CN114867763A - 水性聚氨酯树脂组合物和使用所述组合物的涂料 - Google Patents
水性聚氨酯树脂组合物和使用所述组合物的涂料 Download PDFInfo
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- CN114867763A CN114867763A CN202080091226.0A CN202080091226A CN114867763A CN 114867763 A CN114867763 A CN 114867763A CN 202080091226 A CN202080091226 A CN 202080091226A CN 114867763 A CN114867763 A CN 114867763A
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- polyurethane resin
- compound
- resin composition
- aqueous polyurethane
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Classifications
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/721—Two or more polyisocyanates not provided for in one single group C08G18/73 - C08G18/80
- C08G18/722—Combination of two or more aliphatic and/or cycloaliphatic polyisocyanates
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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
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- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
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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
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- C08G18/0819—Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups
- C08G18/0828—Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups containing sulfonate groups or groups forming them
-
- 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
- C08G18/0838—Manufacture of polymers in the presence of non-reactive compounds
- C08G18/0842—Manufacture of polymers in the presence of non-reactive compounds in the presence of liquid diluents
- C08G18/0861—Manufacture of polymers in the presence of non-reactive compounds in the presence of liquid diluents in the presence of a dispersing phase for the polymers or a phase dispersed in the polymers
- C08G18/0866—Manufacture of polymers in the presence of non-reactive compounds in the presence of liquid diluents in the presence of a dispersing phase for the polymers or a phase dispersed in the polymers the dispersing or dispersed phase being an aqueous medium
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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
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- C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation 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
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- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
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- C08G18/30—Low-molecular-weight compounds
- C08G18/302—Water
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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
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- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
- C08G18/3206—Polyhydroxy compounds aliphatic
