JP5511675B2 - 複層塗膜形成方法 - Google Patents
複層塗膜形成方法 Download PDFInfo
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- JP5511675B2 JP5511675B2 JP2010534832A JP2010534832A JP5511675B2 JP 5511675 B2 JP5511675 B2 JP 5511675B2 JP 2010534832 A JP2010534832 A JP 2010534832A JP 2010534832 A JP2010534832 A JP 2010534832A JP 5511675 B2 JP5511675 B2 JP 5511675B2
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- WMXCDAVJEZZYLT-UHFFFAOYSA-N tert-butylthiol Chemical class CC(C)(C)S WMXCDAVJEZZYLT-UHFFFAOYSA-N 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 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
- 230000008719 thickening Effects 0.000 description 1
- 210000003813 thumb Anatomy 0.000 description 1
- 239000005028 tinplate Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-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
- 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
- RKBCYCFRFCNLTO-UHFFFAOYSA-N triisopropylamine Chemical compound CC(C)N(C(C)C)C(C)C RKBCYCFRFCNLTO-UHFFFAOYSA-N 0.000 description 1
- 239000013638 trimer Substances 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 150000003739 xylenols Chemical class 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
- 229960000314 zinc acetate Drugs 0.000 description 1
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 description 1
- 229910000165 zinc phosphate Inorganic materials 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/50—Multilayers
- B05D7/56—Three layers or more
- B05D7/57—Three layers or more the last layer being a clear coat
- B05D7/572—Three layers or more the last layer being a clear coat all layers being cured or baked together
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2451/00—Type of carrier, type of coating (Multilayers)
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08L61/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08L61/28—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds with melamine
