JP5080322B2 - 複層塗膜形成方法 - Google Patents
複層塗膜形成方法 Download PDFInfo
- Publication number
- JP5080322B2 JP5080322B2 JP2008061595A JP2008061595A JP5080322B2 JP 5080322 B2 JP5080322 B2 JP 5080322B2 JP 2008061595 A JP2008061595 A JP 2008061595A JP 2008061595 A JP2008061595 A JP 2008061595A JP 5080322 B2 JP5080322 B2 JP 5080322B2
- Authority
- JP
- Japan
- Prior art keywords
- coating film
- acid
- clear
- hydroxyl group
- clear 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 - Fee Related
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- XVNKRRXASPPECQ-UHFFFAOYSA-N phenyl n-phenylcarbamate Chemical compound C=1C=CC=CC=1OC(=O)NC1=CC=CC=C1 XVNKRRXASPPECQ-UHFFFAOYSA-N 0.000 description 1
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- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 235000014692 zinc oxide Nutrition 0.000 description 1
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- 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
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Description
本発明の複層塗膜形成方法(以下、「本方法」ということがある)を適用し得る被塗物は、特に制限はないが、例えば、冷延鋼板、亜鉛メッキ鋼板、亜鉛合金メッキ鋼板、ステンレス鋼板、錫メッキ鋼板等の鋼板、アルミニウム板、アルミニウム合金板等の金属基材;各種プラスチック素材等が好ましい。また、これらにより形成される自動車、二輪車、コンテナ等の各種車両の車体等であってもよい。
第1クリヤ塗料
本発明の複層塗膜形成方法に用いられる第1クリヤ塗料は、水酸基含有樹脂及びポリイソシアネート化合物を主成分とし、該塗料を塗装して形成される140℃で30分間加熱して硬化させた膜厚40μmの第1クリヤ塗膜の周波数11Hzでの動的粘弾性測定において、tanδ(損失弾性率/貯蔵弾性率)の最大値を示す温度として測定されるガラス転移温度が70℃未満で、80℃でのtanδが0.4未満であることを特徴とするものである。
水酸基含有アクリル樹脂は、水酸基含有ビニルモノマー(M−1)及びその他の共重合可能なビニルモノマー(M−2)を常法により共重合せしめることによって製造することができる。
樹脂のガラス転移温度
なお、本明細書において、樹脂のガラス転移温度(Tg)は示差走査型熱量計(DSC;セイコー電子工業SSC5200)でJISK7121(プラスチックのガラス転移温度測定方法)に基づいて、不活性気体中で、10℃/分の昇温スピードで測定した値である。測定は、試料をサンプル皿に所定量秤取した後、130℃で3時間乾燥させてから測定を行なった。
ート、脂環族ポリイソシアネート及びこれらポリイソシアネートの誘導体が好ましい。ま
た、特に以下のポリイソシアネート化合物を好適なものとしてあげることができる。
2.イソシアネート骨格の一部に軟質鎖構造を有するポリイソシアネート化合物
3.3官能以上で官能基部分の少なくとも1つに軟質構造成分が結合したポリイソシアネート化合物
具体的には、上記1のタイプとして、ヘキサメチレンジイソシアネート等の脂肪族ポリ
イソシネートやジシクロヘキシルメタンジイソシアネート等の脂環族ポリイソシアネートもしくはそれらの変性品、具体的には、スミジュールN−3300(住化バイエルウレタン社製)等、上記2のタイプとして、デュラネートE−402−90T、E−405−80T(旭化成ケミカルズ社製)、上記3のタイプとして、タケネートD−160N(三井武田薬品工業社製)等をあげることができる。
第2クリヤ塗料
本発明の複層塗膜形成方法に用いられる第2クリヤ塗料は、水酸基含有樹脂及びポリイソシアネート化合物を主成分とし、該塗料を塗装して形成される140℃で30分間加熱して硬化させた膜厚40μmの第2クリヤ塗膜の周波数11Hzでの動的粘弾性測定において、ガラス転移温度が70℃以上であることを特徴とするものである。
塗膜の動的粘弾性
