JP2011515502A - 水性塗料組成物及び複層塗膜形成方法 - Google Patents
水性塗料組成物及び複層塗膜形成方法 Download PDFInfo
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- JP2011515502A JP2011515502A JP2010529160A JP2010529160A JP2011515502A JP 2011515502 A JP2011515502 A JP 2011515502A JP 2010529160 A JP2010529160 A JP 2010529160A JP 2010529160 A JP2010529160 A JP 2010529160A JP 2011515502 A JP2011515502 A JP 2011515502A
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- water
- acid
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- polyester resin
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- GLOBUAZSRIOKLN-UHFFFAOYSA-N pentane-1,4-diol Chemical compound CC(O)CCCO GLOBUAZSRIOKLN-UHFFFAOYSA-N 0.000 description 1
- GTCCGKPBSJZVRZ-UHFFFAOYSA-N pentane-2,4-diol Chemical compound CC(O)CC(C)O GTCCGKPBSJZVRZ-UHFFFAOYSA-N 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 125000002080 perylenyl group Chemical group C1(=CC=C2C=CC=C3C4=CC=CC5=CC=CC(C1=C23)=C45)* 0.000 description 1
- CSHWQDPOILHKBI-UHFFFAOYSA-N peryrene Natural products C1=CC(C2=CC=CC=3C2=C2C=CC=3)=C3C2=CC=CC3=C1 CSHWQDPOILHKBI-UHFFFAOYSA-N 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- XVNKRRXASPPECQ-UHFFFAOYSA-N phenyl n-phenylcarbamate Chemical class C=1C=CC=CC=1OC(=O)NC1=CC=CC=C1 XVNKRRXASPPECQ-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
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- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
- 229920001748 polybutylene Polymers 0.000 description 1
- 229920005906 polyester polyol Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000003505 polymerization initiator Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920006389 polyphenyl polymer Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- DJEHXEMURTVAOE-UHFFFAOYSA-M potassium bisulfite Chemical compound [K+].OS([O-])=O DJEHXEMURTVAOE-UHFFFAOYSA-M 0.000 description 1
- 229940099427 potassium bisulfite Drugs 0.000 description 1
- 235000010259 potassium hydrogen sulphite Nutrition 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- XRVCFZPJAHWYTB-UHFFFAOYSA-N prenderol Chemical compound CCC(CC)(CO)CO XRVCFZPJAHWYTB-UHFFFAOYSA-N 0.000 description 1
