JP5577049B2 - 水性塗料用樹脂組成物を用いた建築外装塗膜の製造方法 - Google Patents
水性塗料用樹脂組成物を用いた建築外装塗膜の製造方法 Download PDFInfo
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- JP5577049B2 JP5577049B2 JP2009133196A JP2009133196A JP5577049B2 JP 5577049 B2 JP5577049 B2 JP 5577049B2 JP 2009133196 A JP2009133196 A JP 2009133196A JP 2009133196 A JP2009133196 A JP 2009133196A JP 5577049 B2 JP5577049 B2 JP 5577049B2
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- UDWIZRDPCQAYRF-UHFFFAOYSA-N 3-[diethoxy(methyl)silyl]propyl prop-2-enoate Chemical compound CCO[Si](C)(OCC)CCCOC(=O)C=C UDWIZRDPCQAYRF-UHFFFAOYSA-N 0.000 description 3
- MCDBEBOBROAQSH-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propyl prop-2-enoate Chemical compound CO[Si](C)(OC)CCCOC(=O)C=C MCDBEBOBROAQSH-UHFFFAOYSA-N 0.000 description 3
- XDQWJFXZTAWJST-UHFFFAOYSA-N 3-triethoxysilylpropyl prop-2-enoate Chemical compound CCO[Si](OCC)(OCC)CCCOC(=O)C=C XDQWJFXZTAWJST-UHFFFAOYSA-N 0.000 description 3
- RYYXDZDBXNUPOG-UHFFFAOYSA-N 4,5,6,7-tetrahydro-1,3-benzothiazole-2,6-diamine;dihydrochloride Chemical compound Cl.Cl.C1C(N)CCC2=C1SC(N)=N2 RYYXDZDBXNUPOG-UHFFFAOYSA-N 0.000 description 3
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- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 3
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- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 description 1
- 239000010438 granite Substances 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 150000004688 heptahydrates Chemical class 0.000 description 1
- VRINOTYEGADLMW-UHFFFAOYSA-N heptyl(trimethoxy)silane Chemical compound CCCCCCC[Si](OC)(OC)OC VRINOTYEGADLMW-UHFFFAOYSA-N 0.000 description 1
- 150000002391 heterocyclic compounds Chemical class 0.000 description 1
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- 150000002430 hydrocarbons Chemical class 0.000 description 1
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- 239000003999 initiator Substances 0.000 description 1
- 239000002563 ionic surfactant Substances 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910000358 iron sulfate Inorganic materials 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 239000004611 light stabiliser Substances 0.000 description 1
- 230000005923 long-lasting effect Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- XJRBAMWJDBPFIM-UHFFFAOYSA-N methyl vinyl ether Chemical compound COC=C XJRBAMWJDBPFIM-UHFFFAOYSA-N 0.000 description 1
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 1
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- 239000000479 mixture part Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- JESXATFQYMPTNL-UHFFFAOYSA-N mono-hydroxyphenyl-ethylene Natural products OC1=CC=CC=C1C=C JESXATFQYMPTNL-UHFFFAOYSA-N 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- OMNKZBIFPJNNIO-UHFFFAOYSA-N n-(2-methyl-4-oxopentan-2-yl)prop-2-enamide Chemical compound CC(=O)CC(C)(C)NC(=O)C=C OMNKZBIFPJNNIO-UHFFFAOYSA-N 0.000 description 1
- LUZMYRZQOMVJCU-UHFFFAOYSA-N n-[2-(diethylamino)ethyl]-2-(5-methyl-2-propan-2-ylphenoxy)acetamide;4-methylbenzenesulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1.CCN(CC)CCNC(=O)COC1=CC(C)=CC=C1C(C)C LUZMYRZQOMVJCU-UHFFFAOYSA-N 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- DCUJJWWUNKIJPH-UHFFFAOYSA-N nitrapyrin Chemical compound ClC1=CC=CC(C(Cl)(Cl)Cl)=N1 DCUJJWWUNKIJPH-UHFFFAOYSA-N 0.000 description 1
- 125000002560 nitrile group Chemical group 0.000 description 1
- 239000007764 o/w emulsion Substances 0.000 description 1
- UHGIMQLJWRAPLT-UHFFFAOYSA-N octadecyl dihydrogen phosphate Chemical compound CCCCCCCCCCCCCCCCCCOP(O)(O)=O UHGIMQLJWRAPLT-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 125000001117 oleyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])/C([H])=C([H])\C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 150000003961 organosilicon compounds Chemical class 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