塗膜の耐擦り傷性を考える上で、塗膜が有する動的粘弾性特性は重要である。塗膜の動的粘弾性の測定は、一般に、塗膜に周期的な微少ひずみを与えて、それに対する応答を測定することによって行なうことができる。塗膜に対して周期的なひずみを与えた場合、完全な弾性体であればそれに応答する時間的な遅れの発生はなく同位相で現れるが、粘性要素が存在すると応答に遅れを生じる。
塗膜のガラス転移温度とはガラス領域からゴム領域への変極点を示す温度のことであり、本明細書においては、動的粘弾性(11Hz、温度分散測定)における上記tanδの値が極大値を示す時の温度をガラス転移温度(Tg)とする。一般に塗膜硬度とガラス転移温度は相関する。
塗料の調整
第1クリヤ塗料及び第2クリヤ塗料は、その使用に際して、水酸基含有樹脂及びポリイソシネート化合物ならびに必要に応じて添加される添加剤を混合し、必要に応じて塗料用有機溶剤等を添加して希釈し、適正粘度に調整することにより塗装することができる。
複層塗膜形成方法
第1クリヤ塗料及び第2クリヤ塗料の塗装方法は、特に限定されるものではなく、常法を用いることができ、例えば、エアスプレー塗装、エアレススプレー塗装、回転霧化塗装、カーテンコート塗装などにより行なうことができる。これらの塗装方法においては、必要に応じて、静電印加を行なってもよい。この中でも特に静電印加による回転霧化塗装が好ましい。また、かかる塗装方法は、所望の膜厚が得られるまで、1回ないし数回に分けて行うことができる。
第1クリヤ塗料の塗装膜厚は、耐擦り傷性及び仕上がり性の点から、通常、硬化膜厚として15〜60μm、とくに20〜40μmであるのが好ましい。
第2クリヤ塗料は、第2クリヤ塗料により形成される第2クリヤ塗膜が、硬化膜厚として2〜15μmの範囲内となるように塗装される。
水酸基含有樹脂の製造
製造例1
撹拌装置、温度計、冷却管、窒素ガス導入口を備えた四ツ口フラスコにエトキシエチルプロピオネート31部を仕込み、窒素ガス通気下で155℃に昇温した。155℃に達した後、窒素ガスの通気を止め、スチレン20部、2−エチルヘキシルアクリレート43部、4−ヒドロキシブチルアクリレート36部、アクリル酸1部、2,2−ジ(t−アミルパーオキシ)ブタン(重合開始剤)3部を4時間かけて滴下した。155℃で窒素ガスを通気しながら2時間熟成させた後、100℃まで冷却し、酢酸ブチル32.5部で希釈することにより、固形分60%の水酸基含有樹脂1の溶液を得た。水酸基含有樹脂1は、水酸基価140mgKOH/g、酸価8mgKOH/g、数平均分子量7500、ガラス転移温度は−30℃であった。樹脂のガラス転移温度は、セイコー電子工業DSC220U(示差走査型熱量計)により測定した。試料50mgを専用のサンプル皿に所定量秤取した後、130℃で3時間乾燥させた後、不活性気体中で、−50℃から10℃/分のスピードで、150℃まで昇温し、得られた熱量変化カーブの変曲点の温度をガラス転移温度とした。
下記表1に示す配合で、製造例1と同様にして合成することにより、水酸基含有樹脂2〜9の溶液を得た。得られた各水酸基含有樹脂の特数値を製造例1で得られた水酸基含有樹脂の溶液の特数値と併せて下記表1に示す。
製造例10〜25
上記製造例1〜9で得られた水酸基含有樹脂及び架橋剤等を後記表2及び表3に示す配合にてディスパーを用いて攪拌混合して塗料化を行い、第1クリヤ塗料として、クリヤ塗料1−1〜10を、第2クリヤ塗料として、クリヤ塗料2−1〜6を得た。なお、後記表2及び表3に示す各クリヤ塗料の配合は各成分の固形分質量比である。なお、後記表2及び表3における(注1)〜(注7)は、それぞれ下記の意味を有する。
(注2)デュラネートE−402−90T:旭化成ケミカルズ社製、ポリイソシアネート化合物
(注3)タケネートD−160N:三井武田薬品工業社製、ポリイソシアネート化合物
(注4)サイメル350:三井サイテック社製、メラミン樹脂
(注5)Nacure5543:キングインダストリー社製、ドデシルベンゼンスルホン酸のアミン中和物
(注6)TINUVIN384:チバ・スペシャルティ・ケミカルズ社製、紫外線吸収剤
(注7)TINUVIN292:チバ・スペシャルティ・ケミカルズ社製、光安定剤
上記製造例10〜25で得られた各第1クリヤ塗料1−1〜10及び第2クリヤ塗料2−1〜6の各塗料を、ブリキ板上に硬化膜厚が40μmになるようにエアスプレー塗装し、140℃で30分間加熱硬化させた後に塗膜を剥離して短冊状(0.5×2cm)の遊離膜に調製したものを試料として、動的粘弾性の測定を行った。
複層塗膜形成方法
実施例1〜15及び比較例1〜8
上記製造例10〜25で得られた各第1クリヤ塗料及び第2クリヤ塗料に、酢酸ブチルを加えて、フォードカップ#4を用いて、第1クリヤ塗料は25秒、そして第2クリヤ塗料は15秒の粘度に調整した。
試験方法
得られた各試験板について、常温で7日間放置してから、以下の方法により耐擦り傷性、耐汚染性、耐酸性、塗面平滑性及びツヤ感の試験を行った。
上記L値は、CIE等色関数に基づくL*値を測定することにより評価した。測定はBYKガードナー社製、カラーガイド45/0を用いて行なった。ΔL*値が小さい程、耐汚染性が良好であることを表わす。目安として一般にΔL*値が1.0未満であれば、耐汚染性は良好であるといえる。
×:塗膜の硫酸滴下部に白化が認められる