- 229950006800 prenderol Drugs 0.000 description 1
- 230000003449 preventive 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
- RLJWTAURUFQFJP-UHFFFAOYSA-N propan-2-ol;titanium Chemical compound [Ti].CC(C)O.CC(C)O.CC(C)O.CC(C)O RLJWTAURUFQFJP-UHFFFAOYSA-N 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- NHARPDSAXCBDDR-UHFFFAOYSA-N propyl 2-methylprop-2-enoate Chemical compound CCCOC(=O)C(C)=C NHARPDSAXCBDDR-UHFFFAOYSA-N 0.000 description 1
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- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
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- XWGJFPHUCFXLBL-UHFFFAOYSA-M rongalite Chemical compound [Na+].OCS([O-])=O XWGJFPHUCFXLBL-UHFFFAOYSA-M 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 239000008159 sesame oil Substances 0.000 description 1
- 235000011803 sesame oil Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 1
- 235000019345 sodium thiosulphate Nutrition 0.000 description 1
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- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 238000001370 static light scattering Methods 0.000 description 1
- KZNICNPSHKQLFF-UHFFFAOYSA-N succinimide Chemical compound O=C1CCC(=O)N1 KZNICNPSHKQLFF-UHFFFAOYSA-N 0.000 description 1
- 229960002317 succinimide Drugs 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 1
- WMXCDAVJEZZYLT-UHFFFAOYSA-N tert-butylthiol Chemical compound CC(C)(C)S WMXCDAVJEZZYLT-UHFFFAOYSA-N 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- VXUYXOFXAQZZMF-UHFFFAOYSA-N tetraisopropyl titanate Substances CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 1
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 150000003606 tin compounds Chemical class 0.000 description 1
- 235000010215 titanium dioxide Nutrition 0.000 description 1
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 1
- RUELTTOHQODFPA-UHFFFAOYSA-N toluene 2,6-diisocyanate Chemical compound CC1=C(N=C=O)C=CC=C1N=C=O RUELTTOHQODFPA-UHFFFAOYSA-N 0.000 description 1
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 1
