JP2022067441A - 鋼材用水性被覆剤、被膜、鋼材の被覆方法、及び鋼材 - Google Patents
鋼材用水性被覆剤、被膜、鋼材の被覆方法、及び鋼材 Download PDFInfo
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- JP2022067441A JP2022067441A JP2020176150A JP2020176150A JP2022067441A JP 2022067441 A JP2022067441 A JP 2022067441A JP 2020176150 A JP2020176150 A JP 2020176150A JP 2020176150 A JP2020176150 A JP 2020176150A JP 2022067441 A JP2022067441 A JP 2022067441A
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- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- JCBJVAJGLKENNC-UHFFFAOYSA-M potassium ethyl xanthate Chemical compound [K+].CCOC([S-])=S JCBJVAJGLKENNC-UHFFFAOYSA-M 0.000 description 1
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- RUELTTOHQODFPA-UHFFFAOYSA-N toluene 2,6-diisocyanate Chemical compound CC1=C(N=C=O)C=CC=C1N=C=O RUELTTOHQODFPA-UHFFFAOYSA-N 0.000 description 1
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- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 1
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- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
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- 238000004383 yellowing Methods 0.000 description 1
- NDKWCCLKSWNDBG-UHFFFAOYSA-N zinc;dioxido(dioxo)chromium Chemical compound [Zn+2].[O-][Cr]([O-])(=O)=O NDKWCCLKSWNDBG-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
また、本発明は、耐食性及び耐候性を維持し、かつ、金属表面に好ましい意匠性を付与できる鋼材用の被膜、鋼材の被覆方法及び鋼材を提供することを目的とする。
本実施形態に係る鋼材用水性被覆剤は、ポリウレタン樹脂粒子(A-1)(以下、単に「樹脂粒子(A-1)」と記載する場合がある)と、エチレン-不飽和カルボン酸共重合樹脂粒子(A-2)(以下、単に「樹脂粒子(A-2)」と記載する場合がある)と、酸化ケイ素粒子(B)と、有機チタン化合物(C)と、フタロシアニン顔料(F)と、を有する。また、ワックス粒子(D)と、酸化ケイ素粒子(E)と、を含んでいてもよい。
