CN1374991A - 有改良外观、改良边角遮盖力和减少焊缝的阴极电涂组合物 - Google Patents
有改良外观、改良边角遮盖力和减少焊缝的阴极电涂组合物 Download PDFInfo
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- CN1374991A CN1374991A CN00812983A CN00812983A CN1374991A CN 1374991 A CN1374991 A CN 1374991A CN 00812983 A CN00812983 A CN 00812983A CN 00812983 A CN00812983 A CN 00812983A CN 1374991 A CN1374991 A CN 1374991A
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- Prior art keywords
- glycidyl
- poly suboxygen
- ether
- improvement
- acid
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- 125000000217 alkyl group Chemical group 0.000 claims description 3
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- IUGYQRQAERSCNH-UHFFFAOYSA-N pivalic acid Chemical compound CC(C)(C)C(O)=O IUGYQRQAERSCNH-UHFFFAOYSA-N 0.000 claims description 3
- 125000003545 alkoxy group Chemical group 0.000 claims 1
- 150000001735 carboxylic acids Chemical class 0.000 claims 1
- 125000001033 ether group Chemical group 0.000 claims 1
- 125000002947 alkylene group Chemical group 0.000 abstract 1
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- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 10
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- MNAHQWDCXOHBHK-UHFFFAOYSA-N 1-phenylpropane-1,1-diol Chemical compound CCC(O)(O)C1=CC=CC=C1 MNAHQWDCXOHBHK-UHFFFAOYSA-N 0.000 description 5
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- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 5
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- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 description 4
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- LCFVJGUPQDGYKZ-UHFFFAOYSA-N Bisphenol A diglycidyl ether Chemical compound C=1C=C(OCC2OC2)C=CC=1C(C)(C)C(C=C1)=CC=C1OCC1CO1 LCFVJGUPQDGYKZ-UHFFFAOYSA-N 0.000 description 1
- 101000822695 Clostridium perfringens (strain 13 / Type A) Small, acid-soluble spore protein C1 Proteins 0.000 description 1
- 101000655262 Clostridium perfringens (strain 13 / Type A) Small, acid-soluble spore protein C2 Proteins 0.000 description 1
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 1
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 description 1
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- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 description 1
- 101000655256 Paraclostridium bifermentans Small, acid-soluble spore protein alpha Proteins 0.000 description 1
- 101000655264 Paraclostridium bifermentans Small, acid-soluble spore protein beta Proteins 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
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- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 1