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L79/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
- C08L79/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08L79/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31721—Of polyimide
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- Paints Or Removers (AREA)
Description
工程(1):被塗物上に、水性中塗り塗料(X)を塗装して中塗り塗膜を形成する工程、
工程(2):工程(1)で形成される未硬化の中塗り塗膜上に、水性ベース塗料(Y)を塗装してベース塗膜を形成する工程、
工程(3):工程(2)で形成される未硬化のベース塗膜上に、クリヤー塗料(Z)を塗装してクリヤー塗膜を形成する工程、及び
工程(4):工程(1)〜(3)で形成される未硬化の中塗り塗膜、未硬化のベース塗膜及び未硬化のクリヤー塗膜を同時に加熱硬化させる工程、
を順次行う複層塗膜形成方法であって、水性中塗り塗料(X)が、樹脂成分として、
(A)水酸基価が60〜200mgKOH/g、酸価が10〜60mgKOH/g、かつ数平均分子量が700〜5,000の範囲内である水酸基及びカルボキシル基含有ポリエステル樹脂、(B)重量平均分子量が500〜4,000の範囲内であるメラミン樹脂、ならびに(C)ポリカルボジイミド化合物を含有することを特徴とする複層塗膜形成方法。
本発明の複層塗膜形成方法によれば、まず、被塗物上に、(A)水酸基価が60〜200mgKOH/g、酸価が10〜60mgKOH/g、数平均分子量が700〜5,000の範囲内である水酸基及びカルボキシル基を含有するポリエステル樹脂、(B)重量平均分子量が500〜4,000の範囲内であるメラミン樹脂、ならびに(C)ポリカルボジイミド化合物を含有する水性中塗り塗料(X)が塗装される。
水性中塗り塗料(X)を適用する被塗物は、特に限定されない。該被塗物としては、例えば、乗用車、トラック、オートバイ、バス等の自動車車体の外板部;バンパー等の自動車部品;携帯電話、オーディオ機器等の家庭電気製品の外板部等を挙げることができる。これらのうち、自動車車体の外板部及び自動車部品が好ましい。
水酸基及びカルボキシル基含有ポリエステル樹脂(A)は、1分子中に1個以上の水酸基と1個以上のカルボキシル基とを有する樹脂である。また、該水酸基及びカルボキシル基含有ポリエステル樹脂(A)は、水酸基価が60〜200mgKOH/gの範囲内であり、かつ、酸価が10〜60mgKOH/gの範囲内であり、かつ、数平均分子量が700〜5,000の範囲内である。
上記モノエポキシ化合物としては、例えば、合成高分岐飽和脂肪酸のグリシジルエステル(商品名「カージュラE10」HEXION Specialty Chemicals社製)を好適に用いることができる。
メラミン樹脂(B)は、メラミンとアルデヒドとの反応により得られる樹脂であり、部分メチロール化メラミン樹脂及び完全メチロール化メラミン樹脂の両者が包含される。また、本発明に従う中塗り塗料(X)として使用されるメラミン樹脂(B)は、得られる複層塗膜の平滑性、鮮映性、耐水性、耐チッピング性等の観点から、一般に、500〜4,000、好ましくは600〜3,000、さらに好ましくは700〜2,000の範囲内の重量平均分子量を有することが好適である。
ポリカルボジイミド化合物(C)は、1分子中に少なくとも2個のカルボジイミド基を有する化合物であって、例えば、イソシアネート基含有化合物のイソシアネート基同士を脱二酸化炭素反応せしめたものを使用することができる。
本発明の複層塗膜形成方法において使用される水性中塗り塗料(X)は、前記水酸基及びカルボキシル基含有ポリエステル樹脂(A)、メラミン樹脂(B)ならびにポリカルボジイミド化合物(C)を含有する水性塗料である。
水酸基及びカルボキシル基含有ポリエステル樹脂(A):5〜95質量部、好ましくは25〜90質量部、さらに好ましくは40〜80質量部、
