JP4958877B2 - 表面処理金属板 - Google Patents
表面処理金属板 Download PDFInfo
- Publication number
- JP4958877B2 JP4958877B2 JP2008271345A JP2008271345A JP4958877B2 JP 4958877 B2 JP4958877 B2 JP 4958877B2 JP 2008271345 A JP2008271345 A JP 2008271345A JP 2008271345 A JP2008271345 A JP 2008271345A JP 4958877 B2 JP4958877 B2 JP 4958877B2
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- JP
- Japan
- Prior art keywords
- resin
- mass
- acrylic
- parts
- meth
- 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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- 229910052751 metal Inorganic materials 0.000 title claims description 64
- 239000002184 metal Substances 0.000 title claims description 64
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- 239000011347 resin Substances 0.000 claims description 173
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 116
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 claims description 76
- -1 glycidoxy group Chemical group 0.000 claims description 72
- OAKJQQAXSVQMHS-UHFFFAOYSA-N hydrazine group Chemical group NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 49
- 239000000178 monomer Substances 0.000 claims description 49
- 229920002803 thermoplastic polyurethane Polymers 0.000 claims description 42
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 41
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 35
- 239000004814 polyurethane Substances 0.000 claims description 34
- 229920002635 polyurethane Polymers 0.000 claims description 33
- 229920000058 polyacrylate Polymers 0.000 claims description 29
- 239000002253 acid Substances 0.000 claims description 23
- 239000002245 particle Substances 0.000 claims description 21
- 239000000126 substance Substances 0.000 claims description 21
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 claims description 18
- 229920005862 polyol Polymers 0.000 claims description 18
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- 239000011342 resin composition Substances 0.000 claims description 11
- 125000003545 alkoxy group Chemical group 0.000 claims description 6
- 125000000217 alkyl group Chemical group 0.000 claims description 4
- 125000002947 alkylene group Chemical group 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 2
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- 238000000576 coating method Methods 0.000 description 25
- 238000004519 manufacturing process Methods 0.000 description 25
- 229910001335 Galvanized steel Inorganic materials 0.000 description 24
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 24
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- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 18
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- 125000000524 functional group Chemical group 0.000 description 9
