキシド、プロピレンオキシド、ブチレンオキシド、テトラヒドロフラン等の環状エーテル化合物の1種以上を開環付加重合あるいは共重合(以下、「重合あるいは共重合」を(共)重合という。)させた、ポリオキシエチレン系ポリオール、ポリオキシプロピレン系ポリオール、ポリオキシブチレン系ポリオール、ポリオキシテトラメチレン系ポリオール、ポリ−(オキシエチレン)−(オキシプロピレン)−ランダムあるいはブロック共重合系ポリオール、さらに、前述のポリエステルポリオールやポリカーボネートポリオールを開始剤としたポリエステルエーテルポリオール、ポリカーボネートエーテルポリオールなどが挙げられる。また、これらの各種ポリオールと有機イソシアネートとを、イソシアネート基に対し水酸基過剰で反応させて、分子末端を水酸基としたポリオールも挙げられる。
ポリオキシアルキレン系ポリオールの1分子当たり平均アルコール性水酸基の数は2個以上、さらに2〜4個、特に2〜3個が好ましい。
Examples of the polyoxyalkylene polyol include low molecular polyols, low molecular polyamines, low molecular amino alcohols, polycarboxylic acids, sorbitol, mannitol, sucrose used for the synthesis of the above-described polyester polyols. 1 or more of cyclic ether compounds such as ethylene oxide, propylene oxide, butylene oxide, and tetrahydrofuran using one or more of low molecular weight polyhydric alcohols such as saccharides such as glucose and low molecular weight polyphenols such as bisphenol A and bisphenol F as initiators A polyoxyethylene-based polyol, a polyoxypropylene-based polyol, a polyoxybutylene-based polyol, a polyoxyethylene, which is obtained by ring-opening addition polymerization or copolymerization (hereinafter, “polymerization or copolymerization” is referred to as (co) polymerization). Ramechiren polyols, poly - (oxyethylene) - (oxypropylene) - random or block copolymer polyols, further polyester polyether polyol initiator polyester polyols and polycarbonate polyols described above, such as polycarbonate polyether polyols. Moreover, the polyol which made these various polyols and organic isocyanate react by hydroxyl group excess with respect to an isocyanate group, and made the molecular terminal a hydroxyl group is also mentioned.
The number of average alcoholic hydroxyl groups per molecule of the polyoxyalkylene polyol is preferably 2 or more, more preferably 2 to 4, and particularly preferably 2 to 3.
さらに、ポリオキシアルキレン系ポリオールは、その製造時に、水素化セシウム、セシウムメトキシド、セシウムエトキシド等のセシウムアルコキシド、水酸化セシウムなどのセシウム系化合物、ジエチル亜鉛、塩化鉄、金属ポルフィリン、ホスファゼニウム化合物、複合金属シアン化錯体など、なかでも亜鉛ヘキサシアノコバルテートのグライム錯体やジグライム錯体等の複合金属シアン化錯体を触媒として使用して得られる、総不飽和度が0.1meq/g以下、さらに0.07meq/g以下、特に0.04meq/g以下のものが好ましく、分子量分布〔ゲルパーミエーションクロマトグラフィー(GPC)によるポリスチレン換算の重量平均分子量(Mw)と数平均分子量(Mn)との比=Mw/Mn〕が1.6以下、特に1.0〜1.3の狭いものが、得られるイソシアネネート基含有ウレタンプレポリマーの粘度を低下でき、かつ得られる硬化組成物の硬化後のゴム弾性物性が良好となる点で好ましい。 Furthermore, the polyoxyalkylene-based polyol is produced at the time of production thereof by cesium hydride, cesium methoxide, cesium alkoxide such as cesium ethoxide, cesium-based compounds such as cesium hydroxide, diethyl zinc, iron chloride, metalloporphyrin, phosphazenium compound, The total unsaturation obtained by using a double metal cyanide complex such as a double metal cyanide complex such as a zinc hexacyanocobaltate glyme complex or diglyme complex as a catalyst is 0.1 meq / g or less. 07 meq / g or less, particularly 0.04 meq / g or less is preferable, and molecular weight distribution [ratio of weight average molecular weight (Mw) and number average molecular weight (Mn) in terms of polystyrene by gel permeation chromatography (GPC) = Mw / Mn] is 1.6 or less, especially 1.0 Having a narrow 1.3, viscosity of the resulting diisocyanate sulfonate group-containing urethane prepolymer can reduce, and rubber elasticity properties after curing of the resulting cured composition is preferable in that is good.
また、イソシアネート基含有ウレタンプレポリマーの変性用として、メチルアルコール、エチルアルコール、プロピルアルコール等の低分子モノアルコール類を開始剤として、前記プロピレンオキシド等の環状エーテル化合物を開環付加重合させたポリオキシプロピレン系モノオール等のポリオキシアルキレン系モノオールなどを場合により使用することもできる。
なお、前記ポリオキシアルキレン系ポリオールあるいはポリオキシアルキレン系モノオールなどの「系」とは、分子1モル中の水酸基を除いた部分の50質量%以上、さらに80質量%以上、特に好ましくは90質量%以上がポリオキシアルキレンで構成されていれば、残りの部分がエステル、ウレタン、ポリカーボネート、ポリアミド、ポリ(メタ)アクリレート、ポリオレフィンなどで変性されていてもよいことを意味するが、水酸基を除いた分子の95質量%以上がポリオキシアルキレンから成るものが最も好ましい。
In addition, for modification of an isocyanate group-containing urethane prepolymer, polyoxyl obtained by ring-opening addition polymerization of a cyclic ether compound such as propylene oxide using a low-molecular monoalcohol such as methyl alcohol, ethyl alcohol or propyl alcohol as an initiator. In some cases, polyoxyalkylene monools such as propylene monools may be used.
The “system” such as the polyoxyalkylene-based polyol or polyoxyalkylene-based monool is 50% by mass or more, further 80% by mass or more, particularly preferably 90% by mass of the portion excluding the hydroxyl group in 1 mol of the molecule. % Or more is composed of polyoxyalkylene, which means that the remaining part may be modified with ester, urethane, polycarbonate, polyamide, poly (meth) acrylate, polyolefin, etc., except for hydroxyl groups. Most preferably, 95% by mass or more of the molecules consist of polyoxyalkylene.
炭化水素系ポリオールとしては、例えば、ポリブタジエンポリオール、ポリイソプレンポリオール等のポリオレフィンポリオール、水添ポリブタジエンポリオール、水添ポリイソプレンポリオール等のポリアルキレンポリオール、塩素化ポリプロピレンポリオール、塩素化ポリエチレンポリオール等のハロゲン化ポリアルキレンポリオールなどが挙げられる。 Examples of the hydrocarbon polyol include polyolefin polyols such as polybutadiene polyol and polyisoprene polyol, polyalkylene polyols such as hydrogenated polybutadiene polyol and hydrogenated polyisoprene polyol, halogenated poly such as chlorinated polypropylene polyol and chlorinated polyethylene polyol. Examples include alkylene polyols.
ポリ(メタ)アクリレート系ポリオールとしては、ヒドロキシエチル(メタ)アクリレート等の水酸基を含有する(メタ)アクリレート単量体類と他の(メタ)アクリル酸アルキルエステル単量体とを、ラジカル重合開始剤の存在下あるいは不存在下に共重合したものなどが挙げられる。 As a poly (meth) acrylate-based polyol, a (meth) acrylate monomer containing a hydroxyl group such as hydroxyethyl (meth) acrylate and another (meth) acrylic acid alkyl ester monomer are used as a radical polymerization initiator. And those copolymerized in the presence or absence of.
動植物系ポリオールとしては、例えば、ヒマシ油系ジオールなどが挙げられる。 Examples of animal and plant-based polyols include castor oil-based diols.
鎖延長剤としては、前記のポリエステルポリオールの合成に用いられる低分子のポリオール類、ポリアミン類、アミノアルコール類の他、前述のポリオキシアルキレンポリオールで、数平均分子量が500未満の低分子量のもの、またはこれらの2種以上の混合物が例示される。
前記の活性水素含有化合物として挙げた化合物は1種または2種以上を組み合わせて使用することができるが、これらのうち、得られる硬化性組成物のゴム弾性物性や接着性が良好な点で、高分子ポリオールが好ましく、さらにポリオキシアルキレン系ポリオールが好ましく、ポリオキシプロピレン系ポリオールが最も好ましい。
As the chain extender, in addition to the low molecular weight polyols, polyamines and amino alcohols used in the synthesis of the polyester polyol, the polyoxyalkylene polyol described above has a low molecular weight with a number average molecular weight of less than 500, Or the mixture of these 2 or more types is illustrated.
The compounds mentioned as the active hydrogen-containing compound can be used alone or in combination of two or more, but among these, the rubber elastic properties and adhesiveness of the resulting curable composition are good, High molecular polyols are preferred, polyoxyalkylene polyols are more preferred, and polyoxypropylene polyols are most preferred.