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- C—CHEMISTRY; METALLURGY
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Abstract
提供了成品外观优异以及耐冲击性,如耐崩裂性和附着力也优异的水性聚氨酯树脂组合物。所述水性聚氨酯树脂组合物包括由至少以下组分获得的聚氨酯树脂:(a)彼此不同的至少两种类型的有机二异氰酸酯化合物和/或多异氰酸酯化合物;(b)多元醇化合物;(c)含酸性基团的化合物,其包含至少两种类型的化合物,它们是含有羧基作为酸基的化合物(含羧基的化合物)和含有磺基作为酸基的化合物(含磺基的化合物);和(d)多胺化合物、二胺化合物、多元醇化合物和/或烷醇胺化合物的扩链剂,其分子量不大于400,其中所述水性聚氨酯树脂组合物在聚氨酯树脂的含量为65重量%时具有不小于500 Pa·s且不大于50,000 Pa·s的粘度。
Description
技术领域
本发明涉及成品外观优异以及耐冲击性,如耐崩裂性和/或附着力优异的水性聚氨酯树脂组合物,还涉及含有所述水性聚氨酯树脂组合物的涂装组合物、涂料组合物、墨水组合物或胶粘剂组合物。
背景技术
由于水性聚氨酯树脂组合物对基底的附着力、耐磨性、耐冲击性、耐溶剂性等优异,水性聚氨酯树脂组合物广泛用作纸、塑料、膜、金属、橡胶、弹性体、纺织品等的涂料、墨水、胶粘剂和各种涂覆剂(专利文献1至3)。为了将水性聚氨酯树脂组合物用于在电沉积金属基底上的单层或多层涂层,特别必须持续改进成品外观、耐冲击性和附着力。
引文列表
专利文献1: JP H08-209066 A
专利文献2: JP H07-166093 A
专利文献3: JP 2004-97917 A。
发明概述
技术问题
本发明的一个目的是提供成品外观优异的水性聚氨酯树脂组合物,以及进一步提供耐冲击性,如耐崩裂性和附着力也优异的水性聚氨酯树脂组合物。
对问题的解决方案
由于深入研究,本发明人发现,在包括由以下成分获得的聚氨酯树脂的水性聚氨酯树脂组合物中:(a) 彼此不同的至少两种类型的有机二异氰酸酯化合物和/或多异氰酸酯化合物;(b) 多元醇化合物;(c) 含酸性基团的化合物,其包含至少两种类型的化合物,它们是含有羧基作为酸基的化合物(含羧基的化合物)和含有磺基作为酸基的化合物(含磺基的化合物);和(d) 选自多胺化合物、二胺化合物、多元醇化合物和烷醇胺化合物并具有不大于400的分子量的扩链剂,如果该水性聚氨酯树脂组合物在聚氨酯树脂的含量为65重量%时具有不小于500 Pa·s且不大于50,000 Pa·s的粘度,该水性聚氨酯树脂组合物由于甚至在施加后的水挥发且树脂颗粒熔结并固化(固含量:65%)的状态下也通过控制树脂粘度获得的良好流动性质而具有优异的成品外观。本发明人还发现,通过调节水性聚氨酯树脂组合物的组分等,有可能产生既有对电沉积膜的优异附着力又有优异耐冲击性,如耐崩裂性的涂膜。因此,本发明人已实现本发明。
本发明提供以下解决方案。
[1] 水性聚氨酯树脂组合物,其包含由至少以下组分(a)至(d)获得的聚氨酯树脂:
(a) 彼此不同的至少两种类型的有机二异氰酸酯化合物和/或多异氰酸酯化合物;
(b) 多元醇化合物;
(c) 含酸性基团的化合物,其包含至少两种类型的化合物,它们是含有羧基作为酸基的化合物(含羧基的化合物)和含有磺基作为酸基的化合物(含磺基的化合物);和
(d) 选自多胺化合物、二胺化合物、多元醇化合物和烷醇胺化合物的扩链剂,所述扩链剂具有不大于400的分子量,
其中所述水性聚氨酯树脂组合物在聚氨酯树脂的含量为65重量%时具有不小于500 Pa·s且不大于50,000 Pa·s的粘度。
[2] 根据[1]的水性聚氨酯树脂组合物,其中组分(c)的含酸性基团的化合物是具有两个或更多个羟基或氨基的化合物。
[3] 根据[1]或[2]的水性聚氨酯树脂组合物,其中作为组分(a)包括彼此不同的至少两种类型的有机二异氰酸酯化合物。
[4] 根据[1]至[3]任一项的水性聚氨酯树脂组合物,其中所述有机二异氰酸酯化合物包括至少一种类型的脂环族二异氰酸酯化合物。
[5] 根据[1]至[4]任一项的水性聚氨酯树脂组合物,其中至少一种类型的有机二异氰酸酯化合物是选自4,4'-二环己基甲烷二异氰酸酯和异佛尔酮二异氰酸酯的脂环族二异氰酸酯化合物,且所述脂环族二异氰酸酯化合物的含量百分比为基于100摩尔%的组分(a)的有机二异氰酸酯化合物计不大于80摩尔%。
[6] 根据[1]至[5]任一项的水性聚氨酯树脂组合物,其中组分(b)的多元醇化合物含有聚醚多元醇。
[7] 根据[1]至[6]任一项的水性聚氨酯树脂组合物,其中组分(b)是聚四亚甲基二醇多元醇。
[8] 根据[1]至[7]任一项的水性聚氨酯树脂组合物,其中组分(b)具有大于400g/mol且不大于6000 g/mol的平均分子量。
[9] 根据[1]至[8]任一项的水性聚氨酯树脂组合物,其中聚氨酯树脂中所含的组分(b)的百分比为不小于60重量%。
[10] 根据[1]至[9]任一项的水性聚氨酯树脂组合物,其中组分(c)在聚氨酯树脂中的存在量使得含羧基的化合物和含磺基的化合物的总重量为0.2至10重量%,优选0.5至5重量%。
[11] 根据[1]至[10]任一项的水性聚氨酯树脂组合物,其中羧基的酸值与组分(c)中的总酸值的比率为0.20至0.95,更优选0.50至0.90,再更优选0.70至0.85。
[12] 根据[1]至[11]任一项的水性聚氨酯树脂组合物,其中所述聚氨酯树脂中的羧基的酸值优选在4.5至30 mgKOH/g的范围内,更优选在5至25 mg KOH/g的范围内,再更优选在6至22 mgKOH/g的范围内。
[13] 根据[1]至[12]任一项的水性聚氨酯树脂组合物,其中所述聚氨酯树脂的含量百分比为20至65重量%。
[14] 涂装组合物、涂料组合物、墨水组合物或胶粘剂组合物,其含有根据[1]至[13]任一项的水性聚氨酯树脂组合物。
本发明的有利效果
根据本发明的水性聚氨酯树脂组合物,有可能提供成品外观优异的水性聚氨酯树脂组合物,以及进一步提供耐冲击性,如耐崩裂性和附着力也优异的水性聚氨酯树脂组合物。
实施方案的描述
本发明提供水性聚氨酯树脂组合物,其包括由以下组分获得的聚氨酯树脂:(a)彼此不同的至少两种类型的有机二异氰酸酯化合物和/或多异氰酸酯化合物;(b) 多元醇化合物;(c) 含酸性基团的化合物,其包含至少两种类型的化合物,它们是含有羧基作为酸基的化合物(含羧基的化合物)和含有磺基作为酸基的化合物(含磺基的化合物);和(d) 选自多胺化合物、二胺化合物、多元醇化合物和烷醇胺化合物的扩链剂,所述扩链剂具有不大于400的分子量,其中所述水性聚氨酯树脂组合物在聚氨酯树脂的含量为65重量%时具有不小于500 Pa·s且不大于50,000 Pa·s的粘度。