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- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 9
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- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 8
- 125000004432 carbon atom Chemical group C* 0.000 description 8
- 239000007810 chemical reaction solvent Substances 0.000 description 8
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- 238000001035 drying Methods 0.000 description 8
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- 238000011282 treatment Methods 0.000 description 8
- 239000011701 zinc Substances 0.000 description 8
- 229910052725 zinc Inorganic materials 0.000 description 8
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 7
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- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 7
- 239000003505 polymerization initiator Substances 0.000 description 7
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- 241001163841 Albugo ipomoeae-panduratae Species 0.000 description 6
- YIMQCDZDWXUDCA-UHFFFAOYSA-N [4-(hydroxymethyl)cyclohexyl]methanol Chemical compound OCC1CCC(CO)CC1 YIMQCDZDWXUDCA-UHFFFAOYSA-N 0.000 description 6
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- RXKJFZQQPQGTFL-UHFFFAOYSA-N dihydroxyacetone Chemical compound OCC(=O)CO RXKJFZQQPQGTFL-UHFFFAOYSA-N 0.000 description 6
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- 239000000377 silicon dioxide Substances 0.000 description 6
- 230000002194 synthesizing effect Effects 0.000 description 6
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 6
- 239000001993 wax Substances 0.000 description 6
- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical compound OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 description 5
- 239000004970 Chain extender Substances 0.000 description 5
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 5
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 5
- 150000002429 hydrazines Chemical class 0.000 description 5
- OMNKZBIFPJNNIO-UHFFFAOYSA-N n-(2-methyl-4-oxopentan-2-yl)prop-2-enamide Chemical compound CC(=O)CC(C)(C)NC(=O)C=C OMNKZBIFPJNNIO-UHFFFAOYSA-N 0.000 description 5
- KIDHWZJUCRJVML-UHFFFAOYSA-N putrescine Chemical compound NCCCCN KIDHWZJUCRJVML-UHFFFAOYSA-N 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- RPACBEVZENYWOL-XFULWGLBSA-M sodium;(2r)-2-[6-(4-chlorophenoxy)hexyl]oxirane-2-carboxylate Chemical compound [Na+].C=1C=C(Cl)C=CC=1OCCCCCC[C@]1(C(=O)[O-])CO1 RPACBEVZENYWOL-XFULWGLBSA-M 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 239000005057 Hexamethylene diisocyanate Substances 0.000 description 4
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 4