メラミン樹脂(B):2〜60質量部、好ましくは5〜50質量部、さらに好ましくは10〜40質量部、
ポリカルボジイミド化合物(C):2〜60質量部、好ましくは5〜40質量部、さらに好ましくは10〜30質量部。
炭素数4〜24のアルキル基を有する重合性不飽和モノマー(g−1):5〜100質量%、好ましくは30〜95質量%、さらに好ましくは50〜90質量%、
水酸基含有重合性不飽和モノマー(g−2):0.5〜40質量%、好ましくは2〜15質量%、さらに好ましくは5〜10質量%、及びカルボキシル基含有重合性不飽和モノマー(g−3):0.5〜20質量%、好ましくは2〜15質量%、さらに好ましくは3〜8質量%。
本明細書において、水分散性を有する水酸基及びカルボキシル基含有アクリル樹脂(G’)の平均粒子径は、サブミクロン粒度分布測定装置を用いて、常法により脱イオン水で希釈してから20℃で測定した値である。サブミクロン粒度分布測定装置としては、例えば、「COULTER N4型」(商品名、ベックマン・コールター社製)を用いることができる。
で表される化合物である。
上記ポリオキシアルキレングリコールの数平均分子量は、100〜1,200程度が好ましく、150〜600程度がより好ましく、200〜400程度がさらに好ましい。
まず、ポリプロピレン板上に本発明の水性中塗り塗料(X)を硬化膜厚が30μmとなるように塗装し、80℃で10分間加熱する。次に、該ポリプロピレン板上の中塗り塗膜を回収し、質量(Wa)を測定する。その後、該塗膜を300メッシュのステンレススチール製の網状容器に入れ、64℃に加温したアセトンとメタノールの等質量混合溶剤中で5時間抽出し、110℃で60分間乾燥した後の塗膜質量(Wb)を測定し、以下の式に従って算出される不溶塗膜残存率(質量%)を算出し、それをゲル分率(G80)とする。
ゲル分率(G80)[質量%]=(Wb/Wa)×100
以上に述べた工程(1)で形成される水性中塗り塗料(X)の塗膜(以下、「中塗り塗膜」という場合がある)上には、次いで、水性ベース塗料(Y)が塗装される。
まず、被塗物上に水性中塗り塗料(X)を塗装すると同時に、予め質量(W1)を測定しておいたアルミホイル上にも水性中塗り塗料(X)を塗装する。続いて、塗装後、プレヒートなどがされた該アルミホイルを水性ベース塗料(Y)が塗装される直前に回収し、その質量(W2)を測定する。次に、回収したアルミホイルを110℃で60分間乾燥し、デシケーター内で室温まで放冷した後、該アルミホイルの質量(W3)を測定し、以下の式に従って固形分含有率を求める。
固形分含有率[質量%]={(W3−W1)/(W2−W1)}×100
まず、被塗物上に水性中塗り塗料(X)を塗装すると同時に、ポリプロピレン板上にも水性中塗り塗料(X)を塗装し、塗装後、プレヒートなどがされた該ポリプロピレン板を水性ベース塗料(Y)が塗装される直前に回収する。次に、該ポリプロピレン板上の中塗り塗膜を回収し、質量(WC)を測定する。その後、該塗膜を300メッシュのステンレススチール製の網状容器に入れ、64℃に加温したアセトンとメタノールの等質量混合溶剤中で5時間抽出し、110℃で60分間乾燥した後の塗膜質量(Wd)を測定し、以下の式に従って得られる不溶塗膜残存率(質量%)を算出し、それをゲル分率とする。
ゲル分率[質量%]=(Wd/WC)×100
本発明の複層塗膜形成方法においては、上記工程(2)で形成される水性ベース塗料(Y)の塗膜(以下、「ベース塗膜」という場合がある)上に、クリヤー塗料(Z)が塗装される。
本発明の第一の複層塗膜形成方法においては、上記工程(1)〜(3)で形成される未硬化の中塗り塗膜、未硬化のベース塗膜及び未硬化のクリヤー塗膜が、同時に加熱硬化せしめられる。
製造例1
温度計、サーモスタット、攪拌装置、還流冷却器及び水分離器を備えた反応容器に、アジピン酸88g、1,2−シクロヘキサンジカルボン酸無水物536g、イソフタル酸199g、2−ブチル−2−エチル−1,3−プロパンジオール288g、ネオペンチルグリコール95g、1,4−シクロヘキサンジメタノール173g及びトリメチロールプロパン287gを仕込み、160℃から230℃まで3時間かけて昇温させた後、縮合水を水分離器により留去させながら230℃で保持し、酸価が5mgKOH/g以下となるまで反応させた。この反応生成物に、無水トリメリット酸86gを添加し、170℃で30分間付加反応を行った後、50℃以下に冷却し、2−(ジメチルアミノ)エタノールを酸基に対して0.9当量添加し中和してから、脱イオン水を徐々に添加することにより、固形分濃度45%、pH7.2の水酸基及びカルボキシル基含有ポリエステル樹脂水分散液(A−1)を得た。得られた水酸基及びカルボキシル基含有ポリエステル樹脂の水酸基価は110mgKOH/g、酸価は33mgKOH/g、数平均分子量は2,050であった。