本発明におけるイソシアネート基含有ウレタンプレポリマーは、一括仕込み反応法、多段階仕込み反応法のいずれでも合成できるが、プレポリマーの分子中にイソシアネート基を残す必要がある。有機イソシアネートのイソシアネート基と高分子ポリオール、場合により更に鎖延長剤等の活性水素含有化合物の活性水素(基)とのイソシアネート基/活性水素(基)の当量比は、1.1〜5.0/1.0が好ましく、更に1.3〜2.0/1.0が好ましい。このようにして得られるイソシアネート基含有ウレタンプレポリマーのイソシアネート基含有量は0.1〜15.0質量%が好ましく、特に0.3〜10.0質量%が好ましく、最も好ましくは0.4〜5.0質量%である。イソシアネート基含有量が0.1質量%未満の場合は、分子量が大きくなりすぎて粘度が増大し作業性が低下する。また、プレポリマー中の架橋点が少ないため、十分な接着性が得られない。イソシアネート基含有量が15.0質量%を超える場合は、イソシアネート基が水分と反応して生成する炭酸ガスによる発泡を防止することが困難になるため好ましくない。 The isocyanate group-containing urethane prepolymer in the present invention can be synthesized by either a batch charge reaction method or a multistage charge reaction method, but it is necessary to leave an isocyanate group in the molecule of the prepolymer. The isocyanate group / active hydrogen (group) equivalent ratio of the isocyanate group of the organic isocyanate and the polymer polyol and optionally the active hydrogen (group) of the active hydrogen-containing compound such as a chain extender is 1.1 to 5.0. /1.0 is preferable, and 1.3 to 2.0 / 1.0 is more preferable. The isocyanate group-containing urethane prepolymer thus obtained preferably has an isocyanate group content of 0.1 to 15.0% by mass, particularly preferably 0.3 to 10.0% by mass, and most preferably 0.4 to 5.0% by mass. When the isocyanate group content is less than 0.1% by mass, the molecular weight becomes too large, the viscosity increases, and the workability decreases. Moreover, since there are few crosslinking points in a prepolymer, sufficient adhesiveness cannot be obtained. When the isocyanate group content exceeds 15.0% by mass, it is difficult to prevent foaming due to carbon dioxide gas generated by the reaction of the isocyanate group with moisture, such being undesirable.
本発明におけるイソシアネート基含有ウレタンプレポリマーの合成には、後述の硬化促進触媒としてあげた化合物と同様の、公知の触媒をウレタン化触媒として用いることができる。これらのうち金属有機酸塩や有機金属と有機酸との塩が好ましく、特にジブチル錫ジラウレートが好ましい。また、さらに公知の有機溶媒を用いることができる。 In the synthesis of the isocyanate group-containing urethane prepolymer in the present invention, a known catalyst similar to the compound mentioned as the curing acceleration catalyst described later can be used as the urethanization catalyst. Among these, metal organic acid salts and salts of organic metals and organic acids are preferable, and dibutyltin dilaurate is particularly preferable. Furthermore, a known organic solvent can be used.
つぎに、架橋性シリル基含有樹脂について説明する。
架橋性シリル基含有樹脂としては、一般に変成シリコーン樹脂と呼ばれているものを挙げることができる。大気中の水分と反応して重合しシロキサン結合を形成することにより架橋してゴム状硬化物を形成する、分子内に架橋性シリル基を0.5個以上含有する樹脂である。
変成シリコーン樹脂としては、例えば特開昭52−73998号公報、特開昭55−9669号公報、特開59−122541号公報、特開昭60−6747号公報、特開昭61−233043号公報、特開昭63−112642号公報、特開平3−79627号公報、特開平4−283259号公報、特開平5−70531号公報、特開平5−287186号公報、特開平11−80571号公報、特開平11−116763号公報、特開平11−130931号公報中に開示されているものを挙げることができる。具体的には、分子内に0.5個以上の架橋性シリル基を含有する、主鎖がポリオキシアルキレン系重合体、ビニル変性ポリオキシアルキレン系重合体、ビニル系重合体、ポリイソプレンやポリブタジエン等のジエン系重合体、ポリエステル系重合体、アクリル及び/またはメタクリル(以下、(メタ)アクリルという。)酸エステル系重合体、ポリサルファイド重合体、これらの共重合体、混合物等が挙げられる。
変成シリコーン樹脂の主鎖は、硬化後の引張接着性、モジュラス等の物性の点から、ポリオキシアルキレン系重合体が好ましく、さらにポリオキシプロピレン系重合体が好ましい。
Next, the crosslinkable silyl group-containing resin will be described.
Examples of the crosslinkable silyl group-containing resin include what is generally called a modified silicone resin. It is a resin containing 0.5 or more crosslinkable silyl groups in the molecule, which reacts with moisture in the atmosphere to form a siloxane bond and crosslink to form a rubber-like cured product.
Examples of the modified silicone resin include JP-A-52-73998, JP-A-55-9669, JP-A-59-122541, JP-A-60-6747, JP-A-61-233043. JP-A-63-112642, JP-A-3-79627, JP-A-4-283259, JP-A-5-70531, JP-A-5-287186, JP-A-11-80571, Examples disclosed in JP-A-11-116763 and JP-A-11-130931 can be mentioned. Specifically, the main chain contains 0.5 or more crosslinkable silyl groups in the molecule and the main chain is a polyoxyalkylene polymer, a vinyl-modified polyoxyalkylene polymer, a vinyl polymer, polyisoprene or polybutadiene. And diene polymers, polyester polymers, acrylic and / or methacrylic (hereinafter referred to as (meth) acrylic) acid ester polymers, polysulfide polymers, copolymers and mixtures thereof.
The main chain of the modified silicone resin is preferably a polyoxyalkylene polymer, more preferably a polyoxypropylene polymer, from the viewpoint of physical properties such as tensile adhesion after curing and modulus.
架橋性シリル基は、組成物の硬化性や硬化後の物性等の点から、分子内に0.5〜5個含まれるのが好ましい。更に架橋性シリル基は、架橋しやすく製造しやすい次の一般式(1)で示されるものが好ましい。
架橋性シリル基の主鎖への導入は、以下の公知の方法で行うことができる。
(1)末端に水酸基等の官能基を有するポリオキシアルキレン系重合体に、この官能基に対して反応性を示す活性基及び不飽和基を有する有機化合物(例えばアリルイソシアネート)を反応させ、ついで得られる反応生成物に加水分解性基を有するヒドロシランを作用させてヒドロシリル化する。
(2)末端に水酸基、アミノ基、エポキシ基、イソシアネート基等の官能基を有するポリオキシアルキレン系重合体に、この官能基に対して反応性を示す官能基及び架橋性シリル基を有する化合物を反応させる。この反応性を示す官能基及び架橋性シリル基を有する化合物は、アミノ基含有シラン類、メルカプト基含有シラン類、エポキシ基含有シラン類、ビニル型不飽和結合含有シラン類、塩素原子含有シラン類、イソシアネー卜基含有シラン類、ハイドロシラン類などが挙げられる。
(3)重合性不飽和結合と架橋性シリル基を有する化合物(例えばCH2=CHSi(OCH3)3)と(メタ)アクリル酸アルキルエステル単量体を共重合させる。
(4)重合性不飽和結合と官能基を有する化合物(例えばヒドロキシエチル(メタ)アクリレート)を(メタ)アクリル酸アルキルエステル単量体に添加して共重合させ、次いで生成する共重合体を前記の反応性官能基及び架橋性シリル基を有する化合物(例えばイソシアネート基と−Si(OCH3)3基を有する化合物)とを反応させる。
架橋性シリル基含有樹脂の数平均分子量は1,000以上、特に6,000〜30,000で分子量分布の狭いものが、硬化前の粘度が低いので取り扱いやすく、硬化後の強度、モジュラス、伸び等の物性が優れているので好適である。
The crosslinkable silyl group can be introduced into the main chain by the following known method.
(1) A polyoxyalkylene polymer having a functional group such as a hydroxyl group at a terminal is reacted with an organic compound (for example, allyl isocyanate) having an active group and an unsaturated group reactive to the functional group, Hydrosilation having hydrolyzable groups is allowed to act on the resulting reaction product to effect hydrosilylation.
(2) A compound having a functional group and a crosslinkable silyl group reactive to this functional group to a polyoxyalkylene polymer having a functional group such as a hydroxyl group, an amino group, an epoxy group or an isocyanate group at the terminal. React. The compound having a reactive functional group and a crosslinkable silyl group includes amino group-containing silanes, mercapto group-containing silanes, epoxy group-containing silanes, vinyl unsaturated bond-containing silanes, chlorine atom-containing silanes, Examples include isocyanate group-containing silanes and hydrosilanes.
(3) A compound having a polymerizable unsaturated bond and a crosslinkable silyl group (for example, CH 2 ═CHSi (OCH 3 ) 3 ) and a (meth) acrylic acid alkyl ester monomer are copolymerized.
(4) A compound having a polymerizable unsaturated bond and a functional group (for example, hydroxyethyl (meth) acrylate) is added to a (meth) acrylic acid alkyl ester monomer for copolymerization, and then the resulting copolymer is the above-mentioned copolymer And a compound having a reactive functional group and a crosslinkable silyl group (for example, a compound having an isocyanate group and —Si (OCH 3 ) 3 group) are reacted.
The number average molecular weight of the crosslinkable silyl group-containing resin is 1,000 or more, particularly 6,000 to 30,000, and a narrow molecular weight distribution is easy to handle because the viscosity before curing is low, and the strength, modulus and elongation after curing. It is preferable because of its excellent physical properties.
つぎに可塑剤について説明する。
本発明における低分子量可塑剤を少なくとも含有する可塑剤とは、低分子量可塑剤が可塑剤成分の一部であってもよいし全部であってもよいが、上塗り塗装仕様向けに適したシーリング材組成物の粘度を低下させ作業性を良好なものとし、
かつ上塗りした塗膜の亀裂防止と汚染防止を両立させるために、可塑剤成分は低分子量可塑剤と高分子量可塑剤の混合物が好ましい。低分子量可塑剤は、シーリング材組成物の硬化後のモジュラスや伸びなどのゴム物性を調節するとともに、
前述したような高耐久性を付与するために伸びが小さく硬いものとなっている塗膜に低分子量可塑剤を汚染を発生させない程度に少量移行(ブリード)させ、硬い塗膜を少し軟化させることにより目地の変位による起こるシーリング材硬化物の伸び等の変化に追従できるようにさせることにより、塗膜が亀裂を発生し難くする効果を発揮させるために必須である。しかし、シーリング材組成物を低粘度化させるため、低分子量可塑剤のみを多量に使用すると上塗りした塗膜にも多量にブリードし、塗膜の耐久性を低下させるとともに、塗膜表面に塵埃等の付着による汚染を発生させてしまうため、塗膜の亀裂防止と汚染防止を両立させ優れたものとするためには低分子量可塑剤の量を適切な量に抑える必要がある。このためシーリング材組成物の粘度低下が不十分になるのを補う目的で高分子量可塑剤を併用する。高分子量可塑剤は、上塗りした塗膜にブリードし難いため、塗膜を汚染させることなくシーリング材組成物の粘度を低下させる効果を発揮する。
Next, the plasticizer will be described.
