JP2008280468A - Impregnating sealer for applying to porous siliceous inorganic body - Google Patents
Impregnating sealer for applying to porous siliceous inorganic body Download PDFInfo
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- JP2008280468A JP2008280468A JP2007127465A JP2007127465A JP2008280468A JP 2008280468 A JP2008280468 A JP 2008280468A JP 2007127465 A JP2007127465 A JP 2007127465A JP 2007127465 A JP2007127465 A JP 2007127465A JP 2008280468 A JP2008280468 A JP 2008280468A
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- isocyanate compound
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- -1 isocyanate compound Chemical class 0.000 claims abstract description 88
- 239000012948 isocyanate Substances 0.000 claims abstract description 65
- 229910000077 silane Inorganic materials 0.000 claims abstract description 33
- 239000007788 liquid Substances 0.000 claims abstract description 29
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims abstract description 25
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 22
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims abstract description 18
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims abstract description 17
- LFSYUSUFCBOHGU-UHFFFAOYSA-N 1-isocyanato-2-[(4-isocyanatophenyl)methyl]benzene Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=CC=C1N=C=O LFSYUSUFCBOHGU-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 238000005470 impregnation Methods 0.000 claims description 50
- 239000011148 porous material Substances 0.000 claims description 26
- 239000003795 chemical substances by application Substances 0.000 claims description 24
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 20
- 229910052710 silicon Inorganic materials 0.000 claims description 20
- 239000010703 silicon Substances 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 6
- 230000003014 reinforcing effect Effects 0.000 claims description 5
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 5
- NNOZGCICXAYKLW-UHFFFAOYSA-N 1,2-bis(2-isocyanatopropan-2-yl)benzene Chemical compound O=C=NC(C)(C)C1=CC=CC=C1C(C)(C)N=C=O NNOZGCICXAYKLW-UHFFFAOYSA-N 0.000 claims description 4
- FKTHNVSLHLHISI-UHFFFAOYSA-N 1,2-bis(isocyanatomethyl)benzene Chemical compound O=C=NCC1=CC=CC=C1CN=C=O FKTHNVSLHLHISI-UHFFFAOYSA-N 0.000 claims description 4
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 4
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 4
- 125000000123 silicon containing inorganic group Chemical group 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims 1
- 239000003960 organic solvent Substances 0.000 abstract description 10
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract description 3
- CZDYPVPMEAXLPK-UHFFFAOYSA-N tetramethylsilane Chemical compound C[Si](C)(C)C CZDYPVPMEAXLPK-UHFFFAOYSA-N 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 42
- 238000002156 mixing Methods 0.000 description 42
- 239000000178 monomer Substances 0.000 description 17
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 14
- 229910052791 calcium Inorganic materials 0.000 description 14
- 239000011575 calcium Substances 0.000 description 14
- 229920001296 polysiloxane Polymers 0.000 description 11
- 150000002513 isocyanates Chemical class 0.000 description 10
- 229940126062 Compound A Drugs 0.000 description 5
- NLDMNSXOCDLTTB-UHFFFAOYSA-N Heterophylliin A Natural products O1C2COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC2C(OC(=O)C=2C=C(O)C(O)=C(O)C=2)C(O)C1OC(=O)C1=CC(O)=C(O)C(O)=C1 NLDMNSXOCDLTTB-UHFFFAOYSA-N 0.000 description 5
- JNGZXGGOCLZBFB-IVCQMTBJSA-N compound E Chemical compound N([C@@H](C)C(=O)N[C@@H]1C(N(C)C2=CC=CC=C2C(C=2C=CC=CC=2)=N1)=O)C(=O)CC1=CC(F)=CC(F)=C1 JNGZXGGOCLZBFB-IVCQMTBJSA-N 0.000 description 4
- 239000004566 building material Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 239000003822 epoxy resin Substances 0.000 description 3
- 230000005484 gravity Effects 0.000 description 3
- 239000003973 paint Substances 0.000 description 3
- 229920000647 polyepoxide Polymers 0.000 description 3
- 230000002787 reinforcement Effects 0.000 description 3
- 150000004756 silanes Chemical class 0.000 description 3
- MPDDTAJMJCESGV-CTUHWIOQSA-M (3r,5r)-7-[2-(4-fluorophenyl)-5-[methyl-[(1r)-1-phenylethyl]carbamoyl]-4-propan-2-ylpyrazol-3-yl]-3,5-dihydroxyheptanoate Chemical compound C1([C@@H](C)N(C)C(=O)C2=NN(C(CC[C@@H](O)C[C@@H](O)CC([O-])=O)=C2C(C)C)C=2C=CC(F)=CC=2)=CC=CC=C1 MPDDTAJMJCESGV-CTUHWIOQSA-M 0.000 description 2
- FMGBDYLOANULLW-UHFFFAOYSA-N 3-isocyanatopropyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)CCCN=C=O FMGBDYLOANULLW-UHFFFAOYSA-N 0.000 description 2
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 description 2
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 2
- XDQWJFXZTAWJST-UHFFFAOYSA-N 3-triethoxysilylpropyl prop-2-enoate Chemical compound CCO[Si](OCC)(OCC)CCCOC(=O)C=C XDQWJFXZTAWJST-UHFFFAOYSA-N 0.000 description 1
- KBQVDAIIQCXKPI-UHFFFAOYSA-N 3-trimethoxysilylpropyl prop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C=C KBQVDAIIQCXKPI-UHFFFAOYSA-N 0.000 description 1
- 239000004641 Diallyl-phthalate Substances 0.000 description 1
- 239000005057 Hexamethylene diisocyanate Substances 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- QUDWYFHPNIMBFC-UHFFFAOYSA-N bis(prop-2-enyl) benzene-1,2-dicarboxylate Chemical compound C=CCOC(=O)C1=CC=CC=C1C(=O)OCC=C QUDWYFHPNIMBFC-UHFFFAOYSA-N 0.000 description 1
- 244000309464 bull Species 0.000 description 1
- 238000006757 chemical reactions by type Methods 0.000 description 1
- 229940125810 compound 20 Drugs 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 239000000539 dimer Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- AYLRODJJLADBOB-QMMMGPOBSA-N methyl (2s)-2,6-diisocyanatohexanoate Chemical compound COC(=O)[C@@H](N=C=O)CCCCN=C=O AYLRODJJLADBOB-QMMMGPOBSA-N 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 238000003900 soil pollution Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- FRGPKMWIYVTFIQ-UHFFFAOYSA-N triethoxy(3-isocyanatopropyl)silane Chemical compound CCO[Si](OCC)(OCC)CCCN=C=O FRGPKMWIYVTFIQ-UHFFFAOYSA-N 0.000 description 1
- JXUKBNICSRJFAP-UHFFFAOYSA-N triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCOCC1CO1 JXUKBNICSRJFAP-UHFFFAOYSA-N 0.000 description 1
- 239000013638 trimer Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Landscapes
- Sealing Material Composition (AREA)
- Paints Or Removers (AREA)
Abstract
Description
本発明は、ケイカル板やフレキシブル板等の珪素質無機多孔体の表面を補強したり、当該無機多孔体に塗布される塗料との密着性を向上させるために使用する含浸シーラー剤に関するものである。 The present invention relates to an impregnating sealer used to reinforce the surface of a silicon-based inorganic porous material such as a calcium plate or a flexible plate, or to improve the adhesion to a coating applied to the inorganic porous material. .
従来より、珪素質無機多孔体の表面補強等のため、含浸シーラー剤として、イソシアネート化合物を有機溶剤で希釈したイソシアネート溶液や、エポキシ樹脂を有機溶剤で希釈したエポキシ樹脂溶液が用いられている。これらの溶液は、有機溶剤で希釈されているため、低粘度となっており、無機多孔体の表面近傍に十分に含浸され、表明補強等の役割を十分に果たすものである。 Conventionally, an isocyanate solution in which an isocyanate compound is diluted with an organic solvent and an epoxy resin solution in which an epoxy resin is diluted with an organic solvent are used as an impregnating sealer for reinforcing the surface of the silicon-based inorganic porous body. Since these solutions are diluted with an organic solvent, they have a low viscosity and are sufficiently impregnated in the vicinity of the surface of the inorganic porous body, thereby sufficiently fulfilling the role of manifestation reinforcement and the like.
