JP2019112644A - 耐黒変性及び耐食性に優れたクロムフリーコーティング組成物及び表面処理鋼板 - Google Patents
耐黒変性及び耐食性に優れたクロムフリーコーティング組成物及び表面処理鋼板 Download PDFInfo
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- JP2019112644A JP2019112644A JP2019026183A JP2019026183A JP2019112644A JP 2019112644 A JP2019112644 A JP 2019112644A JP 2019026183 A JP2019026183 A JP 2019026183A JP 2019026183 A JP2019026183 A JP 2019026183A JP 2019112644 A JP2019112644 A JP 2019112644A
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- chromium
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- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical group CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 3
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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 claims 1
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Classifications
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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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
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- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
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- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
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- B32B15/095—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin comprising polyurethanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08G18/0819—Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups
- C08G18/0823—Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups containing carboxylate salt groups or groups forming them
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/34—Carboxylic acids; Esters thereof with monohydroxyl compounds
- C08G18/348—Hydroxycarboxylic acids
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- C—CHEMISTRY; METALLURGY
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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Abstract
Description
H2NCH2CH2NHCH2CH2CH2−Si−(CxH2x+1)3−z(OCyH2y+1)z
(上記化学式において、xは1〜2の整数であり、y及びzは1〜3の整数である。)
H2NCH2CH2NHCH2CH2CH2−Si−(CxH2x+1)3−z(OCyH2y+1)z
(上記化学式において、xは1〜2の整数であり、y及びzは1〜3の整数である。)
2Lのフラスコ、攪拌機、加熱用メントール、コンデンサ及び温度計を準備し、イソホロンジイソシアネート(IPDI)240g、ポリカーボネートジオール(分子量500)350g、N−メチルピロリドン(NMP)溶剤110gを上記フラスコに投入し、窒素をフラスコ内部に充填して95℃で2時間反応させた。以後、90℃に冷却した後、ジメチロールプロピオン酸(DMPA)35g、トリメチロールプロパン(TMP)15g及びキシレンに10%希釈したジブチル錫ジラウレート(DBTDL)1gを反応器に投入した。投入が終わった後、NCO valueを測定して、5以下になるまで反応温度を維持し、反応が完了したプレポリマーを80℃に冷却させた後、3価アミンであるトリエチルアミン(TEA)を使用して中和させた。