[组分(a): 有机二异氰酸酯化合物和多异氰酸酯化合物]
在本发明中,组分(a)是彼此不同的至少两种类型的有机二异氰酸酯化合物和/或多异氰酸酯化合物。
组分(a)的有机二异氰酸酯化合物是具有每分子两个游离异氰酸酯基团的有机化合物并可以二异氰酸酯Y(NCO)2为例 [其中Y是C4-12二价脂族烃基(= 脂族二异氰酸酯化合物)、C6-15二价脂环族烃基(= 脂环族二异氰酸酯化合物)、C6-15二价芳族烃基(= 芳族二异氰酸酯化合物)或C7-15二价芳脂族烃基]。这样的有机二异氰酸酯化合物的实例包括四亚甲基二异氰酸酯、甲基五亚甲基二异氰酸酯、1,5-五亚甲基二异氰酸酯、六亚甲基二异氰酸酯(=HDI)、十二亚甲基二异氰酸酯、1,2-双(异氰酸根合甲基)环己烷、1,4-环己烷二异氰酸酯、1-异氰酸根合-3,3,5-三甲基-5-异氰酸根合甲基环己烷(= IPDI,异佛尔酮二异氰酸酯)、4,4'-二环己基甲烷二异氰酸酯、4,4'-二环己基丙烷二异氰酸酯-(2,2)、1,4-苯二异氰酸酯、2,4-甲苯二异氰酸酯、2,6-甲苯二异氰酸酯、4,4'-二苯甲烷二异氰酸酯、2,2'-二苯甲烷二异氰酸酯、2,4'-二苯甲烷二异氰酸酯、四甲基苯二亚甲基二异氰酸酯、对苯二亚甲基二异氰酸酯、对异丙叉基二异氰酸酯和1,5-萘二异氰酸酯。
组分(a)的有机多异氰酸酯化合物是具有每分子三个或更多个异氰酸酯基团的多异氰酸酯。这样的有机多异氰酸酯化合物的实例可以是例如通过由至少两种类型的二异氰酸酯组成的脂族、脂环族、芳脂族和/或芳族二异氰酸酯的改性制备并具有脲二酮、异氰脲酸酯、氨基甲酸酯、脲基甲酸酯、缩二脲、碳二亚胺、亚氨基噁二嗪二酮和/或噁二嗪三酮结构的多异氰酸酯。具有每分子三个或更多个异氰酸酯基团的未改性多异氰酸酯的实例包括4-异氰酸根合甲基-1,8-辛烷二异氰酸酯(壬烷三异氰酸酯)。
组分(a)优选包括彼此不同的至少两种类型的有机二异氰酸酯化合物。
为了使涂膜具有高断裂强度和增强耐久性,组分(a)的有机二异氰酸酯化合物优选包括至少一种类型的脂环族二异氰酸酯化合物。
为了有利于反应控制,组分(a)优选包括选自4,4'-二环己基甲烷二异氰酸酯和异佛尔酮二异氰酸酯的至少一种类型的脂环族二异氰酸酯化合物。
组分(a)含有基于100摩尔%的组分(a)的有机二异氰酸酯化合物计优选不大于80摩尔%,更优选20至70摩尔%,再更优选40至60摩尔%的百分比的脂环族二异氰酸酯化合物。由于脂环族二异氰酸酯化合物在一些情况下当其在有机二异氰酸酯化合物中的比例太高时可能降低耐冲击性,如耐崩裂性,脂环族二异氰酸酯化合物优选在上文规定的范围内。
组分(a)优选是脂族二异氰酸酯化合物和选自4,4'-二环己基甲烷二异氰酸酯、异佛尔酮二异氰酸酯及其混合物的脂环族二异氰酸酯化合物的组合。
组分(a)更优选是选自4,4'-二环己基甲烷二异氰酸酯或异佛尔酮二异氰酸酯的脂环族二异氰酸酯化合物和作为脂族二异氰酸酯化合物的六亚甲基二异氰酸酯(= HDI)的组合。
组分(a)在聚氨酯树脂中的含量百分比通常为5至30重量%,优选10至25重量%,更优选13至20重量%。
[组分(b): 多元醇化合物]
组分(b)的多元醇化合物具有大于400的分子量并具有至少两个异氰酸酯反应性羟基。多元醇化合物的实例包括聚醚多元醇、聚酯多元醇、聚碳酸酯多元醇、聚酯聚碳酸酯多元醇、聚内酯多元醇、聚丁二烯多元醇和硅酮多元醇。
优选的组分(b)优选具有2至4,特别优选2至3,最优选2个羟基。此外,组分(b)也可能是这种类型的各种化合物的混合物。
聚醚多元醇的实例包括环醚加聚物和多元醇缩合物。环醚的实例包括氧化苯乙烯、环氧乙烷、环氧丙烷、四氢呋喃、环氧丁烷和表氯醇,并且这些可独自或组合使用。多元醇的实例包括上述二醇和高官能多元醇,并且这些可独自或组合使用。例如,四氢呋喃的加聚物被称为聚四亚甲基醚二醇(PTMG)。
聚酯多元醇可通过调节聚酯的生产条件制成,并且是至少在主链两端都具有羟基的聚酯。聚酯多元醇的实例包括线性聚酯二醇和轻微支化的聚酯多元醇。这些可通过使用脂族、脂环族或芳族二羧酸和二醇以及任选使用多羧酸和/或高官能多元醇的已知方法制备。
聚内酯多元醇是内酯的均聚物或共聚物,其是制备成至少在主链两端都具有羟基的聚内酯。
聚碳酸酯多元醇是至少在主链两端都具有羟基的聚碳酸酯,其通过调节聚碳酸酯的生产条件制成。
硅酮多元醇包括在分子中具有硅氧烷键的末端具有羟基的硅酮油。
组分(b)的多元醇化合物优选包括聚醚多元醇。
当组分(b)包括聚醚多元醇时,组分(b)中所含的聚醚多元醇的百分比优选为50至100重量%,更优选60至100重量%,再更优选75至100重量%。当含量百分比不小于50%时,强度提高。此外,任选组分,如聚碳酸酯多元醇,可组合使用,并且其含量百分比不大于50重量%,优选不大于40重量%,再更优选不大于25%。
组分(b)的多元醇化合物的平均分子量,特别是聚四亚甲基二醇多元醇的平均分子量大于400 g/mol且不大于6000 g/mol,优选800至5000 g/mol,更优选1000至4000 g/mol。当平均分子量大于400 g/mol时,可获得涂膜对基底的足够附着力。当平均分子量不大于6000 g/mol时,可改进水性聚氨酯树脂组合物的分散稳定性和/或涂膜的成品外观。
从涂膜的附着力的角度看,聚氨酯树脂中所含的组分(b)的百分比优选为不小于60重量%,更优选65至85重量%,再更优选70至85重量%。
要指出,在本说明书中,组分(b)的多元醇化合物不包括组分(c)的含酸性基团的二醇化合物。
[组分(c): 含酸性基团的化合物]
组分(c)的含酸性基团的化合物包括至少两种类型的化合物,它们是含有羧基作为酸基的化合物(含羧基的化合物)和含有磺基作为酸基的化合物(含磺基的化合物)。
组分(c)的含酸性基团的化合物优选是具有至少两个或更多个羟基或氨基的化合物。
对于组分(c),含羧基的化合物和含磺基的化合物的组合增强聚氨酯树脂甚至在低酸值下在水中的乳化/可分散性。此外,在将该组合与其它乳液树脂、颜料、添加剂、溶剂等混合以用作涂料时,该混合物具有优异的储存稳定性并且甚至在高固含量下也在低粘度下稳定。
组分(c)以使得含羧基的化合物和含磺基的化合物的总重量优选为0.2至10重量%,更优选0.5至5重量%的量存在于聚氨酯树脂中。当该量不小于0.2重量%时,获得足够的水分散性。当该量不大于10重量%时,改进涂膜的强度和耐水性。
羧基的酸值与组分(c)中的总酸值的比率优选为0.20至0.95,更优选0.50至0.90,再更优选0.70至0.85。酸值在本文中是指以中和聚氨酯树脂中存在的羧基或磺基所需的氢氧化钾的毫克数表示的计算值(mgKOH/g)。总酸值是指羧基的酸值和磺基的酸值的总和。