しかしながら、これらの溶液を用いると、無機多孔体中に有機溶剤が残存するということがあった。有機溶剤が残存していると、無機多孔体を建材等に使用した後、徐々に有機溶剤を環境中に放出するということがあった。そして、大気汚染、水質汚染、土壌汚染等の環境汚染を引き起こし、人体に悪影響を及ぼすということがあった。 However, when these solutions are used, the organic solvent may remain in the inorganic porous material. If the organic solvent remains, the organic solvent may be gradually released into the environment after the inorganic porous material is used as a building material. And it has caused environmental pollution such as air pollution, water pollution, and soil pollution, and has had a bad influence on the human body.
このため、有機溶剤を使用しない含浸シーラー剤が望まれており、特許文献１に記載したような技術が提案されている。すなわち、粘度が１５０ｍＰａ・ｓ以下のイソシアネート化合物のみを用いた含浸シーラー剤が提案されている。具体的には、リジンジイソシアネート、ヘキサメチレンジイソシアネート、ジフェニルメタンジイソシアネートからなる含浸シーラー剤が提案されている。 For this reason, the impregnation sealer agent which does not use an organic solvent is desired, and the technique as described in Patent Document 1 has been proposed. That is, an impregnation sealer using only an isocyanate compound having a viscosity of 150 mPa · s or less has been proposed. Specifically, an impregnated sealer agent composed of lysine diisocyanate, hexamethylene diisocyanate, and diphenylmethane diisocyanate has been proposed.
しかしながら、イソシアネート化合物のみからなる含浸シーラー剤は、有機溶剤で希釈したシーラー剤に比べて、無機多孔体中に含浸されにくいという欠点があった。特許文献１記載の技術では、無機多孔体中に含浸させるのに、当該多孔体を４０〜６０℃程度に加熱し、更に塗布後においては６０〜８０℃に加熱している。すなわち、比較的高温で加熱しなければ、含浸シーラー剤が無機多孔体中に十分に含浸されないのである。 However, the impregnated sealer agent comprising only an isocyanate compound has a drawback that it is less likely to be impregnated in the inorganic porous body than the sealer agent diluted with an organic solvent. In the technique described in Patent Document 1, in order to impregnate the inorganic porous body, the porous body is heated to about 40 to 60 ° C, and further heated to 60 to 80 ° C after coating. That is, unless heated at a relatively high temperature, the impregnated sealer is not sufficiently impregnated in the inorganic porous body.
本発明の課題は、環境汚染を引き起こすような有機溶剤を含有せず、しかも、比較的高温で加熱しなくても、たとえば常温で十分に珪素質無機多孔体表面中に含浸される含浸シーラー剤を提供することにある。 An object of the present invention is to provide an impregnated sealer that does not contain an organic solvent that causes environmental pollution and that is sufficiently impregnated into the surface of a silicon-based inorganic porous body, for example, at room temperature without heating at a relatively high temperature. Is to provide.
本発明は、イソシアネート化合物と、テトラメトキシシラン，テトラエトキシシラン，ビニルトリメトキシシラン及びビニルトリエトキシシランよりなる群から選ばれたシラン化合物とが、相互に混ざり合って透明な液体となっていることを特徴とする珪素質無機多孔体に適用するための含浸シーラー剤に関するものである。 In the present invention, an isocyanate compound and a silane compound selected from the group consisting of tetramethoxysilane, tetraethoxysilane, vinyltrimethoxysilane and vinyltriethoxysilane are mixed with each other to form a transparent liquid. The present invention relates to an impregnated sealer for application to a silicon-based inorganic porous material.
イソシアネート化合物としては、４，４’−ジフェニルメタンジイソシアネート，２，４’−ジフェニルメタンジイソシアネート，イソホロンジイソシアネート，テトラメチルキシリレンジイソシアネート，キシリレンジイソシアネート等が単独で又は混合して用いられる。イソシアネート化合物は、前記シラン化合物と混合したときに、透明な液体となるものを用いる必要がある。どのイソシアネート化合物と、どのシラン化合物とを混合したときに、透明な液体となるかは、両者の配合割合等によるため、一概に言えない。また、一般に市販されているイソシアネート化合物は、単量体だけではなく、二量体や三量体等の多量体が含まれていることがある。特に、市販のジフェニルメタンジイソシアネート（ＭＤＩ）は、一般的に、４，４’−ジフェニルメタンジイソシアネート及び／又は２，４’−ジフェニルメタンジイソシアネートと、これらの多量体との混合物となっている。この多量体の量や、４，４’−ジフェニルメタンジイソシアネートと２，４’−ジフェニルメタンジイソシアネートの組成比によっても、透明な液体となったり、ならなかったりするので、注意が必要である。上記の説明から分かるように、本発明でいうイソシアネート化合物は、イソシアネート化合物の単量体だけではなく、多量体をも含む意味で用いられている。 As the isocyanate compound, 4,4'-diphenylmethane diisocyanate, 2,4'-diphenylmethane diisocyanate, isophorone diisocyanate, tetramethylxylylene diisocyanate, xylylene diisocyanate and the like are used alone or in combination. It is necessary to use an isocyanate compound that becomes a transparent liquid when mixed with the silane compound. Which isocyanate compound and which silane compound are mixed to form a transparent liquid is unclear because it depends on the blending ratio of the two. Moreover, generally the isocyanate compound marketed may contain not only a monomer but multimers, such as a dimer and a trimer. In particular, commercially available diphenylmethane diisocyanate (MDI) is generally a mixture of 4,4'-diphenylmethane diisocyanate and / or 2,4'-diphenylmethane diisocyanate and their multimers. Care must be taken because the amount of this multimer and the composition ratio of 4,4'-diphenylmethane diisocyanate and 2,4'-diphenylmethane diisocyanate may or may not become a transparent liquid. As can be seen from the above description, the isocyanate compound referred to in the present invention is used in the meaning including not only a monomer of the isocyanate compound but also a multimer.
シラン化合物としては、テトラメトキシシラン，テトラエトキシシラン，ビニルトリメトキシシラン又はビニルトリエトキシシランが用いられる。一般のシラン化合物としては、これら四種以外に種々のものが存在する。たとえば、３−グリシドキシプロピ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−イソシアネートプロピルトリメトキシシラン等が存在する。しかし、上記四種以外の他の一般のシラン化合物は、後述する比較例８〜１４で実証されているように、本発明の課題を達成しうるものではなく、珪素質無機多孔体中に十分に含浸されないものである。なお、上記四種のシラン化合物であっても、イソシアネート化合物の種類によっては、混合して透明な液体とならないものがあるので、注意を要する。 As the silane compound, tetramethoxysilane, tetraethoxysilane, vinyltrimethoxysilane, or vinyltriethoxysilane is used. As general silane compounds, there are various types other than these four types. For example, 3-glycidoxypropyltrimethoxysilane, 3-methacryloxypropyltrimethoxysilane, 3-acryloxypropyltrimethoxysilane, 3-mercaptopropyltrimethoxysilane, 3-isocyanatopropyltrimethoxysilane and the like exist. However, other general silane compounds other than the above four types cannot achieve the object of the present invention as demonstrated in Comparative Examples 8 to 14 described later, and are sufficient in the silicon-based inorganic porous body. Is not impregnated. Note that some of the above four types of silane compounds may not be mixed and become a transparent liquid depending on the type of isocyanate compound, so care must be taken.