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- 150000007513 acids Chemical class 0.000 description 4
- IBVAQQYNSHJXBV-UHFFFAOYSA-N adipic acid dihydrazide Chemical compound NNC(=O)CCCCC(=O)NN IBVAQQYNSHJXBV-UHFFFAOYSA-N 0.000 description 4
- 150000001412 amines Chemical class 0.000 description 4
- 150000004985 diamines Chemical class 0.000 description 4
- 235000014113 dietary fatty acids Nutrition 0.000 description 4
- 239000000194 fatty acid Substances 0.000 description 4
- 229930195729 fatty acid Natural products 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 4
- 239000003112 inhibitor Substances 0.000 description 4
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- 239000002685 polymerization catalyst Substances 0.000 description 4
- 230000000379 polymerizing effect Effects 0.000 description 4
- JVYDLYGCSIHCMR-UHFFFAOYSA-N 2,2-bis(hydroxymethyl)butanoic acid Chemical compound CCC(CO)(CO)C(O)=O JVYDLYGCSIHCMR-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
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- 229920000178 Acrylic resin Polymers 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
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- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- SJRJJKPEHAURKC-UHFFFAOYSA-N N-Methylmorpholine Chemical compound CN1CCOCC1 SJRJJKPEHAURKC-UHFFFAOYSA-N 0.000 description 3
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- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 3
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- 239000003760 tallow Substances 0.000 description 1
- MUTNCGKQJGXKEM-UHFFFAOYSA-N tamibarotene Chemical compound C=1C=C2C(C)(C)CCC(C)(C)C2=CC=1NC(=O)C1=CC=C(C(O)=O)C=C1 MUTNCGKQJGXKEM-UHFFFAOYSA-N 0.000 description 1
- SJMYWORNLPSJQO-UHFFFAOYSA-N tert-butyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC(C)(C)C SJMYWORNLPSJQO-UHFFFAOYSA-N 0.000 description 1
- YBRBMKDOPFTVDT-UHFFFAOYSA-N tert-butylamine Chemical compound CC(C)(C)N YBRBMKDOPFTVDT-UHFFFAOYSA-N 0.000 description 1
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- IUTCEZPPWBHGIX-UHFFFAOYSA-N tin(2+) Chemical class [Sn+2] IUTCEZPPWBHGIX-UHFFFAOYSA-N 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 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
- VOZKAJLKRJDJLL-UHFFFAOYSA-N tolylenediamine group Chemical group CC1=C(C=C(C=C1)N)N VOZKAJLKRJDJLL-UHFFFAOYSA-N 0.000 description 1
- 238000013518 transcription Methods 0.000 description 1
- 230000035897 transcription Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- KEROTHRUZYBWCY-UHFFFAOYSA-N tridecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCCOC(=O)C(C)=C KEROTHRUZYBWCY-UHFFFAOYSA-N 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 1
