JP4847680B2 - Water-based paint, method for producing the water-based paint, and coating method - Google Patents
Water-based paint, method for producing the water-based paint, and coating method Download PDFInfo
- Publication number
- JP4847680B2 JP4847680B2 JP2004017753A JP2004017753A JP4847680B2 JP 4847680 B2 JP4847680 B2 JP 4847680B2 JP 2004017753 A JP2004017753 A JP 2004017753A JP 2004017753 A JP2004017753 A JP 2004017753A JP 4847680 B2 JP4847680 B2 JP 4847680B2
- Authority
- JP
- Japan
- Prior art keywords
- water
- solvent
- organic solvent
- coating
- paint
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 239000003973 paint Substances 0.000 title claims description 96
- 238000000576 coating method Methods 0.000 title claims description 87
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims description 81
- 238000004519 manufacturing process Methods 0.000 title claims description 27
- 239000011248 coating agent Substances 0.000 claims description 78
- 239000003960 organic solvent Substances 0.000 claims description 60
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 37
- 239000011347 resin Substances 0.000 claims description 28
- 229920005989 resin Polymers 0.000 claims description 28
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 27
- 239000002904 solvent Substances 0.000 claims description 27
- 239000004925 Acrylic resin Substances 0.000 claims description 22
- 229920000178 Acrylic resin Polymers 0.000 claims description 22
- 239000000839 emulsion Substances 0.000 claims description 20
- 239000003085 diluting agent Substances 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 18
- 239000007787 solid Substances 0.000 claims description 15
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 claims description 14
- JDSQBDGCMUXRBM-UHFFFAOYSA-N 2-[2-(2-butoxypropoxy)propoxy]propan-1-ol Chemical compound CCCCOC(C)COC(C)COC(C)CO JDSQBDGCMUXRBM-UHFFFAOYSA-N 0.000 claims description 12
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 12
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 46
- 239000000049 pigment Substances 0.000 description 35
- 238000001035 drying Methods 0.000 description 20
- -1 3-methoxybutyl Chemical group 0.000 description 15
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 15
- 229910052782 aluminium Inorganic materials 0.000 description 14
- 239000003795 chemical substances by application Substances 0.000 description 14
- 239000000178 monomer Substances 0.000 description 14
- 238000003756 stirring Methods 0.000 description 13
- 239000012141 concentrate Substances 0.000 description 11
- 239000000203 mixture Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 8
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 7
- 229910021641 deionized water Inorganic materials 0.000 description 7
- 239000004210 ether based solvent Substances 0.000 description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 6
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 6
- 229920001228 polyisocyanate Polymers 0.000 description 6
- 239000005056 polyisocyanate Substances 0.000 description 6
- UPGSWASWQBLSKZ-UHFFFAOYSA-N 2-hexoxyethanol Chemical compound CCCCCCOCCO UPGSWASWQBLSKZ-UHFFFAOYSA-N 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 5
- 239000000654 additive Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000010422 painting Methods 0.000 description 5
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 4
- BBMCTIGTTCKYKF-UHFFFAOYSA-N 1-heptanol Chemical compound CCCCCCCO BBMCTIGTTCKYKF-UHFFFAOYSA-N 0.000 description 4
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 description 4
- OHJYHAOODFPJOD-UHFFFAOYSA-N 2-(2-ethylhexoxy)ethanol Chemical compound CCCCC(CC)COCCO OHJYHAOODFPJOD-UHFFFAOYSA-N 0.000 description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000004070 electrodeposition Methods 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000002987 primer (paints) Substances 0.000 description 4
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 description 3
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 3
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 3
- 239000008199 coating composition Substances 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229920005749 polyurethane resin Polymers 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 239000002562 thickening agent Substances 0.000 description 3
- 230000002087 whitening effect Effects 0.000 description 3
- RWNUSVWFHDHRCJ-UHFFFAOYSA-N 1-butoxypropan-2-ol Chemical compound CCCCOCC(C)O RWNUSVWFHDHRCJ-UHFFFAOYSA-N 0.000 description 2
- WMDZKDKPYCNCDZ-UHFFFAOYSA-N 2-(2-butoxypropoxy)propan-1-ol Chemical compound CCCCOC(C)COC(C)CO WMDZKDKPYCNCDZ-UHFFFAOYSA-N 0.000 description 2
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 2
- QCAHUFWKIQLBNB-UHFFFAOYSA-N 3-(3-methoxypropoxy)propan-1-ol Chemical compound COCCCOCCCO QCAHUFWKIQLBNB-UHFFFAOYSA-N 0.000 description 2
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 239000004606 Fillers/Extenders Substances 0.000 description 2
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 2
- 229920000877 Melamine resin Polymers 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 2
- NRCMAYZCPIVABH-UHFFFAOYSA-N Quinacridone Chemical compound N1C2=CC=CC=C2C(=O)C2=C1C=C1C(=O)C3=CC=CC=C3NC1=C2 NRCMAYZCPIVABH-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 2
- 230000005856 abnormality Effects 0.000 description 2
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 2
- 239000005456 alcohol based solvent Substances 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- XXROGKLTLUQVRX-UHFFFAOYSA-N allyl alcohol Chemical compound OCC=C XXROGKLTLUQVRX-UHFFFAOYSA-N 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 2
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000002320 enamel (paints) Substances 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 239000004611 light stabiliser Substances 0.000 description 2
- 239000010445 mica Substances 0.000 description 2
- 229910052618 mica group Inorganic materials 0.000 description 2
- 230000003472 neutralizing effect Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 229920001451 polypropylene glycol Polymers 0.000 description 2
- 239000001054 red pigment Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- DTGKSKDOIYIVQL-WEDXCCLWSA-N (+)-borneol Chemical group C1C[C@@]2(C)[C@@H](O)C[C@@H]1C2(C)C DTGKSKDOIYIVQL-WEDXCCLWSA-N 0.000 description 1
- PSGCQDPCAWOCSH-UHFFFAOYSA-N (4,7,7-trimethyl-3-bicyclo[2.2.1]heptanyl) prop-2-enoate Chemical compound C1CC2(C)C(OC(=O)C=C)CC1C2(C)C PSGCQDPCAWOCSH-UHFFFAOYSA-N 0.000 description 1
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- QWOZZTWBWQMEPD-UHFFFAOYSA-N 1-(2-ethoxypropoxy)propan-2-ol Chemical compound CCOC(C)COCC(C)O QWOZZTWBWQMEPD-UHFFFAOYSA-N 0.000 description 1
- DZSVIVLGBJKQAP-UHFFFAOYSA-N 1-(2-methyl-5-propan-2-ylcyclohex-2-en-1-yl)propan-1-one Chemical compound CCC(=O)C1CC(C(C)C)CC=C1C DZSVIVLGBJKQAP-UHFFFAOYSA-N 0.000 description 1
- OSNILPMOSNGHLC-UHFFFAOYSA-N 1-[4-methoxy-3-(piperidin-1-ylmethyl)phenyl]ethanone Chemical compound COC1=CC=C(C(C)=O)C=C1CN1CCCCC1 OSNILPMOSNGHLC-UHFFFAOYSA-N 0.000 description 1
- SDXHBDVTZNMBEW-UHFFFAOYSA-N 1-ethoxy-2-(2-hydroxyethoxy)ethanol Chemical compound CCOC(O)COCCO SDXHBDVTZNMBEW-UHFFFAOYSA-N 0.000 description 1
- PCJTZWIMKYXOAJ-UHFFFAOYSA-N 1-ethoxy-3-(1-hydroxypropan-2-yloxy)propan-2-ol Chemical compound CCOCC(O)COC(C)CO PCJTZWIMKYXOAJ-UHFFFAOYSA-N 0.000 description 1
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- CSCSROFYRUZJJH-UHFFFAOYSA-N 1-methoxyethane-1,2-diol Chemical compound COC(O)CO CSCSROFYRUZJJH-UHFFFAOYSA-N 0.000 description 1
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- CGLVZFOCZLHKOH-UHFFFAOYSA-N 8,18-dichloro-5,15-diethyl-5,15-dihydrodiindolo(3,2-b:3',2'-m)triphenodioxazine Chemical compound CCN1C2=CC=CC=C2C2=C1C=C1OC3=C(Cl)C4=NC(C=C5C6=CC=CC=C6N(C5=C5)CC)=C5OC4=C(Cl)C3=NC1=C2 CGLVZFOCZLHKOH-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
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Landscapes
- Application Of Or Painting With Fluid Materials (AREA)
- Paints Or Removers (AREA)
Description
本発明は、塗装作業性に優れる水性塗料に関するものである。 The present invention relates to a water-based paint excellent in painting workability.
近年、環境保護の観点から、塗料分野においても塗料の水性化が求められている。水は、他の塗料用有機溶剤と比較して、低分子量の割に高い沸点を有し、表面張力及び誘電率が共に高いという特異な性質を有する。これらの要因は、水性塗料の塗装作業性に大きく影響しており、水性塗料は有機溶剤系の塗料と比較して一般に塗装作業性が悪く、得られる塗膜も高光沢となり難いことが知られている。 In recent years, from the viewpoint of environmental protection, water-based paints are also required in the paint field. Compared to other organic solvents for paints, water has a unique property that it has a high boiling point for its low molecular weight and has a high surface tension and dielectric constant. These factors greatly affect the paint workability of water-based paints. Water-based paints are generally poorer in workability than organic solvent-based paints, and it is known that the resulting coatings are not likely to have high gloss. ing.
水性塗料の塗装作業性や形成塗膜の仕上がり性向上の方策として例えば、水性塗料に用いられる塗料用樹脂を改良するなどの方法が一般に行われているが、この方法では、湿度、温度など随時変動する塗装環境の影響による仕上がり性の変動は避けられない。例えば、水性塗料を用いた自動車補修塗装においては、塗装作業性や該塗料の形成塗膜の仕上がり性が補修塗装現場によってまちまちであった。 As measures for improving the workability of water-based paints and the finish of formed coatings, for example, methods such as improving the resin for paints used in water-based paints are generally used. Variations in the finish due to the influence of the changing coating environment are inevitable. For example, in automotive repair coating using water-based paints, the paint workability and the finish of the paint film formed vary depending on the repair paint site.