イソシアネート化合物とシラン化合物との配合割合は任意であるが、両者がよく混ざり合って、透明な液体となる配合割合であれば、どのような割合であってもよい。透明な液体とならず濁っていると、シラン化合物のみが珪素質無機多孔体中に含浸されやすくなり、イソシアネート化合物がシラン化合物と共に、珪素質無機多孔体中に含浸されにくくなる。イソシアネート化合物とシラン化合物との好ましい配合割合は、イソシアネート化合物が３５〜６５質量％で、シラン化合物が６５〜３５質量％である。イソシアネート化合物の配合割合が６５質量％を超える、すなわち、シラン化合物が３５質量％未満になると、含浸シーラー剤が透明な液体となっても、珪素質無機多孔体中に含浸されにくくなる傾向が生じる。イソシアネート化合物の配合割合が３５質量％未満になる、すなわち、シラン化合物が６５質量％を超えると、珪素質無機多孔体表面の補強効果が低下する傾向が生じる。 The mixing ratio of the isocyanate compound and the silane compound is arbitrary, but any ratio may be used as long as they are mixed well and become a transparent liquid. If it is not transparent and turbid, only the silane compound is easily impregnated in the siliceous inorganic porous body, and the isocyanate compound is difficult to be impregnated in the siliceous inorganic porous body together with the silane compound. The preferable compounding ratio of the isocyanate compound and the silane compound is 35 to 65% by mass of the isocyanate compound and 65 to 35% by mass of the silane compound. When the blending ratio of the isocyanate compound exceeds 65% by mass, that is, the silane compound is less than 35% by mass, the impregnated sealer agent tends to be difficult to be impregnated in the siliceous inorganic porous material even if it becomes a transparent liquid. . When the blending ratio of the isocyanate compound is less than 35% by mass, that is, when the silane compound exceeds 65% by mass, the reinforcing effect on the surface of the silicon-based inorganic porous body tends to be lowered.
本発明に係る含浸シーラー剤は、イソシアネート化合物とシラン化合物とが混ざり合った透明な液体となる必要がある。透明な液体にならなければ、珪素質無機多孔体中に浸透しにくくなるからである。本発明に係る含浸シーラー剤は、イソシアネート化合物とシラン化合物とを混合し、透明な液体として１液の形態で需要者に供給してもよい。また、イソシアネート化合物とシラン化合物とを、各々、別個にして２液の形態で需要者に供給してもよい。すなわち、イソシアネート化合物を容器Ａに収納し、シラン化合物を容器Ｂに収納して、キットの形態で需要者に供給してもよい。需要者は、各容器に収納されたイソシアネート化合物とシラン化合物とを混合攪拌し、透明な液体にして、珪素質無機多孔体に適用することになる。 The impregnated sealer according to the present invention needs to be a transparent liquid in which an isocyanate compound and a silane compound are mixed. This is because if it does not become a transparent liquid, it will be difficult to penetrate into the siliceous inorganic porous material. The impregnated sealer according to the present invention may be mixed with an isocyanate compound and a silane compound, and supplied to the consumer as a transparent liquid in the form of one liquid. Alternatively, the isocyanate compound and the silane compound may be separately supplied to the consumer in the form of two liquids. That is, the isocyanate compound may be stored in the container A and the silane compound may be stored in the container B and supplied to the consumer in the form of a kit. A consumer mixes and stirs the isocyanate compound and silane compound accommodated in each container, makes it a transparent liquid, and applies it to a siliceous inorganic porous material.
本発明に係る含浸シーラー剤は、珪素質無機多孔体に適用される。珪素質無機多孔体とは、珪素化合物を原料として製造された平板等の一定の形状を持つもので、多数の細孔又は空隙を内包しているものである。具体的には、ケイカル板又はフレキシブル板が挙げられる。本発明に係る含浸シーラー剤は、シラン化合物を含有しているので、それを珪素質無機多孔体表面に塗布すると、その細孔又は空隙に良好に浸透する。したがって、本発明に係る含浸シーラー剤を、非珪素質の多孔体に塗布しても、珪素質無機多孔体において得られるような、良好な浸透性は得られない。 The impregnated sealer agent according to the present invention is applied to a siliceous inorganic porous material. The siliceous inorganic porous material has a certain shape such as a flat plate manufactured using a silicon compound as a raw material, and includes a large number of pores or voids. Specifically, a calcium plate or a flexible plate is used. Since the impregnated sealer agent according to the present invention contains a silane compound, when it is applied to the surface of the silicon inorganic porous material, it penetrates well into the pores or voids. Therefore, even if the impregnated sealer according to the present invention is applied to a non-silicon porous material, good permeability as obtained in a silicon inorganic porous material cannot be obtained.
本発明に係る含浸シーラー剤は、一般的に、珪素質無機多孔体表面に塗布することによって、珪素質無機多孔体に適用される。たとえば、ケイカル板又はフレキシブル板の表面に、コーター等によって塗布される。含浸シーラー剤の珪素質無機多孔体に対する適用量（塗布量）は任意であるが、一般的に２０〜８０ｇ／ｍ2程度である。含浸シーラーを珪素質無機多孔体に適用する際、珪素質無機多孔体は加熱されていても、加熱されていなくてもよい。また、適用した後に、適用箇所を乾燥させるために加熱してもよいし、加熱しなくてもよい。本発明に係る含浸シーラー剤は、珪素質無機多孔体表面に対する含浸性乃至は浸透性が良好であるので、加熱せずに常温で適用できる。また、速やかに適用箇所は乾燥するので、適用後に加熱しなくてもよい。しかし、更に含浸性乃至は浸透性を良好にするため、珪素質無機多孔体を加熱しておいてもよい。また、更に適用箇所の乾燥を促進させるために、適用箇所を加熱してもよい。 The impregnation sealer according to the present invention is generally applied to a silicon inorganic porous material by applying it to the surface of the silicon inorganic porous material. For example, it is applied to the surface of a calcium or flexible plate by a coater or the like. The application amount (coating amount) of the impregnated sealer agent to the silicon-based inorganic porous material is arbitrary, but is generally about 20 to 80 g / m 2 . When the impregnated sealer is applied to the siliceous inorganic porous body, the siliceous inorganic porous body may or may not be heated. Moreover, after applying, it may be heated to dry the application site, or may not be heated. Since the impregnating sealer according to the present invention has good impregnation or penetrability with respect to the surface of the silicon inorganic porous material, it can be applied at room temperature without heating. Moreover, since an application location dries quickly, it is not necessary to heat after application. However, in order to further improve the impregnation property or permeability, the silicon-based inorganic porous material may be heated. Further, in order to further accelerate the drying of the application part, the application part may be heated.
含浸シーラー剤が表面に塗布され乾燥した珪素質無機多孔体は、その表面が補強されている。たとえば、表面補強されたケイカル板やフレキシブル板は、そのままで、建材として用いることができる。また、表面補強されているため、そこに各種塗料で塗装を施すと、この塗装が剥げ落ちにくくなる。したがって、本発明に係る含浸シーラー剤を用いて表面補強された珪素質無機多孔体は、壁材や天井材等の各種建材として好適に用いうるものである。 The siliceous inorganic porous material that has been impregnated with the impregnated sealer and dried is reinforced. For example, a surface-reinforced calcium plate or flexible plate can be used as it is as a building material. In addition, since the surface is reinforced, if the paint is applied thereto with various paints, the paint is hardly peeled off. Therefore, the siliceous inorganic porous body whose surface is reinforced by using the impregnated sealer according to the present invention can be suitably used as various building materials such as wall materials and ceiling materials.
以上説明したように、本発明に係る含浸シーラー剤は、イソシアネート化合物と特定のシラン化合物とが、相互に混ざり合って透明な液体となったものである。これを、珪素質無機多孔体の表面に適用すると、シラン化合物は、無機多孔体の珪素質と親和性が良好なので、速やかに無機多孔体に含浸される。一方、イソシアネート化合物はシラン化合物と透明になる程度に混ざり合っているから、シラン化合物と共に速やかに無機多孔体に含浸されるのである。したがって、本発明に係る含浸シーラー剤は、珪素質無機多孔体に速やかに含浸されるという効果を奏する。 As described above, the impregnated sealer according to the present invention is a liquid in which an isocyanate compound and a specific silane compound are mixed with each other. When this is applied to the surface of the silicon inorganic porous body, the silane compound has good affinity with the silicon of the inorganic porous body, so that the inorganic porous body is quickly impregnated. On the other hand, since the isocyanate compound is mixed with the silane compound so as to be transparent, the inorganic porous body is quickly impregnated with the silane compound. Therefore, the impregnated sealer agent according to the present invention has the effect of being rapidly impregnated into the silicon inorganic porous body.