酸価(mgKOH/g)=56.1×V×C/m
V:滴定量(ml)、C:滴定液の濃度(mol/l)、m:試料の固形分質量(g)
水酸基価(mgKOH/g)=〔V×56.1×C/m〕+D
V:滴定量(ml)、C:滴定液の濃度(mol/l)、m:試料の固形分質量(g)、D:試料の酸価(mgKOH/g)(以下、水酸基価及び酸価の測定方法は、本明細書中において同じ)。
炭素数4以上の直鎖アルキレン基のモル数(Wm)
=88/146(アジピン酸)
=0.6[mol]
縮合水の質量
=18×{2×88/146(アジピン酸)+1×536/154(1,2−シクロヘキサンジカルボン酸無水物)+2×199/166(イソフタル酸)}
=127[g]
縮合水を除いた樹脂出来高(Wr)
=88(アジピン酸)+536(1,2−シクロヘキサンジカルボン酸無水物)+199(イソフタル酸)+288(2−ブチル−2−エチル−1,3−プロパンジオール)+95(ネオペンチルグリコール)+173(1,4−シクロヘキサンジメタノール)+287(トリメチロールプロパン)+86(無水トリメリット酸)−127(縮合水)
=1624[g]
=1.624[kg]
炭素数4以上の直鎖アルキレン基の含有量
=炭素数4以上の直鎖アルキレン基のモル数(Wm)/縮合水を除いた樹脂出来高(Wr)
=0.6/1.624
=0.4[mol/kg(樹脂固形分)]
また、得られた水酸基及びカルボキシル基含有ポリエステル樹脂のベンゼン環とシクロヘキサン環の合計含有量は、下記の計算により算出した。
ベンゼン環とシクロヘキサン環の合計モル数(Wn)
=536/154(1,2−シクロヘキサンジカルボン酸無水物)+199/166(イソフタル酸)+173/144(1,4−シクロヘキサンジメタノール)+86/192(無水トリメリット酸)
=6.33[mol]
ベンゼン環とシクロヘキサン環の合計含有量
=ベンゼン環とシクロヘキサン環の合計モル数(Wn)/縮合水を除いた樹脂出来高(Wr)
=6.33/1.624
=3.9[mol/kg(樹脂固形分)]。
下記第1表に示す配合で、製造例1と同様に処理して、固形分濃度45%及びpHが7.2の水酸基及びカルボキシル基含有ポリエステル樹脂水分散液(A−2)〜(A−18)を得た。の得られた各水酸基及びカルボキシル基含有ポリエステル樹脂の、水酸基価、酸価、数平均分子量、炭素数4以上の直鎖アルキレン基の含有量及びベンゼン環とシクロヘキサン環の合計含有量を、製造例1で得た水酸基及びカルボキシル基含有ポリエステル樹脂水分散液(A−1)と併せて、下記第1表に示す。
製造例19
温度計、サーモスタット、撹拌装置、還流冷却器、窒素導入管及び滴下装置を備えた反応容器に、プロピレングリコールモノプロピルエーテル30部を仕込み85℃に昇温した。昇温後、スチレン10部、メチルメタクリレート30部、2−エチルヘキシルアクリレート15部、n−ブチルアクリレート11.5部、ヒドロキシエチルアクリレート30部、アクリル酸3.5部、プロピレングリコールモノプロピルエーテル10部及び2,2’−アゾビス(2,4−ジメチルバレロニトリル)2部の混合物を4時間かけてフラスコに滴下し、滴下終了後1時間熟成した。その後さらにプロピレングリコールモノプロピルエーテル5部及び2,2’−アゾビス(2,4−ジメチルバレロニトリル)1部の混合物を1時間かけてフラスコに滴下し、滴下終了後1時間熟成した。さらに得られた生成物に2−(ジメチルアミノ)エタノール3.03部を加え、脱イオン水を徐々に添加することにより、固形分濃度40%の水酸基含有アクリル樹脂溶液(AC−1)を得た。得られた水酸基含有アクリル樹脂の酸価は27mgKOH/g、水酸基価は145mgKOH/gであった。