こうした問題に対して特許文献１には、水性塗料の溶剤として特定の水混和性有機溶剤と水の混合物を含んでいることを特徴とする補修用エマルション型メタリックベース塗料組成物が記載されている。この塗料組成物によれば、塗装作業性が良好であり、乾燥性が速く、塗膜性能に優れた塗膜を形成できるものであるが、該文献に記載の特定の水混和性有機溶剤は、メタノール、エタノールなどの有機溶剤を多量に含有するので塗装時の臭気が強く、また、かかる溶剤が配合されていることにより塗料中のエマルションが凝集する等の問題があった。 In order to solve these problems, Patent Document 1 describes an emulsion-type metallic base coating composition for repair, which contains a mixture of a specific water-miscible organic solvent and water as a solvent for water-based coatings. . According to this coating composition, the coating workability is good, the drying property is fast, and a coating film excellent in coating film performance can be formed. The specific water-miscible organic solvent described in the document is In addition, since it contains a large amount of organic solvents such as methanol and ethanol, it has a strong odor at the time of painting, and the presence of such a solvent causes problems such as aggregation of the emulsion in the paint.
本発明の目的は、塗装作業性が良好であり、塗装環境の影響を受けることなく形成塗膜の仕上がり性が良好となるような水性塗料の製造方法を提供することである。 An object of the present invention is to provide a method for producing a water-based paint that has good coating workability and that has good finish of the formed coating film without being affected by the coating environment.
本発明者らは、特定組成の有機溶剤、特定の樹脂組成を含有する水性塗料の製造方法により上記した目的を達成できることを見出し、本発明に到達した。即ち本発明は
１．（Ａ）ＨＬＢ値が７以上の有機溶剤及び水のみからなる希釈剤（Ｉ）、（Ｂ）ＨＬＢ値が７未満、且つ分子中に水酸基を有する有機溶剤及び（Ｃ）樹脂成分を含有し、該樹脂成分（Ｃ）がウレタンエマルション及び水溶性アクリル樹脂を含有し、ウレタンエマルション及び水溶性アクリル樹脂の配合割合がウレタンエマルション／水溶性アクリル樹脂の固形分比で３０／７０〜９９／１の範囲内であって、有機溶剤（Ｂ）の量が樹脂成分（Ｃ）固形分に対して３〜８０重量％の範囲内である水性塗料濃厚液（II）に、有機溶剤（Ａ）の量が、水及び全有機溶剤の合計に対して３〜５０重量％の範囲内となるように塗装を行う３時間前までの間に配合してなる水性塗料の製造方法。
２．有機溶剤（Ａ）が、プロピレングリコールエーテル系溶剤を含有し、該プロピレングリコールエーテル系溶剤の含有量が、全有機溶剤の合計に対して５〜９０重量％の範囲内である１項に記載の水性塗料の製造方法、
３．有機溶剤（Ａ）がプロピレングリコールモノエーテル系溶剤であり、有機溶剤（Ｂ）がエチレングリコールエーテル系溶剤であり、該プロピレングリコールモノエーテル系溶剤及び該エチレングリコールエーテル系溶剤の配合比がプロピレングリコールモノエーテル系溶剤／エチレングリコールエーテル系溶剤重量比で９９／1〜５０／５０の範囲内にある１項または２項に記載の水性塗料の製造方法、
４． 希釈剤（Ｉ）が、希釈剤（Ｉ）中に有機溶剤（Ａ）を５〜９０重量％含む１項ないし３項のいずれか１項に記載の製造方法、
に関する。
The present inventors have found that the above-described object can be achieved by a method for producing an aqueous paint containing an organic solvent having a specific composition and a specific resin composition, and have reached the present invention. That is, the present invention is 1. (A) having an HLB value of 7 or more organic solvents and diluents consisting only of water (I), contain an organic solvent and (C) a resin component having a (B) less than HLB value of 7 and a hydroxyl group in the molecule, The resin component (C) contains a urethane emulsion and a water-soluble acrylic resin, and the blending ratio of the urethane emulsion and the water-soluble acrylic resin is in the range of 30/70 to 99/1 as a solid content ratio of the urethane emulsion / water-soluble acrylic resin. The amount of the organic solvent (B) is within the range of 3 to 80% by weight based on the solid content of the resin component (C). A method for producing a water-based paint, which is blended up to 3 hours before coating so that the total amount of water and all organic solvents is within a range of 3 to 50% by weight.
2. 2. The organic solvent (A) contains a propylene glycol ether solvent, and the content of the propylene glycol ether solvent is in the range of 5 to 90% by weight with respect to the total of all organic solvents. Manufacturing method of water-based paint,
3. The organic solvent (A) is a propylene glycol monoether solvent, the organic solvent (B) is an ethylene glycol ether solvent, and the mixing ratio of the propylene glycol monoether solvent and the ethylene glycol ether solvent is propylene glycol mono 3. The method for producing a water-based paint according to 1 or 2, wherein the ether solvent / ethylene glycol ether solvent weight ratio is in the range of 99/1 to 50/50.
4). The production method according to any one of items 1 to 3, wherein the diluent (I) contains 5 to 90% by weight of the organic solvent (A) in the diluent (I).
About.
本発明の水性塗料によれば、乾燥性及び被塗面に対するヌレ性が共に優れ、湿度など塗装環境の変化にも対応ができ、仕上がり外観、耐水性、付着性等が良好な塗膜を常温もしくは強制乾燥の条件でも形成することができる。また、高仕上がり外観を得ることが困難とされているメタリック顔料を含有する水性塗料においても、顔料の配向性や緻密感の良好な塗膜を形成することができる。 According to the water-based paint of the present invention, both dryness and wettability on the surface to be coated are excellent, it can cope with changes in the coating environment such as humidity, and a coating film having good finished appearance, water resistance, adhesion, etc. Alternatively, it can be formed under forced drying conditions. In addition, even a water-based paint containing a metallic pigment, which is difficult to obtain a high-finished appearance, can form a coating film with good pigment orientation and denseness.
本発明の水性塗料の製造方法は、（Ａ）ＨＬＢ値が７以上の有機溶剤及び水のみからなる希釈剤（Ｉ）を、（Ｂ）ＨＬＢ値が７未満、且つ分子中に水酸基を有する有機溶剤及び（Ｃ）樹脂成分を含有し、該樹脂成分（Ｃ）がウレタンエマルション及び水溶性アクリル樹脂を含有し、ウレタンエマルション及び水溶性アクリル樹脂の配合割合がウレタンエマルション／水溶性アクリル樹脂の固形分比で３０／７０〜９９／１の範囲内であって、有機溶剤（Ｂ）の量が樹脂成分（Ｃ）固形分に対して３〜８０重量％の範囲内である水性塗料濃厚液（II）に、有機溶剤（Ａ）の量が、水及び全有機溶剤の合計に対して３〜５０重量％の範囲内となるように塗装を行う３時間前までの間に配合してなる。
Organic production method of an aqueous coating composition of the present invention, with (A) having an HLB value of 7 or more organic solvents and diluents consisting only of water (I), (B) less than HLB value of 7 and a hydroxyl group in the molecule It contains a solvent and a resin component (C), the resin component (C) contains a urethane emulsion and a water-soluble acrylic resin, and the blending ratio of the urethane emulsion and the water-soluble acrylic resin is a solid content of the urethane emulsion / water-soluble acrylic resin. Water-based paint concentrate (II) in which the ratio is within the range of 30/70 to 99/1 and the amount of the organic solvent (B) is within the range of 3 to 80% by weight with respect to the solid content of the resin component (C). ) And 3 hours before coating, so that the amount of the organic solvent (A) is in the range of 3 to 50% by weight with respect to the total of water and all organic solvents.
有機溶剤（Ａ）
本発明において、ＨＬＢ値が７以上の有機溶剤（Ａ）は、本発明の水性塗料の乾燥性又は形成塗膜の造膜性を向上させるために含有されるものである。ＨＬＢ値とは、一般に親水・親油のバランスを数値で定量化した値であり、ＨＬＢ値が大きいほど親水性の性質をあらわす。本明細書においてＨＬＢ値は、デーヴィス計算法により得られる値を採用している。デーヴィス計算法によるＨＬＢ値の算出方法は、Ｐｒｏｃ．２ｎｄ Ｉｎｔｅｒｎ．Ｃｏｎｇｒｅｓｓ ｏｆ Ｓｕｒｆａｃｅ Ａｃｔｉｖｉｔｙ，ｖｏｌ．１（１９５７），Ｐ４２６に記載がされている。
Organic solvent (A)
In the present invention, the organic solvent (A) having an HLB value of 7 or more is contained in order to improve the drying property of the aqueous paint of the present invention or the film forming property of the formed coating film. The HLB value is generally a value obtained by quantifying the balance of hydrophilicity / lipophilicity with a numerical value. The larger the HLB value, the more hydrophilic the property. In this specification, the value obtained by the Davis calculation method is adopted as the HLB value. The calculation method of the HLB value by the Davis calculation method is described in Proc. 2nd Intern. Congress of Surface Activity, vol. 1 (1957), P426.