そして、シラン化合物は含浸された後、無機多孔体の珪素質と結合され、無機多孔体中に残存していても、環境中に放出されることはない。したがって、環境上も安全な無機多孔体を得ることができるという効果を奏する。 The silane compound is impregnated and then bonded to the silicon of the inorganic porous body, and even if it remains in the inorganic porous body, it is not released into the environment. Therefore, there is an effect that an inorganic porous body that is environmentally safe can be obtained.
以下、本発明を実施例に基づいて説明するが、本発明は、実施例に限定されるものではない。本発明は、イソシアネート化合物と特定のシラン化合物とを、透明になるように混合すれば、珪素質無機多孔体中に速やかに含浸され、シラン化合物は無機多孔体中の珪素質と結合し、環境中に放出されないとの知見に基づくものとして、解釈されるべきである。 EXAMPLES Hereinafter, although this invention is demonstrated based on an Example, this invention is not limited to an Example. In the present invention, when an isocyanate compound and a specific silane compound are mixed so as to be transparent, the silicon-containing inorganic porous body is quickly impregnated, and the silane compound is bonded to the silicon-containing inorganic porous body, It should be interpreted as being based on the knowledge that it will not be released into.
実施例１
４，４’−ジフェニルメタンジイソシアネートの単量体５３．３質量％と、２，４’−ジフェニルメタンジイソシアネートの単量体１３．３質量％と、これらの多量体３３．３質量％よりなるイソシアネート化合物Ａを調製した。このようなイソシアネート化合物は、住化バイエルウレタン社製のＭＤＩ［商品名「Ｊ−２４３」（４，４’−ジフェニルメタンジイソシアネートの単量体６０質量％と、２，４’−ジフェニルメタンジイソシアネートの単量体２０質量％と、これらの多量体２０質量％からなるもの。）］と、日本ポリウレタン社製のＭＤＩ［商品名「ＭＲ１００」（４，４’−ジフェニルメタンジイソシアネートの単量体４０質量％と、この多量体６０質量％からなるもの。）］とを適宜混合し、上記のような質量比としたものである。以下、多量体を含むＭＤＩ（ジフェニルメタンジイソシアネート）を使用し、市販のものと異なる質量比としたものについて、このような方法で調製した。また、多量体を含まないＭＤＩは、純品を用いて調製した。
このイソシアネート化合物Ａ５０質量％と、テトラエトキシシラン（東芝シリコーン社製、商品名「ＴＳＬ８１２４」）５０質量％とを混合して含浸シーラー剤を得た。
Example 1
Isocyanate compound A consisting of 53.3% by mass of monomer of 4,4′-diphenylmethane diisocyanate, 13.3% by mass of monomer of 2,4′-diphenylmethane diisocyanate, and 33.3% by mass of these multimers Was prepared. Such an isocyanate compound is MDI [trade name “J-243” (60% by mass of monomer of 4,4′-diphenylmethane diisocyanate and a single amount of 2,4′-diphenylmethane diisocyanate] manufactured by Sumika Bayer Urethane Co., Ltd. And 20% by mass of these multimers.)] And MDI manufactured by Nippon Polyurethane Co., Ltd. [trade name “MR100” (40% by mass of monomer of 4,4′-diphenylmethane diisocyanate, These are composed of 60% by mass of the multimer.)] As appropriate to obtain a mass ratio as described above. Hereinafter, MDI (diphenylmethane diisocyanate) containing a multimer was used, and a mass ratio different from that of a commercially available product was prepared by such a method. Moreover, the MDI which does not contain a multimer was prepared using a pure product.
The isocyanate compound A 50% by mass and tetraethoxysilane (trade name “TSL8124” manufactured by Toshiba Silicone Co., Ltd.) 50% by mass were mixed to obtain an impregnated sealer.
実施例２
４，４’−ジフェニルメタンジイソシアネートの単量体５５質量％と、２，４’−ジフェニルメタンジイソシアネートの単量体１５質量％と、これらの多量体３０質量％よりなるイソシアネート化合物Ｂを調製した。このイソシアネート化合物Ｂ５０質量％と、テトラエトキシシラン５０質量％とを混合して含浸シーラー剤を得た。
Example 2
An isocyanate compound B comprising 55% by mass of a monomer of 4,4′-diphenylmethane diisocyanate, 15% by mass of a monomer of 2,4′-diphenylmethane diisocyanate, and 30% by mass of these multimers was prepared. The isocyanate compound B (50% by mass) and tetraethoxysilane (50% by mass) were mixed to obtain an impregnated sealer agent.
実施例３
「Ｊ−２４３」５０質量％と、テトラエトキシシラン５０質量％とを混合して含浸シーラー剤を得た。
Example 3
An impregnation sealer was obtained by mixing 50% by mass of “J-243” and 50% by mass of tetraethoxysilane.
実施例４
「ＭＲ１００」５０質量％と、ビニルトリメトキシシラン（信越シリコーン社製、商品名「ＫＢＭ１００３」）５０質量％とを混合して含浸シーラー剤を得た。
Example 4
50% by mass of “MR100” and 50% by mass of vinyltrimethoxysilane (manufactured by Shin-Etsu Silicone Co., Ltd., trade name “KBM1003”) were mixed to obtain an impregnated sealer.
実施例５
「Ｊ−２４３」５０質量％と、ビニルトリメトキシシラン５０質量％とを混合して含浸シーラー剤を得た。
Example 5
An impregnation sealer was obtained by mixing 50% by mass of “J-243” and 50% by mass of vinyltrimethoxysilane.
実施例６
４，４’−ジフェニルメタンジイソシアネートの単量体５０質量％と、２，４’−ジフェニルメタンジイソシアネートの単量体１０質量％と、これらの多量体４０質量％よりなるイソシアネート化合物Ｄを調製した。このイソシアネート化合物Ｄ５０質量％と、ビニルトリエトキシシラン（信越シリコーン社製、商品名「ＫＢＥ１００３」）５０質量％とを混合して含浸シーラー剤を得た。
Example 6
An isocyanate compound D comprising 50% by mass of a monomer of 4,4′-diphenylmethane diisocyanate, 10% by mass of a monomer of 2,4′-diphenylmethane diisocyanate, and 40% by mass of these multimers was prepared. The isocyanate compound D 50% by mass and vinyl triethoxysilane (manufactured by Shin-Etsu Silicone Co., Ltd., trade name “KBE1003”) 50% by mass were mixed to obtain an impregnated sealer.
実施例７
「Ｊ−２４３」５０質量％と、ビニルトリエトキシシラン５０質量％とを混合して含浸シーラー剤を得た。
Example 7
An impregnated sealer was obtained by mixing 50% by mass of “J-243” and 50% by mass of vinyltriethoxysilane.
実施例８
「ＭＲ１００」３５質量％と、ビニルトリメトキシシラン６５質量％とを混合して含浸シーラー剤を得た。
Example 8
An impregnating sealer was obtained by mixing 35% by mass of “MR100” and 65% by mass of vinyltrimethoxysilane.
実施例９
「Ｊ−２４３」６５質量％と、ビニルトリメトキシシラン３５質量％とを混合して含浸シーラー剤を得た。
Example 9
An impregnation sealer was obtained by mixing 65% by mass of “J-243” and 35% by mass of vinyltrimethoxysilane.
実施例１０
「Ｊ−２４３」３５質量％と、ビニルトリメトキシシラン６５質量％とを混合して含浸シーラー剤を得た。
Example 10
An impregnation sealer was obtained by mixing 35% by mass of “J-243” and 65% by mass of vinyltrimethoxysilane.