温度計、サーモスタット、撹拌装置、還流冷却器、窒素導入管及び滴下装置を備えた反応容器に脱イオン水70.7部、「アクアロンKH−10」(商品名、第一工業製薬株式会社製、ポリオキシエチレンアルキルエーテル硫酸塩エステルアンモニウム塩、有効成分97%)0.52部を仕込み、窒素気流中で撹拌混合し、80℃に昇温した。次いで下記のモノマー乳化物(1)のうちの全量の1%量、及び6%過硫酸アンモニウム水溶液5部を反応容器内に導入し80℃で15分間保持した。次いで、残りのモノマー乳化物(1)を3時間かけて、同温度に保持した反応容器内に滴下した。滴下終了後、1時間熟成した。次に、5% 2−(ジメチルアミノ)エタノール水溶液40部を反応容器に徐々に加えながら30℃まで冷却し、100メッシュのナイロンクロスで濾過することにより、濾液として、固形分濃度45%の水酸基含有アクリル樹脂分散液(AC−2)を得た。得られた水酸基含有アクリル樹脂の酸価は12mgKOH/g、水酸基価は43mgKOH/gであった。
モノマー乳化物(1):脱イオン水50部、スチレン10部、メチルメタクリレート40部、エチルアクリレート35部、n−ブチルメタクリレート3.5部、2−ヒドロキシエチルメタクリレート10部、アクリル酸1.5部、「アクアロンKH−10」1部及び過硫酸アンモニウム0.03部を混合攪拌して、モノマー乳化物(1)を得た。
温度計、サーモスタット、撹拌装置、還流冷却器、窒素導入管及び滴下装置を備えた反応容器に脱イオン水50部、「アデカリアソープSR−1025」(商品名、ADEKA製、乳化剤、有効成分25%)0.2部を仕込み、窒素気流中で撹拌混合し、80℃に昇温させた。次いで、下記モノマー乳化物の全量のうちの3%量及び5%過硫酸アンモニウム水溶液1部を反応容器内に導入し80℃で20分間保持した。その後、モノマー乳化物の残部を3時間かけて、同温度に保持した反応容器内に滴下し、滴下終了後、90分間熟成を行なった。次いで、反応液を冷却し、該反応液の温度が40℃以下になったところで、5% 2−(ジメチルアミノ)エタノール水溶液10部を反応容器に徐々に加え、冷却を続けながら10分間攪拌した。次いで、100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150nm、固形分45%の水分散性水酸基及びカルボキシル基含有アクリル樹脂水分散液(G−1)を得た。得られた水分散性水酸基及びカルボキシル基含有アクリル樹脂は、水酸基価が41mgKOH/g、酸価が36mgKOH/gであった。
モノマー乳化物:脱イオン水55部、「アデカリアソープSR−1025」8部、過硫酸アンモニウム0.2部、n−ブチルアクリレート40部、2−エチルヘキシルアクリレート35部、2−ヒドロキシエチルメタクリレート9.5部、メタクリル酸5.5部及びスチレン10部を混合攪拌することにより、モノマー乳化物を得た。
下記第2表に示す配合で、製造例21と同様に処理して、固形分45%の水分散性水酸基及びカルボキシル基含有アクリル樹脂水分散液(G−2)〜(G−7)を得た。得られた水分散性水酸基及びカルボキシル基含有アクリル樹脂水分散液の、水酸基価、酸価、モノマー成分(g)の合計質量を基準とした、炭素数4〜24のアルキル基を有する重合性不飽和モノマー(g−1)、水酸基含有重合性不飽和モノマー(g−2)及びカルボキシル基含有重合性不飽和モノマー(g−3)の含有割合を、製造例20で得た水分散性水酸基及びカルボキシル基含有アクリル樹脂水分散液(G−1)と併せて、下記第2表に示す。
製造例28
製造例1で得た水酸基及びカルボキシル基含有ポリエステル樹脂水分散液(A−1)44部(樹脂固形分20部)、ルチル型二酸化チタン(D1−1)(商品名「JR−806」テイカ株式会社製)60部、カーボンブラック(D1−2)(商品名「カーボンMA−100」三菱化学株式会社製)1部、平均一次粒子径が0.5μmの硫酸バリウム粉末(D2−1)(商品名「バリエースB−35」堺化学工業株式会社製)15部、平均一次粒子径が4.8μmのタルク粉末(D2−2)(商品名「MICRO ACE S−3」日本タルク株式会社製)3部及び脱イオン水11部を混合し、2−(ジメチルアミノ)エタノールでpH8.0に調整した後、ペイントシェーカーで30分間分散させて顔料分散ペーストを得た。
次に、得られた顔料分散ペースト134部、製造例1で得た水酸基及びカルボキシル基含有ポリエステル樹脂水分散液(A−1)100部、メラミン樹脂(B−1)(メチル−ブチル混合エーテル化メラミン樹脂、メトキシ基とブトキシ基のモル比がメトキシ基/ブトキシ基=70/30、重量平均分子量800、固形分80%)25部、ポリカルボジイミド化合物(C−1)(商品名「カルボジライトSV−02」日清紡株式会社製、固形分40%)38部及び疎水性溶媒(E−1)(2−エチル−1−ヘキサノール、20℃において100gの水に溶解する質量:0.1g)10部を均一に混合した。