The plasticizer containing at least the low molecular weight plasticizer in the present invention may be a part or all of the plasticizer component of the low molecular weight plasticizer, but is a sealing material suitable for top coating specifications. Reduce the viscosity of the composition to improve workability,
In order to achieve both prevention of cracking and prevention of contamination of the overcoated film, the plasticizer component is preferably a mixture of a low molecular weight plasticizer and a high molecular weight plasticizer. The low molecular weight plasticizer adjusts the rubber properties such as modulus and elongation after curing of the sealant composition,
In order to impart high durability as described above, the low-molecular weight plasticizer should be transferred to a small amount (bleed) to a level that does not cause contamination to soften the hard coating film. Therefore, it is indispensable for the coating film to exhibit the effect of making it difficult to generate cracks by making it possible to follow changes such as elongation of the cured sealing material caused by joint displacement. However, in order to reduce the viscosity of the sealing material composition, if only a small amount of low molecular weight plasticizer is used, a large amount of bleed occurs on the overcoated film, and the durability of the coated film is reduced, and dust or the like is formed on the surface of the coated film. Therefore, it is necessary to suppress the amount of the low molecular weight plasticizer to an appropriate amount in order to achieve both excellent prevention of cracking and prevention of contamination of the coating film. For this reason, a high molecular weight plasticizer is used in combination for the purpose of compensating for the insufficient viscosity reduction of the sealing material composition. Since the high molecular weight plasticizer is difficult to bleed into the overcoated film, it exhibits the effect of reducing the viscosity of the sealing material composition without contaminating the coated film.
低分子量可塑剤を少なくとも含む可塑剤は、シーリング材組成物全体の2〜35質量%が好ましく、さらには2〜25質量%が好ましい。さらに低分子量可塑剤と高分子量可塑剤の割合は、高分子量可塑剤/低分子量可塑剤の質量比が0〜16.5が好ましく、さらには0.1〜12が好ましい。 The plasticizer including at least the low molecular weight plasticizer is preferably 2 to 35% by mass, more preferably 2 to 25% by mass, based on the whole sealing material composition. Furthermore, as for the ratio of the low molecular weight plasticizer and the high molecular weight plasticizer, the mass ratio of high molecular weight plasticizer / low molecular weight plasticizer is preferably 0 to 16.5, and more preferably 0.1 to 12.
具体的に低分子量可塑剤としては、例えばジブチルフタレート、ジヘプチルフタレート、ジオクチルフタレート、ジ(2−エチルヘキシル)フタレート、ジイソノニルフタレート、ブチルベンジルフタレート、ブチルフタリルブチルグリコレート等のフタル酸エステル類、ジオクチルアジペート、ジオクチルセバケート等の非芳香族二塩基酸エステル類、トリクレジルホスフェート、トリブチルホスフェート等のリン酸エステル類などの酸エステル類が好適に挙げられる。しかし配合したときの粘度低下による作業性向上、ゴム物性調節のしやすさ、ブリード汚染が少ないこと及び環境に対する負荷の低減から、フタル酸エステル類が好ましくさらにジイソノニルフタレートが好ましい。低分子量可塑剤は、シーリング材組成物中に2〜12質量%となるように配合するのが好ましい。2質量%未満では上塗り塗膜に対する亀裂防止の効果がなく、12質量%を超えると塗膜へのブリード量が多くなり汚染が発生しやすくなるため好ましくない。数平均分子量は1,000未満が好ましい。この範囲以外では、配合したときの粘度低下効果とブリードが極めて少ないことの両立が難しくなる。 Specific examples of the low molecular weight plasticizer include phthalates such as dibutyl phthalate, diheptyl phthalate, dioctyl phthalate, di (2-ethylhexyl) phthalate, diisononyl phthalate, butyl benzyl phthalate and butyl phthalyl butyl glycolate, and dioctyl. Suitable examples include non-aromatic dibasic acid esters such as adipate and dioctyl sebacate, and acid esters such as phosphate esters such as tricresyl phosphate and tributyl phosphate. However, phthalic acid esters are preferred and diisononyl phthalate is more preferred because of improved workability due to viscosity reduction when blended, ease of rubber property adjustment, low bleed contamination, and reduced environmental burden. The low molecular weight plasticizer is preferably blended in the sealing material composition so as to be 2 to 12% by mass. If it is less than 2% by mass, there is no effect of preventing cracks on the top coat film, and if it exceeds 12% by mass, the amount of bleed to the film increases and contamination is likely to occur. The number average molecular weight is preferably less than 1,000. Outside this range, it is difficult to achieve both the effect of reducing the viscosity when blended and the fact that there is very little bleeding.
高分子量可塑剤としては、前述のイソシアネート基含有ウレタンプレポリマーの合成に使用されるのと同様のポリオキシアルキレン系ポリオールあるいはこれをエーテル化またはエステル化などしたポリエーテル系可塑剤、ウレタン系高分子可塑剤、ポリブタジエン、ブタジエンーアクリロニトリル共重合体、ポリクロロプレン、ポリイソプレンあるいはこれらの水添物等の炭化水素系重合体などが挙げられるが、このうちポリウレタン系高分子可塑剤がイソシアネート基含有ウレタンプレポリマーと相溶性が良好な点で好ましい。 As the high molecular weight plasticizer, the same polyoxyalkylene polyol used for the synthesis of the above-mentioned isocyanate group-containing urethane prepolymer, or a polyether plasticizer obtained by etherification or esterification thereof, a urethane polymer Examples include plasticizers, polybutadiene, butadiene-acrylonitrile copolymers, polychloroprene, polyisoprene, and hydrocarbon polymers such as hydrogenated products thereof. Among these, polyurethane polymer plasticizers are isocyanate group-containing urethane prepolymers. It is preferable in terms of good compatibility with the polymer.
ウレタン系高分子可塑剤としては、活性水素を有するポリオキシアルキレン化合物とイソシアネート基含有化合物の反応物が好ましく、実質的に水酸基またはイソシアネート基を含有しないウレタン系高分子可塑剤が好ましい。具体的にはポリオキシアルキレン系アルコールと有機イソシアネートをイソシアネート基/水酸基の当量比が0.9〜1.1/1.0となる範囲で、最も好ましくは1/1で反応させて好適に製造することができる。当量比が0.9/1.0を下回ると水酸基の含有量が多くなり、配合したときシーリング材の耐水性や貯蔵安定性が悪化し、また1.1/1.0を上回るとイソシアネート基の含有量が多くなり、硬化後のゴム物性に対する悪影響が無視できなくなる点で好ましくない。数平均分子量は1,000以上、好ましくは1,000〜60,000、さらに好ましくは2,000〜20,000である。この範囲以外では、配合したときの粘度低下効果とブリードが極めて少ないことの両立が難しくなる。 As the urethane polymer plasticizer, a reaction product of a polyoxyalkylene compound having active hydrogen and an isocyanate group-containing compound is preferable, and a urethane polymer plasticizer containing substantially no hydroxyl group or isocyanate group is preferable. Specifically, a polyoxyalkylene alcohol and an organic isocyanate are suitably produced by reacting them in an isocyanate group / hydroxyl group equivalent ratio of 0.9 to 1.1 / 1.0, most preferably 1/1. can do. When the equivalence ratio is less than 0.9 / 1.0, the hydroxyl group content increases, and when blended, the water resistance and storage stability of the sealing material deteriorates. This is not preferable because the content of is increased and the adverse effect on the physical properties of the rubber after curing cannot be ignored. The number average molecular weight is 1,000 or more, preferably 1,000 to 60,000, and more preferably 2,000 to 20,000. Outside this range, it is difficult to achieve both the effect of reducing the viscosity when blended and the fact that there is very little bleeding.
なお、前記実質的に水酸基またはイソシアネート基を含有しないとは、反応当量比の選択により、ウレタン系高分子可塑剤に少量の水酸基またはイソシアネート基が残存する場合があるが、貯蔵安定性や硬化後の物性に影響がなく、含有しないとみなしても差し支えがないことを意味する。 Note that the term “substantially free of hydroxyl groups or isocyanate groups” means that a small amount of hydroxyl groups or isocyanate groups may remain in the urethane polymer plasticizer depending on the selection of the reaction equivalent ratio. This means that there is no influence on the physical properties of the product, and there is no problem even if it is regarded as not containing.