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 1
- 235000011054 acetic acid Nutrition 0.000 description 1
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- 150000001298 alcohols Chemical class 0.000 description 1
- 125000002723 alicyclic group Chemical group 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 125000001118 alkylidene group Chemical group 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
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- 239000007864 aqueous solution Substances 0.000 description 1
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- 238000005260 corrosion Methods 0.000 description 1
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- JGFBRKRYDCGYKD-UHFFFAOYSA-N dibutyl(oxo)tin Chemical class CCCC[Sn](=O)CCCC JGFBRKRYDCGYKD-UHFFFAOYSA-N 0.000 description 1
- 125000006182 dimethyl benzyl group Chemical group 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- RUZYUOTYCVRMRZ-UHFFFAOYSA-N doxazosin Chemical compound C1OC2=CC=CC=C2OC1C(=O)N(CC1)CCN1C1=NC(N)=C(C=C(C(OC)=C2)OC)C2=N1 RUZYUOTYCVRMRZ-UHFFFAOYSA-N 0.000 description 1
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- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000007046 ethoxylation reaction Methods 0.000 description 1
- SBRXLTRZCJVAPH-UHFFFAOYSA-N ethyl(trimethoxy)silane Chemical compound CC[Si](OC)(OC)OC SBRXLTRZCJVAPH-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
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- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 description 1
- 150000002923 oximes Chemical class 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
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- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- NVKTUNLPFJHLCG-UHFFFAOYSA-N strontium chromate Chemical compound [Sr+2].[O-][Cr]([O-])(=O)=O NVKTUNLPFJHLCG-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 1
- DENFJSAFJTVPJR-UHFFFAOYSA-N triethoxy(ethyl)silane Chemical compound CCO[Si](CC)(OCC)OCC DENFJSAFJTVPJR-UHFFFAOYSA-N 0.000 description 1
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/44—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications
- C09D5/4419—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications with polymers obtained otherwise than by polymerisation reactions only involving carbon-to-carbon unsaturated bonds
- C09D5/443—Polyepoxides
- C09D5/4457—Polyepoxides containing special additives, e.g. pigments, polymeric particles
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/0834—Compounds having one or more O-Si linkage
- C07F7/0836—Compounds with one or more Si-OH or Si-O-metal linkage
-
- 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