次いで、得られた混合物に、ウレタン会合型増粘剤(商品名「UH−752」株式会社ADEKA製)、2−(ジメチルアミノ)エタノール及び脱イオン水を添加し、pH8.0、塗料固形分48%、20℃におけるフォードカップNo.4による粘度40秒の水性中塗り塗料(X−1)を得た。また、得られた水性中塗り塗料(X−1)の、硬化膜厚が30μmとなるように塗装し、80℃で10分間加熱した後の塗膜のゲル分率(G80)は31%であった。
第3表に示す配合に従って、実施例1と同様の方法により、pH8.0、塗料固形分48%、20℃におけるフォードカップNo.4による粘度40秒である水性中塗り塗料(X−2)〜(X−41)を得た。
製造例69
温度計、サーモスタット、撹拌器、還流冷却器、窒素導入管及び滴下装置を備えた反応容器に脱イオン水130部、「アクアロンKH−10」0.52部を仕込み、窒素気流中で撹拌混合し、80℃に昇温した。次いで下記のモノマー乳化物(1)のうちの全量の1%量及び6%過硫酸アンモニウム水溶液5.3部を反応容器内に導入し80℃で15分間保持した。その後、残りのモノマー乳化物(2)を3時間かけて、同温度に保持した反応容器内に滴下した。滴下終了後、1時間熟成を行なった。次いで、下記のモノマー乳化物(3)を1時間かけて滴下した。1時間熟成した後、5%ジメチルエタノールアミン水溶液40部を反応容器に徐々に加えながら30℃まで冷却し、100メッシュのナイロンクロスで濾過することにより、濾液として、平均粒子径100nm、固形分濃度30%のアクリル樹脂エマルションを得た。
前記平均粒子径は、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。
得られたアクリル樹脂は、酸価が33mgKOH/g、水酸基価が25mgKOH/gであった。
製造例70
温度計、サーモスタット、攪拌装置、還流冷却器及び水分離器を備えた反応容器に、トリメチロールプロパン109部、1,6−ヘキサンジオール141部、ヘキサヒドロ無水フタル酸126部及びアジピン酸120部を仕込み、160℃〜230℃の間を3時間かけて昇温させた後、230℃で4時間縮合反応させた。次いで、得られた縮合反応生成物にカルボキシル基を付加するために、さらに無水トリメリット酸38.3部を加え、170℃で30分間反応させた後、2−エチル−1−ヘキサノール(20℃において100gの水に溶解する質量:0.1g)で希釈し、固形分濃度70%であるポリエステル樹脂溶液を得た。得られたポリエステル樹脂は、酸価が46mgKOH/g、水酸基価が150mgKOH/g、重量平均分子量が6,400であった。
製造例71
攪拌混合容器内において、アルミニウム顔料ペースト(商品名「GX−180A」旭化成メタルズ株式会社製、金属含有量74%)19部、2−エチル−1−ヘキサノール35部、リン酸基含有樹脂溶液(注1)8部及び2−(ジメチルアミノ)エタノール0.2部を均一に混合して、光輝性顔料分散液を得た。
(注1)リン酸基含有樹脂溶液:温度計、サーモスタット、撹拌器、還流冷却器、窒素導入管及び滴下装置を備えた反応容器にメトキシプロパノール27.5部、イソブタノール27.5部の混合溶剤を入れ、110℃に加熱した。次いで、スチレン25部、n−ブチルメタクリレート27.5部、分岐高級アルキルアクリレート(商品名「イソステアリルアクリレート」大阪有機化学工業株式会社製)20部、4−ヒドロキシブチルアクリレート7.5部、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、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時間かけて上記混合溶剤に加え、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部からなる混合物を1時間かけて滴下した。その後、1時間攪拌しながら熟成して固形分濃度50%のリン酸基含有樹脂溶液を得た。リン酸基含有樹脂のリン酸基による酸価は83mgKOH/g、水酸基価は29mgKOH/g、重量平均分子量は10,000であった。