组分(c)的含酸性基团的化合物的具体实例包括N-(2-氨基乙基)-2-氨基乙磺酸、N-(3-氨基丙基)-2-氨基乙磺酸、N-(3-氨基丙基)-3-氨基丙磺酸、N-(2-氨基乙基)-3-氨基丙磺酸、2,2-二羟甲基丙酸、2,2-二羟甲基丁酸、N,N-双羟乙基丙氨酸、3,4-二羟基丁磺酸、3,6-二羟基-2-甲苯磺酸,和钠盐、锂盐、钾盐、叔胺盐等,它们是通过二胺(例如1,2-乙二胺或异佛尔酮二胺)与两倍摩尔量的丙烯酸或马来酸的迈克尔加成获得的反应产物。
组分(c)的含酸性基团的化合物优选是含酸性基团的二醇化合物,包括具有4至12个碳原子的含酸性基团的二醇化合物,如2,2-二羟甲基丙酸、2,2-二羟甲基丁酸、N,N-双羟乙基甘氨酸、N,N-双羟乙基丙氨酸、3,4-二羟基丁磺酸和3,6-二羟基-2-甲苯磺酸。
组分(c)的含酸性基团的化合物可以是包括离子基团的那些,如二羟基羧酸、二氨基羧酸、二羟基磺酸、二氨基磺酸及其盐,或能够形成离子基团的那些。其实例包括二羟甲基丙酸、羟基特戊酸、2-(2-氨基乙基氨基)乙磺酸、乙二胺丙基或丁基磺酸、1,2-或1,3-丙二胺-β-乙基磺酸、赖氨酸、3,5-二氨基苯甲酸及其碱金属和/或铵盐;硫酸氢钠与丁烯-2-二醇-1,4的加合物、聚醚砜、2-丁二醇和NaHSO3的丙氧基化加合物(德国专利说明书DE-A24 46 440),以及例如可转化成阳离子基团的结构单元,如N-甲基二乙醇胺。
[组分(d): 作为扩链剂的多胺化合物、二胺化合物、多元醇化合物和烷醇胺化合物]
组分(d)是作为扩链剂的多胺化合物、二胺化合物、多元醇化合物和/或烷醇胺化合物,这些化合物的分子量不大于400。
组分(d)的多胺化合物是在一个分子中具有总共三个或更多个氨基和/或亚氨基的多胺。多胺化合物的实例包括三胺化合物,如二亚乙基三胺、双(2-氨基丙基)胺和双(3-氨基丙基)胺;四胺化合物,如三亚乙基四胺、三亚丙基四胺、N-(苄基)三亚乙基四胺、N,N'''-(二苄基)三亚乙基四胺和N-(苄基)-N'''-(2-乙基己基)三亚乙基四胺;五胺化合物,如四亚乙基五胺和四亚丙基五胺;六胺化合物,如五亚乙基六胺和五亚丙基六胺;和多胺化合物,如聚乙烯亚胺和聚丙烯亚胺。从与聚氨酯预聚物的反应性的角度看,多胺优选是具有两个氨基和一个或多个亚氨基的多胺,如二亚乙基三胺、三亚乙基四胺、双(2-氨基丙基)胺、双(3-氨基丙基)胺、三亚丙基四胺、四亚乙基五胺、四亚丙基五胺、五亚乙基六胺或五亚丙基六胺。
组分(d)的二胺化合物的实例包括肼、1,2-乙二胺、1,4-四亚甲基二胺、2-甲基-1,5-戊二胺、1,6-六亚甲基二胺、1,4-六亚甲基二胺、3-氨基甲基-3,5,5-三甲基环己基胺、1,3-双(氨基甲基)环己烷、苯二亚甲基二胺、哌嗪、2,5-二甲基哌嗪等。
组分(d)的多元醇化合物是具有两个或更多个羟基的化合物。其实例包括乙二醇、二乙二醇、三乙二醇和四乙二醇、1,2-丙二醇、二丙二醇、三丙二醇、四丙二醇、1,3-丙二醇、1,4-丁二醇、1,3-丁二醇、2,3-丁二醇、1,5-戊二醇、1,6-己二醇、2,2-二甲基-1,3-丙二醇、1,4-二羟基环己烷、1,4-二甲基环己烷、1,8-辛二醇、1,10-癸二醇、1,12-十二烷二醇、新戊二醇、1,4-环己二醇、1,4-环己烷二甲醇、1,4-二羟基苯、1,3-二羟基苯、1,2-二羟基苯、2,2-双(4-羟苯基)-丙烷(双酚A)、TCD-二醇、三羟甲基丙烷、甘油、季戊四醇和二季戊四醇。
组分(d)的烷醇胺化合物的实例包括乙醇胺、丙醇胺、丁基乙醇胺、1-氨基-2-甲基-2-丙醇、2-氨基-2-甲基丙醇、二乙醇胺、二异丙醇胺、二甲基氨基丙基乙醇胺、二丙醇胺、N-甲基乙醇胺、N-乙基乙醇胺等。
对于组分(d)的扩链剂,可独自使用一种类型,或可组合使用多种类型。
组分(d)的扩链剂的量优选不大于聚氨酯预聚物中成为扩链起点的残余异氰酸酯基团的当量,更优选为残余异氰酸酯基团的当量的0.7至0.99。当组分(d)的扩链剂的量不大于残余异氰酸酯基团的当量,优选不大于0.99当量时,倾向于抑制扩链的聚氨酯树脂的分子量降低,并且通过施加所得水性聚氨酯树脂分散体而获得的涂膜的强度倾向于改进。
除组分(d)外,例如,氨基多元醇化合物、水等可用作进一步的扩链剂。
该水性聚氨酯树脂组合物可包括单醇和单胺作为进一步的任选组分。
单醇和单胺的添加量优选为基于水性聚氨酯树脂的固含量计小于5重量%,更优选小于2重量%。
[生产水性聚氨酯树脂组合物的方法]
生产水性聚氨酯树脂组合物的方法不受特别限制,但其实例包括以下方法。
生产水性聚氨酯树脂组合物的方法包括步骤:通过使(a) 彼此不同的至少两种类型的有机二异氰酸酯化合物和/或多异氰酸酯化合物、(b) 多元醇化合物和(c) 含酸性基团的化合物反应而获得聚氨酯预聚物;中和聚氨酯预聚物中的酸性基团;将聚氨酯预聚物分散在水性介质中;和通过使聚氨酯预聚物与(d) 选自多胺化合物、二胺化合物、多元醇化合物和烷醇胺化合物并具有不大于400的分子量的扩链剂反应而获得包括聚氨酯树脂的水性聚氨酯树脂组合物。
在生产水性聚氨酯树脂组合物的方法中,中和酸性基团的步骤和将聚氨酯预聚物分散在水性介质中的步骤可单独或一起进行。在生产水性聚氨酯树脂组合物的方法中,使聚氨酯预聚物与扩链剂反应的步骤可以在将聚氨酯预聚物分散在水性介质中的步骤后,或可以与将聚氨酯预聚物分散在水性介质中的步骤一起进行。
生产水性聚氨酯树脂组合物的方法中的各步骤可在惰性气体气氛下进行,也可在大气中进行。
本发明的聚氨酯树脂组合物优选是包括聚氨酯树脂并分散在水性介质中的分散体。本发明的聚氨酯树脂组合物包括至少水作为水性介质并可含有有机溶剂[酮基溶剂(例如丙酮和甲乙酮)、酯基溶剂(例如乙酸乙酯)、醚基溶剂(例如四氢呋喃)、酰胺基溶剂(例如N,N-二甲基甲酰胺和N-甲基吡咯烷酮)、醇基溶剂(例如异丙醇)和芳烃基溶剂(例如甲苯等)作为助溶剂。本发明的聚氨酯树脂组合物中所含的助溶剂的量优选不大于10重量%。此外,水性介质中的水的比例优选不小于40重量%。
从易于处理水分散体的角度看,本发明中获得的水性聚氨酯树脂的水分散体的固含量浓度(挥发性组分以外的组分含量)优选为20至65重量%,更优选30至60重量%。固含量浓度可如下获得:将大约1克水分散体薄薄地铺开在陪替氏培养皿上;精确称重水分散体;然后精确称重使用循环恒温干燥机在130℃下加热45分钟后的重量;并计算加热后的剩余重量与加热前的重量的比率(百分比)。