活性水素を有するポリオキシアルキレン化合物であるポリオキシアルキレン系アルコールとしては、ポリオキシアルキレン系モノオール、前述のイソシアネート基含有ウレタンプレポリマーの合成に使用されるのと同様のポリオキシアルキレン系ポリオール、これらの混合物が挙げられるが、粘度を下げ且ブリードの極めて少ない高分子量化合物を得る為には、ポリオキシアルキレン系モノオールが好ましい。ポリオキシアルキレン系モノオールは、活性水素を1個有するアルキル化合物などの開始剤に、アルキレンオキシドを開環付加重合させたものなどである。この開始剤は、メタノール、エタノール、n−プロパノール、iso−プロパノール、n−ブタノール、iso−ブタノール、tert−ブタノール、シクロヘキサノール、フェノール、これらの2種以上の混合物などが挙げられるが、これらの内ではメタノール、エタノール等の炭素数5以下の化合物が好ましい。アルキレンオキシドは、エチレンオキシド、プロピレンオキシド、ブチレンオキシド、テトラヒドロフラン、これら2種以上の混合物等が挙げられるが、これらの内ではプロピレンオキシドが好ましい。さらにポリオキシアルキレン系モノオールは、その製造時に使用する触媒としてセシウム系化合物(水酸化セシウム、セシウムメトキシド、セシウムエトキシド等のセシウムアルコキシド、水酸化セシウム)、ジエチル亜鉛、塩化鉄、金属ポルフィリン、ホスファゼニウム化合物、複合金属シアン化合物など、なかでも亜鉛ヘキサシアノコバルテートのグライム錯体やジグライム錯体等の複合金属シアン錯体を使用して得られる、総不飽和度が0.1meq/g以下、更に0.07meq/g以下、特に0.04meq/g以下のものが好ましく、分子量分布[ゲルパーミエーションクロマトグラフィー(GPC)によるポリスチレン換算の重量平均分子量(Mw)と数平均分子量(Mn)の比=Mw/Mn]が1.6以下、特に1.0〜1.3の狭いものが好ましい。特に低粘度の液状ウレタン化合物を得るためには、分子量分布の狭いポリオキシアルキレン系モノオールを使用することが良い。なお、本発明に於いてポリオキシアルキレン系モノオールとは、分子1モルの水酸基を除いた部分の50質量%以上、さらに80質量%以上、好ましくは90質量%以上がポリオキシアルキレンで構成されていれば、残りの部分がエーテル、ウレタン、エステル、ポリカーボネート、ポリアミド、ポリアクリレート、ポリオレフィンなどで変性されていてもよいことを意味するが、本発明においては水酸基を除いた分子の95質量%以上がポリオキシアルキレンからなるモノオールが最も好ましく、ポリオキシプロピレン系モノオールがよい。 Examples of polyoxyalkylene alcohols that are active oxygen-containing polyoxyalkylene compounds include polyoxyalkylene monools, polyoxyalkylene polyols similar to those used in the synthesis of the aforementioned isocyanate group-containing urethane prepolymers, these In order to reduce the viscosity and obtain a high molecular weight compound with very little bleeding, polyoxyalkylene monools are preferred. The polyoxyalkylene monool is obtained by ring-opening addition polymerization of alkylene oxide to an initiator such as an alkyl compound having one active hydrogen. Examples of the initiator include methanol, ethanol, n-propanol, iso-propanol, n-butanol, iso-butanol, tert-butanol, cyclohexanol, phenol, and a mixture of two or more thereof. Then, compounds having 5 or less carbon atoms such as methanol and ethanol are preferable. Examples of the alkylene oxide include ethylene oxide, propylene oxide, butylene oxide, tetrahydrofuran, and a mixture of two or more thereof. Among these, propylene oxide is preferable. Furthermore, polyoxyalkylene monools are cesium compounds (cesium hydroxide, cesium methoxide, cesium alkoxides such as cesium ethoxide, cesium hydroxide), diethyl zinc, iron chloride, metal porphyrin, The total unsaturation obtained by using a complex metal cyanide complex such as a phosphazenium compound, a complex metal cyanide compound, such as a zinc hexacyanocobaltate glyme complex or a diglyme complex, is 0.1 meq / g or less, and further 0.07 meq. / G or less, particularly 0.04 meq / g or less is preferred, and molecular weight distribution [ratio of weight average molecular weight (Mw) and number average molecular weight (Mn) in terms of polystyrene by gel permeation chromatography (GPC) = Mw / Mn ] Is 1.6 or less, especially 1.0-1. A narrow number of 3 is preferred. In particular, in order to obtain a low-viscosity liquid urethane compound, it is preferable to use a polyoxyalkylene monool having a narrow molecular weight distribution. In the present invention, the polyoxyalkylene monool is 50% by mass or more, more preferably 80% by mass or more, and preferably 90% by mass or more of the portion excluding the hydroxyl group of 1 mol of the molecule. Means that the remaining part may be modified with ether, urethane, ester, polycarbonate, polyamide, polyacrylate, polyolefin, etc., but in the present invention, 95% by mass or more of the molecule excluding the hydroxyl group. Is most preferably a monool comprising polyoxyalkylene, and a polyoxypropylene monool is preferred.
イソシアネート基含有化合物としては、前述のイソシアネート基含有ウレタンプレポリマーの合成に使用されるのと同様の有機ポリイソシアネート、有機モノイソシアネート、これらの混合物などが挙げられ、これらのうち得られるウレタン系高分子可塑剤の粘度を低粘度化できる点で脂肪族ジイソシアネート、脂環族ジイソシアネート、芳香脂肪族ジイソシアネートが好ましく、さらに芳香脂肪族ジイソシアネートが好ましく、特にキシリレンジイソシアネートが好ましい。
ウレタン系高分子可塑剤の合成の際にも、前述のイソシアネート基含有ウレタンプレポリマーの合成に使用されるのと同様のウレタン化触媒を反応触媒として用いることができ、さらに公知の有機溶媒を使用することもできる。
Examples of the isocyanate group-containing compound include the same organic polyisocyanates, organic monoisocyanates, and mixtures thereof used in the synthesis of the aforementioned isocyanate group-containing urethane prepolymers. An aliphatic diisocyanate, an alicyclic diisocyanate, and an araliphatic diisocyanate are preferable, an araliphatic diisocyanate is more preferable, and xylylene diisocyanate is particularly preferable in that the viscosity of the plasticizer can be lowered.
When synthesizing urethane polymer plasticizers, the same urethanization catalyst as used for the synthesis of the above-mentioned isocyanate group-containing urethane prepolymer can be used as a reaction catalyst, and a known organic solvent is used. You can also
本発明においてさらに使用することができる添加剤としては、それぞれ耐候性向上、揺変性付与、増量や補強、接着性向上、保存安定性(貯蔵安定性)の向上、着色、硬化促進などのために、耐候安定剤、揺変性付与剤、充填剤、接着性付与剤、保存安定性改良剤(脱水剤)、着色剤、硬化促進触媒などが挙げられる。 Additives that can be further used in the present invention are for improving weather resistance, imparting thixotropic properties, increasing and reinforcing, improving adhesion, improving storage stability (storage stability), coloring, accelerating curing, etc. , Weathering stabilizers, thixotropic agents, fillers, adhesion promoters, storage stability improvers (dehydrating agents), colorants, curing accelerators, and the like.
耐候安定剤としては、硬化物の酸化や光劣化、熱劣化を防止して、耐候性だけでなく耐熱性を更に向上させるために使用されるものである。耐候安定剤としては具体的には、酸化防止剤、紫外線吸収剤などを挙げることができる。 The weather stabilizer is used to prevent oxidation, light degradation, and thermal degradation of the cured product and further improve not only the weather resistance but also the heat resistance. Specific examples of the weather stabilizer include an antioxidant and an ultraviolet absorber.
酸化防止剤としてはヒンダードフェノール系の酸化防止剤が挙げられ、例えば、ペンタエリスリト−ル−テトラキス[3−(3,5−ジ−t e r t−ブチル−4−ヒドロキシフェニル)プロピオネート]、オクタデシル−3−(3,5−ジ−t e r t−ブチル−4−ヒドロキシフェニル)プロピオネート]、N,N′−ヘキサン−1,6−ジイルビス[3−(3,5−ジ−t e r t−ブチル−4−ヒドロキシフェニルプロピオアミド]、ベンゼンプロパン酸3,5−ビス(1,1−ジメチルエチル)−4−ヒドロキシC7−C9側鎖アルキルエステル、2,4−ジメチル−6−(1−メチルペンタデシル)フェノールなどが挙げられる。 Antioxidants include hindered phenol-based antioxidants such as pentaerythritol tetrakis [3- (3,5-di-tert-butyl-4-hydroxyphenyl) propionate], octadecyl- 3- (3,5-di-tert-butyl-4-hydroxyphenyl) propionate], N, N′-hexane-1,6-diylbis [3- (3,5-di-tert-butyl-4-hydroxy Phenylpropioamide], benzenepropanoic acid 3,5-bis (1,1-dimethylethyl) -4-hydroxy C7-C9 side chain alkyl ester, 2,4-dimethyl-6- (1-methylpentadecyl) phenol, etc. Is mentioned.
紫外線吸収剤としては、例えば、2−(3,5−ジ−tert−ブチル−2−ヒドロキシフェニル)−5−クロロベンゾトリアゾール等のベンゾトリアゾール系紫外線吸収剤、2−(4,6−ジフェニル−1,3,5−トリアジン−2−イル)−5−[(ヘキシル)オキシ]−フェノール等のトリアジン系紫外線吸収剤、オクタベンゾン等のべンゾフェノン系紫外線吸収剤、2,4−ジ−tert−ブチルフェニル−3,5−ジ−t e r t−ブチル−4−ヒドロキシベンゾエート等のベンゾエート系紫外線吸収剤が挙げられる。
これらの耐候安定剤は単独あるいは2種以上を組合わせて使用できる。
Examples of the ultraviolet absorber include benzotriazole-based ultraviolet absorbers such as 2- (3,5-di-tert-butyl-2-hydroxyphenyl) -5-chlorobenzotriazole, and 2- (4,6-diphenyl- 1,3,5-triazin-2-yl) -5-[(hexyl) oxy] -phenol and other triazine-based UV absorbers, benzophenone-based UV absorbers such as octabenzone, 2,4-di-tert-butyl Examples thereof include benzoate ultraviolet absorbers such as phenyl-3,5-di-tert-butyl-4-hydroxybenzoate.
These weather stabilizers can be used alone or in combination of two or more.
耐候安定剤は、常温硬化性樹脂100重量部に対して、0.01〜30重量部、特に0.1〜10重量部配合するのが好ましい。 The weathering stabilizer is preferably blended in an amount of 0.01 to 30 parts by weight, particularly 0.1 to 10 parts by weight, based on 100 parts by weight of the room temperature curable resin.