本実施形態に係る鋼材用水性被覆剤により形成される被膜(以下、単に「被膜」と記載する場合がある)は、上記各成分が複合化した複合化樹脂からなる。即ち、各成分の官能基が結合を形成し、複合化された状態である。上記結合は、主に樹脂粒子(A-1)及び(A-2)のSi-OH基、及びSi-OR基の少なくともいずれか、酸化ケイ素粒子(B)、(E)表面のSi-OH基、有機チタン化合物(C)のTi-OH及びTi-OR’基の少なくともいずれか等が反応することによって形成される結合である。上記結合は、例えば、Si-O-Si結合、Si-O-Ti-O-Si結合等であると考えられ、有機樹脂粒子と無機粒子とが化学的に強固な結合を形成する。
本実施形態に係る鋼材は、鋼材(基材)と、鋼材(基材)上に配置されためっき層と、めっき層の表面に配置された被膜とを備える。被膜は、上述したように、ポリウレタン樹脂粒子及びエチレン-不飽和カルボン酸共重合樹脂粒子を含む樹脂と、酸化ケイ素粒子と、Tiと、フタロシアニン顔料とを含む。フタロシアニン顔料の含有量は、ポリウレタン樹脂粒子とエチレン-不飽和カルボン酸共重合樹脂粒子との合計100質量部に対して、0.01~10質量部である。また、フタロシアニン顔料の一次粒子径は0.01~1.0μmである。
(製造例1)
反応容器に4,4-メチレンビス(シクロヘキシルイソシアネート)、分子量2000のポリカーボネートジオール、ネオペンチルグリコール、ジメチロールプロピオン酸、及び溶剤としてN-メチルピロリドンを仕込み、80℃において6時間撹拌後、ジメチルエタノールアミンで中和してポリウレタンプレポリマー溶液を得た。次に、ヒドラジン及びγ-(2-アミノエチル)アミノプロピルトリエトキシシランを含有する水中に、上記反応により得られたポリウレタンプレポリマー溶液をホモディスパーを用いて分散させることにより、シラノール基及び/又はエトキシシリル基を含有するポリカーボネート系ポリウレタン樹脂粒子の水分散液を得た。固形分濃度は30質量%、動的光散乱法によって測定したメジアン径は39nmであった。
上記製造例1と同様にして得られたポリウレタンプレポリマーを、ホモディスパーを用いて、ヒドラジン及びγ-(2-アミノエチル)アミノプロピルメチルジメトキシシランを含有する水中に、上記反応により得られたポリウレタンプレポリマー溶液をホモディスパーを用いて分散させることにより、シラノール基及び/又はエトキシシリル基を含有するポリカーボネート系ポリウレタン樹脂粒子の水分散液を得た。固形分濃度は30質量%、動的光散乱法によって測定したメジアン径は20nmであった。
反応容器に4,4-メチレンビス(シクロヘキシルイソシアネート)、ジメチロールプロピオン酸、及びアセトンを加え、攪拌下50℃に加熱して反応させたのち、更に、アジピン酸、ネオペンチルグリコール、及びエチレングリコールとの反応により得られた分子量2000のポリエステルポリオールを加えて反応させてポリウレタンプレポリマー溶液を得た。次いで、ジメチルエタノールアミン、γ-(2-アミノエチル)アミノプロピルトリエトキシシラン、及び2-(2-アミノエチルアミノ)エタノールを含有する水中に、上記反応により得られたポリウレタンプレポリマー溶液をホモディスパーを用いて分散させ、加熱下にアセトンを留去することにより、シラノール基及び/又はエトキシシリル基を含有するポリエステル系ポリウレタン樹脂粒子の水分散液を得た。固形分濃度は30質量%、メジアン径は32nmであった。
(製造例4)
反応容器にエチレン-メタクリル酸共重合樹脂(メタクリル酸の含有量が20質量%)、樹脂に対して5.6質量%相当の水酸化ナトリウム及び脱イオン水を加え、95℃で6時間攪拌することにより固形分20質量%の水分散樹脂液を得た。この水分散樹脂液に対して、更にγ-グリシドキシプロピルトリメトキシシランを0.8質量%、グリセロールポリグリシジルエーテルを0.8質量%を加えて、85℃で2時間反応させることによって、シラノール基及び/又はメトキシシリル基を有するエチレン-メタクリル酸共重合樹脂粒子の水分散液を得た。固形分濃度は21質量%、メジアン径は50nmであった。