该水性聚氨酯树脂组合物可含有中和剂作为任选组分。中和剂用于中和聚氨酯预聚物的至少一些酸性基团,并将聚氨酯预聚物分散在水性介质中。中和剂的实例包括:叔胺化合物,如三烷基胺,包括三甲胺、三乙胺、三丁胺等,N,N-二烷基烷醇胺,包括N,N-二甲基乙醇胺、N,N-二甲基丙醇胺、N,N-二丙基乙醇胺、1-二甲氨基-2-甲基-2-丙醇等,N-烷基-N,N-二烷醇胺,和三烷醇胺,包括三乙醇胺;氢氧化钾、氢氧化钠等的无机碱金属盐;氨等。这些可独自使用或两种或更多种组合使用。
从可加工性的角度看,中和剂优选是有机胺,更优选N,N-二甲基乙醇胺。中和剂的量为例如水性聚氨酯树脂组合物所具有的每当量酸性基团0.4至1.2当量,优选0.6至1.0当量。
本发明的水性聚氨酯树脂组合物在聚氨酯树脂的含量为65重量%时具有不小于500 Pa·s且不大于50,000 Pa·s的粘度。当聚氨酯树脂的含量为80重量%时,粘度变化率不大于350%,优选不大于250%,特别优选不大于150%。本发明的水性聚氨酯树脂组合物具有上文规定的粘度以提供成品外观优异的涂装组合物、涂料组合物、墨水组合物和胶粘剂组合物。
在本说明书中,在将液体温度调节到25℃后使用流变仪测量在水性聚氨酯树脂组合物的高固含量下的粘度。要指出,当水性聚氨酯树脂组合物中的聚氨酯树脂的含量小于65重量%时,例如有可能通过使用蒸发器等蒸发水性聚氨酯树脂组合物中的水性介质以调节所含聚氨酯树脂的量来测量在聚氨酯树脂的含量不小于65重量%时的粘度。
[粘度变化率]
“粘度变化率”在本发明中是指在将水性聚氨酯树脂组合物的固含量从65重量%增加到80重量%时的粘度变化,并通过以下计算方法测定。要指出,在25℃下用流变仪测得的值用于在高固含量下的粘度。
(粘度变化率(%)) = {(固含量为80重量%时的粘度) − (固含量为65重量%时的粘度)}/(固含量为65重量%时的粘度) × 100。
本发明的水性聚氨酯树脂组合物中的聚氨酯树脂的平均分子量不受特别限制,并可在作为水性涂料提供可分散性和良好涂膜的范围内选择,其优选为5000至500000,更优选10000至100000。在本说明书中,聚氨酯树脂的平均分子量是通过凝胶渗透色谱法测得的重均分子量,并使用聚苯乙烯作为标准物质。
本发明的水性聚氨酯树脂组合物中的聚氨酯树脂中的羧基的酸值优选在4.5至30mgKOH/g的范围内,更优选在5至25 mgKOH/g的范围内,再更优选在6至22 mgKOH/g的范围内。在本说明书中,树脂的酸值是指中和1克树脂所需的氢氧化钾的毫克数。酸值是根据JISK 1557的指示剂滴定法测得的值。
本发明的水性聚氨酯树脂组合物中的聚氨酯树脂的羟值不受特别限制,但通常在1至100 mgKOH/g的范围内。在本说明书中,树脂的羟值是指与1克树脂中的羟基对等的氢氧化钾的毫克(mg)数。羟值是根据JIS K 1557的方法B的指示剂滴定法测得的值。
本发明的水性聚氨酯树脂组合物可独自使用或与涂料和胶粘剂领域中已知的粘合剂、辅助剂和添加剂(特别是乳化剂、光稳定剂如紫外线吸收剂和位阻胺(HALS)、抗氧化剂、填料、辅助剂如抗沉降剂、消泡剂和/或润湿剂、流动改进剂、反应稀释剂、增塑剂、中和剂、催化剂、助溶剂和/或增稠剂,以及添加剂,如颜料、着色剂或流平剂)一起使用。也可加入增粘剂。添加剂可以刚好在加工前添加到本发明的产物中。但是,也可能在粘合剂的分散之前或过程中加入至少一部分添加剂。
[含有水性聚氨酯树脂组合物的涂装组合物等]
本发明还涉及含有上述水性聚氨酯树脂组合物的涂装组合物、涂料组合物、墨水组合物和胶粘剂组合物。
除该水性聚氨酯树脂组合物外,可将另一树脂添加到本发明的涂装组合物、涂料组合物、墨水组合物和胶粘剂组合物中。
另一树脂的实例包括聚酯树脂、丙烯酸系树脂、聚醚树脂、聚碳酸酯树脂、聚氨酯树脂、环氧树脂、醇酸树脂、聚烯烃树脂、氯乙烯树脂等。这些可独自使用或两种或更多种组合使用。
从在水中的可分散性的角度看,另一树脂优选具有一种或多种类型的亲水基团。亲水基团包括羟基、羧基、磺基、聚乙二醇基团等。
聚酯树脂通常可通过酸组分和醇组分之间的酯化或酯交换生产。对于酸组分,可使用通常用作酸组分以生产聚酯树脂的化合物。例如,脂族多元酸、脂环族多元酸、芳族多元酸等可用作酸组分。
丙烯酸系树脂优选是例如含羟基的丙烯酸系树脂。含羟基的丙烯酸系树脂可通过已知方法,例如在有机溶剂中的溶液聚合法或在水中的乳液聚合法生产,其中使含羟基的可聚合不饱和单体与另一种可与含羟基的可聚合不饱和单体共聚的可聚合不饱和单体共聚。
含羟基的可聚合不饱和单体是在一个分子中具有一个或多个羟基和一个或多个可聚合不饱和键的化合物。其实例包括:(甲基)丙烯酸与具有2至8个碳原子的二元醇的单酯化产物,如(甲基)丙烯酸2-羟乙酯、(甲基)丙烯酸2-羟丙酯、(甲基)丙烯酸3-羟丙酯和(甲基)丙烯酸4-羟丁酯;这些单酯化产物的ε-己内酯改性产物;N-羟甲基(甲基)丙烯酰胺;烯丙醇;和具有在分子末端含羟基的聚氧乙烯链的(甲基)丙烯酸;等等。
含羟基的丙烯酸系树脂优选具有阴离子官能团。具有阴离子官能团的含羟基的丙烯酸系树脂可通过例如使用具有阴离子官能团,如羧酸基团、磺酸基团或磷酸基团的可聚合不饱和单体作为一种类型的可聚合不饱和单体制成。
聚醚树脂的实例包括具有醚键的聚合物或共聚物,如基于聚氧乙烯的聚醚、基于聚氧丙烯的聚醚、基于聚氧丁烯的聚醚、衍生自芳族多羟基化合物,包括双酚A、双酚F等的聚醚,等等。
聚碳酸酯树脂的实例包括由双酚A、3-甲基-1,5-戊二醇和1,6-己二醇制成的聚合物。
环氧树脂的实例包括通过双酚化合物与表氯醇等的反应获得的树脂。双酚的实例包括双酚A和双酚F。
醇酸树脂的实例包括例如通过多元酸如邻苯二甲酸、对苯二甲酸或琥珀酸和多元醇进一步与改性剂,如脂肪和油/脂肪和油酸(大豆油、亚麻籽油、棕榈油、硬脂酸等)或天然树脂(松香、琥珀(succinite)等)反应而得的醇酸树脂。
聚烯烃树脂的实例包括酌情通过对聚烯烃树脂(其通过根据正常聚合方法使基于烯烃的单体与另一单体聚合或共聚而得)施以使用乳化剂的水分散或酌情通过基于烯烃的单体与另一单体的乳液聚合获得的树脂。此外,在一些情况下,可使用所谓的氯化聚烯烃改性树脂,其通过将聚烯烃树脂氯化而得。
基于烯烃的单体的实例包括α-烯烃,如乙烯、丙烯、1-丁烯、3-甲基-1-丁烯、4-甲基-1-戊烯、3-甲基-1-戊烯、1-庚烯、1-己烯、1-癸烯和1-十二烯;和共轭二烯和非共轭二烯,如丁二烯、亚乙基降冰片烯、双环戊二烯,1,5-己二烯和苯乙烯。这些单体可独自使用或两种或更多种组合使用。
可与基于烯烃的单体共聚的另一单体的实例包括乙酸乙烯酯、乙烯醇、马来酸、柠康酸、衣康酸、马来酸酐、柠康酸酐和衣康酸酐。这些单体可独自使用或两种或更多种组合使用。
本发明的涂装组合物、涂料组合物、墨水组合物和胶粘剂组合物可进一步包括固化剂。通过包括固化剂,有可能改进使用该涂料组合物、墨水组合物或胶粘剂组合物获得的涂装膜、多层涂装膜、涂膜或印刷品的耐久性。