揺変性付与剤は、本発明のシーリング材組成物に揺変性を付与して、組成物を建築外壁などの垂直面に充填や塗布したときにタレ(スランプ)を起こさないようにするために使用するものであり、たとえば、コロイダルシリカ、有機表面処理炭酸カルシウム等の無機系揺変性付与剤、有機ベントナイト、脂肪酸アマイド等の有機系揺変性付与剤などが挙げられ、これらのものの中から1種あるいは2種以上を適宜選択して添加することができる。これらのうちコロイダルシリカは少量の配合で揺変性を付与できるため好ましいのであるが、硬化性組成物の硬化速度を高めるため後述する硬化促進触媒を使用すると揺変性付与構造が破壊され、垂直面に充填や塗布したときにタレを起こすため使用が制限されてしまうことがあるが、これに対し有機表面処理炭酸カルシウムにはこのような欠点がなく、シーリング材組成物に安定した揺変性を付与することができるため特に好ましい。 The thixotropic agent is used to impart thixotropic properties to the sealing material composition of the present invention so that no sagging (slump) occurs when the composition is filled or applied to a vertical surface such as a building outer wall. Examples thereof include inorganic thixotropic agents such as colloidal silica and organic surface-treated calcium carbonate, organic thixotropic agents such as organic bentonite and fatty acid amide, etc. Two or more kinds can be appropriately selected and added. Of these, colloidal silica is preferable because it can impart thixotropy with a small amount of blending, but if a curing accelerating catalyst described later is used in order to increase the curing rate of the curable composition, the thixotropic structure is destroyed and the vertical plane is broken. The use of organic surface-treated calcium carbonate, which may cause sagging when filled or applied, may be limited. However, organic surface-treated calcium carbonate does not have such disadvantages and imparts stable thixotropic properties to the sealing material composition. It is particularly preferable because it can be used.
本発明において、前記揺変性付与剤の使用量は、常温硬化性樹脂100重量部に対して1〜200重量部、さらに5〜150重量部が好ましい。1重量部を下回ると揺変性付与効果がなくなり、200重量部を超えると得られるシーリング材組成物の粘度が上がり作業性が悪化するため好ましくない。 In the present invention, the thixotropic agent is preferably used in an amount of 1 to 200 parts by weight, more preferably 5 to 150 parts by weight, based on 100 parts by weight of the room temperature curable resin. If the amount is less than 1 part by weight, the thixotropic effect is lost, and if it exceeds 200 parts by weight, the viscosity of the resulting sealing material composition is increased and workability is deteriorated.
充填剤としては、マイカ、カオリン、ゼオライト、グラファイト、珪藻土、白土、クレー、タルク、無水ケイ酸、石英、アルミニウム粉末、亜鉛粉末、沈降性シリカなどの合成シリカ、炭酸カルシウム、水酸化カルシウム、炭酸マグネシウム、アルミナ等の無機粉末状充填剤、ガラス繊維、炭素繊維等の繊維状充填剤、ガラスバルーン、シラスバルーン、シリカバルーン、セラミックバルーン等の無機系バルーン状充填剤などの無機系充填剤、木粉、クルミ穀粉、もみ殻粉、パルプ粉、木綿チップ、ゴム粉末、熱可塑性あるいは熱硬化性樹脂の微粉末、ポリエチレン等の粉末や中空体、サランマイクロバルーン等の有機系バルーン状充填剤などの有機系充填剤などの他、水酸化マグネシウムや水酸化アルミニウムなどの難燃性付与充填剤なども挙げられ、粒径0.01〜1,000μmのものが好ましい。これらは単独あるいは2種以上を組合わせて使用できる。 Fillers include synthetic silica such as mica, kaolin, zeolite, graphite, diatomaceous earth, white clay, clay, talc, silicic anhydride, quartz, aluminum powder, zinc powder, precipitated silica, calcium carbonate, calcium hydroxide, magnesium carbonate Inorganic filler such as alumina, fibrous filler such as glass fiber and carbon fiber, inorganic filler such as glass balloon, shirasu balloon, silica balloon, ceramic balloon and other inorganic balloon filler, wood powder Organic, such as walnut flour, rice husk flour, pulp powder, cotton chips, rubber powder, fine powder of thermoplastic or thermosetting resin, polyethylene powder or hollow body, organic balloon filler such as Saran microballoon Other fillers, flame retardant fillers such as magnesium hydroxide and aluminum hydroxide, etc. Among them, those having a particle size 0.01~1,000μm are preferred. These can be used alone or in combination of two or more.
接着性付与剤としては、カップリング剤の他に、エポキシ樹脂、フェノール樹脂、アルキルチタネ−ト類、有機ポリイソシアネートなどが挙げられる。 Examples of the adhesion-imparting agent include epoxy resins, phenol resins, alkyl titanates, and organic polyisocyanates in addition to the coupling agent.
前記カップリング剤としては、シラン系、アルミニウム系、ジルコアルミネート系などの各種カップリング剤またはその部分加水分解縮合物を挙げることができ、このうちシラン系カップリング剤またはその部分加水分解物が接着性に優れているので好ましい。 Examples of the coupling agent include various coupling agents such as silane-based, aluminum-based, and zircoaluminate-based compounds or partial hydrolysis condensates thereof. Among these, the silane-based coupling agent or partial hydrolyzate thereof is It is preferable because of its excellent adhesiveness.
このシラン系カップリング剤としては、具体的には、メチルシリケート、メチルトリメトキシシラン、エチルトリメトキシシラン、ブチルトリメトキシシラン、オクチルトリメトキシシラン、ドデシルトリメトキシシラン、フェニルトリメトキシシラン、ビニルトリメトキシシラン、3−メタクリロキシプロピルトリメトキシシラン、3−アクリロキシプロピルトリメトキシシラン、3−メルカプトプロピルトリメトキシシラン、3−アミノプロピルトリメトキシシラン、ジメチルジメトキシシラン、ジエチルジメトキシシラン、ジブチルジメトキシシラン、ジフェニルジメトキシシラン、ビニルメチルジメトキシシラン、3−メタクリロキシプロピルメチルジメトキシシラン、トリメチルメトキシシラン、トリエチルメトキシシラン、トリフェニルメトキシシラン、N−(2−アミノエチル)−3−アミノプロピルメチルジメトキシシラン、N−(2−アミノエチル)−3−アミノプロピルトリメトキシシラン、N−(2−アミノエチル)−3−アミノプロピルメチルジメトキシシラン、3−グリシドキシプロピルトリメトキシシラン、3−グリシドキシプロピルメチルジエトキシシランなどのアルコキシシリル基を含有する分子量500以下、好ましくは400以下の低分子化合物またはこれらシラン系カップリング剤の1種または2種以上の部分加水分解縮合物で分子量200〜3,000の化合物を挙げることができる。これらは単独であるいは2種以上を組合せて使用できる。 Specific examples of the silane coupling agent include methyl silicate, methyltrimethoxysilane, ethyltrimethoxysilane, butyltrimethoxysilane, octyltrimethoxysilane, dodecyltrimethoxysilane, phenyltrimethoxysilane, vinyltrimethoxy. Silane, 3-methacryloxypropyltrimethoxysilane, 3-acryloxypropyltrimethoxysilane, 3-mercaptopropyltrimethoxysilane, 3-aminopropyltrimethoxysilane, dimethyldimethoxysilane, diethyldimethoxysilane, dibutyldimethoxysilane, diphenyldimethoxy Silane, vinylmethyldimethoxysilane, 3-methacryloxypropylmethyldimethoxysilane, trimethylmethoxysilane, triethylmethoxysilane, tri Phenylmethoxysilane, N- (2-aminoethyl) -3-aminopropylmethyldimethoxysilane, N- (2-aminoethyl) -3-aminopropyltrimethoxysilane, N- (2-aminoethyl) -3-amino Low molecular weight compounds containing alkoxysilyl groups such as propylmethyldimethoxysilane, 3-glycidoxypropyltrimethoxysilane, 3-glycidoxypropylmethyldiethoxysilane, etc., having a molecular weight of 500 or less, preferably 400 or less, or these silane-based cups A compound having a molecular weight of 200 to 3,000 may be mentioned as one or two or more partially hydrolyzed condensates of the ring agent. These can be used alone or in combination of two or more.
保存安定性改良剤としては、組成物中に存在する水分と反応するビニルトリメトキシシラン、酸化カルシウム、酸化マグネシウム、p−トルエンスルホニルイソシアネートなどが挙げられ、これらは単独あるいは2種以上を組合わせて使用できる。 Examples of the storage stability improver include vinyltrimethoxysilane, calcium oxide, magnesium oxide, p-toluenesulfonyl isocyanate which reacts with moisture present in the composition, and these may be used alone or in combination of two or more. Can be used.
着色剤としては、酸化チタンや酸化鉄などの無機系顔料、銅フタロシアニンなどの有機系顔料、カーボンブラックなどが挙げられる。
これらは単独あるいは2種以上を組合わせて使用できる。
Examples of the colorant include inorganic pigments such as titanium oxide and iron oxide, organic pigments such as copper phthalocyanine, and carbon black.
These can be used alone or in combination of two or more.