反応容器にエチレン-メタクリル酸共重合樹脂(メタクリル酸の含有量が20質量%)、樹脂に対して3.7質量%の水酸化ナトリウム、6.3質量%のアンモニア水、及び脱イオン水を加え、95℃で6時間攪拌することにより固形分20質量%の水分散樹脂液を得た。この水分散樹脂液に対して、更にγ-グリシドキシプロピルトリエトキシシランを1.2質量%、ペンタエリスリトールポリグリシジルエーテルを0.6質量%を加えて、85℃で2時間反応させることによって、シラノール基及び/又はメトキシシリル基を有するエチレン-メタクリル酸共重合樹脂粒子の水分散液を得た。固形分濃度は21質量%、メジアン径は100nmであった。
反応容器にエチレン-メタクリル酸共重合樹脂(メタクリル酸の含有量が20質量%)、樹脂に対して4.7質量%相当の水酸化ナトリウム及び脱イオン水を加え、95℃で2時間攪拌することにより固形分20質量%の水分散樹脂液を得た。この水分散樹脂液に対して、更にγ-グリシドキシプロピルトリメトキシシランを1.2質量%、水添ビスフェノールAジグリシジルエーテルを1.2質量%加えて、85℃で2時間反応させることによって、シラノール基及び/又はメトキシシリル基を有するエチレン-メタクリル酸共重合樹脂粒子の水分散液を得た。固形分濃度は21質量%、メジアン径は70nmであった。
反応容器にエチレン-メタクリル酸共重合樹脂(メタクリル酸の含有量が20質量%)、樹脂に対して21.0質量%のアンモニア水、及び脱イオン水を加え、95℃で2時間攪拌することにより固形分20質量%の水分散樹脂液を得た。この水分散樹脂液に対して、更にγ-グリシドキシプロピルトリメトキシシランを1.2質量%、水添ビスフェノールAジグリシジルエーテルを1.2質量%加えて、85℃で2時間反応させることによって、シラノール基及び/又はメトキシシリル基を有するエチレン-メタクリル酸共重合樹脂粒子の水分散液を得た。固形分濃度は21質量%、メジアン径は150nmであった。
反応容器にエチレン-メタクリル酸共重合樹脂(メタクリル酸の含有量が27質量%)、樹脂に対して28.0質量%のアンモニア水及び脱イオン水を加え、95℃で2時間攪拌することにより固形分20質量%の水分散樹脂液を得た。この水分散樹脂液に対して、さらにγ-グリシドキシプロピルトリメトキシシランを1.6質量%、水添ビスフェノールA ジグリシジルエーテルを1.6質量%加えて、85℃で2時間反応させることによって、シラノール基及び/又はメトキシシリル基を有するエチレン-メタクリル酸共重合樹脂粒子の水分散液を得た。固形分濃度は21質量% 、メジアン径は14nmであった。
反応容器にエポキシ当量190のビスフェノールFエピクロルヒドリン型エポキシ樹脂190質量部にジエタノールアミン30質量部、プロピレングリコールモノメチルエーテルアセテート110質量部を加え、100℃で2時間反応させ、固形分濃度70%の変性エポキシ樹脂を得た。反応容器にNCOが13.3%、不揮発分75%のトリメチロールプロパンの2,4-トルエンジイソシアネートプレポリマーを100質量部、ノニルフェノール44質量部、ジメチルベンジルアミン5質量部、プロピレングリコールモノメチルエーテルアセテート65質量部を混合し、窒素雰囲気下80℃で3時間、反応させ、固形分濃度70%、NCO%が20%のハーフブロック化ポリイソシアネートを得た。上記変性エポキシ樹脂70質量部と上記ハーフブロック化ポリイソシアネート30質量部を混合し、80℃で4時間攪拌して反応させた後、赤外線分光分析でNCO基の吸収が完全になくなることを確認した。その後、イオン交換水で希釈して水性エポキシ樹脂を得た。固形分濃度は25質量%、メジアン径は600nmであった。
(実施例1)