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 1
- 150000003918 triazines Chemical class 0.000 description 1
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- QXJQHYBHAIHNGG-UHFFFAOYSA-N trimethylolethane Chemical compound OCC(C)(CO)CO QXJQHYBHAIHNGG-UHFFFAOYSA-N 0.000 description 1
- 239000002383 tung oil Substances 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- AVWRKZWQTYIKIY-UHFFFAOYSA-N urea-1-carboxylic acid Chemical compound NC(=O)NC(O)=O AVWRKZWQTYIKIY-UHFFFAOYSA-N 0.000 description 1
- 150000003672 ureas Chemical class 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
- 150000003739 xylenols Chemical class 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
- 229960000314 zinc acetate Drugs 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- 235000014692 zinc oxide Nutrition 0.000 description 1
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- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
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- C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
- C09D167/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C08L33/04—Homopolymers or copolymers of esters
- C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
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- C—CHEMISTRY; METALLURGY
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- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
Description
る。しかしながら、該水性中塗り塗料によって得られる塗膜は、十分な鮮映性を得られない場合がある。
ポリエステル樹脂(A)が、酸成分とアルコール成分の反応によって得られ且つ該酸成分中の脂環族多価カルボン酸(酸無水物を含む)(a−1)の含有量が、該酸成分の合計量を基準として少なくとも30モル%である、水酸基価100〜200mgKOH/g及び酸価10〜35mgKOH/gのポリエステル樹脂であり、
重合体粒子(B)が、重量平均分子量が少なくとも110万であり且つ1,4−ジオキサン溶媒中の質量濃度が1.35%の分散液の状態での分光光度計による波長330nmにおける吸光度の値が0.2以下である
ことを特徴とする水性塗料組成物を提供するものである。
本発明の水性塗料組成物において用いられるポリエステル樹脂(A)は、酸成分とアルコール成分の反応によって得られ且つ該酸成分中の脂環族多価カルボン酸(酸無水物を含む)(a−1)の含有量が、該酸成分の合計量を基準として、少なくとも30モル%、好ましくは35〜100モル%、さらに好ましくは40〜90モル%の範囲内にある、水酸基価100〜200mgKOH/g及び酸価10〜35mgKOH/gのポリエステル樹脂である。