例如,多异氰酸酯、封闭型多异氰酸酯、三聚氰胺树脂、碳二亚胺、噁唑啉、氮杂环丙烷、肼等可用作固化剂。要指出,这些固化剂可独自使用或两种或更多种组合使用。
多异氰酸酯不受特别限制,只要该多异氰酸酯在分子中具有两个或更多个异氰酸酯基团,其实例包括与作为多异氰酸酯化合物(a)例举的那些相同的那些。
封闭型多异氰酸酯不受特别限制,只要该封闭型多异氰酸酯在分子中具有两个或更多个封闭型异氰酸酯基团,其实例包括多异氰酸酯化合物(a)或通过向用已知封闭剂[酚、仲醇或叔醇、肟、脂族或芳族仲胺、邻苯二甲酸酰亚胺、内酰胺、活性亚甲基化合物(丙二酸二烷基酯等)、基于吡唑的化合物(吡唑、3,5-二甲基吡唑等)、酸性亚硫酸钠等]封闭的多异氰酸酯化合物(a)提供亲水性而获得的化合物等。
三聚氰胺树脂不受特别限制,并可使用常用作固化剂的那种。例如,三聚氰胺树脂优选是通过烷基醚化获得的烷基醚化三聚氰胺树脂,更优选是被甲氧基和/或丁氧基取代的三聚氰胺树脂。这样的三聚氰胺树脂包括:仅具有甲氧基的那些,如Cymel 325、Cymel327、Cymel 370和My Coat 723;具有甲氧基和丁氧基的那些,如Cymel 202、Cymel 204、Cymel 211、Cymel 232、Cymel 235、Cymel 236、Cymel 238、Cymel 251、Cymel 254、Cymel266、Cymel 267和Cymel 285(它们都是商品名,由Nippon Cytec Industries, Ltd.制造);和仅具有丁氧基的那些,如My Coat 506(商品名,由Mitsui-Cytec Ltd.制造)、U-VAN20N60和U-VAN 20SE(它们都是商品名,由Mitsui Chemicals, Inc.制造)。这些可独自使用或两种或更多种组合使用。其中,Cymel 211、Cymel 251、Cymel 285、Cymel 325、Cymel 327和My Coat 723更优选。
碳二亚胺不受特别限制,只要碳二亚胺是在分子中具有两个或更多个碳二亚胺基团的化合物。例如,可使用脂族聚碳二亚胺[聚(六亚甲基碳二亚胺)等]、脂环族聚碳二亚胺[聚(4,4'-二环己基甲烷碳二亚胺)等]和芳族聚碳二亚胺[聚(对亚苯基碳二亚胺)、聚(4,4'-二苯甲烷碳二亚胺)、聚(二异丙基苯基碳二亚胺)等],它们通过使具有8至26个碳原子的芳族多异氰酸酯、具有4至22个碳原子的脂族多异氰酸酯、具有8至18个碳原子的脂环族多异氰酸酯或具有10至18个碳原子的芳脂族多异氰酸酯聚合而得。作为市售产品,可列举Nisshinbo Chemical Inc.制造的“Carbodilite V-01”、“Carbodilite V-02”、“Carbodilite V-03”、“Carbodilite V-04”、“Carbodilite V-05”、“Carbodilite V-07”、“Carbodilite V-09”、“Carbodilite E-02”、“Carbodilite E-03A”、“Carbodilite E-04”等。
噁唑啉不受特别限制,只要该噁唑啉是在分子中具有两个或更多个噁唑啉基团(噁唑啉骨架)的化合物。其实例包括:具有两个或更多个噁唑啉基团的化合物,如2,2'-异丙叉基双(4-苯基-2-噁唑啉);可聚合噁唑啉化合物,如2-异丙烯基-2-噁唑啉、2-乙烯基-2-噁唑啉和2-乙烯基-4-甲基-2-噁唑啉的(共)聚合物;可聚合噁唑啉化合物和不与噁唑啉基团反应的可共聚单体[(甲基)丙烯酸酯,如(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸羟乙酯和聚乙二醇(甲基)丙烯酸酯、(甲基)丙烯酸酰胺乙酸乙烯酯、苯乙烯、α-甲基苯乙烯、苯乙烯磺酸钠等]的共聚物;等等。作为市售产品,可列举Nippon ShokubaiCo., Ltd.制造的“Epocros K-2010E”、“Epocros K-2020E”和“Epocros WS-500”等。
氮杂环丙烷不受特别限制,只要该氮杂环丙烷是在分子中具有两个或更多个氮杂环丙烷基团的化合物。其实例包括四羟甲基甲烷三(β-氮杂环丙烷基丙酸酯)和三羟甲基丙烷三(β-氮杂环丙烷基丙酸酯)。
肼包括肼和在分子中具有两个或更多个肼基团(肼骨架)的化合物[例如具有2至10个碳原子的二羧酸二酰肼(草酸二酰肼、丙二酸二酰肼、丁二酸二酰肼、戊二酸二酰肼、己二酸二酰肼、癸二酸二酰肼、马来酸二酰肼、富马酸二酰肼、衣康酸二酰肼等)和具有2至10个碳原子的亚烷基二肼(亚乙基二肼、1,3-亚丙基二肼、1,4-亚丁基二肼、1,6-亚己基二肼等)]。
可将着色颜料、体质颜料(extender pigment)和光亮颜料(bright pigment)添加到本发明的涂装组合物、涂料组合物和墨水组合物中。
着色颜料的实例包括氧化钛、锌白、炭黑、钼红、普鲁士蓝、钴蓝、偶氮颜料、酞菁颜料、喹吖啶酮颜料、异吲哚啉颜料、硒基颜料、苝颜料等。优选使用氧化钛和/或炭黑作为着色颜料。要指出,这些可独自使用或两种或更多种组合使用。
体质颜料的实例包括粘土、高岭土、硫酸钡、碳酸钡、碳酸钙、滑石、二氧化硅和氧化铝白。优选使用硫酸钡和/或滑石作为体质颜料,更优选使用硫酸钡。要指出,这些可独自使用或两种或更多种组合使用。
例如,铝、铜、锌、黄铜、镍、氧化铝、云母、被氧化钛或氧化铁涂覆的氧化铝、或被氧化钛或氧化铁涂覆的云母可用作光亮颜料。
本发明的涂装组合物、涂料组合物、墨水组合物和胶粘剂组合物可含有常规添加剂,如增稠剂、固化催化剂、紫外线吸收剂、光稳定剂、消泡剂、增塑剂、表面调节剂(surfaceconditioner)和抗沉降剂,取决于其功能或用途。要指出,这些可独自使用或两种或更多种组合使用,或市售产品可按原样使用。
生产本发明的涂装组合物、涂料组合物、墨水组合物或胶粘剂组合物的方法不受特别限制并可采用已知生产方法。但是,该涂装组合物、涂料组合物、墨水组合物和胶粘剂组合物合适地通过将水性聚氨酯树脂组合物与上文提到的各种树脂和添加剂混合,进一步加入水性介质和为施加方法调节粘度而制成。
对于本发明的涂装组合物、涂料组合物、墨水组合物和胶粘剂组合物所施加的材料,合适的材料包括:通常用于汽车车身或部件的金属材料、路面材料、家用建筑材料等(例如电沉积涂覆的钢板、磷化钢板、镀锌钢板、冷轧钢板、铝板、不锈钢板、磷酸锌处理的钢板、磷酸铁处理的钢板等);或塑料材料,如聚氨酯、聚碳酸酯、聚对苯二甲酸丁二醇酯、聚酰胺、聚苯醚、丙烯腈/丁二烯/苯乙烯共聚物(即ABS树脂)、聚丙烯和不饱和聚酯(通常缩写为SMC)。但是,本发明不限于此。