上記製造例1の樹脂粒子(A-1)の水分散液を固形分換算で80質量部と、上記製造例4の樹脂粒子(A-2)の水分散液を固形分換算で20質量部用いた。酸化ケイ素粒子(B)としては、粒子径(モード径)が15nmのものを用いた。有機チタン化合物(C)としては、ジプロポキシビス(トリエタノールアミナト)チタンを用いた。ワックス粒子(D)としては、粒子径(メジアン径)1.0μm、軟化点115℃のポリエチレン粒子を用いた。酸化ケイ素粒子(E)としては、粒子径(モード径)100nmのものを用いた。フタロシアニン顔料(F)としては、被覆剤として界面活性剤を用いたCuフタロシアニン(一次粒子径0.26μm)を用いた。防錆剤(G)としては、リン酸塩及びチオ尿素を用いた。各成分の含有量は、樹脂粒子(A-1)と樹脂粒子(A-2)の合計100質量部に対する質量部として、表6に示す量を用いて、実施例1に係る鋼材用被覆調整剤を調製した。なお、表6に示す有機チタン化合物(C)の含有量は、チタン原子換算の質量部である。
それぞれ表6に示す原料を用いたこと以外は、実施例1と同様として、実施例2~18、及び比較例1~20に係る鋼材用被覆調整剤を調製した。また比較例12を60℃で経時させて高粘度に調整したものを比較例21とした。なお、表6に示す酸化ケイ素粒子(B)、有機チタン化合物(C)、酸化ケイ素粒子(E)、フタロシアニン顔料(F)及び防錆剤(G)の種類と、表6に示す記号との対応は、以下の表1~表5に示した。
種類k:御国色素株式会社製 「SAブルー 5204」
種類l:トーヨーカラー株式会社製 「LIOFAST SF670ブルー」
種類m:御国色素株式会社製 「SAブルー 5205」
種類n:大日精化工業株式会社社製 「DPカラー 1737 Blue」
種類o:大日精化工業株式会社社製 「DPカラー 1534 Blue」
種類p:大日精化工業株式会社社製 「DP-1957 Yellow」
種類q:大日精化工業株式会社社製 「NAF カラー NAF1032レッド」
種類r:トーヨーカラー株式会社製 「LIOFAST BLUE G227」
種類s:トーヨーカラー株式会社製 「EMF BLUE HG」
種類t:御国色素株式会社製 「PSMスカイブルー FG」
種類u:大日精化工業株式会社社製 「TBカラー TB-700 Blue GA」
上記実施例1~18、比較例1~21の鋼材用水性被覆剤を用い、溶融亜鉛めっき鋼板及びアルミニウム含有亜鉛めっき鋼材の表面に被膜を形成し、評価用サンプルを作成した。鋼材用水性被覆剤の塗布はバーコーターで、乾燥皮膜量1g/m2になるように塗布し、雰囲気温度500℃の熱風乾燥炉を用いて到達板温150℃まで焼き付けて試験板を作成した。
上記作製した実施例及び比較例に係る試験板を用い、耐アルカリ性、耐溶剤性、耐アブレージョン性、平面耐食性、耐候性(彩度変化量)、光沢度、彩度、塗装性について以下の条件で評価を行った。結果を表7に示した。
試験板を55℃のアルカリ脱脂剤(サーフクリーナー53、日本ペイント社製)2質量%水溶液(pH12.5)に攪拌しながら2分間浸漬した後、試験板のエッジと裏面をテープシールし、塩水噴霧試験(JIS-Z-2371)を行った。72時間後の白錆発生状況を観察し下記基準で評価を行い、3を合格とした。結果を表7に示す。
3:白錆ほとんどなし
2:白錆面積30%未満
1:白錆面積30%以上
試験板をラビングテスターに設置後、エタノール、メチルエチルケトン(MEK)又はホワイトガソリンを含浸させた脱脂綿を0.5kgf/cm2の荷重で5回(往復)、擦った後、試験板のエッジと裏面をテープシールし、塩水噴霧試験(JIS-Z-2371)を行った。72時間後の白錆発生状況を観察し下記基準で評価を行い、3を合格とした。結果を表7に示す。
3:白錆ほとんどなし
2:白錆面積30%未満
1:白錆面積30%以上
試験板に、段ボール紙を介して10g/cm2の荷重をかけ、360回/minの楕円運動を加えて摺動部にアブレージョン(摩耗傷)を発生させた。10分間試験を行った後の試験板表面の状態を観察し下記基準で評価を行い、3を合格とした。結果を表7に示す。
3:黒化ほとんどなし
2:摺動部の50%未満の面積が黒化
1:摺動部の50%以上の面積が黒化