- 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
- QXJQHYBHAIHNGG-UHFFFAOYSA-N trimethylolethane Chemical compound OCC(C)(CO)CO QXJQHYBHAIHNGG-UHFFFAOYSA-N 0.000 description 1
- MBYLVOKEDDQJDY-UHFFFAOYSA-N tris(2-aminoethyl)amine Chemical compound NCCN(CCN)CCN MBYLVOKEDDQJDY-UHFFFAOYSA-N 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/48—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
- C23C2/04—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor characterised by the coating material
- C23C2/06—Zinc or cadmium or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/22—Electroplating: Baths therefor from solutions of zinc
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
- C23C2222/20—Use of solutions containing silanes
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Metallurgy (AREA)
- Mechanical Engineering (AREA)
- Wood Science & Technology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Laminated Bodies (AREA)
- Paints Or Removers (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Description
(1−1)アクリルウレタン系樹脂
本発明で使用されるアクリルウレタン系樹脂は、(メタ)アクリル系ポリマーと、ポリウレタンとを含む。このように、(メタ)アクリル系ポリマーとポリウレタンとを併用するのは、樹脂成分を(メタ)アクリル系ポリマーのみとすると、高い硬度を有する樹脂皮膜となるため加工性(耐黒化性)は確保されるものの、柔軟性が低いため、樹脂皮膜にクラックが入り、耐食性の低下が生じ易くなる。そこで、得られる樹脂皮膜に柔軟性を与えることができ、且つ、耐薬品性、耐摩耗性に優れ、さらに、得られる樹脂皮膜に強靭さを与え得るポリウレタンを(メタ)アクリル系ポリマーと併用することとし、樹脂皮膜(表面処理金属板)の加工性と柔軟性を両立させた。
2:アクリルウレタン系樹脂が、少なくとも1種のポリウレタンと、少なくとも1種の(メタ)アクリル系ポリマーとが、それぞれカルボニル基を有し、且つ、少なくとも2個のヒドラジン基を有する化合物を含む態様、
3:アクリルウレタン系樹脂が、少なくとも1種のポリウレタンと、少なくとも1種の(メタ)アクリル系ポリマーとが、それぞれヒドラジン基を有し、且つ、少なくとも2個のカルボニル基を有する化合物を含む態様。
本発明で使用する皮膜形成用樹脂組成物は、上述したアクリルウレタン系樹脂30〜50質量部および、平均粒子径が4〜20nmのシリカ粒子50〜70質量部を合計で100質量部になるように含有し、前記合計100質量部に対して、さらにシランカップリング剤を5〜25質量部の比率で含有することを特徴とする。なお、アクリルウレタン系樹脂の水性分散体を用いる場合は、アクリルウレタン系樹脂水性分散体の不揮発性樹脂成分を30〜50質量部とすることが好ましい。
本発明で使用される皮膜形成用樹脂組成物は、上述したアクリルウレタン系樹脂30〜50質量部に対して、シリカ粒子を50質量部以上、好ましくは60質量部以上であって、70質量部以下、好ましくは65質量部以下含有する(ただし、アクリルウレタン系樹脂成分とシリカ粒子との合計量を100質量部とする)。
本発明で使用する皮膜形成用樹脂組成物は、シランカップリング剤を含有する。シランカップリング剤は、耐食性、深絞り加工性、塗装性等の向上に加えて、金属板と金属板上に形成される樹脂皮膜との密着性の向上にも寄与する。
本発明では、より強固な皮膜を形成させるため、官能基間反応を利用した化学結合によってポリマー鎖同士を架橋させてもよい。このポリマー鎖同士の架橋形成に用いられる架橋剤としては、カルボキシル基と反応し得る官能基を1分子中に2個以上有する架橋剤であれば特に限定されず、例えば、ソルビトールポリグリシジルエーテル、(ポリ)グリセロールポリグリシジルエーテル、ペンタエリストールポリグリシジルエーテル、トリメチロールプロパンポリグリシジルエーテル、ネオペンチルグリコールジグリシジルエーテル、(ポリ)エチレングリコールグリシジルエーテル等のポリグリシジルエーテル類や、ポリグリシジルアミン類等のグリシジル基含有架橋剤;4,4−ビス(エチレンイミンカルボニルアミノ)ジフェニルメタン、N,N−ヘキサメチレン−1,6−ビス(1−アジリジンカルボキシアミド)、N,N−ジフェニルメタン−4,4−ビス(1−アジリジンカルボキシアミド)、トルエンビスアジリジンカルボキシアミド等の2官能アジリジン化合物;トリ−1−アジリジニルホスフィンオキサイド、トリス〔1−(2−メチル)アジリジニル〕ホスフィンオキサイド、トリメチロ−ルプロパントリス(β−アジリジニルプロピオネート)、トリス−2,4,6−(1−アジリジニル)−1,3,5−トリアジン、テトラメチルプロパンテトラアジリジニルプロピオネート等の3官能以上のアジリジン化合物あるいはこれらの誘導体等のアジリジニル基含有架橋剤が好適例として挙げられ、これらのうちの1種または2種以上を用いることができる。