実施例１１
イソシアネート化合物Ｄ５０質量％と、ビニルトリエトキシシラン５０質量％とを混合して含浸シーラー剤を得た。
Example 11
An impregnation sealer was obtained by mixing 50% by mass of isocyanate compound D and 50% by mass of vinyltriethoxysilane.
実施例１２
「Ｊ−２４３」６５質量％と、ビニルトリエトキシシラン３５質量％とを混合して含浸シーラー剤を得た。
Example 12
An impregnation sealer was obtained by mixing 65% by mass of “J-243” and 35% by mass of vinyltriethoxysilane.
実施例１３
「Ｊ−２４３」３５質量％と、ビニルトリエトキシシラン６５質量％とを混合して含浸シーラー剤を得た。
Example 13
An impregnation sealer was obtained by mixing 35% by mass of “J-243” and 65% by mass of vinyltriethoxysilane.
実施例１４
「Ｊ−２４３」５０質量％と、テトラメトキシシラン（東芝シリコーン社製、商品名「ＴＳＬ８１１４」）５０質量％とを混合して含浸シーラー剤を得た。
Example 14
An impregnation sealer was obtained by mixing 50% by mass of “J-243” and 50% by mass of tetramethoxysilane (trade name “TSL8114”, manufactured by Toshiba Silicone Co., Ltd.).
実施例１５
４，４’−ジフェニルメタンジイソシアネートの単量体５０質量％と、２，４’−ジフェニルメタンジイソシアネートの単量体５０質量％よりなるイソシアネート化合物Ｅを調製した。このイソシアネート化合物Ｅ５０質量％と、テトラエトキシシラン５０質量％とを混合して含浸シーラー剤を得た。
Example 15
An isocyanate compound E comprising 50% by mass of 4,4′-diphenylmethane diisocyanate monomer and 50% by mass of 2,4′-diphenylmethane diisocyanate monomer was prepared. The isocyanate compound E (50% by mass) and tetraethoxysilane (50% by mass) were mixed to obtain an impregnated sealer agent.
実施例１６
イソシアネート化合物Ｅ５０質量％と、ビニルトリメトキシシラン５０質量％とを混合して含浸シーラー剤を得た。
Example 16
An impregnation sealer was obtained by mixing 50% by mass of the isocyanate compound E and 50% by mass of vinyltrimethoxysilane.
実施例１７
イソシアネート化合物Ｅ５０質量％と、ビニルトリエトキシシラン５０質量％とを混合して含浸シーラー剤を得た。
Example 17
An impregnation sealer was obtained by mixing 50% by mass of isocyanate compound E and 50% by mass of vinyltriethoxysilane.
実施例１８
イソホロンジイソシアネート５０質量％と、テトラエトキシシラン５０質量％とを混合して含浸シーラー剤を得た。
Example 18
An impregnation sealer was obtained by mixing 50% by mass of isophorone diisocyanate and 50% by mass of tetraethoxysilane.
実施例１９
テトラメチルキシリレンジイソシアネート５０質量％と、テトラエトキシシラン５０質量％とを混合して含浸シーラー剤を得た。
Example 19
Tetramethylxylylene diisocyanate 50% by mass and tetraethoxysilane 50% by mass were mixed to obtain an impregnation sealer.
実施例２０
キシリレンジイソシアネート５０質量％と、テトラエトキシシラン５０質量％とを混合して含浸シーラー剤を得た。
Example 20
An impregnated sealer was obtained by mixing 50% by mass of xylylene diisocyanate and 50% by mass of tetraethoxysilane.
実施例２１
イソホロンジイソシアネート５０質量％と、ビニルトリメトキシシラン５０質量％とを混合して含浸シーラー剤を得た。
Example 21
An impregnation sealer was obtained by mixing 50% by mass of isophorone diisocyanate and 50% by mass of vinyltrimethoxysilane.
実施例２２
テトラメチルキシリレンジイソシアネート５０質量％と、ビニルトリメトキシシラン５０質量％とを混合して含浸シーラー剤を得た。
Example 22
Tetramethylxylylene diisocyanate 50% by mass and vinyltrimethoxysilane 50% by mass were mixed to obtain an impregnation sealer.
実施例２３
キシリレンジイソシアネート５０質量％と、ビニルトリメトキシシラン５０質量％とを混合して含浸シーラー剤を得た。
Example 23
An impregnated sealer was obtained by mixing 50% by mass of xylylene diisocyanate and 50% by mass of vinyltrimethoxysilane.
比較例１
「ＭＲ１００」５０質量％と、テトラエトキシシラン５０質量％とを混合して含浸シーラー剤を得た。
Comparative Example 1
50% by mass of “MR100” and 50% by mass of tetraethoxysilane were mixed to obtain an impregnated sealer.
比較例２
イソシアネート化合物Ｄ５０質量％と、テトラエトキシシラン５０質量％とを混合して含浸シーラー剤を得た。
Comparative Example 2
An impregnation sealer was obtained by mixing 50% by mass of isocyanate compound D and 50% by mass of tetraethoxysilane.
比較例３
イソシアネート化合物Ａ３５質量％と、テトラエトキシシラン６５質量％とを混合して含浸シーラー剤を得た。
Comparative Example 3
An impregnation sealer was obtained by mixing 35% by mass of isocyanate compound A and 65% by mass of tetraethoxysilane.
比較例４
「Ｊ−２４３」３５質量％と、テトラエトキシシラン６５質量％とを混合して含浸シーラー剤を得た。
Comparative Example 4
An impregnating sealer was obtained by mixing 35% by mass of “J-243” and 65% by mass of tetraethoxysilane.
比較例５
「ＭＲ１００」５０質量％と、ビニルトリエトキシシラン５０質量％とを混合して含浸シーラー剤を得た。
Comparative Example 5
50% by mass of “MR100” and 50% by mass of vinyltriethoxysilane were mixed to obtain an impregnated sealer.
比較例６
４，４’−ジフェニルメタンジイソシアネートの単量体４６．７質量％と、２，４’−ジフェニルメタンジイソシアネートの単量体６．７質量％と、これらの多量体４６．７質量％よりなるイソシアネート化合物Ｆを調製した。このイソシアネート化合物Ｆ５０質量％と、テトラエトキシシラン５０質量％とを混合して含浸シーラー剤を得た。
Comparative Example 6
Isocyanate compound F comprising 46.7% by weight of monomer of 4,4′-diphenylmethane diisocyanate, 6.7% by weight of monomer of 2,4′-diphenylmethane diisocyanate, and 46.7% by weight of these multimers. Was prepared. The isocyanate compound F (50% by mass) and tetraethoxysilane (50% by mass) were mixed to obtain an impregnated sealer agent.
比較例７
イソシアネート化合物Ｄ３５質量％と、ビニルトリエトキシシラン６５質量％とを混合して含浸シーラー剤を得た。
Comparative Example 7
An impregnation sealer was obtained by mixing 35% by mass of the isocyanate compound D and 65% by mass of vinyltriethoxysilane.
比較例８
「Ｊ−２４３」５０質量％と、３−グリシドキシプロピルトリメトキシシラン（信越シリコーン社製、商品名「ＫＢＭ４０３」）５０質量％とを混合して含浸シーラー剤を得た。
Comparative Example 8
An impregnation sealer was obtained by mixing 50% by mass of “J-243” and 50% by mass of 3-glycidoxypropyltrimethoxysilane (manufactured by Shin-Etsu Silicone, trade name “KBM403”).
比較例９
「Ｊ−２４３」５０質量％と、３−グリシドキシプロピルトリエトキシシラン（信越シリコーン社製、商品名「ＫＢＥ４０３」）５０質量％とを混合して含浸シーラー剤を得た。
Comparative Example 9
An impregnation sealer was obtained by mixing 50% by mass of “J-243” and 50% by mass of 3-glycidoxypropyltriethoxysilane (manufactured by Shin-Etsu Silicone, trade name “KBE403”).