硬化促進触媒としては、たとえば、テトラ−n−ブチルチタネート等の金属のアルコキシド、オクチル酸第一錫、オクテン酸錫などの、亜鉛、錫、鉛、ジルコニウム、ビスマス、コバルト、マンガン、鉄等の金属とオクチル酸、オクテン酸、ナフテン酸等の有機酸との塩、ジブチル錫ビス(アセチルアセトナート)、ジルコニウムテトラキス(アセチルアセトナート)、チタンテトラキス(アセチルアセトナート)等の金属キレート化合物、ジブチル錫ジラウレート、ジオクチル錫ジラウレート等の有機金属と有機酸との塩、トリエチレンジアミン、トリエチルアミン、トリ−n−ブチルアミン、ヘキサメチレンテトラミン、1,8−ジアザビシクロ〔5,4、0〕ウンデセン−7(DBU)、1,4−ジアザビシクロ〔2,2,2〕オクタン(DABCO)、N−メチルモルホリン、N−エチルモルホリン等の第3級アミン類、あるいはこれらのアミン類と有機酸との塩類などが挙げられる。これらは単独であるいは2種以上組み合わせて使用できる。これらのうち硬化を促進する効果が高い点で、金属キレート化合物や有機金属と有機酸との塩が好ましく、さらにジブチル錫ジラウレートが好ましい。
硬化促進触媒は硬化速度、硬化物の物性などの点から、常温硬化性樹脂100重量部に対して、0〜10重量部、特に0.01〜2重量部配合するのが好ましい。
Examples of the curing accelerating catalyst include metals such as zinc, tin, lead, zirconium, bismuth, cobalt, manganese, iron, such as metal alkoxides such as tetra-n-butyl titanate, stannous octylate and tin octenoate. Salts with organic acids such as octylic acid, octenoic acid, naphthenic acid, metal chelate compounds such as dibutyltin bis (acetylacetonate), zirconium tetrakis (acetylacetonate), titanium tetrakis (acetylacetonate), dibutyltin dilaurate , Salts of organic metals and organic acids such as dioctyltin dilaurate, triethylenediamine, triethylamine, tri-n-butylamine, hexamethylenetetramine, 1,8-diazabicyclo [5,4,0] undecene-7 (DBU), 1 , 4-Diazabicyclo [2,2,2] octane Tertiary amines such as (DABCO), N-methylmorpholine and N-ethylmorpholine, or salts of these amines with organic acids. These can be used alone or in combination of two or more. Of these, a metal chelate compound or a salt of an organic metal and an organic acid is preferable, and dibutyltin dilaurate is more preferable because it has a high effect of promoting curing.
The curing accelerating catalyst is preferably blended in an amount of 0 to 10 parts by weight, particularly 0.01 to 2 parts by weight, based on 100 parts by weight of the room temperature curable resin, from the viewpoint of curing speed and physical properties of the cured product.
充填剤、接着性付与剤、保存安定性改良剤、着色剤および硬化促進触媒の合計の配合量は、常温硬化性樹脂100重量部に対して0〜500重量部、特に5〜300重量部であることが好ましい。 The total amount of the filler, the adhesion-imparting agent, the storage stability improver, the colorant and the curing accelerating catalyst is 0 to 500 parts by weight, particularly 5 to 300 parts by weight, based on 100 parts by weight of the room temperature curable resin. Preferably there is.
本発明のシーリング材組成物において、前記各添加剤成分はそれぞれ1種類または2種以上を混合して使用することができる。 In the sealing material composition of the present invention, each additive component may be used alone or in combination of two or more.
本発明において、必要に応じて、酢酸エチル等のエステル系溶剤、メチルエチルケトン等のケトン系溶剤、n−ヘキサン等の脂肪族系溶剤、シクロヘキサン等の脂環族系溶剤、トルエンやキシレン等の芳香族系溶剤、灯油、ミネラルスピリット、工業ガソリン等の石油留分系溶剤など従来公知の有機溶剤を使用することができる。しかし、常温硬化性のシーリング材組成物の各成分に反応しないものであることが必要である。その使用量は常温硬化性のシーリング材組成物中に20質量%以下、さらに10質量%以下が好ましい。 In the present invention, if necessary, ester solvents such as ethyl acetate, ketone solvents such as methyl ethyl ketone, aliphatic solvents such as n-hexane, alicyclic solvents such as cyclohexane, aromatics such as toluene and xylene. Conventionally known organic solvents such as petroleum solvents such as petroleum solvents, kerosene, mineral spirits, and industrial gasoline can be used. However, it is necessary that it does not react with each component of the room temperature curable sealing material composition. The amount used is 20% by mass or less, more preferably 10% by mass or less, in the room temperature curable sealing material composition.
本発明におけるシーリング材組成物の製造方法としては、特に限定はされない。例えば、常温硬化性樹脂と、可塑剤成分と、場合により、さらに添加剤とを、ステンレス製や鉄製などで湿気を遮断できる攪拌、混合装置に仕込み、常圧下、減圧下、加圧下、窒素気流下などの各種の条件下に、バッチ式あるいは連続式に攪拌、混合して製造することができる。前記攪拌、混合装置としては、例えばプラネタリーミキサー、ニーダー、アジター、ナウタミキサー、ラインミキサーなど各種挙げられる。製造した、シーリング材組成物は、湿気等により増粘、硬化するものであるため、内容物の貯蔵安定性を保つため湿気等を遮断できる容器に詰め、密封して貯蔵するのが好ましい。前記容器としては湿気等を遮断できる容器であれば何でもよいが、例えばドラム缶、金属製や合成樹脂製のペール缶や袋状容器、紙製や合成樹脂製のカートリッジ状容器など各種の容器が挙げられる。 The method for producing the sealing material composition in the present invention is not particularly limited. For example, a room temperature curable resin, a plasticizer component, and, optionally, an additive are charged into a stirrer / mixer that can block moisture with stainless steel, iron, etc., under normal pressure, under reduced pressure, under pressure, under nitrogen flow It can be produced by stirring and mixing batchwise or continuously under various conditions such as below. Examples of the agitation and mixing device include a planetary mixer, a kneader, an agitator, a nauta mixer, and a line mixer. Since the produced sealing material composition is thickened and hardened by moisture or the like, it is preferably stored in a container that can block moisture and the like in order to maintain the storage stability of the contents, and sealed and stored. The container may be anything as long as it is capable of blocking moisture and the like, and examples include various kinds of containers such as drum cans, metal or synthetic resin pail cans and bag-like containers, and paper or synthetic resin cartridge-like containers. It is done.
本発明のシーリング材組成物は用途に応じて一液型としても二液型としても使用できるが、主剤と硬化剤を混合する手間なく、また混合不良による硬化不良などの不具合もなく作業性に優れているため、一液型のシーリング材組成物が好ましくさらに一液湿気硬化型シーリング材組成物が好ましい。
本発明の上塗り塗装仕様向け常温硬化性シーリング材組成物の施工方法について説明するが、これに限定されるものではない。まず建築物の外壁等に形成されている目地に付着している埃などの汚れを刷毛や布を使用して取り除き清掃する。その後三面接着を防止するためのボンドブレーカーやバックアップ材を装填し、次に目地に沿って、目地の両側にマスキングテープを貼り付ける。シーリング材組成物が基材に十分に接着するようプライマーを塗布する。30分程度の所定の時間放置した後シーリング材組成物を充填、施工する。シーリング材組成物の充填、施工は、ノズルを目地幅に合わせてカットし、押出し用ガンに装填し、カートリッジ等の容器を開封し、ノズルを目地底にあてがい、シーリング材をノズルから押出し目地内に充填する。次いで金属製などのヘラを用いて余分なシーリング材をかきとり、シーリング材表面を平滑に仕上げ、シーリング材の表面が硬化する前にマスキングテープを取り除き、シーリング材を養生硬化させる。
シーリング材の押出し用器具は、手動押出しガンのほか電導式のもの、空気圧を利用するものなどがあり、適且選択する。
The sealing material composition of the present invention can be used as a one-pack type or a two-pack type depending on the application, but there is no need to mix the main agent and the curing agent, and there is no problem such as poor curing due to poor mixing, and workability is improved. Since it is excellent, a one-pack type sealant composition is preferable, and a one-part moisture curable sealant composition is more preferable.
Although the construction method of the room temperature curable sealing material composition for topcoat application specification of this invention is demonstrated, it is not limited to this. First, dirt such as dust adhering to the joints formed on the outer wall of the building is removed and cleaned using a brush or cloth. After that, a bond breaker or a backup material for preventing three-sided adhesion is loaded, and then a masking tape is applied to both sides of the joint along the joint. A primer is applied so that the sealant composition is sufficiently adhered to the substrate. After leaving for a predetermined time of about 30 minutes, the sealing material composition is filled and applied. Filling and installing the sealing material composition, cut the nozzle to fit the joint width, load it into the extrusion gun, open the container such as the cartridge, place the nozzle on the joint bottom, push the sealing material through the nozzle, To fill. Next, an excess sealing material is scraped off using a spatula made of metal or the like, the surface of the sealing material is finished smoothly, the masking tape is removed before the surface of the sealing material is cured, and the sealing material is cured and cured.
Equipment for extruding the sealing material includes a manual extruding gun, a conductive type, and an apparatus using air pressure, which are appropriately selected.
つぎに上塗り塗装工程に移る。シーリング材組成物の所定の養生期間後、上塗り塗料をスプレーガン、ローラー、刷毛、へら、コテなどの器具を使用して、被塗装面全体にシーリング材組成物充填目地をも含めて塗装し、養生硬化させて仕上げる。上塗り塗料としては、水性アクリル塗料、水性アクリルシリコン塗料、水性ウレタン塗料などの水性塗料、エポキシ系塗料、ウレタン溶剤系塗料が挙げられるが、環境に対する負荷が少ない点で水性塗料が好ましい。さらに上塗り塗装仕様の塗膜の伸びが、常温において100%以下、さらに70%以下である高耐久性で長寿命の水性塗料が特に好ましい。 Next, the top coating process is started. After a predetermined curing period of the sealant composition, the top coat paint is applied to the entire surface to be coated, including the sealant composition filling joints, using a device such as a spray gun, roller, brush, spatula, or iron, Finish by curing. Examples of the top coating include water-based paints such as water-based acrylic paints, water-based acrylic silicone paints, and water-based urethane paints, epoxy-based paints, and urethane solvent-based paints. Further, a highly durable and long-life water-based paint having an extension of the coating film of the top coat specification of 100% or less at room temperature and further 70% or less is particularly preferable.
本願の施工方法は、上塗り塗装仕様であればどのような外壁を構成する部材であってもよく、したがって限定されるものではないが、高耐久性、長寿命の硬く伸びの少ない塗膜を形成する上塗り塗装仕様の塗料を用いた、建築物の外装材としてコンクリート、モルタル、窯業系サイディング、ALC板、特にALC板を使用する場合に本発明の効果を最大限発揮できるので好ましい。 The construction method of the present application may be any member that constitutes the outer wall as long as it is a top coat coating specification, and therefore is not limited, but it forms a highly durable, long-life, hard, low-elongation coating film. In the case of using concrete, mortar, ceramics siding, ALC plate, especially ALC plate as a building exterior material using a paint having a top coating specification to be used, the effect of the present invention can be maximized, which is preferable.