- 125000005459 perfluorocyclohexyl group Chemical group 0.000 description 1
- 150000004714 phosphonium salts Chemical class 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
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- 229920000570 polyether Polymers 0.000 description 1
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- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000011178 precast concrete Substances 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- HJWLCRVIBGQPNF-UHFFFAOYSA-N prop-2-enylbenzene Chemical compound C=CCC1=CC=CC=C1 HJWLCRVIBGQPNF-UHFFFAOYSA-N 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000011833 salt mixture Substances 0.000 description 1
- 150000003342 selenium Chemical class 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- 125000003808 silyl group Chemical group [H][Si]([H])([H])[*] 0.000 description 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- DEWNCLAWVNEDHG-UHFFFAOYSA-M sodium;2-(2-methylprop-2-enoyloxy)ethanesulfonate Chemical compound [Na+].CC(=C)C(=O)OCCS([O-])(=O)=O DEWNCLAWVNEDHG-UHFFFAOYSA-M 0.000 description 1
- MNCGMVDMOKPCSQ-UHFFFAOYSA-M sodium;2-phenylethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=CC1=CC=CC=C1 MNCGMVDMOKPCSQ-UHFFFAOYSA-M 0.000 description 1
- 238000005063 solubilization Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
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- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
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- 238000003786 synthesis reaction Methods 0.000 description 1
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- 125000002889 tridecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- DENFJSAFJTVPJR-UHFFFAOYSA-N triethoxy(ethyl)silane Chemical compound CCO[Si](CC)(OCC)OCC DENFJSAFJTVPJR-UHFFFAOYSA-N 0.000 description 1
- WUMSTCDLAYQDNO-UHFFFAOYSA-N triethoxy(hexyl)silane Chemical compound CCCCCC[Si](OCC)(OCC)OCC WUMSTCDLAYQDNO-UHFFFAOYSA-N 0.000 description 1
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 1
- FZMJEGJVKFTGMU-UHFFFAOYSA-N triethoxy(octadecyl)silane Chemical compound CCCCCCCCCCCCCCCCCC[Si](OCC)(OCC)OCC FZMJEGJVKFTGMU-UHFFFAOYSA-N 0.000 description 1
- FHVAUDREWWXPRW-UHFFFAOYSA-N triethoxy(pentyl)silane Chemical compound CCCCC[Si](OCC)(OCC)OCC FHVAUDREWWXPRW-UHFFFAOYSA-N 0.000 description 1
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 description 1
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 description 1
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- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- JZZBTMVTLBHJHL-UHFFFAOYSA-N tris(2,3-dichloropropyl) phosphate Chemical compound ClCC(Cl)COP(=O)(OCC(Cl)CCl)OCC(Cl)CCl JZZBTMVTLBHJHL-UHFFFAOYSA-N 0.000 description 1
- GTRSAMFYSUBAGN-UHFFFAOYSA-N tris(2-chloropropyl) phosphate Chemical compound CC(Cl)COP(=O)(OCC(C)Cl)OCC(C)Cl GTRSAMFYSUBAGN-UHFFFAOYSA-N 0.000 description 1
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- 229920001567 vinyl ester resin Polymers 0.000 description 1
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical class [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Paints Or Removers (AREA)
Description
すなわち、
1).
(I)合成樹脂エマルジョン
(II)下記一般式(1)で示されるシリコン化合物および/またはその部分加水分解縮合物
(R1O)4-aSiR2 a (1)
(式中、R1は同じかまたは異なり、炭素数1〜10のアルキル基、炭素数6〜10のアリール基または炭素数7〜10のアラルキル基、R2は同じかまたは異なり、炭素数1〜10のアルキル基、炭素数6〜10のアリール基、または炭素数7〜10のアラルキル基、aは0〜2の整数。)
(III)光酸発生剤
を含有する水性塗料用樹脂組成物、
2).
前記(II)シリコン化合物および/またはその部分加水分解縮合物が、オルガノシリケート(下記一般式(2)で示される化合物および/またはその部分加水分解縮合物)および/またはその変性物
(R3O)4Si (2)
(式中、R3は同じかまたは異なり、炭素数1〜10のアルキル基、炭素数6〜10のアリール基または炭素数7〜10のアラルキル基である1)に記載の水性塗料用樹脂組成物、
3).