比較例１０
「Ｊ−２４３」５０質量％と、３−メタクリロキシプロピルトリメトキシシラン（信越シリコーン社製、商品名「ＫＢＥ５０３」）５０質量％とを混合して含浸シーラー剤を得た。
Comparative Example 10
An impregnation sealer was obtained by mixing 50% by mass of “J-243” and 50% by mass of 3-methacryloxypropyltrimethoxysilane (manufactured by Shin-Etsu Silicone Co., Ltd., trade name “KBE503”).
比較例１１
「Ｊ−２４３」５０質量％と、３−アクリロキシプロピルトリエトキシシラン（信越シリコーン社製、商品名「ＫＢＥ５１０３」）５０質量％とを混合して含浸シーラー剤を得た。
Comparative Example 11
An impregnation sealer was obtained by mixing 50% by mass of “J-243” and 50% by mass of 3-acryloxypropyltriethoxysilane (manufactured by Shin-Etsu Silicone, trade name “KBE5103”).
比較例１２
「Ｊ−２４３」５０質量％と、３−メルカプトプロピルトリメトキシシラン（信越シリコーン社製、商品名「ＫＢＭ８０３」）５０質量％とを混合して含浸シーラー剤を得た。
Comparative Example 12
An impregnation sealer was obtained by mixing 50% by mass of “J-243” and 50% by mass of 3-mercaptopropyltrimethoxysilane (trade name “KBM803”, manufactured by Shin-Etsu Silicone Co., Ltd.).
比較例１３
「Ｊ−２４３」５０質量％と、３−イソシアネートプロピルトリエトキシシラン（信越シリコーン社製、商品名「ＫＢＥ９００７」）５０質量％とを混合して含浸シーラー剤を得た。
Comparative Example 13
An impregnation sealer was obtained by mixing 50% by mass of “J-243” and 50% by mass of 3-isocyanatopropyltriethoxysilane (manufactured by Shin-Etsu Silicone Co., Ltd., trade name “KBE9007”).
比較例１４
「Ｊ−２４３」５０質量％と、３−イソシアネートプロピルトリメトキシシラン（信越シリコーン社製、商品名「ＫＢＭ９００７」）５０質量％とを混合して含浸シーラー剤を得た。
Comparative Example 14
An impregnation sealer was obtained by mixing 50% by mass of “J-243” and 50% by mass of 3-isocyanatopropyltrimethoxysilane (manufactured by Shin-Etsu Silicone Co., Ltd., trade name “KBM9007”).
比較例１５
４，４’−ジフェニルメタンジイソシアネートの単量体１００質量％からなるイソシアネート化合物を調製した。このイソシアネート化合物５０質量％と、テトラエトキシシラン５０質量％とを混合して含浸シーラー剤を得た。
Comparative Example 15
An isocyanate compound consisting of 100% by mass of a monomer of 4,4′-diphenylmethane diisocyanate was prepared. An impregnation sealer was obtained by mixing 50% by mass of this isocyanate compound and 50% by mass of tetraethoxysilane.
比較例１６
４，４’−ジフェニルメタンジイソシアネートの単量体１００質量％からなるイソシアネート化合物を調製した。このイソシアネート化合物５０質量％と、ビニルトリメトキシシラン５０質量％とを混合して含浸シーラー剤を得た。
Comparative Example 16
An isocyanate compound consisting of 100% by mass of a monomer of 4,4′-diphenylmethane diisocyanate was prepared. An impregnation sealer was obtained by mixing 50% by mass of this isocyanate compound and 50% by mass of vinyltrimethoxysilane.
比較例１７
４，４’−ジフェニルメタンジイソシアネートの単量体１００質量％からなるイソシアネート化合物を調製した。このイソシアネート化合物５０質量％と、ビニルトリエトキシシラン５０質量％とを混合して含浸シーラー剤を得た。
Comparative Example 17
An isocyanate compound consisting of 100% by mass of a monomer of 4,4′-diphenylmethane diisocyanate was prepared. An impregnation sealer was obtained by mixing 50% by mass of this isocyanate compound and 50% by mass of vinyltriethoxysilane.
実施例１〜２３及び比較例１〜１７に係る含浸シーラー剤を用いて、以下の評価を行い、その結果を表１に示した。
［混合性］
液温を２３℃として、含浸シーラー剤を混合攪拌したときに、相互によく混ざり合い、透明な液体になるか否かを、目視にて観察した。そして、以下の基準で評価した。
○：よく混ざり合い、透明な液体となる。
×：混ざり合わず、濁りのある液体となる。
［シーラー剤の含浸性］
次の方法で、三種の珪素質無機多孔体表面への含浸時間（秒）を測定した。すなわち、２３℃の温度下で、ニチアス社製の０．８比重ケイカル板１（厚さ６ｍｍ）、１．０比重ケイカル板２（厚さ６ｍｍ）及びＡ＆Ａ社製のフレキシブル板（厚さ４ｍｍ）の表面にスポイトで、各含浸シーラー剤を０．１５ｍｌ滴下し、その表面が乾くまでの時間を測定した。３００秒以上経過しても乾かないものは、その時点で測定を中止した。
［表面補強性］
縦・横４０ｍｍ角に調整した０．８比重ケイカル板２枚の表面にシーラー剤を約６０ｇ／ｍ2塗布する。その後、２３℃・５５％ＲＨ環境下で、３００秒養生した。そして、シーラー剤の塗布面を対向させ、その間に２０ｍｍ角のジアリルフタレート樹脂含浸紙を挟んで、ホットプレス（温度１３０℃で圧力９８１ｋＰａ）を１０分間行い、２枚のケイカル板を接着する。解圧後、２３℃・５５％ＲＨ環境下で、２４時間養生した。その後、接着されている２枚のケイカル板の両面に、金属アタッチメントを２液反応型エポキシ樹脂系接着剤で接着した。そして、金属アタッチメントを島津製作所社製のオートグラフ試験機に装着して、単軸平面引張接着強さ（Ｎ／ｍｍ2）を測定した。なお、シーラー剤の含浸が３００秒以上のものについては、表面補強性の試験は行わなかった。
The following evaluation was performed using the impregnated sealer agents according to Examples 1 to 23 and Comparative Examples 1 to 17, and the results are shown in Table 1.
[Mixability]
When the liquid temperature was 23 ° C. and the impregnated sealer agent was mixed and stirred, it was visually observed whether or not it mixed well and became a transparent liquid. And it evaluated on the following references | standards.
○: It mixes well and becomes a transparent liquid.
X: It does not mix and becomes a turbid liquid.
[Impregnation of sealer]
The impregnation time (seconds) on the surfaces of the three types of silicon-containing inorganic porous bodies was measured by the following method. That is, at a temperature of 23 ° C., 0.8 specific gravity calcium plate 1 (thickness 6 mm) manufactured by Nichias, 1.0 specific gravity calcium plate 2 (thickness 6 mm), and flexible plate manufactured by A & A (thickness 4 mm). 0.15 ml of each impregnating sealer agent was dropped on the surface with a dropper, and the time until the surface was dried was measured. For those that did not dry after 300 seconds, the measurement was stopped at that time.
[Surface reinforcement]
About 60 g / m 2 of sealer is applied to the surface of two 0.8 specific gravity calcium plates adjusted to 40 mm square. Thereafter, it was cured for 300 seconds in an environment of 23 ° C. and 55% RH. Then, the application surface of the sealer is made to face each other, and a 20 mm square diallyl phthalate resin impregnated paper is sandwiched between them, and hot pressing (at a temperature of 130 ° C. and a pressure of 981 kPa) is performed for 10 minutes to bond the two calcium plates. After decompression, it was cured for 24 hours in an environment of 23 ° C. and 55% RH. Thereafter, a metal attachment was bonded to both surfaces of the two bonded calcium plates with a two-component reaction type epoxy resin adhesive. Then, the metal attachment was attached to an autograph tester manufactured by Shimadzu Corporation, and the uniaxial planar tensile adhesive strength (N / mm 2 ) was measured. In addition, the surface reinforcing property test was not performed for the impregnated sealer agent for 300 seconds or more.