〔合成例1〕
攪拌機、温度計、窒素シール管及び加温・冷却装置付反応容器に、窒素ガスを流しながらポリオキシプロピレングリコール(旭硝子社製、エクセノール3021、数平均分子量3,200、分子量分布(Mw/Mn)1.1〜1.2)を340g、ポリオキシプロピレントリオール(三井化学社製、MN−4000、数平均分子量4,000、分子量分布(Mw/Mn)1.1〜1.2)を100g、石油系溶剤(日本鉱業社製、カクタスソルベント)を90g仕込み、攪拌しながら4,4’−ジフェニンルメタンジイソシアネート(日本ポリウレタン工業社製、ミリオネートMT、分子量250)を54g仕込み、さらに反応触媒としてジブチル錫ジラウレート0.05gを加え、70〜80℃で2時間攪拌しながら反応させ、滴定によるイソシアネート基含有量が理論値(1.04質量%)以下になった時点で反応を終了し、冷却してイソシアネート基含有ウレタンプレポリマーP−1を合成した。
得られたイソシアネート基含有ウレタンプレポリマーP−1は、滴定によるイソシアネート基含有量1.00質量%、25℃における粘度32,000mPa・sの常温で粘稠な透明液体であった。
(Synthesis Example 1)
Polyoxypropylene glycol (Asahi Glass Co., Ltd., Exenol 3021, number average molecular weight 3,200, molecular weight distribution (Mw / Mn) while flowing nitrogen gas into a reactor equipped with a stirrer, thermometer, nitrogen seal tube and heating / cooling device 1.1 to 1.2) 340 g, polyoxypropylene triol (Mitsui Chemicals, MN-4000, number average molecular weight 4,000, molecular weight distribution (Mw / Mn) 1.1 to 1.2) 100 g, 90 g of petroleum solvent (Nippon Mining Co., Cactus Solvent) is charged, and 54 g of 4,4′-diphenylmethane diisocyanate (manufactured by Nippon Polyurethane Industry Co., Ltd., Millionate MT, molecular weight 250) is added while stirring. Add 0.05 g of dibutyltin dilaurate and react at 70-80 ° C. with stirring for 2 hours. The reaction was terminated when the Aneto group content is below the theoretical value (1.04 wt%) was synthesized an isocyanate group-containing urethane prepolymer P-1 by cooling.
The obtained isocyanate group-containing urethane prepolymer P-1 was a viscous transparent liquid at room temperature with an isocyanate group content of 1.00% by mass and a viscosity of 32,000 mPa · s at 25 ° C.
〔合成例2〕
攪拌機、温度計、窒素シール管及び加温・冷却装置付反応容器に、窒素ガスを流しながらポリオキシプロピレンモノオール(旭硝子社製、XS−M3000、数平均分子量3,243、分子量分布(Mw/Mn)1.0〜1.1)300g(OH当量:0.0925)を仕込み、攪拌しながらジブチル錫ジラウレート0.1gとm−キシリレンジイソシアネート(武田薬品社製、タケネート500、分子量188)9.1g(NCO当量:0.0968)(R値(NCO当量/OH当量=1.05)を加えたのち、加温して70〜80℃で4時間攪拌して、イソシアネート基含有量が理論値(0.06質量%)以下となった時点で反応を終了し、液状のウレタン系高分子可塑剤U−1を製造した。
この液状のウレタン系高分子可塑剤U−1は、滴定による実測イソシアネート基含有量0.04質量%、粘度3,300mPa・s/25℃、分子量分布(Mw/Mn)1.0〜1.1、常温で透明の液体であった。
[Synthesis Example 2]
A polyoxypropylene monool (manufactured by Asahi Glass Co., Ltd., XS-M3000, number average molecular weight 3,243, molecular weight distribution (Mw / Mn) was introduced into a reaction vessel equipped with a stirrer, thermometer, nitrogen seal tube and heating / cooling device. Mn) 1.0 to 1.1) 300 g (OH equivalent: 0.0925) was charged, and while stirring, 0.1 g of dibutyltin dilaurate and m-xylylene diisocyanate (Takeda 500, Takenate 500, molecular weight 188) 9 0.1 g (NCO equivalent: 0.0968) (R value (NCO equivalent / OH equivalent = 1.05) was added, and the mixture was heated and stirred at 70-80 ° C. for 4 hours. The reaction was terminated when the value (0.06% by mass) or less was reached, and a liquid urethane polymer plasticizer U-1 was produced.
This liquid urethane polymer plasticizer U-1 has a measured isocyanate group content of 0.04 mass% by titration, a viscosity of 3,300 mPa · s / 25 ° C., and a molecular weight distribution (Mw / Mn) of 1.0 to 1. 1. It was a transparent liquid at room temperature.
〔実施例1〕
冷却装置及び窒素シール管付き混練容器に、窒素ガスを流しながら合成例1で得たイソシアネート基含有ウレタンプレポリマーP−1を100g、ジイソノニルフタレート(新日本理化社製、DINP、分子量419)を8.1g、実質的にイソシアネート基と水酸基とを有しない液状のウレタン系高分子可塑剤U−1を41.9g、石油系溶剤(日本鉱業社製、カクタスソルベント)10g、酸化チタン10g、3−グリシドキシプロピルトリメトキシシラン(信越化学工業社製、KBM403)0.5g、ヒンダードフェノール系酸化防止剤(チバ・スペシャルテイ・ケミカルズ社製、IRGANOX1010、ペンタエリスリトールテトラキス〔3−(3,5−ジ−tert−ブチル−4−ヒドロキシフェニル)プロピオネート〕)1gを順次仕込み、60℃以下で、内容物が均一になるまで攪拌、混練りした。次いで予め80〜100℃の乾燥器中で1日乾燥した脂肪酸表面処理炭酸カルシウム(白石工業社製、白艶華CCR)100gとジブチル錫ジラウレート0.05gを順次仕込み、均一になるまで更に混練した。次いで30〜100hPaで減圧脱泡し、容器に充填、密封して、ペースト状の一液型湿気硬化性ウレタン系シーリング材組成物を調整した。
[Example 1]
100 g of the isocyanate group-containing urethane prepolymer P-1 obtained in Synthesis Example 1 while flowing nitrogen gas into a kneading vessel equipped with a cooling device and a nitrogen seal tube, and diisononyl phthalate (DINP, molecular weight 419, manufactured by Shin Nippon Rika Co., Ltd.) 8 .1 g, 41.9 g of a liquid urethane polymer plasticizer U-1 having substantially no isocyanate group and hydroxyl group, 10 g of petroleum solvent (Cactus Solvent manufactured by Nippon Mining Co., Ltd.), 10 g of titanium oxide, 3- 0.5 g of glycidoxypropyltrimethoxysilane (manufactured by Shin-Etsu Chemical Co., Ltd., KBM403), hindered phenol antioxidant (manufactured by Ciba Specialty Chemicals, IRGANOX 1010, pentaerythritol tetrakis [3- (3,5- Di-tert-butyl-4-hydroxyphenyl) propionate]) They were charged, at 60 ° C. or less, and the mixture was stirred, kneaded until the contents became homogeneous. Subsequently, 100 g of fatty acid surface-treated calcium carbonate (Shiraishi Kogyo Co., Ltd., Hakujyo Hana CCR) dried in an oven at 80 to 100 ° C. for 1 day in advance and 0.05 g of dibutyltin dilaurate were sequentially charged and further kneaded until uniform. Subsequently, it was degassed under reduced pressure at 30 to 100 hPa, filled in a container, and sealed to prepare a paste-like one-component moisture-curable urethane-based sealing material composition.
〔実施例2〕
実施例1において、ジイソノニルフタレート(新日本理化社製、DINP、分子量419)8.1g、ウレタン系高分子可塑剤U−1の41.9gの代わりに、ジイソノニルフタレートを13.6g、ウレタン系高分子可塑剤U−1を36.4g使用した以外は同様にして、ペースト状の一液型湿気硬化性ウレタン系シーリング材組成物を調整した。
[Example 2]
In Example 1, instead of 8.1 g of diisononyl phthalate (manufactured by Shin Nippon Rika Co., Ltd., DINP, molecular weight 419) and 41.9 g of urethane polymer plasticizer U-1, 13.6 g of diisononyl phthalate, urethane type high A paste-like one-component moisture-curable urethane-based sealing material composition was prepared in the same manner except that 36.4 g of the molecular plasticizer U-1 was used.
〔実施例3〕
実施例1において、ジイソノニルフタレート(新日本理化社製、DINP、分子量419)8.1g、ウレタン系高分子可塑剤U−141.9gの代わりに、ジイソノニルフタレートを24.4g、ウレタン系高分子可塑剤U−1を25.6g使用した以外は同様にして、ペースト状の一液型湿気硬化性ウレタン系シーリング材組成物を調整した。
Example 3
In Example 1, instead of 8.1 g of diisononyl phthalate (Shin Nippon Rika Co., Ltd., DINP, molecular weight 419) and urethane polymer plasticizer U-141.9 g, 24.4 g of diisononyl phthalate, urethane polymer plastic A paste-like one-component moisture-curable urethane-based sealing material composition was prepared in the same manner except that 25.6 g of the agent U-1 was used.
〔実施例4〕
実施例2において、合成例1で得たイソシアネート基含有ウレタンプレポリマーP−1の代わりに加水分解性シリル基含有ポリオキシプロピレン系ポリマー(カネカ社製、S−303)を使用した以外は同様にして、ペースト状の一液型湿気硬化性シリル基含有ポリオキシプロピレン系シーリング材組成物を調整した。
Example 4
In Example 2, a hydrolyzable silyl group-containing polyoxypropylene polymer (manufactured by Kaneka Corporation, S-303) was used instead of the isocyanate group-containing urethane prepolymer P-1 obtained in Synthesis Example 1. Thus, a paste-like one-component moisture-curable silyl group-containing polyoxypropylene-based sealing material composition was prepared.