前記(II)シリコン化合物および/またはその部分加水分解縮合物をノニオン系界面活性剤および/またはアニオン系界面活性剤を用いて水性媒体中に分散して得られる乳化物として添加する1)または2)に記載の水性塗料用樹脂組成物、
4).
前記(I)合成樹脂エマルジョンが、アルコキシシリル基含有単量体単位を有するアクリル系樹脂エマルジョンである1)〜3)のいずれか1項に記載の水性塗料用樹脂組成物、
5).
さらに(IV)酸により活性化するアルコキシシリル基の加水分解・縮合を促進する化合物を含有する1)〜4)のいずれか1項に記載の水性塗料用樹脂組成物、
6).
(IV)酸により活性化するアルコキシシリル基の加水分解・縮合を促進する化合物が酸性リン酸化合物の塩である5)に記載の水性塗料用樹脂組成物、
7)
(III)光酸発生剤が、有機ハロゲン化合物である1)〜6)の何れか1項に記載の水性塗料用樹脂組成物、
8)
(III)光酸発生剤が、ハロゲン含有トリアジン化合物、塩化ビニリデン共重合体、塩化ビニル共重合体、塩素化ポリオレフィンである1)〜7)の何れか1項に記載の水性塗料用樹脂組成物、
9)
1)〜8)の何れか1項に記載の(I)、(II)、(III)および必要に応じて(IV)を含有してなる一液型水性塗料用樹脂組成物、
に関する。
本発明に使用可能な合成樹脂エマルションとしては、アクリル系樹脂エマルジョン、ウレタン樹脂エマルジョン、ふっ素樹脂エマルジョン、エポキシ樹脂エマルジョン、ポリエステル樹脂エマルジョン、アルキド樹脂エマルジョン、メラミン樹脂エマルジョンなどが挙げられるが、これらに限定されるわけではない。また、これらは単独で使用しても2種以上を併用しても良い。これらの中でコスト、樹脂設計の自由度の高さなどからアクリル系樹脂エマルジョンが有利である。
R4R5 (3-b)Si(OR6)b (3)
(式中、R4は重合性二重結合を有する1価有機基、R5は炭素数1〜4のアルキル基、R6は炭素数1〜4のアルキル基、bは1〜3)で示される有機ケイ素化合物で、アルコキシ基を有し、反応性二重結合を有する化合物である。その具体例としては、ビニルトリメトキシシラン、ビニルトリエトキシシラン、ビニルトリプロポキシシラン、ビニルトリイソプロポキシシラン、ビニルメチルジメトキシシラン、ビニルメチルジエトキシシランなどのビニルシラン類;γ−(メタ)アクリロキシプロピルトリメトキシシラン、γ−(メタ)アクリロキシプロピルトリエトキシシラン、γ−(メタ)アクリロキシプロピルトリプロポキシシラン、γ−(メタ)アクリロキシプロピルトリイソプロポキシシラン、γ−(メタ)アクリロキシプロピルトリブトキシシラン、γ−(メタ)アクリロキシプロピルメチルジメトキシシラン、γ−(メタ)アクリロキシプロピルメチルジエトキシシラン、γ−(メタ)アクリロキシプロピルメチルジプロポキシシラン、γ−(メタ)アクリロキシプロピルメチルジイソプロポキシシラン、γ−(メタ)アクリロキシプロピルメチルジブトキシシランなどのアクリルシラン類などがあげられ、これらを1種又は2種以上併用して用いることができる。
本発明における(II)成分であるシリコン化合物は、一般式(1)で示される。
(R1O)4-aSiR2 a (1)
(式中、R1は同じかまたは異なり、炭素数1〜10のアルキル基、炭素数6〜10のアリール基または炭素数7〜10のアラルキル基、R2は同じかまたは異なり、炭素数1〜10のアルキル基、炭素数6〜10のアリール基、または炭素数7〜10のアラルキル基、aは0〜2の整数。)
(R3O)4Si (2)
(式中、R3は同じかまたは異なり、炭素数1〜10のアルキル基、炭素数6〜10のアリール基または炭素数7〜10のアラルキル基)