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/04—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers only
- C08G65/22—Cyclic ethers having at least one atom other than carbon and hydrogen outside the ring
-
- 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
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/329—Polymers modified by chemical after-treatment with organic compounds
- C08G65/336—Polymers modified by chemical after-treatment with organic compounds containing silicon
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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
- C08L71/00—Compositions of polyethers obtained by reactions forming an ether link in the main chain; Compositions of derivatives of such polymers
- C08L71/02—Polyalkylene oxides
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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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/44—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications
- C09D5/4419—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications with polymers obtained otherwise than by polymerisation reactions only involving carbon-to-carbon unsaturated bonds
- C09D5/443—Polyepoxides
- C09D5/4434—Polyepoxides characterised by the nature of the epoxy binder
- C09D5/4438—Binder based on epoxy/amine adducts, i.e. reaction products of polyepoxides with compounds containing amino groups only
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Engineering & Computer Science (AREA)
- Molecular Biology (AREA)
- General Chemical & Material Sciences (AREA)
- Paints Or Removers (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
- Conductive Materials (AREA)
Abstract
一种阴极电涂组合物,包括含水载体,分散在该载体中的成膜粘结剂,其包含环氧胺加合物和封闭的多异氰酸酯交联剂,和新的添加剂,其包括由(1)聚亚氧烷基二或一胺(2)环氧丙氧基烷基烷氧基硅烷和(3)选自羧酸缩水甘油酯和烷基缩水甘油醚的缩水甘油基化合物反应所生成的产物,该反应产物在酸或水存在下水解,将烷氧基硅烷部分转变为硅烷醇部分。这种电涂组合物生产出具有较好的边角遮盖力和较少的焊缝的较光滑外观的涂层。
Description
发明背景
本发明涉及一种阴极电涂组合物，特别是一种含有能显著地减少焊缝和改良组合物的电沉积膜的边角遮盖力的防缩孔剂的阴极电涂组合物。
通过电沉积法，也称为电涂法，使导电基材涂覆，是一种众所周知的重要的工业方法。对于汽车基材的底漆电沉积法被广泛应用于汽车工业。在此方法中，一种导电部件，例如汽车车身或汽车零件，被浸泡在成膜聚合物的水乳液的涂料组合物的浴(bath)中，并且作为电沉积过程的电极。电流在部件与水乳液实现电接触的相反电极之间通过，直到所需的涂层沉积到此部件上。在此阴极电涂方法中，被涂覆的部件是阴极，相反的电极是阳极。
在典型的阴极电沉积方法的浴中使用的树脂组合物在本领域是公知的。这些树脂典型地是由已经扩链的聚环氧化物树脂制成，然后形成在树脂中包含胺基的加合物。典型地，通过树脂和胺化合物的反应引入胺基。这些树脂和交联剂掺混，然后用酸中和形成水乳液，其为经常提及的基本乳液。将颜料浆、结合溶剂、水和其它添加剂与基本乳液混合形成电涂浴。
电涂浴放置在一个包含阳极的绝缘槽中。被涂覆的部件是阴极，并且穿过含有电沉积浴的槽。沉积在被电涂的部件上的涂层的厚度是电涂浴的性质、槽的电操作特性、浸渍时间等的函数。在一个设定的时间段之后，把得到的涂覆部件从浴中取出，并且用去离子水进行清洗。典型地是在烘箱中，在足以在部件上产生交联涂层的温度下，将部件上的涂层固化。
有关阴极电涂组合物持续存在的问题是固化涂层表面缺乏光滑度，固化涂层表面焊缝的存在，以及缺乏组合物的边角保护或边角遮盖力。在本领域中，已提出各种各样的添加剂来解决上述一或多个问题。例如，US 5,356,960公开了一种防缩孔添加剂。然而，经过烘培之后，这种添加剂有迁移到电涂表面上的倾向，导致底漆或者其他在汽车和其他工业中使用的涂层的粘附力较差。US 5,723,519公开了一种在烘培过程中不会迁移的防缩孔剂，因此克服了上述缺点，另外据说可以改良边角遮盖力。然而，仍然需要改良外观、减少焊缝和改良在被涂覆基料的边角遮盖力的电涂组合物。