(注2)リン酸基含有重合性モノマー:温度計、サーモスタット、撹拌器、還流冷却器、窒素導入管及び滴下装置を備えた反応容器にモノブチルリン酸57.5部及びイソブタノール41部を入れ、90℃に昇温した後、グリシジルメタクリレート42.5部を2時間かけて滴下した。その後、さらに1時間攪拌しながら熟成した後、イソプロパノ−ル59部を加えて、固形分濃度50%のリン酸基含有重合性モノマー溶液を得た。得られたモノマーのリン酸基による酸価は285mgKOH/gであった。
製造例72
製造例69で得たアクリル樹脂エマルション100部、製造例70で得たポリエステル樹脂溶液57部、製造例71で得た光輝性顔料分散液62部及びメラミン樹脂(商品名「サイメル325」日本サイテックインダストリーズ株式会社製、固形分80%)37.5部を均一に混合し、更に、ポリアクリル酸系増粘剤(商品名「プライマルASE−60」ロームアンドハース社製)、2−(ジメチルアミノ)エタノール及び脱イオン水を加えてpH8.0、塗料固形分25%、20℃におけるフォードカップNo.4による粘度40秒の水性ベース塗料(Y−1)を得た。
製造例28〜68で得た水性中塗り塗料(X−1)〜(X−41)、及び製造例72で得た水性ベース塗料(Y−1)を用いて、以下のようにしてそれぞれ試験板を作製し、評価試験を行なった。
リン酸亜鉛化成処理を施した冷延鋼板に、カチオン電着塗料(商品名「エレクロンGT−10」関西ペイント株式会社製)を硬化膜厚20μmとなるように電着塗装し、170℃で30分間加熱して硬化させて試験用被塗物とした。
上記試験用被塗物に、前記製造例28で得た水性中塗り塗料(X−1)を、回転霧化型の静電塗装機を用いて、硬化膜厚25μmとなるように静電塗装し、2分間放置後、80℃で8分間プレヒートを行なった。次いで、該未硬化の中塗り塗膜上に製造例72で得た水性ベース塗料(Y−1)を、回転霧化型の静電塗装機を用いて、硬化膜厚15μmとなるように静電塗装し、2分間放置後、80℃で3分間プレヒートを行なった。次いで、該未硬化のベース塗膜上にアクリル樹脂系溶剤型上塗りクリヤー塗料(商品名「マジクロンKINO−1210」関西ペイント株式会社製、以下「クリヤー塗料(Z−1)」ということがある)を硬化膜厚35μmとなるように静電塗装し、7分間放置した後、140℃で30分間加熱して、該クリヤー塗膜を硬化させることにより試験板を作製した。
実施例1において、製造例21で得た水性中塗り塗料(X−1)を下記第4表に示す水性中塗り塗料(X−2)〜(X−41)のいずれかに変更する以外は、実施例1と同様にして試験板を作製した。
上記実施例1〜30及び比較例1〜11で得られた各試験板について、下記の試験方法により評価を行なった。評価結果を下記第4表に示す。
平滑性:商品名「Wave Scan」(BYK Gardner社製)によって測定されるLong Wave(LW)値を用いて評価した。Long Wave(LW)値が小さいほど塗面の平滑性が高いことを示し、自動車車体等に塗装される塗料としては、通常、10以下であることが必要となる。
◎:ゴバン目塗膜が100個残存し、カッターの切り込みの縁において塗膜の小さなフチカケが生じていない
○:ゴバン目塗膜が100個残存するが、カッターの切り込みの縁において塗膜の小さなフチカケが生じている
△:ゴバン目塗膜が90〜99個残存する
×:ゴバン目塗膜の残存数が89個以下である。
◎:キズの大きさが極めて小さく、電着面又は素地の鋼板が露出していない
○:キズの大きさが小さく、電着面又は素地の鋼板が露出していない
△:キズの大きさは小さいが、電着面又は素地の鋼板が露出している
×: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。
本願発明の属する技術分野においては、塗膜は、平滑性、鮮映性、耐水性及び耐チッピング性の全てにおいて優れていることが重要である。従って、以下のように総合評価を行った:
◎:前述の平滑性が10以下を示し、鮮映性が16以下を示し、かつ耐水性及び耐チッピング性が共に◎である
○:平滑性が10以下を示し、鮮映性が16以下を示し、かつ耐水性及び耐チッピング性が○又は◎であり、かつ少なくとも一方が○である
△:平滑性が10以下を示し、鮮映性が16以下を示し、かつ耐水性及び耐チッピング性が△、○又は◎であり、かつ少なくとも一つが△である
×:平滑性が10を超えるか、鮮映性が16を超えるか、または耐水性及び耐チッピング性の少なくとも一方が×である
Claims (9)
- 下記の工程(1)〜(4)