这些材料可以就这样使用或可经过表面处理,如去油或底漆涂装和/或中间涂装。这些处理可独自或两种或更多种组合进行。
为了通过使用本发明的涂装组合物、涂料组合物、墨水组合物或胶粘剂组合物来修复先前施加在该材料上的多层涂膜,优选首先对需要修复的涂膜部分施以溶剂清洁或砂磨处理,然后涂装。
本发明的涂装组合物、涂料组合物、墨水组合物和胶粘剂组合物可在使用前进行调节以具有适用于常规涂覆方法,如空气喷涂、无气喷涂或静电涂覆或用于获得所需膜厚度的特定粘度。例如,为了涂覆塑料材料,水性涂装组合物优选在使用前通过加入去离子水和如果必要,添加剂,如增稠剂和消泡剂而进行调节以具有大约10至40重量%的固含量和大约800至5,000 cps/6 rpm的粘度(用B型粘度计测得)。
上述合适的材料可用本发明的涂装组合物、涂料组合物、墨水组合物或胶粘剂组合物的单涂层涂覆,但可在本发明的涂装组合物、涂料组合物、墨水组合物或胶粘剂组合物的施加涂料上通过所谓的湿对湿法或在预热后的湿对湿法施加中间涂层材料。同时,在电沉积膜上施加本发明的涂装组合物、涂料组合物、墨水组合物或胶粘剂组合物的涂料后,可通过湿对湿法或在预热后的湿对湿法进行顶部涂覆。预热是在40至80℃下加热5至60分钟的方法,例如,在80℃下加热5分钟,并通过热风加热、红外照射等进行。
用于涂覆的涂装组合物、涂料组合物、墨水组合物或胶粘剂组合物的干膜厚度可随涂覆方法和必要性而变,但可通常为大约10至50 μm。
施加的涂装组合物、涂料组合物、墨水组合物或胶粘剂组合物随后通过放置在室温下、空气干燥或使用热风干燥或红外加热器的强制干燥等完全或不完全干燥,或在一些情况下,通过在不大于120℃的温度下烘烤而完全或不完全固化,以获得水性涂膜。特别地,为了根据本发明在塑料材料上形成水性涂膜,优选通过在涂覆后用空气干燥或热风干燥在40至120℃下将含水量干燥至大约不大于25重量%来获得水性膜。或者,为了修复多层涂膜,优选通过在涂覆后用吹气或最多80℃的热空气进行干燥来获得水性膜。
由于本发明的水性聚氨酯树脂组合物甚至在该组合物具有高固含量时也具有良好流动性,使用该组合物的涂料具有良好的成品外观。此外,使用该组合物的涂膜对基底的附着力,特别是对电沉积涂膜的附着力良好,并且甚至在单个涂层(单涂层)体系和多层涂层体系中也提供优异的耐冲击性。本发明的水性聚氨酯树脂组合物适合作为水性涂料的原料以涂覆电沉积膜。
实施例
通过以下具体实施例更详细描述本发明。
PolyTHF2000是可获自BASF AG的聚四亚甲基醚二醇(OH值: 56 mgKOH/g;数均分子量: 2000 g/mol)。
PolyTHF1000是可获自BASF AG的聚四亚甲基醚二醇(OH值: 112 mgKOH/g;数均分子量: 1000 g/mol)。
Desmophen 3600Z是可获自Sumika Covestro Urethane Co., Ltd.的聚环氧丙烷聚醚多元醇(OH值: 56 mg KOH/g;数均分子量: 2000 g/mol)。
PolyTHF650是可获自BASF AG的聚四亚甲基醚二醇(OH值: 173 mg KOH/g;数均分子量 650 g/mol)。
Desmophen C2202是可获自Sumika Covestro Urethane Co., Ltd.的聚碳酸酯多元醇(OH值: 56 mgKOH/g;数均分子量: 2000 g/mol)。
Desmophen 2028I是可获自Sumika Covestro Urethane Co., Ltd.的聚酯多元醇(OH值: 56 mgKOH/g;数均分子量: 2000 g/mol)。
IPDI是可获自Sumika Covestro Urethane Co., Ltd.的异佛尔酮二异氰酸酯(Desmodur I)。
HDI是可获自Sumika Covestro Urethane Co., Ltd.的六亚甲基二异氰酸酯(Desmodur H)。
W是可获自Sumika Covestro Urethane Co., Ltd.的4,4'-二环己基甲烷二异氰酸酯(Desmodur W)。
AAS是可获自FUJIFILM Wako Pure Chemical Corporation的2-[(2-氨基乙基)氨基]乙磺酸钠(产品号: W01COBQV-7243)。
DMPA是可获自Tokyo Chemical Industry Co., Ltd.的二羟甲基丙酸(双-MPA)。
AAP是可获自FUJIFILM Wako Pure Chemical Corporation的3-[(2-氨基乙基)氨基]丙酸钠(产品号: W01COBQV-3340)。
EDA是可获自Tokyo Chemical Industry Co., Ltd.的乙二胺(E0077)。
TMP是可获自Tokyo Chemical Industry Co., Ltd.的三羟甲基丙烷(T0480)。
DEOA是可获自Tokyo Chemical Industry Co., Ltd.的二乙醇胺(S0376)。
DMEA是可获自Tokyo Chemical Industry Co., Ltd.的N,N-二甲基乙醇胺(D0649)。
[测量水性聚氨酯树脂组合物的一般粘度的方法]
根据JIS Z8803通过使用B型旋转粘度计在25℃下进行测量。
[测量在水性聚氨酯树脂组合物的高固含量下的粘度的方法,特别是其中水性聚氨酯树脂组合物在聚氨酯树脂的含量为65重量%时具有不小于500 Pa·s且不大于50,000Pa·s的粘度。]
对于在高固含量下的粘度,例如有可能通过使用蒸发器等蒸发水性聚氨酯树脂组合物中的水性介质以调节所含聚氨酯树脂的量来测量在聚氨酯树脂的含量不小于65重量%时的粘度。在25℃下用流变仪(例如TA Instruments制造的AR-G2)测量粘度。使用的测量条件是间隙:0.25毫米;几何:锥板型;直径:20毫米;锥角:0.042弧度;和转速:0.1 S-1。
[测量组分(b)的多元醇化合物的平均分子量的方法]
为了测量组分(b)的多元醇化合物的平均分子量,写入由使用凝胶渗透色谱法(GPC)预先创建的标准聚苯乙烯校准曲线获得的转换值。
[测量聚氨酯树脂的平均分子量的方法]
为了测量聚氨酯树脂的平均分子量,写入由使用凝胶渗透色谱法(GPC)预先创建的标准聚苯乙烯校准曲线获得的转换值。
[计算聚氨酯树脂的酸值的方法]
计算值(mgKOH/g)以中和聚氨酯树脂中存在的羧基或磺基所需的氢氧化钾的毫克数表示。通过以下公式计算羧基的酸值与总酸值的比率。总酸值是指羧基的酸值和磺基的酸值的总和。
羧基的酸值与总酸值的比率 = AV[COOH]/(AV[COOH] + AV[SO3H])
AV(总): 聚氨酯树脂中的总酸值(AV[COOH] + AV[SO3H]).