塗面平滑性:BYK Gardner社製のWave Scan(商品名)により測定した。Wave ScanによりShort Wave値(SW)を測定した。Short Wave値は、300〜1200μm程度の波長における表面粗度の振幅の指標であり、塗面の微少肌の具合を評価することができる。また、Wave Scan値は、測定値が小さいほど塗面平滑性が高いことを示す。目安として、一般にWave Scan値が10未満であれば、塗面平滑性は良好とされる。
上記性能試験結果を動的粘弾性測定結果と併せて下記表4及び表5に示す。
Claims (7)
- 被塗物に、第1クリヤ塗料を塗装し、未硬化の又は加熱硬化した第1クリヤ塗膜上に第2クリヤ塗料を塗装して、第2クリヤ塗膜を形成させる複層塗膜形成方法であって、第1クリヤ塗膜及び第2クリヤ塗膜各々を膜厚40μmで、140℃で30分間加熱して硬化させた時の周波数11Hzでの動的粘弾性測定において、第1クリヤ塗膜のガラス転移温度が70℃未満、でかつ80℃でのtanδ(損失弾性率/貯蔵弾性率)が0.4未満、第2クリヤ塗膜のガラス転移温度が70℃以上となる、水酸基含有樹脂及びポリイソシアネート化合物を主成分とする、第1クリヤ塗料及び第2クリヤ塗料を使用し、第1クリヤ塗膜が800〜10000Kgf/cm 2 の範囲内のヤング率を有し、かつ、第2クリヤ塗膜の加熱硬化後の膜厚が2〜15μmの範囲内となるように塗装することを特徴とする複層塗膜形成方法。
- 被塗物表面が、着色塗料を塗装することにより塗膜が形成された未硬化又は硬化された塗面である請求項1に記載の複層塗膜形成方法。
- 第1クリヤ塗料が、水酸基含有樹脂として、−60〜30℃の範囲内のガラス転移温度を有する水酸基含有アクリル樹脂を含有する請求項1又は2に記載の複層塗膜形成方法。
- 第1クリヤ塗料が、ポリイソシアネート化合物として、脂肪族ポリイソシアネート、脂環族ポリイソシアネート及びこれらポリイソシアネートの誘導体のうちの少なくとも1種を含有する請求項1〜3のいずれか1項に記載の複層塗膜形成方法。
- 第2クリヤ塗料が、水酸基含有樹脂として、−30〜70℃の範囲内のガラス転移温度
を有する水酸基含有アクリル樹脂を含有する請求項1〜4のいずれか1項に記載の複層塗膜形成方法。 - 第2クリヤ塗料が、1分子中に3個以上のイソシアネート基を有する多官能ポリイソシアネート化合物を含有する請求項1〜5のいずれか1項に記載の複層塗膜形成方法。
- 請求項1〜6のいずれかに記載の方法で塗装された物品。
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JP5260255B2 (ja) * | 2008-12-17 | 2013-08-14 | 株式会社豊田中央研究所 | 塗装方法およびそれにより得られる塗装体 |
US20100181201A1 (en) * | 2009-01-20 | 2010-07-22 | Bibber John W | Electrolytic passivated tin plated steel |
JP5382611B2 (ja) * | 2009-02-16 | 2014-01-08 | 日産自動車株式会社 | 微粒子含有軟質塗膜及び積層塗膜 |
JP2011057955A (ja) * | 2009-09-10 | 2011-03-24 | E I Du Pont De Nemours & Co | クリヤコート被覆組成物及びベースコート/クリヤコート2層被覆物の調製におけるその使用 |
JP5685505B2 (ja) * | 2010-08-19 | 2015-03-18 | オリジン電気株式会社 | 金属めっき用塗膜 |
JP2012097173A (ja) * | 2010-11-01 | 2012-05-24 | Dic Corp | 耐傷性に優れるコーティング樹脂組成物 |
JP5605195B2 (ja) * | 2010-12-08 | 2014-10-15 | Dic株式会社 | 耐傷性に優れるコーティング樹脂組成物 |
JP2012121985A (ja) * | 2010-12-08 | 2012-06-28 | Dic Corp | 耐傷性に優れるコーティング樹脂組成物 |
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JP5991822B2 (ja) * | 2012-02-10 | 2016-09-14 | Basfジャパン株式会社 | 1液型クリヤー塗料組成物及びそれを用いた複層塗膜形成方法 |
US9815084B2 (en) | 2013-05-13 | 2017-11-14 | Nissan Motor Co., Ltd. | Clear coating method, coating method, and coating film structure |
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Free format text: JAPANESE INTERMEDIATE CODE: R250 |
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LAPS | Cancellation because of no payment of annual fees |