ングリコール、ジエチレングリコール、トリメチレングリコール、トリエチレングリコール、テトラエチレングリコール、ジプロピレングリコール、1,4−ブタンジオール、1,3−ブタンジオール、2,3−ブタンジオール、1,2−ブタンジオール、3−メチル−1,2−ブタンジオール、2,2−ジエチル−1,3−プロパンジオール、2−ブチル−2−エチル−1,3−プロパンジオール、1,2−ペンタンジオール、1,5−ペンタンジオール、1,4−ペンタンジオール、2,4−ペンタンジオール、2,3−ジメチルトリメチレングリコール、テトラメチレングリコール、3−メチル−4,3−ペンタンジオール、3−メチル−1,5−ペンタンジオール、2,2,4−トリメチル−1,3−ペンタンジオール、1,6−ヘキサンジオール、1,5−ヘキサンジオール、1,4−ヘキサンジオール、2,5−ヘキサンジオール、ネオペンチルグリコール、ヒドロキシピバリン酸ネオペンチルグリコールエステルなどの2価アルコール;これらの2価アルコールにε−カプロラクトンなどのラクトン類を付加したポリラクトンジオール;ビス(ヒドロキシエチル)テレフタレートなどのエステルジオール類;ビスフェノールAのアルキレンオキサイド付加物、ポリエチレングリコール、ポリプロピレングリコール、ポリブチレングリコールなどのポリエーテルジオール類;グリセリン、トリメチロールプロパン、トリメチロールエタン、ジグリセリン、トリグリセリン、1,2,6−ヘキサントリオール、ペンタエリスリトール、ジペンタエリスリトール、ソルビトール、マンニトールなどの3価以上のアルコール;これらの3価以上のアルコールにε−カプロラクトンなどのラクトン類を付加させたポリラクトンポリオール類;1,3−シクロヘキサンジメタノール、1,4−シクロヘキサンジメタノール、トリシクロデカンジメタノール、水添ビスフェノールA、水添ビスフェノールF等の脂環族多価アルコールなどが挙げられる。
ール又はポリエーテルポリオール等を挙げることができる。
Specialty Chemicals社製、合成高分岐飽和脂肪酸のグリシジルエステル)などが挙げられる。
本塗料において用いられる水分散性アクリル重合体粒子(B)は、重量平均分子量が少なくとも110万であり且つ1,4−ジオキサン溶媒中の質量濃度が1.35%の分散液の状態での分光光度計による波長330nmにおける吸光度の値が0.2以下である水分散性アクリル重合体粒子である。
クリレート、3−ヒドロキシプロピルメタクリレート、4−ヒドロキシブチルメタクリレート等の水酸基含有メタクリレートモノマー;N−メチロールアクリルアミド、N−メチロールメタクリルアミド等を挙げることができる。
(1) アクリル酸又はメタクリル酸と炭素数1〜20の1価アルコールとのモノエステル化物:例えば、メチルアクリレート、メチルメタクリレート、エチルアクリレート、エチルメタクリレート、プロピルアクリレート、プロピルメタクリレート、ブチルアクリレート、ブチルメタクリレート、2−エチルヘキシルアクリレート、2−エチルヘキシルメタクリレート、シクロヘキシルアクリレート、シクロヘキシルメタクリレート、ラウリルアクリレート、ラウリルメタクリレート、ステアリルアクリレート、ステアリルメタクリレート等。
(2) 芳香族系ビニルモノマー:例えば、スチレン、α−メチルスチレン、ビニルトルエン等。
(3) グリシジル基含有ビニルモノマー:1分子中に少なくとも1個のグリシジル基と1個の重合性不飽和結合とを有する化合物、具体的には、例えば、グリシジルアクリレート、グリシジルメタクリレート等。
(4) 含窒素C1〜20アルキル(メタ)アクリレート:例えばジメチルアミノエチルアクリレート、ジメチルアミノエチルメタクリレート等。
(5) 重合性不飽和基含有アミド系化合物:1分子中に少なくとも1個のアミド基と1個の重合性不飽和結合とを有する化合物、例えば、アクリルアミド、メタクリルアミド、ジメチルアクリルアミド、N,N−ジメチルプロピルアクリルアミド、N−ブトキシメチルアクリルアミド、ジアセトンアクリルアミド等。
(6) 重合性不飽和基含有ニトリル系化合物:例えば、アクリロニトリル、メタクリロニトリル等。
(7) ジエン系化合物:例えばブタジエン、イソプレン等。
(8) ビニル化合物:例えば酢酸ビニル、プロピオン酸ビニル、塩化ビニル等。
ポリオキシエチレン基及び重合性不飽和基を有する反応性乳化剤が特に好ましい。かかる反応性乳化剤の具体例としては、アデカリアソープER−30、アデカリアソープER−40(以上、旭電化社製、商品名)、ラテムルPD−450(花王社製、商品名)等を挙げることができる。
る。
EC−MALLS法により重量平均分子量の測定を行なうことにより得られるものである。
Kc/R(θ)=1/MwP(θ)+2A2c+・・・ (1)
R(θ)=角度θにおける散乱光(レイリー係数)の還元強度
c=サンプル濃度
Mw=重量平均分子量
A2=第2ビリアル係数
K=光学パラメーター
P(θ)=角度散乱関数
が用いられるが、本発明における重量平均分子量は、サイズ排除クロマトグラフに多角度光散乱検出器を接続したSEC−MALLS法と同様、上記式(1)において、第2ビリアル係数とサンプル濃度との積である第2項以降を無視した式から求めた値である。