上記ＨＬＢ値が７以上の有機溶剤（Ａ）として具体的には、例えばメタノール、エタノール、イソプロパノール、ｎ−ブタノール、イソブタノール等のアルコール系溶剤；ジオキサン、テトラヒドロフラン等のエーテル系溶剤；エチレングリコールモノメチルエーテル、エチレングリコールモノエチルエーテル、エチレングリコールモノｎ−プロピルエーテル、エチレングリコールモノイソプロピルエーテル、エチレングリコールモノｎ−ブチルエーテル、エチレングリコールモノイソブチルエーテル、エチレングリコールモノｔｅｒｔ−ブチルエーテル、ジエチレングリコールモノメチルエーテル、ジエチレングリコールモノエチルエーテル、ジエチレングリコールモノｎ−プロピルエーテル、ジエチレングリコールモノイソプロピルエーテル、ジエチレングリコールモノｎ−ブチルエーテル、ジエチレングリコールモノイソブチルエーテル、ジエチレングリコールモノｔｅｒｔ−ブチルエーテル等のエチレングリコールエーテル系溶剤；プロピレングリコールモノメチルエーテル、プロピレングリコールモノエチルエーテル、プロピレングリコールモノｎ−プロピルエーテル、プロピレングリコールモノイソプロピルエーテル、ジプロピレングリコールモノメチルエーテル、ジプロピレングリコールモノエチルエーテル、ジプロピレングリコールモノｎ−プロピルエーテル、ジプロピレングリコールモノイソプロピルエーテル等のプロピレングリコールエーテル系溶剤；酢酸エチル、酢酸ブチル、酢酸イソブチル、３−メトキシブチルアセテート等のエステル系溶剤が挙げられ、これらは単独で、又は併用して使用できる。 Specific examples of the organic solvent (A) having an HLB value of 7 or more include alcohol solvents such as methanol, ethanol, isopropanol, n-butanol and isobutanol; ether solvents such as dioxane and tetrahydrofuran; ethylene glycol monomethyl ether , Ethylene glycol monoethyl ether, ethylene glycol mono n-propyl ether, ethylene glycol monoisopropyl ether, ethylene glycol mono n-butyl ether, ethylene glycol monoisobutyl ether, ethylene glycol mono tert-butyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, Diethylene glycol mono n-propyl ether, diethylene glycol monoisopropyl ether Ethylene glycol ether solvents such as diethylene glycol mono n-butyl ether, diethylene glycol monoisobutyl ether, diethylene glycol mono tert-butyl ether; propylene glycol monomethyl ether, propylene glycol monoethyl ether, propylene glycol mono n-propyl ether, propylene glycol monoisopropyl ether , Propylene glycol ether solvents such as dipropylene glycol monomethyl ether, dipropylene glycol monoethyl ether, dipropylene glycol mono n-propyl ether, dipropylene glycol monoisopropyl ether; ethyl acetate, butyl acetate, isobutyl acetate, 3-methoxybutyl And ester solvents such as acetate These alone, or in combination can be used.
本発明の水性塗料において、上記有機溶剤（Ａ）の量は、最終的に得られる水性塗料に含有される水及び全有機溶剤の合計に対して３〜５０重量％であり、好ましくは５〜４５重量％の範囲内であることが望ましい。 In the aqueous paint of the present invention, the amount of the organic solvent (A) is 3 to 50% by weight, preferably 5 to 5%, based on the total amount of water and all organic solvents contained in the finally obtained aqueous paint. It is desirable to be within the range of 45% by weight.
上記ＨＬＢ値が７以上の有機溶剤（Ａ）の量が、３重量％未満では、乾燥性向上に効果がなく、５０重量％以上では、水性塗料の安定性、特に塗料中のエマルションの安定性が低下し、形成塗膜の仕上がり性が低下するので好ましくない。 When the amount of the organic solvent (A) having an HLB value of 7 or more is less than 3% by weight, there is no effect in improving the drying property, and when it is 50% by weight or more, the stability of the aqueous paint, particularly the stability of the emulsion in the paint. Decreases, and the finish of the formed coating film decreases, which is not preferable.
本発明において、上記有機溶剤（Ａ）としては、プロピレングリコールエーテル系溶剤を含有することが望ましい。有機溶剤（Ａ）が、プロピレングリコールエーテル系溶剤を含有することにより、乾燥性を早めることができ、しかも形成塗膜の仕上がり性を向上させることができる。該プロピレングリコールエーテル系溶剤の配合量は、水性塗料に含有される全有機溶剤の合計に対して５〜９０重量％、好ましくは３０〜９０重量％の範囲内であることが望ましい。 In the present invention, the organic solvent (A) preferably contains a propylene glycol ether solvent. When the organic solvent (A) contains a propylene glycol ether solvent, the drying property can be accelerated and the finish of the formed coating film can be improved. The blending amount of the propylene glycol ether solvent is 5 to 90% by weight, preferably 30 to 90% by weight, based on the total of all organic solvents contained in the aqueous coating material.
有機溶剤（Ｂ）
本発明の水性塗料は、ＨＬＢ値が７未満、且つ分子中に水酸基を有する有機溶剤（Ｂ）を含有する。上記有機溶剤（Ｂ）は、塗料表面張力を低下させ、被塗面に対するヌレ性を向上させることができる効果を有する。
Organic solvent (B)
The water-based paint of the present invention contains an organic solvent (B) having an HLB value of less than 7 and having a hydroxyl group in the molecule. The organic solvent (B) has an effect of reducing the coating surface tension and improving the wettability with respect to the coated surface.
上記有機溶剤（Ｂ）としては、例えば、ｎ−ペンチルアルコール、ｎ−ヘキシルアルコール、ｎ−ヘプチルアルコール、シクロヘキシルアルコール、ｎ−オクチルアルコール、ベンジルアルコール等のアルコール系溶剤；エチレングリコールモノヘキシルエーテル、エチレングリコールモノ２−エチルヘキシルエーテル等のエチレングリコールエーテル系溶剤；プロピレングリコールノルマルブチルエーテル、ジプロピレングリコールノルマルブチルエーテル、トリプロピレングリコールｎ−ブチルエーテル等のプロピレングリコールエーテル系溶剤等を挙げることができ、これらは単独で或いは２種以上を選択して使用できる。 Examples of the organic solvent (B) include alcohol solvents such as n-pentyl alcohol, n-hexyl alcohol, n-heptyl alcohol, cyclohexyl alcohol, n-octyl alcohol, benzyl alcohol; ethylene glycol monohexyl ether, ethylene glycol Examples include ethylene glycol ether solvents such as mono 2-ethylhexyl ether; propylene glycol ether solvents such as propylene glycol normal butyl ether, dipropylene glycol normal butyl ether, and tripropylene glycol n-butyl ether. You can select and use more than species.
本発明においては、水性塗料をスプレー塗装した場合などに微粒化が向上するという点から、上記有機溶剤（Ｂ）のＨＬＢ値としては、５以上で且つ７未満であることが特に望ましい。ＨＬＢ値が５以上で且つ７未満である有機溶剤（Ｂ）の具体例としては、ｎ−ヘキシルアルコール、ｎ−ヘプチルアルコール、ｎ−オクチルアルコール、エチレングリコールモノ２−エチルヘキシルエーテル、エチレングリコールモノヘキシルエーテル、プロピレングリコールノルマルブチルエーテル、ジプロピレングリコールノルマルブチルエーテル、トリプロピレングリコールノルマルブチルエーテル等を挙げることができ、これらの中でもエチレングリコールモノヘキシルエーテル及びエチレングリコールモノ２−エチルヘキシルエーテルが好適である。 In the present invention, the HLB value of the organic solvent (B) is particularly preferably 5 or more and less than 7 from the viewpoint that atomization is improved when a water-based paint is spray-coated. Specific examples of the organic solvent (B) having an HLB value of 5 or more and less than 7 include n-hexyl alcohol, n-heptyl alcohol, n-octyl alcohol, ethylene glycol mono-2-ethylhexyl ether, ethylene glycol monohexyl ether. , Propylene glycol normal butyl ether, dipropylene glycol normal butyl ether, tripropylene glycol normal butyl ether, and the like. Among these, ethylene glycol monohexyl ether and ethylene glycol mono 2-ethylhexyl ether are preferable.
上記有機溶剤（Ｂ）は、樹脂成分（Ｂ）固形分に対して３〜８０重量％であり、好ましくは５〜５０重量％の範囲内で含有することが望ましい。３重量％未満では、ヌレ性向上効果が低く、一方８０重量％を超えると、水性塗料の安定性が不十分となり望ましくない。 The organic solvent (B) is 3 to 80% by weight, preferably 5 to 50% by weight, based on the solid content of the resin component (B). If it is less than 3% by weight, the effect of improving the wettability is low. On the other hand, if it exceeds 80% by weight, the stability of the water-based paint is undesirably insufficient.
本発明の水性塗料において、上記有機溶剤（Ａ）及び有機溶剤（Ｂ）の組み合わせにおいて、造膜性、乾燥性及びヌレ性の点から、特に好ましいものは、有機溶剤（Ａ）としては、ＨＬＢ値が７以上のプロピレングリコールエーテル系溶剤、特にプロピレングリコールモノメチルエーテルが挙げられ、有機溶剤（Ｂ）としては、ＨＬＢ値が７未満のエチレングリコールエーテル系溶剤、特にエチレングリコールモノヘキシルエーテル、エチレングリコールモノ２エチルヘキシルエーテルが挙げられる。また、上記ＨＬＢが７以上のプロピレングリコールモノエーテル系溶剤及びＨＬＢが７未満のエチレングリコールモノエーテル系溶剤の配合比としては、上記ＨＬＢが７以上のプロピレングリコールモノエーテル系溶剤及びＨＬＢが７未満のエチレングリコールモノエーテル系溶剤の重量比で、９９／１〜５０／５０、好ましくは９９／１〜８０／２０の範囲内であることが望ましい。 In the water-based paint of the present invention, the combination of the organic solvent (A) and the organic solvent (B) is particularly preferable as the organic solvent (A) from the viewpoint of film forming property, drying property and wettability. Examples include propylene glycol ether solvents having a value of 7 or more, particularly propylene glycol monomethyl ether. As the organic solvent (B), ethylene glycol ether solvents having an HLB value of less than 7, particularly ethylene glycol monohexyl ether, ethylene glycol mono 2 ethyl hexyl ether is mentioned. The blending ratio of the propylene glycol monoether solvent with HLB of 7 or more and the ethylene glycol monoether solvent with HLB of less than 7 is the propylene glycol monoether solvent with HLB of 7 or more and HLB of less than 7. The weight ratio of the ethylene glycol monoether solvent is 99/1 to 50/50, preferably 99/1 to 80/20.
樹脂成分（Ｃ）
本発明の水性塗料に含有される樹脂成分（Ｃ）としては、通常、水性塗料の膜形成成分として使用される樹脂が制限なく使用でき、アクリル樹脂、ウレタン樹脂、アルキド系樹脂、ポリエステル系樹脂、セルロ−ス系樹脂等の水溶性及び／又は水分散性樹脂を挙げることができ、ポリイソシアネート硬化剤、ブロックイソシアネート硬化剤、メラミン硬化剤、オキサゾリン硬化剤、カルボジイミド硬化剤等の硬化剤を包含せしめたものであってもよい。
Resin component (C)
As the resin component (C) contained in the water-based paint of the present invention, resins that are usually used as film-forming components of water-based paints can be used without limitation, and acrylic resins, urethane resins, alkyd resins, polyester resins, Examples include water-soluble and / or water-dispersible resins such as cellulose resins, and include curing agents such as polyisocyanate curing agents, blocked isocyanate curing agents, melamine curing agents, oxazoline curing agents, and carbodiimide curing agents. It may be.