发明概述
改良的含水阴极电涂组合物，其含有一种环氧胺加合物的粘结剂和一种封闭型多异氰酸酯交联剂；新的添加剂提供改良外观，改良边角遮盖力和降低在涂覆组合物的基底上焊缝的出现率。这种新的添加剂是聚亚氧烷基胺(二胺或一元胺)；环氧丙氧基烷基烷氧基硅烷和选自羧酸缩水甘油酯和烷基缩水甘油醚中的缩水甘油基化合物的反应物。在水中用酸将添加剂乳化以将烷氧基硅烷部分水解为硅烷醇部分。
发明详述
这种构成本发明基础的新添加剂，可通过将它用有机酸或无机酸在水中乳化，然后添加到含水电涂组合物中而容易地掺入电涂组合物。在传统浴操作条件下的延长时间内，添加剂在组合物和电涂浴中仍然保持稳定，这是由于添加剂不与组合物中的其它组份反应，它对于电涂浴或电涂组合物的涂层的性质没什么不利影响，并且改良了边缘保护和焊缝的减少，形成了比现有技术更光滑的固化涂层。
这种添加剂通过聚亚氧烷基胺(二胺或一元胺)与环氧丙氧基烷基烷氧基硅烷和羧酸缩水甘油酯或烷基缩水甘油醚反应制备。聚亚氧烷基胺和环氧丙氧基烷基烷氧基硅烷和缩水甘油酯或者醚的摩尔比为1∶0.2∶1.8～1∶1.2∶0.8。通常，该反应在50℃～130℃进行，直到没有残余环氧化物存在(大约1～6小时)。然后将添加剂在水中用有机酸或无机酸乳化，这将烷氧基硅烷基团水解为稳定的硅烷醇部分。合适的有机酸包括：乳酸、醋酸和甲酸。也可使用无机酸，例如氨基磺酸和链烷磺酸例如甲磺酸，或磷酸。
用于形成新的添加剂的聚亚氧烷基二元或一元胺，在亚烷基中有2-4个碳原子，优选聚亚氧烷基二元或一元胺的数均分子量为230～3000，更优选1500～2500，例如构自Huntsman Corporation的数均分子量大约为2000的JeffamineD-2000。其它有用的聚亚氧烷基胺包括类似分子量的聚氧乙烯二元或一元胺和聚氧丁烯二元或一元胺。
典型地，用于生产新的添加剂的有用的环氧丙氧基烷基烷氧基硅烷具有通式：
其中R是甲基、乙基或甲基和乙基的混合，n是1～3。典型的硅烷是γ-环氧丙氧基丙基三甲氧基硅烷、γ-环氧丙氧基乙基三甲氧基硅烷、γ-环氧丙基甲基三甲氧基硅烷、γ-环氧丙氧基甲基三乙氧基硅烷、γ-环氧丙氧基乙基三乙氧基硅烷、γ-环氧丙氧基丙基三乙氧基硅烷。优选γ-环氧丙氧基丙基三甲氧基硅烷以生产高质量的添加剂。
典型地，有用的缩水甘油酯和醚包括单缩水甘油酯、单缩水甘油醚、多缩水甘油酯和多缩水甘油醚。优选单缩水甘油酯和单缩水甘油醚。有利的单缩水甘油酯和单缩水甘油醚的典型例子，包括2-乙基己基缩水甘油醚、丁基缩水甘油醚、十二烷基缩水甘油醚、新癸酸缩水甘油酯和新戊酸缩水甘油酯。特别优选新癸酸单缩水甘油酯，其提供低光泽和较好(平滑)外观。
将添加剂用有机酸或无机酸(上述)在水中乳化，以将硅烷基团水解形成硅烷醇基团。添加剂几乎可随时加到电涂组合物中，并可加到基本乳液，或所述浴中。
完全水解后的添加剂有如下的结构式：
其中：R、R1和R2独立地是H或CaH2a+1，a为0～22的整数，n为5～40的整数；m为1～3的整数；X是醚键或酯键。
通常，用于电涂组合物的添加剂至少为电涂组合物中固体粘结剂总重量的2％，优选2％～10％。最优选所用添加剂为4％～8％。
大多数应用于电涂组合物的基本乳液包含一种与交联剂混合的环氧胺加合物的粘结剂的含水乳液，其已被酸中和以形成水溶性产物。电涂组合物粘结剂典型地是环氧胺加合物和封闭的多异氰酸酯交联剂的混合物。尽管新的添加剂可潜在地与多种不同的阴极电涂树脂使用，但特别优选环氧胺加合物树脂。这些树脂一般公开在US4,419,467中，其在此引用作为参考。
用于环氧胺加合物树脂的优选交联剂也是现有技术领域是公知的。有脂肪族、脂环族、芳香族异氰酸酯，例如：二异氰酸六亚甲基酯、二异氰酸环六亚甲基酯、甲苯二异氰酸酯、二异氰酸亚甲基二苯基酯等。采用封闭剂，例如肟类、醇类或己内酰胺对这些异氰酸酯进行预处理，这些封闭剂封闭了异氰酸酯的官能度，即交联官能度。加热使封闭剂分离，因而，提供反应性的异氰酸酯基团并发生交联。异氰酸酯交联剂和封闭剂是现有技术中公知的并也公开在前述的US4,419,467中。
在电涂组合物中，阴极环氧胺加合物粘结剂和封闭的异氰酸酯是主要的树脂成分并通常占组合物中固体重量的30％～50％。为了形成电涂浴，所述固体通常用含水介质稀释。
除上述树脂粘结剂之外，电涂组合物通常包括颜料，它以颜料浆的形式被引入到组合物中。通过将颜料研磨或分散到研磨漆料，和任选的成分如润湿剂、表面活性剂和去泡剂中制备颜料浆。可应用任何一种本领域公知的颜料研磨漆料或可应用上述新的添加剂。研磨之后，颜料颗粒的尺寸应尽可能的小，通常，用赫格曼细度计测量粒子的尺寸为6～8。
可用于本发明的颜料包括：二氧化钛、碱式硅酸铅、铬酸锶、炭黑、氧化铁、粘土等。使用高表面和吸油性的颜料应当多加注意，因为这些对于电沉积的涂层的聚结和流动有不良的影响。
颜料与粘结剂的重量比也是很重要的，最好小于0.5∶1，优选小于0.4∶1，通常为0.2∶1到0.4∶1。已经发现，较高的颜料与粘结剂的重量比对聚结和流动产生不利的影响。
本发明的涂层组合物可包括任选组分，比如润湿剂，表面活性剂，去泡剂等。表面活性剂和润湿剂的例子包括烷基咪唑啉，如可从Ciba-Geigy Industrial Chemicals购得的“Amine C”，炔醇，如可从Air Products and Chemical购得的“Surfynol104”。当这些任选组分存在时，组分的重量为组合物中粘结剂固体的0.1～20％。
任选地，可用增塑剂以促进流动。可用的增塑剂的例子是高沸点的水不混溶性物质，例如：壬基酚或双酚A的环氧乙烷和环氧丙烷加合物。通常增塑剂的用量大约占树脂固体重量的0.1～15％。
本发明的电涂组合物是一个水分散体。在本发明的上下文中，“分散体”这个词，被认为是两相半透明的或不透明的含水树脂粘结剂体系，其中粘结剂在分散相中，水是连续相。粘结剂相粒子的平均直径大约是0.1～10μm，优选小于5μm。通常，在含水介质中，粘结剂的浓度不是关键，但是通常水分散体的主要部分是水。通常，水分散体包含约3～50％，优选5～40％重量的粘结剂固体。当加入电涂浴中时，要把含水的粘结剂浓缩物用水进行稀释。通常该浓缩物含有10～30％重量的粘结剂固体。