本発明における(III)成分である光酸発生剤は、光暴露により酸を発生する化合物であり、たとえばトルエンスルホン酸などの強酸または四フッ化ホウ素などのスルホニウム塩、アンモニウム塩、ホスホニウム塩、ヨードニウム塩またはセレニウム塩などのオニウム塩類;鉄−アレン錯体類;シラノール−金属キレート錯体類;ジスルホン類、ジスルホニルジアゾメタン類、ジスルホニルメタン類、スルホニルベンゾイルメタン類、イミドスルホネート類、ベンゾインスルホネート類などのスルホン酸誘導体;有機ハロゲン化合物類など、特開平5−134412号公報に示される放射線の照射により酸を発生する化合物があげられる。
本発明の水性塗料用樹脂組成物は、(I)合成樹脂エマルジョン、(II)シリコン化合物および/またはその部分加水分解縮合物、(III)光酸発生剤、必要であれば(IV)加水分解・縮合を促進する化合物を、任意の順番で加え混合することにより得られる。混合方法は、一般的な混合方法を使用することができ特に限定されない。
撹拌機、還流冷却器、窒素ガス導入管および滴下ロートを備えた反応容器に、初期仕込みとして脱イオン水160重量部、Newcol−707SN(日本乳化剤(株)製:有効成分30%、ポリオキシエチレン多環フェニルエーテル硫酸エステルナトリウム塩)0.35重量部、5%炭酸水素ナトリウム水溶液0.25重量部を仕込み、窒素ガスを導入しつつ50℃に昇温した。昇温後、7%t−ブチルハイドロパーオキサイド水溶液0.5重量部、20%Bruggolite FF−6水溶液0.28重量部、0.10%硫酸第一鉄・7水和物と0.40%エチレンジアミン四酢酸二ナトリウムの混合水溶液0.35部を添加し、1段目として2−エチルヘキシルアクリレート16.04重量部、ブチルメタクリレート33重量部、γ−メタクリロキシプロピルメチルジメトキシシラン0.94重量部の混合物50重量部にアデカリアソープSR−10S((株)ADEKA製:有効成分100%、ポリオキシエチレン−1−アルコキシメチル−2−(2−プロペニルオキシ)エチルエーテル硫酸エステルナトリウム塩)0.75重量部、アデカリアソープER−20((株)ADEKA製:有効成分75%、ポリオキシエチレン−1−アルコキシメチル−2−(2−プロペニルオキシ)エチルエーテル)0.47重量部、および脱イオン水20重量部を加え乳化したモノマー乳化液を200分かけて等速追加した。その間、7%t−ブチルハイドロパーオキサイド水溶液0.55重量部および2.5%Bruggolite FF−6水溶液0.43重量部を3回に分けて添加した。モノマー乳化液追加終了後、1時間後重合を行った。さらに、7%t−ブチルハイドロパーオキサイド水溶液0.25重量部、2.5%Bruggolite FF−6水溶液0.55重量部および0.10%硫酸第一鉄・7水和物と0.40%エチレンジアミン四酢酸二ナトリウムの混合水溶液0.35部を添加し、2段目としてメチルメタクリレート9.25重量部、ブチルメタクリレート37重量部、γ−メタクリロキシプロピルトリエトキシシラン0.5重量部、ポリオキシエチレン鎖を有するビニル系単量体であるブレンマーPE−200(日油(株)製)3重量部、n−ドデシルメルカプタン0.25重量部の混合物50重量部にアデカリアソープSR−10S 0.75重量部、アデカリアソープER−20 0.47重量部、および脱イオン水20重量部を加え乳化したモノマー乳化液を200分かけて等速追加した。その間、7%t−ブチルハイドロパーオキサイド水溶液0.6重量部および2.5%Bruggolite FF−6水溶液0.85重量部を4回に分けて添加した。モノマー乳化液追加終了後、1.5時間後重合を行った。得られたエマルジョンに5%炭酸水素ナトリウム水溶液5.5部を添加後、脱イオン水で固形分50%に調整しアクリル系樹脂エマルジョン(I−1)を得た。得られたエマルジョンは、日機装(株)製動的光散乱法粒子径測定機MICROTRAC UPA MODEL9340−UPAによる体積平均粒子径が200nmであった。
室温にて、縮合度5〜6のテトラ−n−プロピルシリケート部分加水分解縮合物30重量部とネオコールSW−C(第一工業製薬(株)製:有効成分70%、ジアルキルスルホコハク酸ナトリウム塩)10重量部を攪拌しながら、脱イオン水を60重量部を滴下して、有効固形分濃度30%のシリコン化合物(II−1)の乳化物を得た。