本発明の水性塗料においては、上記有機溶剤（Ｂ）の配合により水性塗料の粘度を適度に上昇させることができ、ヌレ性を向上させる効果が特に顕著であることから、樹脂成分（Ｃ）としてウレタンエマルションを含有することが望ましい。 In the water-based paint of the present invention, the viscosity of the water-based paint can be appropriately increased by blending the organic solvent (B), and the effect of improving the wettability is particularly remarkable. Therefore, as the resin component (C) It is desirable to contain a urethane emulsion.
上記ウレタンエマルションとしては、従来公知のものが制限なく使用でき、例えば、ポリイソシアネ−ト、ポリオ−ル及びヒドロキシ酸とによるイソシアネ−ト基含有プレポリマ−を水及び鎖伸長剤の存在下で反応させることにより得られる平均粒子径が、０．１〜１μｍの範囲内の粒子形態のエマルションを挙げることができる。本明細書において、平均粒子径とは、「ＳＡＬＤ−３１００」（商品名、島津製作所社製、レーザー回折式粒度分布測定装置）にて、試料を脱イオン水で希釈して、常温（２０℃程度）下で測定したピークトップの値とする。 As the urethane emulsion, conventionally known ones can be used without limitation, for example, reacting an isocyanate group-containing prepolymer with polyisocyanate, polyol and hydroxy acid in the presence of water and a chain extender. The emulsion of the particle form in the range whose average particle diameter obtained by 0.1-1 micrometer can be mentioned. In the present specification, the average particle size means “SALD-3100” (trade name, manufactured by Shimadzu Corporation, laser diffraction particle size distribution measuring device), diluted with deionized water at room temperature (20 ° C. About the peak top value measured below.
また、形成塗膜の耐水性、仕上がり性の点から、樹脂成分（Ｃ）として、さらに水溶性アクリル樹脂を含有することが望ましい。かかる水溶性アクリル樹脂としては、例えば、酸基含有重合性不飽和モノマー、水酸基含有重合性不飽和モノマー及びその他の重合性不飽和モノマーを含む重合性不飽和モノマー混合物を、有機溶剤の存在下で重合開始剤により重合させることにより得られるアクリル共重合体を中和剤により中和し、水溶化せしめた樹脂を挙げることができる。 Moreover, it is desirable to contain a water-soluble acrylic resin as the resin component (C) from the viewpoint of the water resistance and finish of the formed coating film. Examples of the water-soluble acrylic resin include a polymerizable unsaturated monomer mixture containing an acid group-containing polymerizable unsaturated monomer, a hydroxyl group-containing polymerizable unsaturated monomer, and other polymerizable unsaturated monomers in the presence of an organic solvent. A resin obtained by neutralizing an acrylic copolymer obtained by polymerization with a polymerization initiator with a neutralizing agent to be water-soluble can be mentioned.
上記酸基含有重合性不飽和モノマーとしては、例えばアクリル酸、メタクリル酸、クロトン酸、マレイン酸、イタコン酸、βーカルボキシエチルアクリレート、２ーアクリルアミドー２ーメチルプロパンスルホン酸、アリルスルホン酸、スチレンスルホン酸ナトリウム塩、スルホエチルメタクリレート及びそのナトリウム塩やアンモニウム塩、「ライトエステルＰＭ」（ライトエステル社製）などのリン酸基含有重合性不飽和モノマーなどが挙げられ、これらは１種又は２種以上併用して用いることができる。このうち（メタ）アクリル酸が好適である。 Examples of the acid group-containing polymerizable unsaturated monomer include acrylic acid, methacrylic acid, crotonic acid, maleic acid, itaconic acid, β-carboxyethyl acrylate, 2-acrylamide-2-methylpropanesulfonic acid, allylsulfonic acid, and styrene. Examples thereof include sulfonic acid sodium salt, sulfoethyl methacrylate and its sodium salt and ammonium salt, and phosphoric acid group-containing polymerizable unsaturated monomers such as “Light Ester PM” (manufactured by Light Ester Co., Ltd.). These can be used in combination. Of these, (meth) acrylic acid is preferred.
水酸基含有重合性不飽和モノマーとしては、２ーヒドロキシエチル（メタ）アクリレート、２ーヒドロキシプロピル（メタ）アクリレート、３−ヒドロキシプロピル（メタ）アクリレート、ヒドロキシブチル（メタ）アクリレートなどの（メタ）アクリル酸の炭素数２〜８個のヒドロキシアルキル（メタ）アクリレート；Ｎーメチロールアクリルアミド、アリルアルコール、εーカプロラクトン変性アクリルモノマーなどが挙げられ、これらは１種又は２種以上併用して用いることができる。 Examples of the hydroxyl group-containing polymerizable unsaturated monomer include (meth) acrylic acid such as 2-hydroxyethyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, 3-hydroxypropyl (meth) acrylate, and hydroxybutyl (meth) acrylate. Of C2-C8 hydroxyalkyl (meth) acrylate; N-methylolacrylamide, allyl alcohol, ε-caprolactone-modified acrylic monomer, and the like. These may be used alone or in combination of two or more.
その他の重合性不飽和モノマーとしては、メチル(メタ)アクリレート、エチル（メタ）アクリレート、ｎ−プロピル(メタ)アクリレート、イソプロピル(メタ)アクリレート、ｎ−ブチル（メタ）アクリレート、イソブチル(メタ)アクリレート、ヘキシル(メタ)アクリレート、２−エチルヘキシル(メタ)アクリレート、ｎ−オクチル(メタ)アクリレート、デシル(メタ)アクリレート、ステアリル(メタ)アクリレート、イソステアリル(メタ)アクリレート、ラウリル（メタ）アクリレート等の直鎖状もしくは分岐状のアルキル（メタ）アクリレート；シクロヘキシル（メタ）アクリレート、ｔ−ブチルシクロヘキシル（メタ）アクリレート、イソボルニル(メタ)アクリレート、アダマンチル(メタ)アクリレート、ビシクロ［３，３，１］ノニル（メタ）アクリレート等の環状の炭化水素基を有するアルキル（メタ）アクリレート等；ジエチレングリコール（メタ）アクリレート、トリエチレングリコール（メタ）アクリレート、ポリエチレングリコール（メタ）アクリレート、ジプロピレングリコール（メタ）アクリレート、トリプロピレングリコール（メタ）アクリレート、ポリプロピレングリコール（メタ）アクリレート、ポリエチレンポリプロピレングリコール（メタ）アクリレート、メトキシエチレングリコール（メタ）アクリレート、エトキシエチレングリコール（メタ）アクリレート、エトキシジエチレングリコール（メタ）アクリレート、エトキシトリエチレングリコール（メタ）アクリレート、エトキシポリエチレングリコール（メタ）アクリレート、プロポキシトリエチレングリコール（メタ）アクリレート、メトキシプロピレングリコール（メタ）アクリレート、エトキシプロピレングリコール（メタ）アクリレート、エトキシジプロピレングリコール（メタ）アクリレート、エトキシトリプロピレングリコール（メタ）アクリレート、エトキシポリプロピレングリコール（メタ）アクリレート、プロポキシトリプロピレングリコール（メタ）アクリレート等のポリオキシアルキレン鎖含有重合性不飽和モノマー；ジメチルアミノエチル(メタ)アクリレート、Ｎ−ブトキシメチルアクリルアミド、Ｎ，Ｎ−ジメチルアクリルアミドなどの含窒素化合物；グリシジル(メタ)アクリレ−トなどのエポキシ基含有（メタ）アクリレート；酢酸ビニル、プロピオン酸ビニル、スチレン、α−メチルスチレン、ビニルトルエン、アクリロニトリル、メタクリロニトリル、ブタジエン、イソプレン等のビニルモノマー等が挙げられ、これらは１種もしくは２種以上用いることができる。 Other polymerizable unsaturated monomers include methyl (meth) acrylate, ethyl (meth) acrylate, n-propyl (meth) acrylate, isopropyl (meth) acrylate, n-butyl (meth) acrylate, isobutyl (meth) acrylate, Straight chain such as hexyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, n-octyl (meth) acrylate, decyl (meth) acrylate, stearyl (meth) acrylate, isostearyl (meth) acrylate, lauryl (meth) acrylate, etc. Or branched alkyl (meth) acrylate; cyclohexyl (meth) acrylate, t-butylcyclohexyl (meth) acrylate, isobornyl (meth) acrylate, adamantyl (meth) acrylate, bicyclo [3,3,1] nonyl (meth) A Alkyl (meth) acrylates having cyclic hydrocarbon groups such as relate; diethylene glycol (meth) acrylate, triethylene glycol (meth) acrylate, polyethylene glycol (meth) acrylate, dipropylene glycol (meth) acrylate, tripropylene glycol ( (Meth) acrylate, polypropylene glycol (meth) acrylate, polyethylene polypropylene glycol (meth) acrylate, methoxyethylene glycol (meth) acrylate, ethoxyethylene glycol (meth) acrylate, ethoxydiethylene glycol (meth) acrylate, ethoxytriethylene glycol (meth) acrylate , Ethoxypolyethylene glycol (meth) acrylate, propoxytriethylene Recall (meth) acrylate, methoxypropylene glycol (meth) acrylate, ethoxypropylene glycol (meth) acrylate, ethoxydipropylene glycol (meth) acrylate, ethoxytripropylene glycol (meth) acrylate, ethoxypolypropylene glycol (meth) acrylate, propoxytri Polyoxyalkylene chain-containing polymerizable unsaturated monomers such as propylene glycol (meth) acrylate; nitrogen-containing compounds such as dimethylaminoethyl (meth) acrylate, N-butoxymethylacrylamide, N, N-dimethylacrylamide; glycidyl (meth) acrylate Epoxy group-containing (meth) acrylates such as vinyl acetate, vinyl acetate, vinyl propionate, styrene, α-methylstyrene, vinyltoluene, Examples thereof include vinyl monomers such as acrylonitrile, methacrylonitrile, butadiene and isoprene, and these can be used alone or in combination of two or more.