下面的例子将举例说明本发明。如果没有别的说明，所有的份数和百分数都以重量为基础。
实施例防缩孔剂的制备
防缩孔剂的制备是通过将1000份的Jeffamine D2000(数均分子量为2000和996.5胺当量的聚氧丙烯二胺)、100份CarduraE-10(新癸酸缩水甘油酯)、141.6份的SilquestA-187(环氧丙氧基丙基三甲氧基硅烷)和130份2-乙基己醇加入到合适的反应器中，在干燥的氮气氛中加热到110℃，将反应混合物保持在110℃，直到得到S-T加德纳-霍尔特粘度。接着，将加合物分散到4049.6份去离子水和66.3份的乳酸的含水介质中。得到的加合物溶液不挥发物含量为22％。交联树脂溶液的制备
乙醇封闭的多异氰酸酯交联树脂溶液的制备是通过将317.14份的MondurMR(二异氰酸亚甲基二苯基酯)、47.98份甲基异丁基酮和0.064份二月桂酸二丁基锡加入到合适的反应器中并在氮氛中加热到37℃。在反应混合物保持在低于93℃下，将323.10份的二甘醇一丁基醚和13.04份三羟甲基丙烷的混合物慢慢加入反应器中。然后使反应混合物保持在110℃，直到用红外扫描反应混合物表明所有异氰酸酯已经基本反应。然后加入2.30份的丁醇和167.37份的甲基异丁基酮。得到的树脂溶液的不挥发物含量为75％。扩链的聚环氧化物乳液的制备
将下述组份加入到合适的反应容器中：1478份的Epon 828(环氧当量为188的双酚A二缩水甘油醚环氧化物树脂)；427份双酚A；533份羟基当量为247的乙氧基化双酚A(Synfac8009)和121份二甲苯。在氮气氛下将最终反应混合物加热到160℃并在室温条件下保持1小时。加入5.1份二甲基苄基胺并且将混合物的温度保持在182℃，直到达到环氧当量为1050。当反应混合物的温度降低到149℃时，将2061份的交联树脂溶液(上面得到)加入。当反应温度降低到107℃时，加入168份的二酮亚胺(diketimine)(不挥发物含量为72.27％的二亚乙基三胺和甲基异丁基酮的反应产物)和143份的甲基乙醇胺。所得反应混合物温度升高，并在120℃时保持1小时，然后分散到3886份的去离子水和182.6份的乳酸(乳酸含量为88％在去离子水中)的含水介质中。再加入2741份的去离子水。持续搅拌乳液直至甲基异丁基酮蒸发。得到的树脂乳液的不挥发物含量为38％。季铵化剂的制备
季铵化剂的制备是通过在室温下，将87份二甲基乙醇胺加到有320份乙基己醇半封闭的甲苯二异氰酸酯的反应器中，发生放热反应并在80℃下搅拌反应混合物1小时。加入118份乳酸水溶液(不挥发物的含量为75％)，然后加入39份的2-丁氧基乙醇。将反应混合物在65℃下保持约1小时并不断搅拌以形成季铵化剂。颜料研磨漆料的制备
颜料研磨漆料是通过：在氮气氛下，将710份的Epon828(环氧当量为188的双酚A的二缩水甘油醚)和290份双酚A加入到合适的容器中，并且加热到150℃-160℃引发放热反应。放热反应在150℃-160℃下继续约1小时。然后，将反应混合物降温到120℃，再加入496份2-乙基己醇半封闭的甲苯二异氰酸酯。将反应混合物的温度在110℃～120℃保持1小时，然后加入1095份2-丁氧基乙醇，接着将反应混合物的温度降到85℃～90℃，加入71份去离子水，然后加入496份季铵化剂(上述制备)。将反应混合物的温度保持在85℃～90℃，直到达到酸度值大约为1。颜料浆的制备
组份 重量份数颜料研磨漆料(如上制备) 608.52去离子水 1244.42二氧化钛颜料 713.81硅酸铝颜料 149.12硅酸铅颜料 114.71炭黑颜料 19.61氧化二丁基锡 149.81
将上述组份在合适的容器中混合，直到形成均匀的混合物。然后通过将混合物加入Eiger碾磨机中，并进行研磨直至达到Hegman读数为7或更大而将混合物分散。电涂浴的制备
| 重量份数 | ||||
| 组份 | 浴I | 浴II | 浴III | 浴IV |
| 乳液 | 1503.08 | 1518.90 | 1503.08 | 1487.26 |
| 去离子水 | 2013.49 | 1974.25 | 1962.74 | 1951.23 |
| 颜料浆 | 397.54 | 397.54 | 397.54 | 397.54 |
| 防缩孔剂 | 85.89* | 109.31 | 136.64 | 163.97 |
| 总计 | 4000.00 | 4000.00 | 4000.00 | 4000.00 |
* 应用于浴I的防缩孔剂包括传统的防缩孔剂，它是
JeffamineD2000(聚亚氧烷基二胺)和Epon1001环氧树脂的反应产
物。
每种阳极电涂浴的制备都是通过将组份混合在一起，然后超滤这些混合物。每种浴在240～280伏下进行电涂，以得到0.8～1.0密耳(20.23～25.4微米)。在抗焊缝、表面粗糙度、边缘耐腐蚀性方面对这些浴进行比较。浴I用作对照。
ASSP吹焊缝试验(blow out cratertest)用于测试每一个浴。根据下面的A-E的等级评估耐焊缝等级：
A-0-10％缺陷
B-11-20％缺陷
C-21-40％缺陷
D-41-80％缺陷
E-大于80％缺陷
浴I(对照)的耐焊缝等级是E。浴II、III、IV的耐焊缝等级是A。
为了测量边缘耐腐蚀度，将剃刀片在浴I、II、III、IV中分别进行电涂，并在360℃金属温度下焙烧10分钟。然后将剃刀片暴露在盐雾中7天。用显微镜来观察剃刀片，计数每个刀片上锈点的数量。用浴I得到的刀片有100-140个锈点，用浴II得到的刀片有60-80个锈点，用浴III得到的刀片有20-40个锈点，用浴IV用的刀片没有锈点。
电涂固化膜的表面粗糙度的测量通过在浴I、II、III、IV中涂覆磷化的冷轧钢板，并在360℃金属温度下焙烧10分钟。所得膜的厚度为0.8-0.9密耳。用Taylor-Hobson Surtronic 3+表面光度仪对表面粗糙度进行测定。用浴I得到的钢板的表面粗糙度为254nm(10微英寸)；用浴II为356nm(14微英寸)；用浴III为457nm(18微英寸)；用浴IV为559nm(22微英寸)。
Claims (14)
1.一种阴极电涂组合物，包含
a)含水载体；
b)分散在载体中的成膜粘结剂，所述的粘结剂包含环氧胺加合物和封闭的多异氰酸酯交联剂；以及
c)添加剂，包含以下的反应产物：
1) 聚亚氧烷基胺