本発明の表面処理金属板(樹脂皮膜)の製造には、上記皮膜形成用樹脂組成物が水あるいは水を主成分とする溶媒に分散された樹脂水性分散液を用いる。本発明で使用する樹脂水性分散液には、樹脂塗膜の形成及び得られる皮膜の物性を向上させるため、本発明の目的を阻害しない範囲で、希釈溶媒、皮張り防止剤、レべリング剤、消泡剤、浸透剤、乳化剤、造膜助剤、着色顔料、増粘剤、および潤滑剤等を含有させてもよい。
得られた表面処理金属板(樹脂塗装鋼板)について、エッジシールをした平板材の塩水噴霧試験をJIS−Z2371(11.1 中性塩水噴霧試験)に従って実施し、以下の評価基準に沿って、白錆の発生量が、平板材の面積の5%に達するまでの時間にて評価した。
(評価基準)
◎:白錆発生 240時間以上
○:白錆発生 120時間以上〜240時間未満
△:白錆発生 72時間以上〜120時間未満
×:白錆発生 72時間未満
得られた表面処理金属板(樹脂塗装鋼板)について、80トンのクランクプレス装置(アイダエンジニアリング社製、80TONクランクプレス、図5参照)でプレス成形品を作製し、成形品の摺動面の型かじり及び黒化現象(耐黒化性)について目視で観察して評価した。
・しわ押さえ圧=9.8N
・成形速度=40SPM
・ビード高さ=3mm
・ミゾR(r4)=2mm
・ダイR(r3)=0.5mm
・ダイ径:51.640mm
・ポンチ径:50.120mm
◎:かじりが生じている部分の面積が全体の40%未満。
○:かじりが生じている部分の面積が全体の40%以上、60%未満。
△:かじりが生じている部分の面積が全体の60%以上、80%未満。
×:かじりが生じている部分の面積が全体の80%以上。
◎:プレス成形品の摺動面に黒化現象は認められなかった(極めて良い)。
○:良い(図6(a)参照)。
△:悪い。
×:極めて悪い(図6(b)参照)。
得られた表面処理金属板(樹脂塗装鋼板)に、メラミンアルキッド系塗料(関西ペイント社製「アミラック(登録商標)#1000」)を、乾燥後の塗膜厚が約20μmになるようにスプレー塗装し、130℃で20分間焼き付けて、後塗装を行った。続いて、この供試材を沸騰水に1時間浸漬した後、取り出し、室温(25℃)で1時間放置した後、供試材表面に、カッターナイフで1mm角の碁盤目を100升刻み、これにテープ剥離試験(JIS K5600、使用したテープはニチバン社製「セロテープ(登録商標)品番No.405」)を実施して、塗膜の残存升目数によって塗膜密着性を下記4段階の評価基準で評価した。
(評価基準)
◎:残存率 95%以上
○:残存率 80%以上95%未満
△:残存率 70%以上80%未満
×:残存率 70%未満
下記製造例で得られた各樹脂の水系分散体を、縦200mm、横150mmのガラス板上に、#20のバーコーターで塗布して評価用の試料を作成し、前記した方法で、樹脂皮膜のスォードロッカー値を測定し、スォードロッカー硬度を求めた。
樹脂皮膜の軟化点を熱機械分析(TMA:「TMA/SS120」:セイコーインスツルメンツ社製)で測定した。試料は、樹脂の水系分散体を適量ポリテトラフルオロエチレン製の皿に入れて、40℃の乾燥機で12時間以上乾燥させたものとした。測定温度範囲は室温から250℃までとし、昇温速度:5℃/分、測定荷重:5gf、アルゴンガス100ml/minの気流中で、針入法にて行った。
製造例1 アクリルウレタン系樹脂水系分散体1の調製(H−MDI系ウレタンアクリル樹脂)
攪拌機、加熱用ヒーター、温度計、温度コントローラーを備えた内容量1.0Lの加圧対応合成装置に、ポリオール成分として、ダイマー酸、トリメチロールプロパンおよびジエチレングリコールからなるポリエステルポリオール24.3g(「TA22−636」、日立化成ポリマー株式会社製)、1,4−シクロヘキサンジメタノール3.89g、ジメチロールプロピオン酸22.52g、ジヒドロキシアセトン8.82g(Merck Ltd., JAPAN製)を仕込み、ここに、アクリル酸ブチル370.01g,メタクリル酸n−ブチル370.01g,ジアセトンアクリルアミド13.32g,メチルエチルケトン13.32gおよびメトキノン1.51gを混合した反応溶媒96.01gを加えて、系全体が均一に分散するように攪拌した。
攪拌機、加熱用ヒーター、温度計、温度コントローラーを備えた内容量1.0Lの加圧対応合成装置に、ポリオール成分として、ダイマー酸、トリメチロールプロパンおよびジエチレングリコールからなるポリエステルポリオール24.3g(「TA22−636」、日立化成ポリマー株式会社製)、1,4−シクロヘキサンジメタノール3.89g、ジメチロールプロピオン酸22.52g、ジヒドロキシアセトン8.82g(Merck Ltd., JAPAN製)を仕込み、ここに、アクリル酸ブチル370.01g,メタクリル酸n−ブチル370.01g,ジアセトンアクリルアミド13.32g,メチルエチルケトン13.32gおよびメトキノン1.51gを混合した反応溶媒96.01gを加えて、系全体が均一に分散するように攪拌した。
攪拌機、加熱用ヒーター、温度計、温度コントローラを備えた内容量0.8Lの合成装置に、ポリオール成分としてポリテトラメチレンエーテルグリコール60g(平均分子量1000、保土ヶ谷化学工業株式会社製)、1,4−シクロヘキサンジメタノール14g、ジメチロールプロピオン酸20gを仕込み、反応溶媒としてN−メチルピロリドン30.0gを加えた。ここに、イソシアネート成分としてトリレンジイソシアネート104gを添加し、この混合溶液を80〜85℃まで昇温させて5時間反応させた。得られたプレポリマーのNCO含有率は8.9%であった。
攪拌機、加熱用ヒーター、温度計、温度コントローラを備えた内容量0.8Lの乳化設備を有するオートクレーブに、水626質量部、エチレン−アクリル酸共重合体(アクリル酸20質量%、メルトインデックス(MI):1300、質量平均分子量(Mw):20,000、酸価:150、ダウケミカル社製「プリマコール(登録商標)5990I」)160質量部に加え、上記エチレン−アクリル酸共重合体の有する全カルボキシル基に対して、トリエチルアミンを0.6当量、水酸化ナトリウムを0.15当量加えて、150℃、0.5MPaの雰囲気下で高速攪拌を行い、反応溶液を40℃まで冷却してエチレン−アクリル酸共重合体の水系分散体を得た。