本明細書において、（メタ）アクリレートとは、「（メタ）アクリレート」と「アクリレート」の両方を意味するものとする。 In the present specification, (meth) acrylate means both “(meth) acrylate” and “acrylate”.
上記水溶性アクリル樹脂としては、酸価が５〜１００ｍｇＫＯＨ／ｇ、水酸基価が１０〜１５０ｍｇＫＯＨ／ｇ、重量平均分子量が５０００〜１０００００であることが望ましい。本発明において重量平均分子量は、ゲルパーミエーションクロマトグラフィーで測定した値をポリスチレンの重量平均分子量を基準にして換算した値である。 The water-soluble acrylic resin preferably has an acid value of 5 to 100 mgKOH / g, a hydroxyl value of 10 to 150 mgKOH / g, and a weight average molecular weight of 5,000 to 100,000. In the present invention, the weight average molecular weight is a value obtained by converting a value measured by gel permeation chromatography based on the weight average molecular weight of polystyrene.
本発明の水性塗料において、樹脂成分（Ｃ）が、ウレタンエマルション及び水溶性アクリル樹脂を含有することにより、形成塗膜が、耐水性等の十分な塗膜性能を有し、且つ被塗面に対するヌレ性並びに被塗面もしくは後述のトップクリヤー塗料による塗膜に対する付着性を確保することができる。また、ウレタンエマルション及び水溶性アクリル樹脂の配合割合は、ウレタンエマルション／水溶性アクリル樹脂の固形分比で３０／７０〜９９／１、好ましくは５０／５０〜９５／５の範囲内であることが好適である。 In the water-based paint of the present invention, the resin component (C) contains a urethane emulsion and a water-soluble acrylic resin, so that the formed coating film has sufficient coating film performance such as water resistance and is suitable for the coated surface. It is possible to ensure wettability and adhesion to the surface to be coated or a coating film with a top clear paint described later. The blending ratio of the urethane emulsion and the water-soluble acrylic resin is 30/70 to 99/1, preferably 50/50 to 95/5, as a solid content ratio of the urethane emulsion / water-soluble acrylic resin. Is preferred.
水性塗料
本発明の水性塗料としては、顔料を実質的に含有しないクリヤー塗料であっても顔料を含有するエナメル塗料であってもよく、エナメル塗料である場合において、用いられる顔料としては、通常塗料分野で用いられる光輝性顔料、着色顔料、体質顔料等の顔料が特に制限なく使用できる。光輝性顔料として例えば、アルミニウム粉、ブロンズ粉、銅粉、錫粉、鉛粉、亜鉛末、リン化鉄等のメタリック顔料；パール状金属コーティング雲母粉、マイカ状酸化鉄等のパール顔料を挙げることができ、着色顔料としては、酸化チタン等の白色顔料；カーボンブラック、アセチレンブラック、ランプブラック、ボーンブラック、黒鉛、鉄黒、アニリンブラックなどの黒色顔料；黄色酸化鉄、チタンイエロー、モノアゾイエロー、縮合アゾイエロー、アゾメチンイエロー、ビスマスバナデート、ベンズイミダゾロン、イソインドリノン、イソインドリン、キノフタロン、ベンジジンイエロー、パーマネントイエロー等の黄色顔料；パーマネントオレンジ等の橙色顔料；赤色酸化鉄、ナフトールＡＳ系アゾレッド、アンサンスロン、アンスラキノニルレッド、ペリレンマルーン、キナクリドン系赤顔料、ジケトピロロピロール、ウォッチングレッド、パーマネントレッド等の赤色顔料；コバルト紫、キナクリドンバイオレット、ジオキサジンバイオレット等の紫色顔料；コバルトブルー、フタロシアニンブルー、スレンブルーなどの青色顔料；フタロシアニングリーンなどの緑色顔料；等をあげることができ、体質顔料としては、バリタ粉、沈降性硫酸バリウム、炭酸バリウム、炭酸カルシム、石膏、クレー、シリカ、ホワイトカーボン、珪藻土、タルク、炭酸マグネシウム、アルミナホワイト、グロスホワイト、マイカ粉などを挙げることができる。
Water-based paint The water-based paint of the present invention may be a clear paint substantially not containing a pigment or an enamel paint containing a pigment. In the case of an enamel paint, the pigment used is usually a paint. Pigments such as glitter pigments, colored pigments and extender pigments used in the field can be used without particular limitation. Examples of glitter pigments include metallic pigments such as aluminum powder, bronze powder, copper powder, tin powder, lead powder, zinc powder, and iron phosphide; pearl pigments such as pearl-like metal-coated mica powder and mica-like iron oxide Color pigments include white pigments such as titanium oxide; black pigments such as carbon black, acetylene black, lamp black, bone black, graphite, iron black, aniline black; yellow iron oxide, titanium yellow, monoazo yellow, condensation Yellow pigments such as azo yellow, azomethine yellow, bismuth vanadate, benzimidazolone, isoindolinone, isoindoline, quinophthalone, benzidine yellow, permanent yellow; orange pigments such as permanent orange; red iron oxide, naphthol AS azo red, ansan Throne, Anthra Red pigments such as nonyl red, perylene maroon, quinacridone red pigment, diketopyrrolopyrrole, watching red and permanent red; purple pigments such as cobalt purple, quinacridone violet and dioxazine violet; blue such as cobalt blue, phthalocyanine blue and slen blue Examples of extender pigments include barita powder, precipitated barium sulfate, barium carbonate, calcium carbonate, gypsum, clay, silica, white carbon, diatomaceous earth, talc, and magnesium carbonate. , Alumina white, gloss white, mica powder and the like.
上記メタリック顔料の形状は特に限定されないが、例えば燐片状が好適であり、またメタリック顔料は、リン酸基あるいはスルホン酸基を含有する処理剤で分散処理され被覆されていることが水素ガス発生抑制の点から好適である。リン酸基あるいはスルホン酸基含有処理剤には従来公知の低分子化合物や共重合体が特に制限なく適用できる。 The shape of the metallic pigment is not particularly limited. For example, a flake shape is preferable, and the metallic pigment is dispersed and coated with a treatment agent containing a phosphate group or a sulfonate group to generate hydrogen gas. It is preferable from the viewpoint of suppression. Conventionally known low molecular weight compounds and copolymers can be applied to the phosphoric acid group or sulfonic acid group-containing treatment agent without any particular limitation.
本発明の水性塗料は、さらに必要に応じて、紫外線吸収剤、光安定剤、表面調整剤、増粘剤、ポリマー微粒子、分散助剤、塩基性中和剤、防腐剤、シランカップリング剤、増粘剤、消泡剤、硬化触媒、有機溶剤（Ａ）、（Ｂ）以外の有機溶剤など、水性塗料調整の際に通常用いられる塗料用添加剤など他の成分を含んでいてもよい。 The water-based paint of the present invention further contains an ultraviolet absorber, a light stabilizer, a surface conditioner, a thickener, polymer fine particles, a dispersion aid, a basic neutralizer, an antiseptic, a silane coupling agent, if necessary. Other components such as paint additives that are usually used in the preparation of water-based paints, such as thickeners, antifoaming agents, curing catalysts, and organic solvents other than organic solvents (A) and (B) may be included.
本発明の水性塗料の塗料固形分としては、１〜３０重量％、好ましくは３〜２０重量％が望ましく、表面張力としては、３３ｄｙｎｅ／ｃｍ２以下、好ましくは１０〜３０ｄｙｎｅ／ｃｍ２以下であることが望ましい。表面張力が３３ｄｙｎｅ／ｃｍ２を超えると、素地への濡れ性が不十分となり、塗膜外観が低下することがある。 The solid content of the aqueous paint of the present invention is 1 to 30% by weight, preferably 3 to 20% by weight, and the surface tension is 33 dyne / cm 2 or less, preferably 10 to 30 dyne / cm 2 or less. It is desirable. When surface tension exceeds 33 dyne / cm < 2 >, the wettability to a base material becomes inadequate and a coating-film external appearance may fall.
本明細書において、水性塗料の表面張力は、試料の粘度を２０℃に調整し、「ＢＹＫダイノメータ」（商品名、白金リング式液体表面張力測定装置、ＢＹＫ−ＣＨＥＭＩＥ 社製）を使用した値とする。 In this specification, the surface tension of the water-based paint is a value obtained by adjusting the viscosity of the sample to 20 ° C. and using a “BYK dynometer” (trade name, platinum ring liquid surface tension measuring device, manufactured by BYK-CHEMIE). To do.
本発明の水性塗料の製造方法としては、特に限定されるものではないが、例えば、有機溶剤（Ａ）及び水を含む希釈剤（Ｉ）を、上記有機溶剤（Ｂ）及び樹脂成分（Ｃ）を含有する水性塗料濃厚液（II）に、塗装直前に配合する方法等を挙げることができる。該方法により製造することにより、水性塗料濃厚液としては貯蔵安定性が良好であり、水性塗料として塗装直前に希釈されることにより、塗装環境によらず仕上がり性の良好な塗膜を形成でき、好適である。尚、本明細書において、塗装直前とは、例えば、塗装を行う３時間前までの間を挙げることができる。 Although it does not specifically limit as a manufacturing method of the aqueous coating material of this invention, For example, the diluent (I) containing an organic solvent (A) and water, the said organic solvent (B), and resin component (C). And the like. A method of blending into a water-based paint concentrate liquid (II) containing a solution immediately before coating can be exemplified. By producing by this method, as a water-based paint concentrate, the storage stability is good, and as a water-based paint is diluted immediately before painting, a coating film with good finish can be formed regardless of the coating environment, Is preferred. In the present specification, the term “immediately before painting” may include, for example, up to 3 hours before painting.