硬化剤(C)は、特に制限されるものではないが、例えば、以下に挙げるメラミン樹脂、ブロック化ポリイソシアネート化合物を好適に用いることができる。硬化剤は、それぞれ単独で用いてもよく、また、2種以上併用してもよい。
ロール基を平均少なくとも3個有するメラミン樹脂;重量平均分子量が500〜1000程度の親水性イミノ基含有アルキルエーテル化メラミン樹脂等を好適に使用することができる。
トメチル)−ビシクロ(2.2.1)ヘプタン、5−(2−イソシアナトエチル)−2−イソシアナトメチル−3−(3−イソシアナトプロピル)−ビシクロ(2.2.1)ヘプタン、6−(2−イソシアナトエチル)−2−イソシアナトメチル−3−(3−イソシアナトプロピル)−ビシクロ(2.2.1)ヘプタン、5−(2−イソシアナトエチル)−2−イソシアナトメチル−2−(3−イソシアナトプロピル)−ビシクロ(2.2.1)−ヘプタン、6−(2−イソシアナトエチル)−2−イソシアナトメチル−2−(3−イソシアナトプロピル)−ビシクロ(2.2.1)ヘプタン等の脂環族トリイソシアネート等を挙げることができる。
キシム、ベンゾフェノンオキシム、シクロヘキサンオキシム等のオキシム系化合物;マロン酸ジメチル、マロン酸ジエチル、アセト酢酸エチル、アセト酢酸メチル、アセチルアセトン等の活性メチレン系化合物;ブチルメルカプタン、t−ブチルメルカプタン、ヘキシルメルカプタン、t−ドデシルメルカプタン、2−メルカプトベンゾチアゾール、チオフェノール、メチルチオフェノール、エチルチオフェノール等のメルカプタン系化合物;アセトアニリド、アセトアニシジド、アセトトルイド、アクリルアミド、メタクリルアミド、酢酸アミド、ステアリン酸アミド、ベンズアミド等の酸アミド系化合物;コハク酸イミド、フタル酸イミド、マレイン酸イミド等のイミド系化合物;ジフェニルアミン、フェニルナフチルアミン、キシリジン、N−フェニルキシリジン、カルバゾール、アニリン、ナフチルアミン、ブチルアミン、ジブチルアミン、ブチルフェニルアミン等アミン系化合物;イミダゾール、2−エチルイミダゾール等のイミダゾール系化合物;3,5−ジメチルピラゾール等のピラゾール系;尿素、チオ尿素、エチレン尿素、エチレンチオ尿素、ジフェニル尿素等の尿素系化合物;N−フェニルカルバミン酸フェニル等のカルバミン酸エステル系化合物;エチレンイミン、プロピレンイミン等のイミン系化合物;重亜硫酸ソーダ、重亜硫酸カリ等の亜硫酸塩系化合物等のブロック剤を挙げることができる。
本発明の水性塗料組成物中のポリエステル樹脂(A)、水分散性アクリル重合体粒子(B)、及び硬化剤(C)の含有量は、(A)成分、(B)成分及び(C)成分の合計固形分を基準として、不揮発分として、ポリエステル樹脂(A)は一般に1〜90質量%、好ましくは3〜80質量%、さらに好ましくは5〜70質量%の範囲内;水分散性アクリル重合体粒子(B)は一般に1〜80質量%、好ましくは3〜70質量%、さらに好ましくは5〜60質量%の範囲内;硬化剤(C)は一般に5〜60質量%、好ましくは7.5〜50質量%、さらに好ましくは10〜40質量%の範囲内であることができる。
に使用することができる。
本発明によれば、被塗物に、中塗塗料及び上塗塗料を順次塗装することからなる複層塗膜形成方法において、中塗塗料として、上記の水性塗料組成物を塗装することを特徴とする複層塗膜形成方法が提供される。
酢酸、ヒドロキシル酢酸、プロピオン酸、酪酸、乳酸、グリシン等の有機酸;硫酸、塩酸、リン酸等の無機酸を使用することができる。これらの中和剤の配合量は、上記樹脂のアミン価(通常、約30〜約200mgKOH/gの範囲内にある)に対する中和当量が約0.1〜約1の範囲内となるようにするのが適当である。
とする複層塗膜形成方法は、具体的には、例えば、中塗塗料として、本発明の塗料組成物を硬化塗膜として約10〜約50μm、好ましくは約20〜約40μmの膜厚となるように塗装し、必要に応じて約50〜約80℃の温度で3〜10分間程度のプレヒートを行なった後、その未硬化の塗面上に、水性ベースコート塗料を硬化膜厚として約10〜約30μm、好ましくは約10〜約20μmの膜厚となるように塗装し、必要に応じて約50〜約80℃の温度で3〜10分間程度のプレヒートを行なった後、さらにその未硬化の塗面上に、クリヤコート塗料を硬化膜厚として約20〜約60μm、好ましくは約30〜約50μmの膜厚となるように塗装し、必要に応じて約50〜約80℃の温度で3〜10分間程度のプレヒートを行なった後、約100〜約160℃の温度で10〜40分間加熱して、この3層の塗膜を同時に硬化させることにより行なうことができる。
製造例1〜18
加熱装置、攪拌装置、温度計、還流冷却器及び精留塔を備えた4つ口フラスコに、下記表1に示すモル比の酸成分及びアルコール成分を仕込み、160℃まで昇温させた後、160℃から230℃まで3時間かけて生成する縮合水を精留塔を用いて溜去しながら昇温させ、その後230℃で2時間反応させた。