2) 环氧丙氧基烷基烷氧基硅烷；和
3) 缩水甘油基化合物，选自：
(a)羧酸缩水甘油酯，和
(b)烷基缩水甘油醚；
该反应产物在酸和水存在下水解，将烷氧基硅烷部分转变为硅烷醇部分。
2.如权利要求1所述的改良电涂组合物，其中缩水甘油基化合物选自2-乙基己基缩水甘油醚、丁基缩水甘油醚、十二烷基缩水甘油醚、新癸酸缩水甘油酯和新戊酸缩水甘油酯。
3.如权利要求2所述的改良电涂组合物，其中缩水甘油基化合物是新癸酸单缩水甘油酯。
4.如权利要求2所述的改良电涂组合物，其中聚亚氧烷基胺是重均分子量为230-3000的聚亚氧丙基胺。
5.如权利要求2所述的改良电涂组合物，其中环氧丙氧基烷基烷氧基硅烷是γ-环氧丙氧基丙基三甲氧基硅烷。
6.如权利要求1所述的改良电涂组合物，其中聚亚氧烷基胺选自聚亚氧烷基二胺和聚亚氧烷基一元胺。
7.如权利要求1所述的改良电涂组合物，其中聚亚氧烷基胺是重均分子量为230-3000的聚亚氧丙基二胺；其中环氧丙氧基烷基烷氧基用硅烷是γ-环氧丙氧基丙基三甲氧基硅烷；和其中缩水甘油基化合物是羧酸单缩水甘油酯。
8.如权利要求1所述的改良电涂组合物，其中聚亚氧烷基胺和环氧丙氧基烷基硅烷和缩水甘油基化合物摩尔比为1∶0.2∶1.8～1∶1.2∶0.8。
9.如权利要求1所述的改良阴极电涂组合物，其中以组合物成膜粘结剂的重量为基础，添加剂的存在量为2％-10％重量。
10.具有下列结构式(水解后的)的用于阴极电涂组合物的添加剂：
其中：R1、R2和R3独立地是H或CaH2a+1，其中a为0～22的整数，n为5～40的整数；m为1～3的整数；X是醚或酯键。
11.生产阴极电涂组合物的方法中，在任何切实可行的顺序下，包括以下步骤：
(a) 制备环氧胺加合物；
(b) 制备封闭的多异氰酸酯交联剂；
(c) 环氧胺加合物和封闭的多异氰酸酯交联剂的掺混；
(d) 使用有机酸中和环氧胺加合物以形成乳液；
(e) 将乳液与颜料浆混合；和
(f) 将添加剂混入电涂组合物中；其中添加剂基本上由聚亚氧烷基胺、环氧丙氧基烷基烷氧基硅烷和选自羧酸缩水甘油酯和烷基缩水甘油醚的缩水甘油基化合物的反应产物组成，该反应产物被水解以将烷氧基硅烷部分转变为硅烷醇部分。
12.如权利要求11所述的方法，其中缩水甘油基化合物选自2-乙基己基缩水甘油醚、丁基缩水甘油醚、十二烷基缩水甘油醚、新癸酸缩水甘油酯和新戊酸缩水甘油酯。
13.如权利要求12所述的方法，其中缩水甘油基化合物是新癸酸单缩水甘油酯。
14.如权利要求11所述的方法，其中聚亚氧烷基胺和环氧丙氧基烷基硅烷和缩水甘油基化合物的摩尔比为1∶0.2∶1.8～1∶1.2∶0.8。
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US09/401,697 US6207731B1 (en) | 1999-09-23 | 1999-09-23 | Cathode electrocoating compositions having improved appearance, improved edge coverage and reduced craters |
| US09/401697 | 1999-09-23 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1374991A true CN1374991A (zh) | 2002-10-16 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN00812983A Pending CN1374991A (zh) | 1999-09-23 | 2000-09-21 | 有改良外观、改良边角遮盖力和减少焊缝的阴极电涂组合物 |
Country Status (15)
| Country | Link |
|---|---|
| US (1) | US6207731B1 (zh) |
| EP (1) | EP1226217B1 (zh) |
| JP (1) | JP4722358B2 (zh) |
| KR (1) | KR100713732B1 (zh) |
| CN (1) | CN1374991A (zh) |
| AT (1) | ATE286948T1 (zh) |
| AU (1) | AU777593B2 (zh) |
| BR (1) | BR0014618B1 (zh) |
| CA (1) | CA2380628C (zh) |
| DE (1) | DE60017441T2 (zh) |
| ES (1) | ES2234667T3 (zh) |
| IL (1) | IL147973A0 (zh) |
| MX (1) | MXPA02003086A (zh) |
| NZ (1) | NZ517033A (zh) |
| WO (1) | WO2001021718A1 (zh) |
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| CN100383174C (zh) * | 2003-04-10 | 2008-04-23 | 关西涂料株式会社 | 聚加成物和含有该聚加成物的阳离子电淀积涂料 |
| CN101514243B (zh) * | 2008-02-21 | 2014-08-13 | 赢创戈尔德施米特有限公司 | 带有烷氧基甲硅烷基的聚醚醇及其制备方法 |
| CN106318114A (zh) * | 2016-08-19 | 2017-01-11 | 浩力森涂料（上海）有限公司 | 阳离子电沉积涂料 |
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| US20020056641A1 (en) * | 1999-12-15 | 2002-05-16 | December Timothy S. | Cured multilayer coating providing improved edge corrosion resistance to a substrate and a method of making same |