［表１］
━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━
シ ー ラ ー 剤 の 含 浸 性（秒）
────────────────────
混合性 ケイカル ケイカル フレキシ 表面補強性
板１ 板２ ブル板 (N/mm2)
━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━
実施例１ ○ １４０ １６０ ２６０ ０．３２
実施例２ ○ １１０ １５０ ２４０ ０．２４
実施例３ ○ １００ １４０ ２３０ ０．２６
実施例４ ○ ７０ ７５ １００ ０．２３
実施例５ ○ ４０ ４０ ４５ ０．２０
実施例６ ○ １０５ １２０ １４５ ０．２１
実施例７ ○ ９０ ９０ １２０ ０．３５
実施例８ ○ ４０ ５０ ６０ ０．２７
実施例９ ○ ６５ ８０ １５０ ０．４２
実施例１０ ○ ３０ ３０ ４０ ０．１５
実施例１１ ○ １０５ １２０ １４５ ０．２１
実施例１２ ○ １８０ １８０ ３００ ０．４６
実施例１３ ○ ６５ ６０ ９０ ０．１９
実施例１４ ○ ６０ ６０ ８０ ０．２１
実施例１５ ○ ６５ ７０ １５０ ０．２２
実施例１６ ○ ３５ ３５ ４０ ０．２２
実施例１７ ○ ５５ ５５ ９０ ０．２０
実施例１８ ○ ６０ ８０ ９０ ０．２６
実施例１９ ○ ６０ ６０ ９０ ０．２０
実施例２０ ○ ６０ ６０ ９０ ０．２８
実施例２１ ○ ３０ ３５ ４５ ０．３５
実施例２２ ○ ３０ ３０ ４０ ０．２９
実施例２３ ○ ３０ ３０ ４５ ０．２５
比較例１ × ３００＜ ３００＜ ３００＜ −
比較例２ × ３００＜ ３００＜ ３００＜ −
比較例３ × ３００＜ ３００＜ ３００＜ −
比較例４ × ３００＜ ３００＜ ３００＜ −
比較例５ × ３００＜ ３００＜ ３００＜ −
比較例６ × ３００＜ ３００＜ ３００＜ −
比較例７ × ３００＜ ３００＜ ３００＜ −
比較例８ × ３００＜ ３００＜ ３００＜ −
比較例９ ○ ３００＜ ３００＜ ３００＜ −
比較例１０ × ３００＜ ３００＜ ３００＜ −
比較例１１ ○ ３００＜ ３００＜ ３００＜ −
比較例１２ × ３００＜ ３００＜ ３００＜ −
比較例１３ ○ ３００＜ ３００＜ ３００＜ −
比較例１４ × ３００＜ ３００＜ ３００＜ −
比較例１５ × ３００＜ ３００＜ ３００＜ −
比較例１６ × ３００＜ ３００＜ ３００＜ −
比較例１７ × ３００＜ ３００＜ ３００＜ −
━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━
[Table 1]
━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━
Impregnation of sealer (seconds)
────────────────────
Mixability Keical Keical Flexi Surface reinforcement
Board 1 Board 2 Bull board (N / mm 2 )
━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━
Example 1 ○ 140 160 260 0.32
Example 2 ○ 110 150 240 0.24
Example 3 ○ 100 140 230 0.26
Example 4 ○ 70 75 100 0.23
Example 5 ○ 40 40 45 0.20
Example 6 ○ 105 120 145 0.21
Example 7 ○ 90 90 120 0.35
Example 8 ○ 40 50 60 0.27
Example 9 ○ 65 80 150 0.42
Example 10 ○ 30 30 40 0.15
Example 11 ○ 105 120 145 0.21
Example 12 ○ 180 180 300 0.46
Example 13 ○ 65 60 90 0.19
Example 14 ○ 60 60 80 0.21
Example 15 ○ 65 70 150 0.22
Example 16 ○ 35 35 40 0.22
Example 17 ○ 55 55 90 0.20
Example 18 ○ 60 80 90 0.26
Example 19 ○ 60 60 90 0.20
Example 20 ○ 60 60 90 0.28
Example 21 ○ 30 35 45 0.35
Example 22 ○ 30 30 40 0.29
Example 23 ○ 30 30 45 0.25
Comparative Example 1 × 300 <300 <300 <−
Comparative Example 2 × 300 <300 <300 <−
Comparative Example 3 × 300 <300 <300 <−
Comparative Example 4 × 300 <300 <300 <−
Comparative Example 5 × 300 <300 <300 <−
Comparative Example 6 × 300 <300 <300 <−
Comparative Example 7 × 300 <300 <300 <−
Comparative Example 8 × 300 <300 <300 <−
Comparative Example 9 ○ 300 <300 <300 <-
Comparative Example 10 × 300 <300 <300 <−
Comparative Example 11 ○ 300 <300 <300 <−
Comparative Example 12 × 300 <300 <300 <−
Comparative Example 13 ○ 300 <300 <300 <-
Comparative Example 14 × 300 <300 <300 <−
Comparative Example 15 × 300 <300 <300 <−
Comparative Example 16 × 300 <300 <300 <−
Comparative Example 17 × 300 <300 <300 <−
━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━
実施例１〜２３に係る含浸シーラー剤は、２３℃下において、相互に混ざり合い透明な液体となって、ケイカル板及びフレキシブル板への含浸性に優れたものであった。また、ケイカル板表面の補強性も十分なものであった。なお、実施例１５に係る含浸シーラー剤は、２３℃の液温では相互に混ざり合い透明な液体になったが、液温が１０℃以下になると、イソシアネート化合物が結晶化して、濁りが生じた。したがって、この含浸シーラー剤は、常温以上にて作業する必要がある。一方、比較例１〜７に係る含浸シーラー剤は、所定のイソシアネート化合物と所定のシラン化合物とを混合したが、相互に混ざり合わずに、濁ったままであり、含浸性の悪いものであった。また、比較例８〜１４に係る含浸シーラー剤は、本発明で用いるシラン化合物以外のものを使用したため、比較例９，１１及び１３を除き、いずれも相互に混ざり合わずに濁りが生じたままであった。したがって、比較例８、１０、１２及び１４に係るシーラー剤は、含浸性は悪かった。また、その理由は定かではないが、透明な液体となった比較例９、１１及び１３についても、含浸性が悪かった。さらに、比較例１６〜１７は、４，４’−ジフェニルメタンジイソシアネートが結晶化しており、シラン化合物と混合しても、透明な液体とならず、含浸性の悪いものであった。 The impregnated sealer agents according to Examples 1 to 23 were mixed with each other at 23 ° C. to become a transparent liquid, and were excellent in impregnation properties for the calcium and flexible plates. In addition, the reinforcing property of the surface of the calcium plate was sufficient. The impregnated sealer according to Example 15 mixed with each other at a liquid temperature of 23 ° C. and became a transparent liquid. However, when the liquid temperature became 10 ° C. or less, the isocyanate compound crystallized and became turbid. . Therefore, it is necessary to work this impregnated sealer at room temperature or higher. On the other hand, the impregnated sealer agents according to Comparative Examples 1 to 7 were prepared by mixing a predetermined isocyanate compound and a predetermined silane compound, but remained turbid without being mixed with each other, and had poor impregnation properties. Moreover, since the impregnating sealer agents according to Comparative Examples 8 to 14 were other than the silane compound used in the present invention, except for Comparative Examples 9, 11 and 13, none of them mixed with each other and remained turbid. there were. Therefore, the sealer agents according to Comparative Examples 8, 10, 12 and 14 had poor impregnation properties. Moreover, although the reason is not certain, the impregnation property was also bad also about the comparative examples 9, 11, and 13 used as the transparent liquid. Further, in Comparative Examples 16 to 17, 4,4'-diphenylmethane diisocyanate was crystallized, and even when mixed with a silane compound, it was not a transparent liquid and was poor in impregnation properties.