〔比較例1〕
実施例1において、ジイソノニルフタレートを使用しないでウレタン系高分子可塑剤U−1を50g使用した以外は同様にして、ペ−スト状の一液型湿気硬化性ウレタン系シーリング材組成物を調整した。
[Comparative Example 1]
In Example 1, a paste-like one-component moisture-curable urethane-based sealing material composition was prepared in the same manner except that 50 g of the urethane-based polymer plasticizer U-1 was used without using diisononyl phthalate. .
〔比較例2〕
比較例1において、ウレタン系高分子可塑剤U−1の50gの代わりに、ジイソノニルフタレートを50g使用した以外は同様にして、ペースト状の一液型湿気硬化性ウレタン系シーリング材組成物を調整した。
[Comparative Example 2]
In Comparative Example 1, a paste-like one-component moisture-curable urethane-based sealing material composition was prepared in the same manner except that 50 g of diisononyl phthalate was used instead of 50 g of the urethane-based polymer plasticizer U-1. .
試験方法
実施例1〜4及び比較例1と2で得られた一液型湿気硬化性ウレタン系シーリング材組成物と一液型湿気硬化性架橋性シリル基含有樹脂シーリング材組成物を用いて以下の試験をした。
(1)塗膜の割れ
シーリング材組成物を厚さ3mmのシート状にし、23℃、50%相対湿度で3日間養生硬化し、さらに水性アクリルシリコン塗料(藤倉化成社製、セラミトーンフレック、塗布量:上塗り・中塗を各300〜500g/m2)を塗布し23℃、50%相対湿度で14日間養生した。次に幅25mm長さ100mmの短冊状に切り出し、80℃7日間の加熱処理をした。この試料を5℃に24時間以上静置後恒温槽付きの引張試験機を用い、5℃、引張速度5mm/min、標線間距離40mmの条件で引張試験を行ない、目視により標線間の塗膜に亀裂が生じたときの伸び率を求め評価した。
この場合の判定基準は、以下のとおりである。
○:伸び率が5%以上。
×;伸び率が5%未満。
なお、水性アクリルシリコン塗料(藤倉化成社製、セラミトーンフレック、上塗り・中塗りを各300〜500g/m2)の塗膜の伸び;40〜50%以下(23℃50%相対湿度7日間養生、試験体形状 幅20mm×長さ100mm、引張速度20mm/min・23℃)である。
Test Method Using the one-component moisture-curable urethane-based sealant composition and the one-component moisture-curable crosslinkable silyl group-containing resin sealant composition obtained in Examples 1 to 4 and Comparative Examples 1 and 2 below Was tested.
(1) Cracking of the coating film The sealing material composition was formed into a sheet having a thickness of 3 mm, cured at 23 ° C. and 50% relative humidity for 3 days, and further water-based acrylic silicone paint (manufactured by Fujikura Kasei Co., Ltd., ceramic tone fleck, coating) Amount: 300-500 g / m 2 ) of each of the top coat and the intermediate coat was applied and cured at 23 ° C. and 50% relative humidity for 14 days. Next, it cut out into the strip shape of width 25mm length 100mm, and heat-processed at 80 degreeC for 7 days. This sample was allowed to stand at 5 ° C. for 24 hours or longer and then a tensile tester with a thermostatic bath was used to conduct a tensile test at 5 ° C., a tensile speed of 5 mm / min, and a distance between marked lines of 40 mm. The elongation when the crack occurred in the coating film was determined and evaluated.
The judgment criteria in this case are as follows.
○: Elongation rate is 5% or more.
X: Elongation rate is less than 5%.
In addition, the elongation of the coating film of water-based acrylic silicone paint (manufactured by Fujikura Kasei Co., Ltd., ceramic tone fleck, top coat and intermediate coat each 300 to 500 g / m 2 ); 40 to 50% or less (23 ° C., 50% relative humidity for 7 days , Specimen shape width 20 mm × length 100 mm, tensile speed 20 mm / min · 23 ° C.).
(2)汚染性
試験体の作製を次のように行なった。厚さ5mmのスレート板を使用し、幅25mm×深さ15mm×長さ150mmの目地を作製した。その目地にシーリング材組成物を充填し、余分な組成物をヘラでかきとり、表面を平らに仕上げる。次に標準状態(23℃50%相対湿度)で14日間養生しシーリング材組成物を硬化させ、表面に水性アクリルシリコン塗料(藤倉化成社製、セラミトーンフレック、塗布量:上塗り・中塗を各300〜500g/m2)を刷毛により塗布し、さらに標準状態(23℃50%相対湿度)で14日間養生して試験体とした。
次に試験体を80℃の恒温槽中で30日間熱処理した後、恒温槽より取り出し試験体の表面に黒色ケイ砂(粒径70〜110μm)をふりかける。直ちに試験体を裏返し、表面を手で軽く叩いて余分な黒色ケイ砂をおとす。表面に付着して残った黒色ケイ砂(汚れ)の状態を目視により観察し汚染性を評価した。
判定基準は、以下のとおりである。
○:目地上の水性アクリルシリコン塗料表面に黒色ケイ砂の付着がなくきれいな状態。
×:目地上の水性アクリルシリコン塗料表面に黒色ケイ砂が付着し汚れた状態。
(2) Contamination property A test specimen was prepared as follows. A 5 mm thick slate plate was used to produce a joint having a width of 25 mm, a depth of 15 mm, and a length of 150 mm. The sealant composition is filled in the joint, and the excess composition is scraped off with a spatula to finish the surface flat. Next, it was cured for 14 days in a standard state (23 ° C. and 50% relative humidity), and the sealing material composition was cured. Aqueous acrylic silicone paint (manufactured by Fujikura Kasei Co., Ltd., ceramic tone flex, coating amount: 300 for each of top coat and intermediate coat) ˜500 g / m 2 ) was applied with a brush, and further cured for 14 days in a standard state (23 ° C. and 50% relative humidity) to obtain a test specimen.
Next, after heat-treating a test body for 30 days in an 80 degreeC thermostat, it takes out from a thermostat and sprinkles black quartz sand (particle diameter of 70-110 micrometers) on the surface of a test body. Immediately turn the specimen over and tap the surface with your hand to remove excess black silica sand. The state of the black silica sand (dirt) remaining on the surface was visually observed to evaluate the contamination.
Judgment criteria are as follows.
○: Black silica sand is not adhered to the surface of the water-based acrylic silicone paint on the surface, and the surface is clean.
X: A state in which black silica sand adheres to the surface of the water-based acrylic silicone paint surface on the surface and becomes dirty.
(3)押出し性
JIS A1439:1997「建築用シーリング材の試験方法」の「4.14試験用カートリッジによる押出し試験」に準拠して測定(測定温度23℃)した。押出し時間が5秒以下のものを○と評価した。
(3) Extrudability Measured (measurement temperature: 23 ° C.) in accordance with “4.14 Extrusion Test with Cartridge for Testing” of JIS A1439: 1997 “Testing Method of Sealant for Building”. Those having an extrusion time of 5 seconds or less were evaluated as ◯.
(4)スランプ
JIS A1439:1997「建築用シーリング材の試験方法」の「4.1スランプ試験」に準拠してスランプ(縦)を測定(測定温度23℃)した。
(4) Slump The slump (longitudinal) was measured (measurement temperature: 23 ° C.) in accordance with “4.1 slump test” in JIS A1439: 1997 “Testing method of sealing material for building”.
(5)タックフリー
JIS A1439:1997「建築用シーリング材の試験方法」の「4.19タックフリー試験」に準拠して測定(測定温度23℃)した。タックフリー時間が5時間以内を○と評価した。
(5) Tack-free Measured in accordance with “4.19 Tack-free test” in JIS A1439: 1997 “Testing method of sealing material for building” (measurement temperature: 23 ° C.). A tack-free time of 5 hours or less was rated as “good”.
(6)伸び
シーリング材組成物について、厚さが約2mmのシート状になるように離型紙上に塗布し、23℃50%相対湿度で14日間養生し硬化させた後離型紙を取り除き、JIS K6251:1993「加硫ゴム物理試験方法」により3号形ダンベル状に打ち抜いたものを試験片として、試験温度23℃で硬化物の切断時の伸びを測定した。伸びが200%以上を○と評価した。
(6) Elongation The sealing material composition was applied onto a release paper so as to form a sheet having a thickness of about 2 mm, cured at 23 ° C. and 50% relative humidity for 14 days, cured, and then released from the release paper. K6251: 1993 A vulcanized rubber physical test method punched into a No. 3 type dumbbell was used as a test piece, and the elongation at the time of cutting the cured product was measured at a test temperature of 23 ° C. An elongation of 200% or more was evaluated as ◯.
これらの結果をつぎの表1に示す。
このように本発明のシーリング材組成物とそれを用いた施工法は、硬化後のモジュラス、伸び等のゴム物性を調節し、さらに上塗り塗料の割れが生じ難くブリード汚染の極めて少ないという優れた効果を奏するものである。
As described above, the sealing material composition of the present invention and the construction method using the sealing material have excellent effects of adjusting the rubber physical properties such as modulus and elongation after curing, and further preventing the occurrence of cracks in the top coating and causing very little bleed contamination. It plays.
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JP5545588B2 (en) * | 2008-07-14 | 2014-07-09 | セメダイン株式会社 | Polyurethane sealant composition |
JP2010037866A (en) * | 2008-08-07 | 2010-02-18 | Asahi Kasei Homes Co | Exterior wall structure of building |
JP5609165B2 (en) * | 2009-04-30 | 2014-10-22 | 横浜ゴム株式会社 | Topcoat composition for sealant |
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