製造例19
温度計、サーモスタット、撹拌器、還流冷却器及び滴下装置を備えた反応容器に、脱イオン水82部、アデカリアソープSR−1025(注1)1.0部を仕込み、窒素気流中で撹拌混合し、75℃に昇温した。次いで下記のモノマーと開始剤の乳化物(注2)全量
のうちの3%量及び0.5%過硫酸アンモニウム水溶液10部とを反応容器内に導入し75℃で2時間保持した。その後、残りのモノマーと開始剤の乳化物を5時間かけて反応容器内に滴下し、滴下終了後6時間熟成を行なった。その後、30℃まで冷却し、5.0%ジメチルエタノールアミン水溶液と脱イオン水を用いて固形分40%、pH6.8となるように調整した。ついで、200メッシュのナイロンクロスで濾過しながら排出し、平均粒子径140nm(サブミクロン粒度分布測定装置「COULTER N4型」(ベックマン・コールター社製)を用いて、脱イオン水で希釈し20℃で測定した。)、酸価11mgKOH/g、水酸基価24mgKOH/gの水分散性アクリル重合体粒子1(固形分40%)を得た。
モノマーと開始剤の乳化物を下記表2に示す配合とする以外、製造例19と同様にして処理して、水分散性アクリル重合体粒子2〜5を得た。なお、製造例21〜23においては、開始剤として、上記(注2)中の2,2′−アゾビス〔2−(2−イミダゾリン−2−イル)プロパン〕にかえて、過硫酸アンモニウムを使用した。
製造例24
加熱装置、攪拌装置、温度計、還流冷却器及び精留塔を備えた4つ口フラスコに、カージュラE10P(ジャパンエポキシレジン社製、商品名、ネオデカン酸モノグリシジルエステル)274部、トリメチロールプロパン382部、無水フタル酸650部、アジピン酸350部及び1,6−ヘキサンジオール486部を仕込み、160℃に昇温後、生成する縮合水を精留塔を用いて溜去しながら、160から230℃まで3時間かけて昇温した。その後230℃で2時間反応させた後、精留塔を水分離器に付け替え、トルエンを適宜加え、230℃で還流状態を保持し、縮合水を水分離器で分離、溜去しながら樹脂酸価が2以下となるまで縮合反応させた。次いで減圧下でトルエンを溜去し、170℃まで冷却した。その後、無水トリメリット酸127.4部を加え、170℃で30分付加反応させた後、プロピレングリコールモノプロピルエーテルを反応生成物に対して10質量%加え、温度を85℃とした後、N,N−ジメチルエタノールアミンで中和し、さらに脱イオン水を徐々に添加して水分散体とすることにより、固形分40%の顔料分散ペースト用樹脂1を得た。
実施例1
製造例24で得た顔料分散ペースト用樹脂1 37.5部に、カーボンMA100(カーボンブラック、三菱化学社製)1部、JR806(チタン白、テイカ社製)70部及びMICRO ACE S−3(日本タルク社製、商品名、微粉タルク)10部を順次加え
ながら混合し、ペイントシェーカーで30分間分散し、顔料分散ペースト1を得た。
50部、及びサイメル250(三井サイテック社製、商品名、メトキシ・ブトキシ混合アルキル化メラミン樹脂、固形分70%)35.7部を加えて混合攪拌し、さらに、脱イオン水、ジメチルエタノールアミンを加えて、pH8.5、フォードカップNo.4で20℃にて、40秒の粘度に調整して水性塗料組成物1を得た。
下記表3に示す配合で、実施例1と同様にして混合攪拌を行なうことにより、水性塗料組成物2〜24を得た。
◎:粘度変化、沈降物及び相分離が認められず良好。
○:若干の粘度変化は認められるが、沈降物及び相分離は認められない。
△:沈降物が認められるが、相分離は認められない。
×:沈降物が認められ、相分離している。
実施例1〜14及び比較例1〜10で得られた水性塗料組成物1〜24を使用して、それぞれについて以下のようにして試験板を作製した。
◎:キズの大きさは小さく、水性中塗塗料(本塗料組成物)の塗膜が少し露出している
。
○:キズの大きさは小さく、水性中塗塗料の塗膜と一部電着塗膜が少し露出しているが
、素地は露出していない。
△:キズの大きさは小さいが、電着塗膜面や素地の鋼板が少し露出している。
×:キズの大きさはかなり大きく、素地の鋼板も大きく露出している。
○:ツヤ感が良好、
△:ツヤ感が劣るが、塗面に濁りは認められない、
×:ツヤ感が劣り、塗面が白く濁っている
実施例15及び比較例11〜13
実施例4、比較例1、2及び7で得られた水性塗料組成物4、15、16及び21については、さらに、それぞれについて以下のようにして試験板を作製した。
法は試験板の作製1で示した方法と同じである。
Claims (14)
- ポリエステル樹脂(A)、水分散性アクリル重合体粒子(B)及び硬化剤(C)を含有する水性塗料組成物であって、
ポリエステル樹脂(A)が、酸成分とアルコール成分の反応によって得られ且つ該酸成分中の脂環族多価カルボン酸(酸無水物を含む)(a−1)の含有量が、該酸成分の合計量を基準として少なくとも30モル%である、水酸基価100〜200mgKOH/g及び酸価10〜35mgKOH/gのポリエステル樹脂であり、