実施例２４
イソシアネート化合物Ａ６５質量％と、テトラエトキシシラン３５質量％とを混合して含浸シーラー剤を得た。
Example 24
An impregnation sealer was obtained by mixing 65% by mass of isocyanate compound A and 35% by mass of tetraethoxysilane.
実施例２５
「Ｊ−２４３」８０質量％と、テトラエトキシシラン２０質量％とを混合して含浸シーラー剤を得た。
Example 25
80% by mass of “J-243” and 20% by mass of tetraethoxysilane were mixed to obtain an impregnated sealer agent.
実施例２６
「Ｊ−２４３」６５質量％と、テトラエトキシシラン３５質量％とを混合して含浸シーラー剤を得た。
Example 26
An impregnation sealer was obtained by mixing 65% by mass of “J-243” and 35% by mass of tetraethoxysilane.
実施例２７
「ＭＲ１００」６５質量％と、ビニルトリメトキシシラン３５質量％とを混合して含浸シーラー剤を得た。
Example 27
“MR100” 65 mass% and vinyltrimethoxysilane 35 mass% were mixed to obtain an impregnated sealer.
実施例２８
「ＭＲ１００」８０質量％と、ビニルトリメトキシシラン２０質量％とを混合して含浸シーラー剤を得た。
Example 28
80% by mass of “MR100” and 20% by mass of vinyltrimethoxysilane were mixed to obtain an impregnated sealer.
実施例２９
イソシアネート化合物Ｄ８０質量％と、ビニルトリエトキシシラン２０質量％とを混合して含浸シーラー剤を得た。
Example 29
An impregnation sealer was obtained by mixing 80% by mass of the isocyanate compound D and 20% by mass of vinyltriethoxysilane.
実施例３０
イソシアネート化合物Ｄ６５質量％と、ビニルトリエトキシシラン３５質量％とを混合して含浸シーラー剤を得た。
Example 30
An impregnation sealer was obtained by mixing 65% by mass of the isocyanate compound D and 35% by mass of vinyltriethoxysilane.
実施例３１
「Ｊ−２４３」８０質量％と、ビニルトリエトキシシラン２０質量％とを混合して含浸シーラー剤を得た。
Example 31
80% by mass of “J-243” and 20% by mass of vinyltriethoxysilane were mixed to obtain an impregnated sealer agent.
実施例２４〜３１に係る含浸シーラー剤に関して、混合性と、ケイカル板１及び２への含浸性を評価した結果は、表２に示すとおりであった。 Regarding the impregnated sealer agents according to Examples 24-31, the results of evaluating the mixing property and the impregnating property to the calcium plates 1 and 2 were as shown in Table 2.
［表２］
━━━━━━━━━━━━━━━━━━━━━━━━━━━━
シーラー剤の含浸性（秒）
───────────────
混合性 ケイカル板１ ケイカル板２
━━━━━━━━━━━━━━━━━━━━━━━━━━━━
実施例２４ ○ ２７０ ２７０
実施例２５ ○ ２７０ ３００＜
実施例２６ ○ ２１０ ２１０
実施例２７ ○ ９０ １８０
実施例２８ ○ １５０ １６０
実施例２９ ○ ２７０ ３００＜
実施例３０ ○ ２２０ ２１０
実施例３１ ○ ２１０ ２４０
━━━━━━━━━━━━━━━━━━━━━━━━━━━━
[Table 2]
━━━━━━━━━━━━━━━━━━━━━━━━━━━━
Sealer impregnation (seconds)
───────────────
Mixing Calcium board 1 Calcium board 2
━━━━━━━━━━━━━━━━━━━━━━━━━━━━
Example 24 ○ 270 270
Example 25 ○ 270 300 <
Example 26 ○ 210 210
Example 27 ○ 90 180
Example 28 ○ 150 160
Example 29 ○ 270 300 <
Example 30 ○ 220 210
Example 31 ○ 210 240
━━━━━━━━━━━━━━━━━━━━━━━━━━━━
実施例３２
イソシアネート化合物Ａ８０質量％と、テトラエトキシシラン２０質量％とを混合して含浸シーラー剤を得た。これは、相互に混ざり合い、濁りのない透明な液体になった。
Example 32
An impregnation sealer was obtained by mixing 80% by mass of isocyanate compound A and 20% by mass of tetraethoxysilane. This blended with each other and became a clear liquid without turbidity.
実施例３３
「ＭＲ１００」８０質量％と、ビニルトリメトキシシラン２０質量％とを混合して含浸シーラー剤を得た。これは、相互に混ざり合い、濁りのない透明な液体になった。
Example 33
80% by mass of “MR100” and 20% by mass of vinyltrimethoxysilane were mixed to obtain an impregnated sealer. This blended with each other and became a clear liquid without turbidity.
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Citations (9)
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|---|---|---|---|---|
| JPS5540722A (en) * | 1978-09-19 | 1980-03-22 | Nippon Polyurethan Kogyo Kk | Primer composition |
| JPH04306283A (en) * | 1991-04-03 | 1992-10-29 | Cemedine Co Ltd | Primer composition |
| JPH07278494A (en) * | 1994-04-15 | 1995-10-24 | Yokohama Rubber Co Ltd:The | Primer composition for coating composition with resistance to acid rain |
| JPH08199066A (en) * | 1995-01-27 | 1996-08-06 | Shin Etsu Chem Co Ltd | Waterproof composition |
| JPH1113250A (en) * | 1997-06-19 | 1999-01-19 | Asahi Glass Co Ltd | Curtain plate with excellent stain resistance |
| JP2002308961A (en) * | 2001-04-13 | 2002-10-23 | Asia Kogyo Kk | Moisture-curable resin composition and sealer for inorganic material |
| JP2004339278A (en) * | 2003-05-13 | 2004-12-02 | Chugoku Marine Paints Ltd | Non-solvent type substrate treating agent for inorganic substrate, and method for substrate treating inorganic substrate using the treating agent |
| JP2005015676A (en) * | 2003-06-27 | 2005-01-20 | Kaneka Corp | Composition affording antifouling property, coating composition using the same and coated film using the coating composition |
| JP2005139426A (en) * | 2003-10-16 | 2005-06-02 | Shinko Paint Kk | Non-solvent normal temperature-curable type silicone resin coating composition |
-
2007
- 2007-05-12 JP JP2007127465A patent/JP5083947B2/en not_active Expired - Fee Related
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5540722A (en) * | 1978-09-19 | 1980-03-22 | Nippon Polyurethan Kogyo Kk | Primer composition |
| JPH04306283A (en) * | 1991-04-03 | 1992-10-29 | Cemedine Co Ltd | Primer composition |
| JPH07278494A (en) * | 1994-04-15 | 1995-10-24 | Yokohama Rubber Co Ltd:The | Primer composition for coating composition with resistance to acid rain |
| JPH08199066A (en) * | 1995-01-27 | 1996-08-06 | Shin Etsu Chem Co Ltd | Waterproof composition |
| JPH1113250A (en) * | 1997-06-19 | 1999-01-19 | Asahi Glass Co Ltd | Curtain plate with excellent stain resistance |
| JP2002308961A (en) * | 2001-04-13 | 2002-10-23 | Asia Kogyo Kk | Moisture-curable resin composition and sealer for inorganic material |
| JP2004339278A (en) * | 2003-05-13 | 2004-12-02 | Chugoku Marine Paints Ltd | Non-solvent type substrate treating agent for inorganic substrate, and method for substrate treating inorganic substrate using the treating agent |
| JP2005015676A (en) * | 2003-06-27 | 2005-01-20 | Kaneka Corp | Composition affording antifouling property, coating composition using the same and coated film using the coating composition |
| JP2005139426A (en) * | 2003-10-16 | 2005-06-02 | Shinko Paint Kk | Non-solvent normal temperature-curable type silicone resin coating composition |
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