| US20040238362A1 (en) * | 1999-12-15 | 2004-12-02 | December Timothy S. | Cured multilayer coating providing improved edge corrosion to a substrate and a method of making same |
| US6846400B2 (en) * | 2002-01-10 | 2005-01-25 | E. I. Du Pont De Nemours And Company | Cathodic electrodeposition coating agents |
| WO2004090055A1 (ja) * | 2003-04-10 | 2004-10-21 | Kansai Paint Co., Ltd. | 重付加体及び該重付加体を含有するカチオン電着塗料 |
| US20060024511A1 (en) * | 2004-07-29 | 2006-02-02 | Joseph Elmer | Electro-coat adhesion layer with a siloxane top coat |
| US7264706B2 (en) * | 2004-10-18 | 2007-09-04 | E. I. Du Pont De Nemours And Company | Cathodic electrocoating compositions containing an anti-crater agent |
| US7264705B2 (en) * | 2004-10-18 | 2007-09-04 | E. I. Dupont De Nemours And Company | Cathodic electrocoating compositions containing an anti-crater agent |
| US7772333B2 (en) * | 2007-03-13 | 2010-08-10 | Basf Coatings Gmbh | Film-forming material containing resin with -Si(OR)3 and crosslinkable groups |
| WO2009045558A2 (en) * | 2007-03-13 | 2009-04-09 | Basf Corporation | Film-forming material, crosslinkers and coating compositions containing silane, methods for producing a coating composition and a coated substrate |
| DE102009028636A1 (de) | 2009-08-19 | 2011-02-24 | Evonik Goldschmidt Gmbh | Neuartige Urethangruppen enthaltende silylierte Präpolymere und Verfahren zu deren Herstellung |
| DE102009028640A1 (de) * | 2009-08-19 | 2011-02-24 | Evonik Goldschmidt Gmbh | Härtbare Masse enthaltend Urethangruppen aufweisende silylierte Polymere und deren Verwendung in Dicht- und Klebstoffen, Binde- und/oder Oberflächenmodifizierungsmitteln |
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| US9133350B2 (en) | 2011-01-11 | 2015-09-15 | Axalta Coating Systems Ip Co., Llc | Anticrater agent for electrocoat composition |
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| EP3212720B8 (en) * | 2014-10-31 | 2020-01-15 | Swimc Llc | High edge cathodic epoxy electrocoat composition |
| WO2016130656A1 (en) | 2015-02-10 | 2016-08-18 | Valspar Sourcing, Inc. | Novel electrodeposition system |
| BR112018013275A2 (pt) | 2015-12-31 | 2018-12-11 | Henkel Ag & Co Kgaa | revestimentos de autodeposição de baixo cozimento |
| DE102017100961A1 (de) * | 2017-01-19 | 2018-07-19 | GEDIA Gebrüder Dingerkus GmbH | Verfahren zur Vorbereitung von Metallblech für eine Beschichtung |
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| ATE29145T1 (de) * | 1985-02-27 | 1987-09-15 | Corona Peintures | Umsetzungsprodukte von polyoxyalkylenpolyaminen und ihre verwendung in der cationischen elektrotauchlackierung. |
| JPH06287267A (ja) * | 1993-04-07 | 1994-10-11 | Kansai Paint Co Ltd | カチオン電着性微粒子及びそれを含む電着塗料組成物 |