上記製造方法においては、水及び有機溶剤（Ａ）は、希釈剤（Ｉ）に含有されることが望ましいが、必要に応じて樹脂成分（Ｃ）を製造する際の反応溶媒に使用するなどして、水性塗料濃厚液（II）に一部含有されていてもよい。また、上記水性塗料濃厚液（II）は、塗料固形分が５〜６０重量％、好ましくは１２〜３０重量％の範囲内であることが望ましく、樹脂成分（Ｃ）及び有機溶剤（Ｂ）以外に、上記で例示した顔料、塗料用添加剤など通常水性塗料調整の際にもちいられる成分を含むことができる。 In the above production method, water and the organic solvent (A) are desirably contained in the diluent (I), but may be used as a reaction solvent when producing the resin component (C), if necessary. In addition, it may be partly contained in the aqueous paint concentrate (II). The aqueous paint concentrate (II) preferably has a paint solid content in the range of 5 to 60% by weight, preferably 12 to 30% by weight, except for the resin component (C) and the organic solvent (B). In addition, components such as pigments and paint additives exemplified above, which are usually used when preparing an aqueous paint, can be included.
有機溶剤（Ａ）を希釈剤（Ｉ）に配合する場合において、その配合量としては、希釈剤（Ｉ）中、有機溶剤（Ａ）が、５〜９０重量％の範囲内、好ましくは８〜８５重量％、さらに好ましくは５〜７０重量％の範囲内であることが望ましい。
希釈剤（Ｉ）に含有される有機溶剤（Ａ）としては、水への溶解性、塗膜の乾燥性等の点から、特にプロピレングリコールエーテル系溶剤が好適である。
In the case where the organic solvent (A) is blended with the diluent (I), the blending amount of the organic solvent (A) in the diluent (I) is within the range of 5 to 90% by weight, preferably 8 to It is desirable to be within the range of 85% by weight, more preferably 5 to 70% by weight.
As the organic solvent (A) contained in the diluent (I), a propylene glycol ether solvent is particularly preferable from the viewpoints of solubility in water, drying properties of the coating film, and the like.
また、上記希釈剤（Ｉ）は、上記で例示した水性塗料調整の際に通常用いられる塗料用添加剤など他の成分を含んでいてもよい。 Further, the diluent (I) may contain other components such as paint additives that are usually used in preparing the water-based paint exemplified above.
希釈剤（Ｉ）の配合量としては、塗装環境に応じて適宜調整することができ、例えば、水性塗料濃厚液（II）に対して一般に、３０〜２００重量％、好ましくは４０〜１５０重量％の範囲内とすることができる。 As a compounding quantity of diluent (I), it can adjust suitably according to coating environment, for example, generally 30-200 weight% with respect to water-based paint concentrate (II), Preferably it is 40-150 weight% Can be within the range.
塗装
本発明の塗装方法は、被塗面に上記水性塗料を塗装する塗装方法である。
Coating The coating method of the present invention is a coating method in which the water-based paint is applied to the surface to be coated.
被塗面としては、従来公知の基材面や該基材に設けられた塗膜面を例示することができ、該基材としては、特に制限されるものではないが、例えば、鉄、アルミニウム等の金属；プラスチック；コンクリート、木材等の無機質基材等が挙げられ、また該基材に設けられる塗膜としては特に制限はないが、例えば自動車車体などに設けられている着色ベース塗料によるベース塗膜及びトップクリヤー塗膜から形成されてなる複層塗膜を挙げることができ、該ベース塗膜の下層にプライマー塗膜、電着塗膜、中塗り塗膜等の塗膜が適宜設けられたものであってもよい。 Examples of the surface to be coated include a conventionally known base material surface and a coating surface provided on the base material, and the base material is not particularly limited. Metals such as plastics; inorganic base materials such as concrete and wood, etc., and the coating film provided on the base material is not particularly limited. For example, a base made of a colored base paint provided on an automobile body or the like A multilayer coating film formed from a coating film and a top clear coating film can be mentioned, and a coating film such as a primer coating film, an electrodeposition coating film, and an intermediate coating film is appropriately provided below the base coating film. It may be.
着色ベース塗料によるベース塗膜とは一般に、被塗面に美粧性を与える目的で塗装される着色顔料を含有する塗料により設けられる塗膜を表し、トップクリヤー塗膜とは一般に、透明な塗膜を形成することができる最上層に設けられる塗膜を表す。プライマー塗膜とは一般に、付着性向上等の理由で基材面に直接設けられる塗料を表し、電着塗膜とは一般に、電着塗装に使用される塗料による塗膜を表し、中塗り塗膜とは一般に、プライマー塗膜あるいは電着塗膜のような下塗り塗膜による塗膜とベース塗膜あるいはトップクリヤー塗膜のような上塗り塗膜の間に設けられる塗膜を表す。 A base coating film by a colored base coating generally represents a coating film provided by a coating containing a coloring pigment applied for the purpose of giving cosmetics to the coated surface, and a top clear coating film is generally a transparent coating film. The coating film provided in the uppermost layer which can form is represented. The primer coating generally represents a coating directly provided on the substrate surface for reasons such as improved adhesion, and the electrodeposition coating generally represents a coating with a coating used for electrodeposition coating. The film generally represents a coating film provided between a coating film by an undercoating film such as a primer coating film or an electrodeposition coating film and a top coating film such as a base coating film or a top clear coating film.
塗装手段としては、スプレー塗装、静電塗装、ハケ塗装、ローラー塗装等特に制限はなく、乾燥方法としては、加熱乾燥、強制乾燥、常温乾燥のいずれであってもよい。本明細書では４０℃未満の乾燥条件を常温乾燥とし、４０℃以上で且つ８０℃未満の乾燥条件を強制乾燥とし、８０℃以上の乾燥条件を加熱乾燥とする。 The coating means is not particularly limited, such as spray coating, electrostatic coating, brush coating, or roller coating, and the drying method may be any of heat drying, forced drying, and room temperature drying. In this specification, the drying condition of less than 40 ° C. is room temperature drying, the drying condition of 40 ° C. or more and less than 80 ° C. is forced drying, and the drying condition of 80 ° C. or more is heat drying.
本発明の塗装方法においては、上記水性塗料を塗装した後、該塗面上にトップクリヤー塗料を塗装することができる。 In the coating method of the present invention, after applying the water-based paint, a top clear paint can be applied on the coated surface.
上記水性塗料による塗膜はトップクリヤー塗料を塗装する前に硬化乾燥させてもよいし、該塗膜上にトップクリヤー塗料をウェットオンウェットで塗装し、乾燥することもできる。 The coating film made of the water-based paint may be cured and dried before the top clear paint is applied, or the top clear paint may be applied wet-on-wet on the paint film and dried.
本発明方法に用いられるトップクリヤー塗料としては、従来公知のものが特に制限なく使用でき、例えば水酸基などの架橋性官能基を含有するアクリル樹脂やフッ素樹脂を主剤とし、ブロックポリイソシアネート、ポリイソシアネートやメラミン樹脂などを硬化剤として含有する硬化型塗料、あるいはセルロースアセテートブチレート変性のアクリル樹脂を主成分とするラッカー塗料などが好適に使用でき、さらに必要に応じて顔料類、繊維素誘導体類、添加樹脂、紫外線吸収剤、光安定剤、表面調整剤、硬化触媒などの塗料用添加剤を含有することができる。
このうち水酸基含有アクリル樹脂及びポリイソシアネート硬化剤を含有する塗料を用いた場合、トップクリヤー塗膜から水性塗料により塗膜中にポリイソシアネート硬化剤が一部しみ込んでくるので、水性塗料による塗膜が水酸基を含有する場合は、該水酸基と反応することができ、水性塗料中に硬化剤成分を用いない或いは減量できる上、水性塗料による塗膜とトップクリヤー塗膜間の付着性が向上させることができるので好適である。
As the top clear coating used in the method of the present invention, conventionally known top clear coatings can be used without any particular limitation. For example, acrylic resins or fluororesins containing a crosslinkable functional group such as a hydroxyl group as a main agent, block polyisocyanate, polyisocyanate, A curable paint containing a melamine resin or the like as a curing agent, or a lacquer paint mainly composed of a cellulose acetate butyrate-modified acrylic resin can be suitably used. Furthermore, pigments, fiber derivatives, and additives can be added as necessary. Additives for coating materials such as resins, ultraviolet absorbers, light stabilizers, surface conditioners, and curing catalysts can be contained.
Of these, when a coating containing a hydroxyl group-containing acrylic resin and a polyisocyanate curing agent is used, the polyisocyanate curing agent partially penetrates into the coating from the top clear coating with an aqueous coating. When it contains a hydroxyl group, it can react with the hydroxyl group, the curing agent component can be used in the aqueous paint or the amount can be reduced, and the adhesion between the aqueous paint and the top clear paint can be improved. This is preferable because it is possible.
実施例を記載する。 Examples will be described.
アルミニウム顔料ペーストの調製
製造例１
攪拌混合容器にアルミニウム顔料ペースト「ＭＧ−５１」（旭化成社製、アルミニウム含有量６６％、炭化水素系及び石油系有機溶剤３４％）４５．５部、エチレングリコールモノブチルエーテル３５部（ＨＬＢ値＝７．３３）、リン酸基含有樹脂溶液（注１）３部を添加し、攪拌混合してアルミニウム顔料ペースト（Ｃ１）を得た。
（注１）リン酸基含有樹脂溶液：攪拌器、温度調節器および冷熱器を備えた反応容器にメトキシプロパノール（ＨＬＢ値＝８．２８）２７．５部、イソブタノール２７．５部（ＨＬＢ値＝７．００）の混合溶剤を入れ、１１０℃に加熱し、スチレン２５部、ｎ−ブチルメタクリレート２７．５部、「イソステアリルアクリレート」（大阪有機化学社製、イソステアリルアクリレート）２０部、ヒドロキシブチルアクリレート７．５部、５０％リン酸基含有重合性モノマー（注２）１５部、２−メタクリロイルオキシエチルアシッドホスフェート１２．５部、イソブタノール１０部（ＨＬＢ値＝７．００）、ｔ−ブチルパーオキシオクタノエート４部からなる混合物１２１．５部を４時間で上記の混合溶剤に加え、さらにｔ−ブチルパーオキシオクタノエート０．５部とイソプロパノール２０部（ＨＬＢ値＝７．４８）からなる混合物を１時間で滴下した。その後、１時間攪拌熟成して固形分５０％のリン酸基含有樹脂溶液を得た。
Preparation of aluminum pigment paste Production Example 1
Aluminum pigment paste “MG-51” (Asahi Kasei Co., Ltd., aluminum content 66%, hydrocarbon-based and petroleum-based organic solvent 34%) 45.5 parts, ethylene glycol monobutyl ether 35 parts (HLB value = 7) .33), 3 parts of a phosphoric acid group-containing resin solution (Note 1) was added and mixed by stirring to obtain an aluminum pigment paste (C1).