工程(1):被塗物上に、水性中塗り塗料(X)を塗装して中塗り塗膜を形成する工程、
工程(2):工程(1)で形成される未硬化の中塗り塗膜上に、水性ベース塗料(Y)を塗装してベース塗膜を形成する工程、
工程(3):工程(2)で形成される未硬化のベース塗膜上に、クリヤー塗料(Z)を塗装してクリヤー塗膜を形成する工程、及び
工程(4):工程(1)〜(3)で形成される未硬化の中塗り塗膜、未硬化のベース塗膜及び未硬化のクリヤー塗膜を同時に加熱硬化させる工程、
を順次行う複層塗膜形成方法であって、水性中塗り塗料(X)が、樹脂成分として、
(A)水酸基価が60〜200mgKOH/g、酸価が10〜60mgKOH/g、かつ数平均分子量が700〜5,000の範囲内である水酸基及びカルボキシル基含有ポリエステル樹脂、(B)重量平均分子量が500〜4,000の範囲内であるメラミン樹脂、ならびに(C)ポリカルボジイミド化合物を含有することを特徴とする複層塗膜形成方法であって、
水酸基及びカルボキシル基含有ポリエステル樹脂(A)が、分子中に炭素数4以上の直鎖アルキレン基を0.3〜2.5mol/kg(樹脂固形分)含有するポリエステル樹脂であるか、又は
水酸基及びカルボキシル基含有ポリエステル樹脂(A)が、分子中にベンゼン環及び/又はシクロヘキサン環を含有し、且つそれらの合計含有量が1.5〜4.0mol/kg(樹脂固形分)の範囲内にあるポリエステル樹脂である、
複層塗膜形成方法。 - メラミン樹脂(B)が、メトキシ基とブトキシ基とのモル比がメトキシ基/ブトキシ基のモル比で95/5〜5/95の範囲内であるメチル−ブチル混合エーテル化メラミン樹脂である請求項1に記載の複層塗膜形成方法。
- 水性中塗り塗料(X)における水酸基及びカルボキシル基含有ポリエステル樹脂(A)、メラミン樹脂(B)ならびにポリカルボジイミド化合物(C)の配合割合が、水酸基及びカルボキシル基含有ポリエステル樹脂(A)、メラミン樹脂(B)ならびにポリカルボジイミド化合物(C)の合計固形分100質量部を基準として、水酸基及びカルボキシル基含有ポリエステル樹脂(A)が5〜95質量部、メラミン樹脂(B)が2〜60質量部、ポリカルボジイミド化合物(C)が2〜60質量部である請求項1又は2に記載の複層塗膜形成方法。
- 水性中塗り塗料(X)が、着色顔料(D1)及び/又は体質顔料(D2)を含有し、かつ、該着色顔料(D1)及び体質顔料(D2)の合計含有量が、水酸基及びカルボキシル基含有ポリエステル樹脂(A)、メラミン樹脂(B)ならびにポリカルボジイミド化合物(C)の合計固形分100質量部を基準として、40〜300質量部の範囲内である請求項1〜3のいずれか1項に記載の複層塗膜形成方法。
- 水性中塗り塗料(X)が、さらに、アクリル樹脂を含む、請求項1〜4のいずれか1項に記載の複層塗膜形成方法。
- 水性ベース塗料(Y)が光輝性顔料(D3)を含有する塗料である請求項1〜5のいずれか1項に記載の複層塗膜形成方法。
- 被塗物が、電着塗料によって下塗り塗膜が形成された車体である請求項1〜6のいずれか1項に記載の複層塗膜形成方法。
- (A)水酸基価が60〜200mgKOH/g、酸価が10〜60mgKOH/g、かつ数平均分子量が700〜5,000の範囲内である水酸基及びカルボキシル基含有ポリエステル樹脂、(B)重量平均分子量が500〜4,000の範囲内であるメラミン樹脂、ならびに(C)ポリカルボジイミド化合物を含有する、水性中塗り塗料であって、
水酸基及びカルボキシル基含有ポリエステル樹脂(A)が、分子中に炭素数4以上の直鎖アルキレン基を0.3〜2.5mol/kg(樹脂固形分)含有するポリエステル樹脂であるか、又は
水酸基及びカルボキシル基含有ポリエステル樹脂(A)が、分子中にベンゼン環及び/又はシクロヘキサン環を含有し、且つそれらの合計含有量が1.5〜4.0mol/kg(樹脂固形分)の範囲内にあるポリエステル樹脂である、水性中塗り塗料。 - 請求項1〜7のいずれか1項に記載の方法により複層塗膜が形成された物品。
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WO2019159453A1 (ja) * | 2018-02-13 | 2019-08-22 | 東洋製罐グループホールディングス株式会社 | 水性塗料組成物 |
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