室温にて、縮合度5〜6のテトラエチルシリケート部分加水分解縮合物30重量部とネオコールSW−C(第一工業製薬(株)製:有効成分70%、ジアルキルスルホコハク酸ナトリウム塩)10重量部、ハイテノールXJ−630S(第一工業製薬(株)製:有効成分30%、ポリオキシアルキレンデシルエーテル硫酸エステルナトリウム塩)5重量部を混合し、攪拌しながら、脱イオン水を55重量部を滴下して、有効固形分濃度30%のシリコン化合物(II−2)の乳化物を得た。
室温にて、縮合度5〜6、エチル基/i−プロピル基が8/2 mol/molであるテトラアルコキシシランの部分加水分解縮合物30重量部とポリオキシエチレンラウリル硫酸エステルナトリウム塩5重量部、ポリオキシエチレンノニルフェニルエーテル3重量部を混合し、1000rpm以上で高速攪拌しながら、ゆっくりと脱イオン水を62重量部加えて、有効固形分濃度30%のシリコン化合物(II−3)の乳化物を得た。
アクリル系樹脂エマルジョン(I−1)100重量部に、シリコン化合物の乳化物の製造例1〜3のシリコン化合物(II−1)〜(II−3)の乳化物16.7重量部{(I)の固形分100重量部に対し、(II)のシリコン化合物および/またはその部分加水分解縮合物10重量部}を加え、室温下、攪拌機により30分混合した。この混合物に表1に示す光酸発生剤(III−1)〜(III−5)の溶液、懸濁液または水分散液を添加、混合して水性樹脂組成物A〜Kを得た。
水性樹脂組成物A〜C、Iに表2に示す添加剤を室温、攪拌下で加えクリアー塗料を得た。これらを6ミルのアプリケーターを使用してガラス板上に塗装し、表2に示す露光、養生を行って塗板を作製した。これらの塗板の露光、養生完了時の水接触角(初期)および室温で14日水浸漬し、室内で約6時間乾燥後の水接触角(水浸漬後)の測定を行った。結果を表2に示す。
実施例7、8は、水性樹脂組成物D、Eに表3に示す添加剤を室温、攪拌下で加えクリアー塗料を得た。これらを密閉容器に入れ、直射日光の当たらない条件下で表3に示す貯蔵を行った後、6ミルのアプリケーターを使用してガラス板上に塗装し、表3に示す露光、養生を行って塗板を作製した。比較例3、4は、水性樹脂組成物I、Jに表4に示す成膜助剤を室温、攪拌下で加えてクリアー塗料とし、これらにアルコキシシリル基の加水分解・縮合を促進する化合物である加水分解縮合触媒を加えて混合し、混合後30分後もしくは1日後に塗装を行う、2液形態とした。これらの塗板の露光、養生完了時の水接触角(初期)および室温で7日水浸漬し、室内で約6時間乾燥後の水接触角(水浸漬後)の測定を行った。結果を表3、表4に示す。
水性樹脂組成物F、Kに表5に示す添加剤を室温、攪拌下で加えクリアー塗料を得た。これらを密閉容器に入れ、直射日光の当たらない条件下で表5に示す貯蔵を行った後、6ミルのアプリケーターを使用してガラス板上に塗装し、表5に示す露光、養生を行って塗板を作製した。比較例6は、比較例5のクリアー塗料に室温でアルコキシシリル基の加水分解・縮合を促進する化合物である加水分解縮合触媒を加えて混合、30分後に塗装を行う、2液形態とした。これらの塗板の露光、養生完了時の水接触角(初期)および室温で14日水浸漬し、室内で約6時間乾燥後の水接触角(水浸漬後)の測定を行った。結果を表5に示す。
水性樹脂組成物D、Iに表6に示す顔料ペースト、表7に示す添加剤を室温、攪拌下で加え白エナメル塗料を得た。比較例8は、比較例7の白エナメル塗料に室温でアルコキシシリル基の加水分解・縮合を促進する化合物である加水分解縮合触媒を加えて混合、30分後に塗装を行う、2液形態とした。比較例9は、市販の1液水系アクリル塗料である亜細亜工業(株)製ネオグロスG−80(白)をそのまま用いた。厚さ4mm、幅40mm、長さ150mmのJIS A5430スレート板に関西ペイント(株)製アレスゴムタイルシーラーを室温下エアスプレーで塗装、1日乾燥し、これに白エナメル塗料を室温下、塗装間隔24時間でエアスプレー2回塗装(塗布量合計約0.3Kg/m2)、直射日光の当たらない室内で室温下、7日養生を行って塗板を作製した。これらの塗板を兵庫県高砂市内で南面45°で固定し、屋外暴露を行った。この際の養生完了時の水接触角(初期)および各暴露期間での水接触角、各暴露期間での耐汚染性、養生完了時の光沢の測定を行った。結果を表7に示す。