(Note 1) Phosphate group-containing resin solution: 27.5 parts of methoxypropanol (HLB value = 8.28), 27.5 parts of isobutanol (HLB value) in a reaction vessel equipped with a stirrer, a temperature controller and a refrigerator. = 7.00), heated to 110 ° C., 25 parts of styrene, 27.5 parts of n-butyl methacrylate, 20 parts of “isostearyl acrylate” (produced by Osaka Organic Chemical Co., Ltd.), hydroxy 7.5 parts of butyl acrylate, 15 parts of 50% phosphoric acid group-containing polymerizable monomer (Note 2), 12.5 parts of 2-methacryloyloxyethyl acid phosphate, 10 parts of isobutanol (HLB value = 7.00), t- 121.5 parts of a mixture of 4 parts of butyl peroxyoctanoate is added to the above mixed solvent over 4 hours, and t-butyl peroxy Kutanoeto 0.5 parts of isopropanol 20 parts (HLB value = 7.48) mixture consisting was added dropwise over 1 hour. Thereafter, the mixture was aged and stirred for 1 hour to obtain a phosphate group-containing resin solution having a solid content of 50%.
（注２）リン酸基含有重合性モノマー：攪拌器、温度調節器および冷熱器を備えた反応容器にモノブチルリン酸５７．５部、イソブタノール４１．１（ＨＬＢ値＝７．００）を入れ、空気通気下でグリシジルメタクリレート４２．５部を２時間で滴下した後、さらに１時間攪拌熟成した。その後、イソプロパノール５．９部（ＨＬＢ値＝７．４８）を加えて、固形分５０％のリン酸基含有重合性モノマー溶液を得た。 (Note 2) Phosphoric acid group-containing polymerizable monomer: 57.5 parts of monobutyl phosphoric acid and 41.1 of isobutanol (HLB value = 7.00) are placed in a reaction vessel equipped with a stirrer, a temperature controller and a refrigerator. 42.5 parts of glycidyl methacrylate was added dropwise over 2 hours under air ventilation, and the mixture was further aged and stirred for 1 hour. Thereafter, 5.9 parts of isopropanol (HLB value = 7.48) was added to obtain a phosphate group-containing polymerizable monomer solution having a solid content of 50%.
製造例２
攪拌混合容器にアルミニウム顔料ペースト「ＭＧ−５１」（旭化成社製、金属含有量６６％）４５．５部、エチレングリコールモノヘキシルエーテル３５部（ＨＬＢ値＝６．３８）、リン酸基含有樹脂溶液（注１）３部を添加し、攪拌混合してアルミニウム顔料ペースト（Ｃ２）を得た。
Production Example 2
Aluminum pigment paste “MG-51” (manufactured by Asahi Kasei Co., Ltd., metal content 66%) 45.5 parts, ethylene glycol monohexyl ether 35 parts (HLB value = 6.38), phosphate group-containing resin solution in a stirring and mixing container (Note 1) 3 parts were added and stirred and mixed to obtain an aluminum pigment paste (C2).
製造例３
攪拌混合容器にアルミニウム顔料ペースト「ＭＧ−５１」（旭化成社製、金属含有量６６％）４５．５部、エチレングリコールモノ２−エチルヘキシルエーテル３５部（ＨＬＢ値＝５．１０）、リン酸基含有樹脂溶液（注１）３部を添加し、攪拌混合してアルミニウム顔料ペースト（Ｃ３）を得た。
Production Example 3
45.5 parts of aluminum pigment paste “MG-51” (manufactured by Asahi Kasei Co., Ltd., metal content 66%), 35 parts of ethylene glycol mono-2-ethylhexyl ether (HLB value = 5.10), phosphate group contained in a stirring and mixing container 3 parts of a resin solution (Note 1) was added and mixed by stirring to obtain an aluminum pigment paste (C3).
希釈剤の作成
製造例４
攪拌混合容器に脱イオン水９００部、プロピレングリコールモノメチルエーテル１００部（ＨＬＢ値＝８．２８）を添加し、攪拌混合して希釈剤（Ｉ−１）を得た。
製造例５
攪拌混合容器に脱イオン水９００部、ジプロピレングリコールモノメチルエーテル１００部（ＨＬＢ値＝ ８．１３）を添加し、攪拌混合して希釈剤（Ｉ−２）を得た。
製造例６
攪拌混合容器に脱イオン水２００部、プロピレングリコールモノメチルエーテル８００部（ＨＬＢ値＝８．２８）を添加し、攪拌混合して希釈剤（Ｉ−３）を得た。
Preparation of diluent <Production Example 4>
In a stirring and mixing vessel, 900 parts of deionized water and 100 parts of propylene glycol monomethyl ether (HLB value = 8.28) were added and stirred and mixed to obtain a diluent (I-1).
Production Example 5
To a stirring and mixing vessel, 900 parts of deionized water and 100 parts of dipropylene glycol monomethyl ether (HLB value = 8.13) were added and stirred and mixed to obtain a diluent (I-2).
Production Example 6
200 parts of deionized water and 800 parts of propylene glycol monomethyl ether (HLB value = 8.28) were added to the stirring and mixing vessel, and stirring and mixing were performed to obtain a diluent (I-3).
水性塗料濃厚液の作成
製造例７
アルミニウム顔料ペースト（Ｃ２）８３．５部と水溶性アクリル樹脂溶液（注３）４０部を攪拌混合容器中に加え、１時間攪拌した後、ポリウレタン樹脂エマルション（注４）２６６．７部、「プライマールＡＳＥ６０」（ローム・アンド・ハース社製、増粘剤）１６．７部を添加し、さらに１時間攪拌を続けた。得られた混合物を２−（ジメチルアミノ）エタノールでｐＨ８．０に調整した後、脱イオン水を添加し、固形分２０％の水性塗料濃厚液（II−１）を得た。
Preparation of water-based paint concentrate liquid Production Example 7
83.5 parts of aluminum pigment paste (C2) and 40 parts of a water-soluble acrylic resin solution (Note 3) were added to a stirring and mixing vessel and stirred for 1 hour, and then 266.7 parts of a polyurethane resin emulsion (Note 4), “Primer 16.7 parts of “Lu ASE60” (Rohm and Haas, thickener) was added, and stirring was continued for another hour. The resulting mixture was adjusted to pH 8.0 with 2- (dimethylamino) ethanol, and then deionized water was added to obtain an aqueous paint concentrate (II-1) having a solid content of 20%.
（注３）水溶性アクリル樹脂： 反応容器にエチレングリコールモノブチルエーテル（ＨＬＢ値＝７．３３）５００部を加え、窒素気流中で１１５℃に昇温した。１１５℃に達した後、メチルメタクリレート２００部、ｎ−ブチルアクリレート２００部、イソボルニルアクリレート３００部、スチレン１１０部、ヒドロキシエチルアクリレート５０部、アクリル酸４０部、「ＮＦバイソマーＳ２０Ｗ」（商品名、第一工業製薬社製、分子末端がメトキシ基であり、分子内にＣ２Ｈ４Ｏ基の４５量体を含有するメタクリレート）１００部およびアゾビスイソブチロニトリル１０部の混合物を３時間かけて加え、２時間熟成を行った。反応終了後、ジメチルエタノールアミンで当量中和し、さらにプロピレングリコールモノプロピルエーテル（ＨＬＢ値＝７．３３）を２５０部を加えて、酸価３１ｍｇＫＯＨ／ｇ、水酸基価４０ｍｇＫＯＨ／ｇ、重量平均分子量４５０００、固形分５０％の水溶性アクリル樹脂溶液を得た。 (Note 3) Water-soluble acrylic resin: 500 parts of ethylene glycol monobutyl ether (HLB value = 7.33) was added to the reaction vessel, and the temperature was raised to 115 ° C. in a nitrogen stream. After reaching 115 ° C., 200 parts of methyl methacrylate, 200 parts of n-butyl acrylate, 300 parts of isobornyl acrylate, 110 parts of styrene, 50 parts of hydroxyethyl acrylate, 40 parts of acrylic acid, “NF biisomer S20W” (trade name, Made by Dai-ichi Kogyo Seiyaku Co., Ltd., a mixture of 100 parts of methacrylate having a molecular end of methoxy group and a 45-mer of C 2 H 4 O group in the molecule and 10 parts of azobisisobutyronitrile over 3 hours In addition, aging was performed for 2 hours. After completion of the reaction, the reaction mixture was neutralized with dimethylethanolamine in an equivalent amount, and further 250 parts of propylene glycol monopropyl ether (HLB value = 7.33) was added. A water-soluble acrylic resin solution having a solid content of 50% was obtained.
（注４）ポリウレタン樹脂エマルション：数平均分子量２０００のポリブチレンアジペート１１５．５部、数平均分子量２０００のポリカプロラクトンジオール１１５．５部、ジメチロールプロピオン酸２３．２部、１，４−ブタンジオール６．５部及び１−イソシアナート−３−イソシアナートメチル−３，５，６−トリメチルシクロヘキサン１２０．１部を重合容器に仕込み、撹拌下に窒素気流中で８５℃で７時間反応せしめてＮＣＯ含有量４．０％の末端ＮＣＯプレポリマーを得た。次いで該プレポリマーを５０℃まで冷却し、アセトン１６５部を加え均一に溶解した後、撹拌下にトリエチルアミン１５．７部を加え、５０℃以下に保ちながら脱イオン水６００部を加え、得られた水分散体を５０℃で２時間保持し水伸長反応を完結させた後、減圧下７０℃以下でアセトンを留去し、トリエチルアミンと脱イオン水でｐＨを８．０に調整し固形分３０％のポリウレタン樹脂エマルションを得た。 (Note 4) Polyurethane resin emulsion: 115.5 parts of polybutylene adipate having a number average molecular weight of 2000, 115.5 parts of polycaprolactone diol having a number average molecular weight of 2000, 23.2 parts of dimethylolpropionic acid, 6 of 1,4-butanediol .5 parts and 120.1 parts of 1-isocyanate-3-isocyanatomethyl-3,5,6-trimethylcyclohexane were charged in a polymerization vessel and reacted for 7 hours at 85 ° C. in a nitrogen stream with stirring to contain NCO. An amount of 4.0% terminal NCO prepolymer was obtained. Next, the prepolymer was cooled to 50 ° C., and 165 parts of acetone was added and dissolved uniformly. Then, 15.7 parts of triethylamine was added with stirring, and 600 parts of deionized water was added while maintaining the temperature at 50 ° C. or lower. After maintaining the aqueous dispersion at 50 ° C. for 2 hours to complete the water elongation reaction, acetone was distilled off at 70 ° C. or lower under reduced pressure, and the pH was adjusted to 8.0 with triethylamine and deionized water to obtain a solid content of 30%. A polyurethane resin emulsion was obtained.