重合体粒子(B)が、重量平均分子量が少なくとも110万であり且つ1,4−ジオキサン溶媒中の質量濃度が1.35%の分散液の状態での分光光度計による波長330nmにおける吸光度の値が0.2以下である
ことを特徴とする水性塗料組成物。 - ポリエステル樹脂(A)が120〜180mgKOH/gの範囲内の水酸基価及び12〜30mgKOH/gの範囲内の酸価を有するものである請求項1に記載の水性塗料組成物
- ポリエステル樹脂(A)が、アルコール成分として、分岐アルキレン基を有する炭素原子数が少なくとも5のジオール(a−2)を含んでなり、且つ該アルコール成分中の(a−2)の含有量が、該アルコール成分の合計量を基準として少なくとも40モル%である請求項1に記載の水性塗料組成物。
- ポリエステル樹脂(A)が、アルコール成分として、水酸基を少なくとも2個有するヒドロキシ酸(a−3)を含んでなり、且つ該アルコール成分中の(a−3)の含有量が、該アルコール成分の合計量を基準として1〜20モル%の範囲内である請求項1に記載の水性塗料組成物。
- ポリエステル樹脂(A)が300〜50000の範囲内の数平均分子量を有するものである請求項1に記載の水性塗料組成物。
- 水分散性アクリル重合体粒子(B)が110万〜1000万の範囲内の重量平均分子量を有するものである請求項1に記載の水性塗料組成物。
- 重合体粒子(B)の1,4−ジオキサン溶媒中の質量濃度が1.35%の分散液の状態での分光光度計による波長330nmにおける吸光度の値が0.15以下である請求項1に記載の水性塗料組成物。
- 水分散性アクリル重合体粒子(B)が、重合性不飽和モノマーを、1分子中に−(CH2CH2O)n−(ここで、nは5〜60の整数である)で表わされるポリオキシエチレン基及び重合性不飽和基を有する反応性乳化剤の存在下に共重合することにより得られるものである請求項1に記載の水性塗料組成物。
- 水分散性アクリル重合体粒子(B)が0〜150mgKOH/gの範囲内の水酸基価及び0.1〜100mgKOH/gの範囲内の酸価を有するものである請求項1に記載の水性塗料組成物。
- 硬化剤(C)がメラミン樹脂及びブロック化ポリイソシアネート化合物よりなる群から選ばれるものである請求項1に記載の水性塗料組成物。
- (A)成分、(B)成分及び(C)成分の合計樹脂固形分を基準にして、不揮発分とし
て、ポリエステル樹脂(A)を1〜90質量%、水分散性アクリル重合体粒子(B)を1〜80質量%、硬化剤(C)を5〜60質量%の範囲内で含有する請求項1に記載の水性塗料組成物。 - 被塗物に、中塗塗料及び上塗塗料を順次塗装する複層塗膜形成方法において、中塗塗料として、請求項1〜11のいずれかに記載の水性塗料組成物を用いることを特徴とする複層塗膜形成方法。
- 被塗物に、請求項1〜11のいずれかに記載の水性塗料組成物を中塗塗料として塗装し、その未硬化の塗面上に水性ベースコート塗料を塗装し、さらにその未硬化の塗面上にクリヤコート塗料を塗装して、中塗、ベースコート及びクリヤコートの3層の塗膜を同時に硬化させることを特徴とする複層塗膜形成方法。
- 請求項1〜11のいずれかに記載の水性塗料組成物が塗装された、或いは
請求項12又は13に記載の複層塗膜形成方法により塗装された物品。
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JP2012224731A (ja) * | 2011-04-19 | 2012-11-15 | Honda Motor Co Ltd | 水性中塗り塗料組成物 |
JP2015105297A (ja) * | 2013-11-29 | 2015-06-08 | 関西ペイント株式会社 | 塗料組成物及び塗装物品 |
Also Published As
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GB201013781D0 (en) | 2010-09-29 |
GB2470505A (en) | 2010-11-24 |
CN101978007B (zh) | 2014-07-23 |
JP5661464B2 (ja) | 2015-01-28 |
US8404776B2 (en) | 2013-03-26 |
GB2470505B (en) | 2012-10-24 |
US20100323211A1 (en) | 2010-12-23 |
WO2009116454A1 (en) | 2009-09-24 |
CN101978007A (zh) | 2011-02-16 |
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