| JPH06287484A (ja) * | 1993-04-01 | 1994-10-11 | Kansai Paint Co Ltd | カチオン電着塗料 |
| JP3287643B2 (ja) * | 1993-04-07 | 2002-06-04 | 関西ペイント株式会社 | カチオン電着塗料組成物及びその調製方法 |
| US5356960A (en) | 1993-08-11 | 1994-10-18 | E. I. Du Pont De Nemours And Company | Cathodic electrocoating compositions containing an anticrater agent |
| US5723519A (en) | 1997-02-25 | 1998-03-03 | E. I. Du Pont De Nemours And Company | Cathodic electrocoating compositions containing an anticrater agent |
-
1999
- 1999-09-23 US US09/401,697 patent/US6207731B1/en not_active Expired - Lifetime
-
2000
- 2000-09-21 DE DE60017441T patent/DE60017441T2/de not_active Expired - Lifetime
- 2000-09-21 MX MXPA02003086A patent/MXPA02003086A/es active IP Right Grant
- 2000-09-21 AU AU75983/00A patent/AU777593B2/en not_active Ceased
- 2000-09-21 WO PCT/US2000/025859 patent/WO2001021718A1/en active IP Right Grant
- 2000-09-21 AT AT00965237T patent/ATE286948T1/de not_active IP Right Cessation
- 2000-09-21 ES ES00965237T patent/ES2234667T3/es not_active Expired - Lifetime
- 2000-09-21 IL IL14797300A patent/IL147973A0/xx unknown
- 2000-09-21 EP EP00965237A patent/EP1226217B1/en not_active Expired - Lifetime
- 2000-09-21 CA CA002380628A patent/CA2380628C/en not_active Expired - Fee Related
- 2000-09-21 NZ NZ517033A patent/NZ517033A/en unknown
- 2000-09-21 CN CN00812983A patent/CN1374991A/zh active Pending
- 2000-09-21 KR KR1020027003770A patent/KR100713732B1/ko active IP Right Grant
- 2000-09-21 BR BRPI0014618-8A patent/BR0014618B1/pt not_active IP Right Cessation
- 2000-09-21 JP JP2001525282A patent/JP4722358B2/ja not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100383174C (zh) * | 2003-04-10 | 2008-04-23 | 关西涂料株式会社 | 聚加成物和含有该聚加成物的阳离子电淀积涂料 |
| CN101514243B (zh) * | 2008-02-21 | 2014-08-13 | 赢创戈尔德施米特有限公司 | 带有烷氧基甲硅烷基的聚醚醇及其制备方法 |
| CN106318114A (zh) * | 2016-08-19 | 2017-01-11 | 浩力森涂料（上海）有限公司 | 阳离子电沉积涂料 |
Also Published As
| Publication number | Publication date |
|---|---|
| EP1226217B1 (en) | 2005-01-12 |
| IL147973A0 (en) | 2002-09-12 |
| NZ517033A (en) | 2004-01-30 |
| AU7598300A (en) | 2001-04-24 |
| JP2003510399A (ja) | 2003-03-18 |
| MXPA02003086A (es) | 2002-10-31 |
| JP4722358B2 (ja) | 2011-07-13 |
| CA2380628C (en) | 2009-05-19 |
| EP1226217A1 (en) | 2002-07-31 |
| AU777593B2 (en) | 2004-10-21 |
| BR0014618A (pt) | 2002-06-18 |
| ATE286948T1 (de) | 2005-01-15 |
| US6207731B1 (en) | 2001-03-27 |
| DE60017441D1 (de) | 2005-02-17 |
| WO2001021718A1 (en) | 2001-03-29 |
| CA2380628A1 (en) | 2001-03-29 |
| BR0014618B1 (pt) | 2009-05-05 |
| KR100713732B1 (ko) | 2007-05-02 |
| DE60017441T2 (de) | 2005-12-22 |
| KR20020031198A (ko) | 2002-04-26 |
| ES2234667T3 (es) | 2005-07-01 |
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