攪拌機、加熱用ヒーター、温度計、温度コントローラを備えた内容量1.0Lの乳化設備を有するオートクレーブに、エチレン−アクリル酸共重合体(上記「プリマコール(登録商標)5990I」)200質量部、ポリマレイン酸水溶液(日油社製「ノンポール(登録商標)PMA−50W」、Mw:約1100(ポリスチレン換算)、固形分50質量%品)8.0質量部、トリエチルアミン33.5質量部(上記エチレン−アクリル酸共重合体の有する全カルボキシル基に対して0.63当量分)、48%水酸化ナトリウム水溶液6.9質量部(上記エチレン−アクリル酸共重合体の有する全カルボキシル基に対して0.15当量)、トール油脂肪酸(ハリマ化成社製「ハートールFA3」)3.5質量部、イオン交換水792.6質量部を加えて密封し、150℃、0.5MPa(5気圧)で3時間、500rpmで攪拌し、反応溶液を30℃まで冷却した。次いでシランカップリング剤(モメンティブ・パフォーマンス・マテリアルズ(旧社名:GE東芝シリコーン)社製「TSL8350」、γ−グリシドキシプロピルトリメトキシシラン)10.4質量部、ポリカルボジイミド(日清紡社製「カルボジライト(登録商標)SV−02」、Mw:2,700、固形分40質量%品)31.2質量部、イオン交換水72.8質量部を添加し、10分間攪拌した。エチレン−アクリル酸共重合体を主成分とする水系分散体を得た。
(実験例1)
上記製造例1〜5で得られたアクリルウレタン系樹脂水系分散体1および2、カルボキシル基含有ポリウレタン樹脂水系分散体、エチレン−不飽和カルボン酸共重合体水系分散体およびエチレン−アクリル酸共重合体を主成分とする水系分散体を用いて、樹脂皮膜の軟化点とスォードロッカー硬度を測定した。結果を表1に示す。
(実験例2)
上述の各製造例で得られたアクリルウレタン系樹脂水系分散体1および2、カルボキシル基含有ポリウレタン樹脂水系分散体、エチレン−不飽和カルボン酸共重合体水系分散体の混合液、エチレン−アクリル酸共重合体を主成分とする水系分散体のそれぞれに、表2に示す配合組成に従ってシリカ粒子(日産化学株式会社製「スノーテックス(登録商標)XS」、平均粒子径4〜6nm)を配合して不揮発性成分換算による両者の合計が100質量部となるようにし、ここに、シランカップリング剤としてγ−グリシドキシプロピルトリメトキシシラン(信越化学工業製「KBM403」)を10質量部添加して皮膜形成用樹脂水性分散液を調製した。
上記製造例1で得たアクリルウレタン系樹脂水系分散体1または製造例2で得たアクリルウレタン系樹脂水系分散体2と、シリカ粒子(日産化学製「スノーテックス(登録商標)XS」、平均粒子径4〜6nm)とを、表3に示す配合組成にしたがって、不揮発性成分で換算した両者の合計が100質量部となるように配合し、ここに、シランカップリング剤としてγ−グリシドキシプロピルトリメトキシシラン(信越化学工業製「KBM403」)を10質量部添加して皮膜形成用樹脂水性分散液を調製した。
上記で得たアクリルウレタン系樹脂水系分散体1または2と、シリカ粒子(日産化学株式会社製「スノーテックス(登録商標)XS」、平均粒子径4〜6nm)とを、アクリルウレタン系樹脂水系分散体の不揮発性樹脂成分が40質量部、シリカ粒子が60質量部となるように配合し、両者の合計100質量部に対して、シランカップリング剤(γ−グリシドキシプロピルトリメトキシシラン、信越化学工業製「KBM403」)を0〜30質量部添加して皮膜形成用樹脂水性分散液を調製した。
上記アクリルウレタン系樹脂水系分散体1または2を40質量部(不揮発性樹脂成分換算)と、平均粒子径が4〜100nmのシリカ粒子(日産化学製「スノーテックス(登録商標)」XS)60質量部とを混合し、両者の合計100質量部に対して、シランカップリング剤(γ−グリシドキシプロピルトリメトキシシラン、信越化学工業製「KBM403」)を10質量部添加して皮膜形成用樹脂水性分散液を調製した。
上記アクリルウレタン系樹脂水系分散体1または2を40質量部(不揮発性樹脂成分換算)と、シリカ粒子(日産化学株式会社製「スノーテックス(登録商標)XS」、平均粒子径4〜6nm)60質量部とを配合し、両者の合計100質量部に対して、表6に示す各種シランカップリング剤を10質量部添加して皮膜形成用樹脂水性分散液を調製した。
上記アクリルウレタン系樹脂水系分散体1または2を40質量部(不揮発性樹脂成分換算)と、シリカ粒子(日産化学製「スノーテックス(登録商標)XS」、平均粒子径4〜6nm)60質量部とを混合し、両者の合計100質量部に対して、シランカップリング剤(γ−グリシドキシプロピルトリメトキシシラン、信越化学工業製「KBM403」)を10質量部添加して、皮膜形成用樹脂水性分散液を調製した。
Claims (7)
- 金属板表面に樹脂皮膜を有する表面処理金属板であって、
前記樹脂皮膜が、アクリルウレタン系樹脂30〜50質量部と、平均粒子径が4〜20nmのシリカ粒子50〜70質量部とを、両者の合計が100質量部となるように含有し、さらに、
前記アクリルウレタン系樹脂とシリカ粒子の合計100質量部に対して、シランカップリング剤を5〜25質量部の比率で含有する皮膜形成用樹脂組成物から形成されたものであることを特徴とする表面処理金属板。 - 前記アクリルウレタン系樹脂が、原料として、ポリイソシアネート、ポリオール、および、ジヒドロキシアルカン酸を含み、これらの合計3〜80質量部から合成されたウレタンプレポリマーから得られたポリウレタンと、10〜97質量部の(メタ)アクリルモノマーから得られた(メタ)アクリル系ポリマーとを含むものである請求項1に記載の表面処理金属板。
- 前記アクリルウレタン系樹脂が、ポリウレタンおよび/または(メタ)アクリル系ポリマーの構造中に、カルボニル基および/またはヒドラジン基を有するものである請求項1または2に記載の表面処理金属板。
- 前記アクリルウレタン系樹脂の軟化点が120℃以上であり、かつ、スォードロッカー硬度が25以上である請求項1〜3のいずれかに記載の表面処理金属板。
- 前記樹脂皮膜が、アゾメチン架橋構造を有するものである請求項1〜4のいずれかに記載の表面処理金属板。
- 前記シランカップリング剤が、下記化学式(1)で表される構造を有するものである請求項1〜5のいずれかに記載の表面処理金属板。
- 前記樹脂皮膜の付着量が0.05〜1g/m2である請求項1〜6のいずれかに記載の表面処理金属板。
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