製造例８
上記製造例７において、アルミニウム顔料ペースト（Ｃ２）をアルミニウム顔料ペースト（Ｃ３）とする以外は、製造例７と同様にして水性塗料濃厚液（II−２）を得た。
Production Example 8
A water-based paint concentrate (II-2) was obtained in the same manner as in Production Example 7 except that the aluminum pigment paste (C2) was changed to the aluminum pigment paste (C3) in Production Example 7.
製造例９
上記製造例７において、アルミニウム顔料ペースト（Ｃ２）をアルミニウム顔料ペースト（Ｃ１）とする以外は、製造例７と同様にして水性塗料濃厚液（II−３）を得た。
Production Example 9
A water-based paint concentrate (II-3) was obtained in the same manner as in Production Example 7 except that the aluminum pigment paste (C2) was changed to the aluminum pigment paste (C1) in Production Example 7.
水性塗料の製造
実施例１
水性塗料濃厚液（II−１）１００部と希釈剤（Ｉ−１）１５０部を手攪拌によって十分に混合し、水性塗料（III-１）を得た。
Production of water-based paint Example 1
100 parts of aqueous paint concentrate (II-1) and 150 parts of diluent (I-1) were sufficiently mixed by hand stirring to obtain an aqueous paint (III-1).
実施例２〜４及び比較例１〜５
配合組成を下記表１に示す通りとする以外は実施例１と同様にして水性塗料（ＩＩＩ−２）〜（ＩＩＩ−１１）を得た。表１には、各水性塗料の温度を２０℃に調整し、表面張力を「ＢＹＫダイノメータ」（商品名、表面張力測定計、ＢＹＫ−ＣＨＥＭＩＥ 社製）により測定した値を併記した。
Examples 2 to 4 and Comparative Examples 1 to 5
Aqueous paints (III-2) to (III-11) were obtained in the same manner as in Example 1 except that the composition was as shown in Table 1 below. In Table 1, the temperature of each water-based paint was adjusted to 20 ° C., and the surface tension was measured with a “BYK dynometer” (trade name, surface tension meter, manufactured by BYK-CHEMIE).
比較例６
上記水性塗料（III-７）を１週間２５℃の条件で貯蔵し、水性塗料（III−１２）とした。かかる水性塗料（III-１２）は顔料沈降の現象が見られた。表面張力は３０ｄｙｎｅ／ｃｍ２であった。
Comparative Example 6
The aqueous paint (III-7) was stored at 25 ° C. for 1 week to obtain an aqueous paint (III-12). In this water-based paint (III-12), a phenomenon of pigment sedimentation was observed. The surface tension was 30 dyne / cm 2 .
塗装
自動車車体用クリヤー塗料を塗装した工程板を、＃８００耐水ペーパーで研磨、脱脂し、被塗板とした。該被塗面に上記で作成した各水性塗料（III−１）〜（III-１２）を２０℃、６０％ＲＨ雰囲気下でエアスプレー塗装し、６０℃強制乾燥した後、乾燥膜厚が１５μｍの塗膜を得た。その後、「レタンＰＧマルチクリヤーＨＸ（Ｑ）」（商品名、関西ペイント社製、ウレタン硬化系クリヤー塗料）を乾燥膜厚５０μｍとなるようにエアスプレー塗装し、６０℃で２０分間強制乾燥し、各試験塗板を得た。
Coating The process board coated with the clear paint for automobile bodies was polished and degreased with # 800 water-resistant paper to obtain a coated board. Each of the aqueous paints (III-1) to (III-12) prepared above is applied to the surface to be coated by air spraying in an atmosphere of 20 ° C. and 60% RH, and after forced drying at 60 ° C., the dry film thickness is 15 μm. Coating film was obtained. Thereafter, “Letane PG Multi Clear HX (Q)” (trade name, manufactured by Kansai Paint Co., Ltd., urethane-cured clear paint) is air sprayed to a dry film thickness of 50 μm, and forcedly dried at 60 ° C. for 20 minutes. Each test coating was obtained.
評価試験
上記水性塗料、およびそれらを用いて作成した試験塗板に関し、以下の各項目について評価試験を行った。結果を表２に示す。
（＊１）素地濡れ性：スプレー塗装した各水性塗料の被塗板上での外観を目視で評価することにより濡れ性を評価した。
○：良好、△：塗膜欠陥がわずかに見られる、×：不良（ピンホールが見られる）
（＊２）乾燥性：２０℃、６０％ＲＨ条件下において、水性塗料をエアスプレーし、放置して指で触れてタック感がない状態になるまでの時間によって評価した。
○：良好（１時間未満）、△：やや不良（１時間〜３時間未満）、×：不良（３時間以上）
（＊３）塗膜外観 ：各試験板の塗膜面を目視で評価した。
○：アルミ顔料が塗面に対して平行かつ均一に配向し、メタリックムラの発生が全く認められない、△：メタリックムラの発生が少し認められた、×：メタリックムラの発生が多く認められた
（＊４）初期付着性：各試験板状に素地に達するようにカッターで切り込みを入れ、大きさ２ｍｍ×２ｍｍのゴバン目を１００個作り、その表面に粘着テープを貼着し、２０℃においてそのテープを急激に剥離した跡のゴバン目塗膜の残存数を調べた。
○：１００個残存、△：９９〜８１個残存、□：８０〜４１個残存、×：４０個
（＊５）耐水性：各試験塗板を４０℃の温水に１０日間浸漬し、引き上げてから各塗膜表面を観察した
◎：異常なし、○：わずかに白化が見られる、△：白化がみられる、×：フクレ、白化などの異常が見られる
（＊６）耐水付着性：試験塗板を４０℃の温水に１０日間浸漬し、引き上げ、室温で１時間乾燥してから、上記初期付着性と同様にしてゴバン目試験を行った。評価基準も初期付着性と同じである。
Evaluation Test With respect to the above water-based paints and test coating plates prepared using them, evaluation tests were performed on the following items. The results are shown in Table 2.
(* 1) Substrate wettability: The wettability was evaluated by visually evaluating the appearance of each water-based paint that was spray-coated on the coated plate.
○: Good, Δ: Slight coating defects are observed, ×: Poor (pinholes are observed)
(* 2) Drying: Evaluation was made by the time until the water-based paint was sprayed with air under 20 ° C. and 60% RH conditions, and left to touch with a finger until there was no tackiness.
○: Good (less than 1 hour), Δ: Slightly poor (1 hour to less than 3 hours), X: Bad (3 hours or more)
(* 3) Coating film appearance: The coating film surface of each test plate was visually evaluated.
○: The aluminum pigment is oriented in a parallel and uniform manner with respect to the coating surface, and no occurrence of metallic unevenness is observed. Δ: The occurrence of metallic unevenness is observed a little. ×: The occurrence of metallic unevenness is observed. (* 4) Initial adhesion: Cut with a cutter to reach the substrate in each test plate shape, make 100 goby meshes with a size of 2 mm x 2 mm, stick adhesive tape on the surface, and at 20 ° C The remaining number of the goby eye coatings after the tape was abruptly peeled was examined.
○: 100 remaining, Δ: 99-81 remaining, □: 80-41 remaining, ×: 40 (* 5) Water resistance: Each test coating plate was immersed in warm water at 40 ° C. for 10 days and pulled up. Observed surface of each coating film ◎: No abnormality, ○: Slight whitening, △: Whitening is observed, X: Abnormality such as blistering, whitening, etc. are observed (* 6) Water resistance: Test coating plate After dipping in warm water of 40 ° C. for 10 days, lifting and drying at room temperature for 1 hour, a gobang test was performed in the same manner as the above initial adhesion. The evaluation criteria are the same as the initial adhesion.
特に自動車補修塗装の分野における水性塗料として有用である。
It is particularly useful as a water-based paint in the field of automobile repair coating.
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| JP4828225B2 (en) * | 2005-12-28 | 2011-11-30 | 新日本製鐵株式会社 | Manufacturing method of plated steel strip |
| JP4895098B2 (en) * | 2006-03-30 | 2012-03-14 | Ｄｉｃ株式会社 | Method for producing aqueous resin dispersion for metallic paint, method for producing water-based metallic paint, and method for producing water-based metallic paint for plastic substrate |
| DE102007023539A1 (en) * | 2007-05-18 | 2008-11-20 | Basf Coatings Ag | Aqueous, pigmented coating compositions, process for their preparation and their use for the production of multicoat paint systems |
| JP6525559B2 (en) * | 2013-11-29 | 2019-06-05 | 花王株式会社 | Hard surface treatment composition |
| JP2015124360A (en) * | 2013-12-27 | 2015-07-06 | 大日本塗料株式会社 | Far infrared reflective coating material, formation method of coating film, and coated article |
| KR101797373B1 (en) | 2016-07-12 | 2017-11-13 | (주)에코리엔트글로벌 | Two-component type luminescent paint composition comprising acrylic urethane resin and road line marking method |
| WO2020153023A1 (en) * | 2019-01-21 | 2020-07-30 | Dic株式会社 | Aqueous resin composition, film, and moisture-permeable waterproof fabric |
| CN112552772B (en) * | 2020-12-08 | 2022-04-19 | 重庆海联水性涂料有限公司 | Water-based environment-friendly self-spraying paint for repairing commercial vehicle chassis paint film and preparation method thereof |
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