水性樹脂組成物E、G、H、Jに表6に示す顔料ペースト、表8に示す添加剤を室温、攪拌下で加え白エナメル塗料を得た。比較例11は、比較例10の白エナメル塗料に室温でアルコキシシリル基の加水分解・縮合を促進する化合物である加水分解縮合触媒を加えて混合、30分後に塗装を行う、2液形態とした。厚さ4mm、幅40mm、長さ150mmのJIS A5430スレート板に関西ペイント(株)製アレスゴムタイルシーラーを室温下エアスプレーで塗装、1日乾燥し、これに白エナメル塗料を室温下、塗装間隔24時間でエアスプレー2回塗装(塗布量合計約0.3Kg/m2)、直射日光の当たらない室内で室温下、7日養生を行って塗板を作製した。これらの塗板を兵庫県高砂市内で南面45°で固定し、屋外暴露を行った。
・水接触角
協和界面科学(株)製接触角測定機CA−S150を使用し、純水の接触角を測定した。値が低いほど表面親水性が高く、耐汚染性に優れることを示し、70°以下であれば実際の屋外暴露試験での耐汚染性の効果が顕著となる傾向がある。特に水浸漬後の値は、降雨後の状態を想定しており、この値が低いことは、表面親水性の耐久性、持続性が高く、長期にわたる耐汚染性の効果が顕著となる傾向がある。
・耐汚染性
ミノルタ(株)製測色計CR−300を使用し、暴露開始前と各暴露期間でL*、a*、b*値を測定し、各暴露期間でのL*と暴露開始前のL*から明度差(ΔL)を算出した。値が大きい(0に近い)ほど汚染物質の付着による色相変化が小さく、耐汚染性に優れることを示す。
・光沢
ミノルタ(株)製光沢計Multi−Gloss268を使用し、入射角60°の光沢値を測定した。値が高いほど外観に優れることを示す。
Claims (7)
- (I)下記一般式(3)で示されるアルコキシシリル基含有単量体単位を有するアクリル系樹脂エマルジョン
R 4 R 5 (3-b) Si(OR 6 ) b (3)
(式中、R 4 はγ−(メタ)アクリロキシ基、R 5 は炭素数1〜4のアルキル基、R 6 は炭素数1〜4のアルキル基、bは1〜3を表す。)
(II)下記一般式(2)で示されるテトラアルキルシリケートの部分加水分解縮合物の乳化物
(R 3 O) 4 Si (2)
(式中、R 3 は同じかまたは異なり、炭素数2〜4のアルキル基を表す。)
(III)光酸発生剤
を含有する水性塗料用樹脂組成物を塗布し屋外暴露することによる建築外装塗膜の製造方法。 - 前記(II)のテトラアルキルシリケートの部分加水分解縮合物の乳化物がノニオン系界面活性剤および/またはアニオン系界面活性剤を用いて水性媒体中に分散して得られる乳化物である、請求項1に記載の建築外装塗膜の製造方法。
- さらに(IV)酸により活性化するアルコキシシリル基の加水分解・縮合を促進する化合物を含有する請求項1または2に記載の建築外装塗膜の製造方法。
- (IV)酸により活性化するアルコキシシリル基の加水分解・縮合を促進する化合物が酸性リン酸化合物の塩である請求項3に記載の建築外装塗膜の製造方法。
- (III)光酸発生剤が、有機ハロゲン化合物である請求項1〜4の何れか1項に記載の建築外装塗膜の製造方法。
- (III)光酸発生剤が、ハロゲン含有トリアジン化合物、塩化ビニリデン共重合体、塩化ビニル共重合体、または塩素化ポリオレフィンである請求項1〜4の何れか1項に記載の建築外装塗膜の製造方法。
- 水性塗料用樹脂組成物が一液型水性塗料用樹脂組成物である、請求項1〜6の何れか1項に記載の建築外装塗膜の製造方法。
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