合成例1のように水分散ポリウレタンの製造が完了した状態で、アミノシラン系製品であるKBM−603(日本信越社製)20g及び30%のヒドラジンハイドレート50gをそれぞれ10分間均一滴下させた。均一滴下が完了すると、50℃で2時間反応を維持し、反応が終わった後、固形分34%の均質なシラン変性水分散ポリウレタンを得た。
合成例2と同様に装置と過程を経るが、鎖延長剤を下記の表1のように投入反応して、シラン変性水分散ポリウレタンを製造した。
ASTM B117に規定した方法に基づいて、表面処理鋼板の時間経過とともに白錆発生率(72時間基準)を確認して平板耐食性を評価した。
◎:白錆が発生せず
○:5%未満の白錆発生
X:5%以上の白錆発生
液温40〜45℃で強アルカリ脱脂剤(FC−4460、日本パーカライジング製造)20g/Lに準備した試片を2分間浸漬した後、流水に水洗して乾燥した後、外観の変色や剥離有無を評価した。
◎:無変色、無剥離
○:色差1以内の変色、無剥離
X:剥離
50℃、95%RHが維持される恒温恒湿器に10〜20kgf/cmの圧力で試片を120時間放置して、実験前後の色相変化(ΔE)を測定し、下記の基準によって評価した。
◎:ΔE<2
○:2≦≦ΔE<3
X:ΔE≧≧3
純度98%以上のエタノールとアセトンを十分に含ませたガーゼを準備し、試片に対して、5Nの力で溶剤を含ませたガーゼを5回往復した後、外観の変化を評価した。
◎:外観変化なし
○:往復3回以上で剥離
X:往復3回未満で剥離
アクリルメラミン系焼付型塗料を試片に厚さ30μmとなるようにスプレー塗装乾燥後、1mm間隔の100個のマスが出るようにコーティング層に微細切れ目を入れた。以後、マス部分にセロハンテープで付着性を評価した。
◎:マス脱落なし
○:マス1つの一部分脱落
X:マス1つ以上脱落
準備された試片にワセリンの塗布1時間前後の色差値(ΔL)を測定評価した。
◎:ΔL<1
○:1≦≦ΔE<2
X:ΔE≧≧2
Claims (12)
- シラン変性水分散ポリウレタン20〜70重量%、硬化剤0.5〜5重量%、黒変防止剤0.5〜5重量%、防錆剤0.5〜5重量%、潤滑剤0.5〜5重量%及び残部溶媒を含む、耐黒変性及び耐食性に優れたクロムフリーコーティング組成物。
- 前記シラン変性水分散ポリウレタンは、数平均分子量が10,000〜60,000である、請求項1に記載の耐黒変性及び耐食性に優れたクロムフリーコーティング組成物。
- 前記シラン変性水分散ポリウレタンは、シラン変性水分散ポリウレタン全量に対して、有機シランの含量が1〜5重量%である、請求項1に記載の耐黒変性及び耐食性に優れたクロムフリーコーティング組成物。
- 前記有機シランは、下記化学式の構造を有する化合物である、請求項3に記載の耐黒変性及び耐食性に優れたクロムフリーコーティング組成物。
H2NCH2CH2NHCH2CH2CH2−Si−(CxH2x+1)3−z(OCyH2y+1)z
(前記化学式において、xは1〜2の整数であり、y及びzは1〜3の整数である。) - 前記有機シランは、
N−(2−アミノエチル)−3−アミノプロピルメチルジメトキシシラン、
N−(2−アミノエチル)−3−アミノプロピルトリメトキシシラン、
N−(2−アミノエチル)−3−アミノプロピルトリエトキシシラン、及び
N−(2−アミノエチル)−3−アミノプロピルトリプロポキシシランからなる群より選択されたいずれか一つ以上である、請求項3に記載の耐黒変性及び耐食性に優れたクロムフリーコーティング組成物。 - 前記硬化剤は、
3−グリシドキシプロピルトリメトキシシラン、
3−グリシドキシプロピルトリエトキシシラン、
3−グリシドキシプロピルトリプロピルシラン、
3−グリシドキシプロピルトリイソプロピルシラン、
2−(3,4−エポキシシクロヘキシル)エチルトリメトキシシラン、及び
2−(3,4−エポキシシクロヘキシル)エチルトリエトキシシランからなる群より選択されたいずれか一つ以上である、請求項1に記載の耐黒変性及び耐食性に優れたクロムフリーコーティング組成物。 - 前記黒変防止剤は、ニッケル化合物、バナジウム系化合物、ジルコニウム系化合物、セリウム系化合物及びモリブデン系化合物からなる群より選択されたいずれか一つ以上である、請求項1に記載の耐黒変性及び耐食性に優れたクロムフリーコーティング組成物。
- 前記防錆剤は、リチウムシリケート、ナトリウムシリケート及びカリウムシリケートからなる群より選択されたいずれか一つ以上である、請求項1に記載の耐黒変性及び耐食性に優れたクロムフリーコーティング組成物。
- 前記防錆剤は、防錆剤全量に対して、金属の含量が0.1〜2重量%である、請求項1に記載の耐黒変性及び耐食性に優れたクロムフリーコーティング組成物。
- マグネシウムを含有する鋼板と、
前記鋼板の少なくとも一面に形成されるコーティング層とを含み、
前記コーティング層は、請求項1乃至9のいずれか一項に記載のクロムフリーコーティング組成物の硬化物である、耐黒変性及び耐食性に優れた表面処理鋼板。 - 前記コーティング層は、乾燥皮膜付着量が300〜1200mg/m2である、請求項10に記載の耐黒変性及び耐食性に優れた表面処理鋼板。
- 前記クロムフリーコーティング組成物は、硬化温度が70〜180℃である、請求項10に記載の耐黒変性及び耐食性に優れた表面処理鋼板。
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