試験板を、試験板のエッジと裏面をテープシールし、塩水噴霧試験SST(JIS-Z-2371)を行った。溶融亜鉛めっきの試験片では72時間後、アルミニウム含有亜鉛めっきの試験片は120時間後の白錆発生状況を観察し下記基準で評価を行い、3を合格とした。結果を表7に示す。
3:白錆ほとんどなし
2:白錆面積30%未満
1:白錆面積30%以上
試験板をサンシャインウェザーメーター試験機にいれ、促進耐候試験500時間を実施し、初期値と試験後の彩度の変化量を測定した。彩度は以下に示す彩度測定と同様の方法で、彩度C*として算出した。彩度C*の変化量は以下式(2)にて算定し、以下の基準で評価を行い、3を合格とした。試験機はスガ試験機株式会社製サンシャインウェザーメーターを用いた。結果を表7に示す。
変化量(%)=試験後彩度C*/初期値彩度C*×100 …(2)
3:変化量(%)=95%~100%
2:変化量(%)=90%~95%未満
1:変化量(%)=80%~90%未満
光沢計(日本電色工業株式会社製 VG2000)を用い、JIS Z 8741に規定される方法に基づいて試験板表面の60°光沢度(%)を測定した。以下の基準で評価を行い、2を合格とした。結果を表7に示す。
2:50~200%
1:50%未満
分光色差計(日本電色工業株式会社製 SE6000)を用い、試験板表面のL*a*b*値を測定し、以下の式により彩度C*を算出した。以下の基準で評価を行い、3を合格とした。結果を表7に示す。
3:C*=2.0~50
2:C*=50超、100未満
1:C*=2.0未満
自動バーコーター(安田精機製作所製 No 542-AB)を用い、鋼材用水性被覆剤を塗布し、塗装外観ムラを以下の基準で評価を行い、2を合格とした。結果を表7に示す。
2:ムラなし
1:ムラあり
Claims (9)
- それぞれ、メジアン径が20~100nmであり、かつ、シラノール基及びアルコキシシリル基のうち少なくともいずれかを有する、ポリウレタン樹脂粒子(A-1)及びエチレン-不飽和カルボン酸共重合樹脂粒子(A-2)と、
モード径が5~20nmである酸化ケイ素粒子(B)と、
有機チタン化合物(C)と、
樹脂及び界面活性剤のうち、少なくともいずれかで被覆されたフタロシアニン顔料(F)と、を有し、
前記フタロシアニン顔料(F)の含有量は、前記ポリウレタン樹脂粒子(A-1)と、前記エチレン-不飽和カルボン酸共重合樹脂粒子(A-2)との合計100質量部に対して、0.01~10質量部であり、一次粒子径は、0.01~1.0μmである、鋼材用水性被覆剤。 - 前記フタロシアニン顔料(F)におけるフタロシアニンは、金属フタロシアニン及び無金属フタロシアニンのうち少なくともいずれかであり、
前記金属フタロシアニンの金属は、Ca、Ba、Cd、Na、Cu、Ni、Co、Fe、Mg、Zn、Al、Mn、V、Ti及びSnのうちいずれかである、請求項1に記載の鋼材用水性被覆剤。 - 20℃粘度が100mPa・s以下である、請求項1又は2に記載の鋼材用水性被覆剤。
- 前記ポリウレタン樹脂粒子(A-1)と、前記エチレン-不飽和カルボン酸共重合樹脂粒子(A-2)との質量比は、(A-1):(A-2)=20:80~90:10である、請求項1~3のいずれか一項に記載の鋼材用水性被覆剤。
- モード径が70~200nmである酸化ケイ素粒子(E)を更に有する、請求項1~4のいずれか一項に記載の鋼材用水性被覆剤。
- 請求項1~5のいずれか一項に記載の鋼材用水性被覆剤により形成され、彩度C*が2.0以上50以下である、被膜。
- 請求項1~5のいずれか一項に記載の鋼材用水性被覆剤を鋼材表面に塗布して被膜を形成する、鋼材の被覆方法。
- 請求項1~5のいずれかに記載の鋼材用水性被覆剤により、表面に被膜が形成され、60°光沢度が50%以上である、鋼材。
- 前記鋼材は、溶融亜鉛めっき鋼及びアルミニウム含有亜鉛めっき鋼のうちいずれかである、請求項8に記載の鋼材。
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