AV[COOH]: 由聚氨酯树脂中的羧基导出的酸值
AV[SO3H]: 由聚氨酯树脂中的磺基导出的酸值。
[测量聚氨酯树脂的羟值的方法]
根据JIS K 1557的B方法测量聚氨酯树脂的羟值。
[生产实施例1: 水性聚氨酯树脂组合物实施例1(PUD 1号)]
在配备搅拌器和加热装置的反应容器中,装载4.19重量份的PolyTHF1000(组分b1)、19.59重量份的PolyTHF2000(组分b2)和0.69重量份的DMPA(组分c)并加热至70℃。接下来,加入2.28重量份的六亚甲基二异氰酸酯(组分a1)和3.02重量份的异佛尔酮二异氰酸酯(组分a2)的混合物,并将混合物在100至115℃下搅拌直至该混合物具有略低于理论NCO值的值。将成品预聚物在50℃下溶解在丙酮中以得到浓度为大约40%的溶液。然后在通过加入0.46重量份的DMEA进行中和处理后,测量0.28重量份乙二胺(组分d1)、0.31重量份AAS(组分c)和5.0重量份去离子水的溶液并输入。第二次搅拌时间为15分钟。然后通过加入64.18重量份去离子水进行分散。接下来,通过真空蒸馏除去溶剂以获得固含量为30.82重量%和粘度为2194 mPa·s(25℃,B型粘度计,JIS Z8803)的分散体。
[生产实施例2至10(水性聚氨酯树脂组合物实施例2至10(PUD 2至10号))和水性聚氨酯树脂组合物对比例1至6(PUD 11至16号)]
通过与水性聚氨酯树脂组合物(PUD 1号)的生产实施例中相同的操作,用下表1中所示的配方获得水性聚氨酯树脂组合物2至16号。
表1显示水性聚氨酯树脂组合物的组成和在各浓度下的粘度值(除非另行规定,表中的值代表重量份)。
Setaqua B E270是可获自Nuplex Industries Ltd.的聚酯分散体(OH值: 96mgKOH/g;数均分子量: 1000 g/mol)。
Envirogem AD-01是可获自Air Products Japan K.K.的表面调节剂(surfaceconditioner)。
TEGO WET 775W是可获自Evonik Japan Co., Ltd.的颜料分散剂。
JR-806是可获自Teyka Corporation的钛白。
[颜料分散浆]
将11.30重量份的聚酯分散体Setaqua B E 270装载到带有搅拌器的不锈钢圆柱形搅拌釜中,并在搅拌下加入25.30重量份的离子交换水。接下来,加入1.60重量份的DMEA10%水溶液,并在搅拌下加入1.60重量份的颜料分散剂TEGO WET 775W。在充分搅拌下,加入1.30重量份的表面调节剂Envirogem AD-01。在继续搅拌的同时,然后装载58.90重量份的氧化钛JR-806并搅拌15分钟,直至整体在充分搅拌下变得均匀以制成颜料漆浆。使用漆摇动器对该漆浆施以颜料分散,以制成用于水性底漆的颜料分散浆。其非挥发物含量为68.8%且颜料浓度(PWC)为85.0%。
颜料分散浆的配混比如下表2中所示。
Cymel 327是可获自Mitsui-Cytec Ltd.的三聚氰胺树脂。
Bayhydrol A 2770是可获自Sumika Covestro Urethane Co., Ltd.的丙烯酸系分散体。
Byhidule BL 2781是可获自Sumika Covestro Urethane Co., Ltd.的封闭型异氰酸酯。
[水性涂装组合物1号的生产]
加入31.1重量份基于表2制成的颜料分散浆、21.8重量份在生产实施例1中制成的水性聚氨酯树脂组合物1号、1.6重量份的三聚氰胺树脂Cymel 327、19.4重量份的丙烯酸系分散体Bayhydrol A 2770、21.8重量份的封闭型异氰酸酯Byhidule BL 2781和4.3重量份的去离子水并充分搅拌以获得具有47重量%的固含量的水性涂装组合物1号。此后,为了获得能够喷涂的粘度,使用福特杯4号以通过加入去离子水进行调节,以在20℃下获得大约40秒的粘度。
[用于评估的涂覆板的制造]
空气喷涂水性涂装组合物1号以涂覆电沉积的钢板,以使干膜厚度为35至40 μm,在140℃下烘烤30分钟以获得用于评估的试验板。
水性涂装组合物2至10号的生产(实施例2至10)
通过用下表3中所示的配方进行与水性涂装组合物1号的生产实施例中相同的操作,制备水性涂装组合物2至10号,并用相同程序制造用于评估的涂覆板。
水性涂装组合物11至16号(对比例1至6)
通过用下表3中所示的配方进行与水性涂装组合物1号的生产实施例中相同的操作,制备水性涂装组合物11至16号,并用相同程序制造用于评估的涂覆板。
[测试方法]
[测量成品外观的方法]
通过垂直涂覆制造多层涂膜,并根据JIS K-5400 7.6 (1990)的60°镜面光泽度测量涂膜的光泽度水平。不小于90的光泽度值表明成品外观优异并由表示。不小于80且小于90的光泽度值由○表示,不小于70且小于80由△表示,且小于70由×表示。
[测量耐冲击性的方法]
耐崩裂性: 将试验板安装在碎石试验仪器JA-400(Suga Test Instruments Co.,Ltd.制造,商品名,崩裂试验装置)的样品支架上;在-20℃下通过0.441 MPa(4.5 kgf/cm2)的压缩空气将50克粒度号为7的花岗岩碎石吹向涂覆表面;目视观察和评估涂膜上由碎石造成的损伤程度。
评估: 涂膜的状态
○: 损伤尺寸小到暴露出电沉积膜的程度
△: 损伤尺寸小,但暴露出基础钢板
×: 损伤尺寸极大,并且也很大暴露出基础钢板。
[测量附着力的方法]
进行划格法附着力试验(100个尺寸为1 × 1 mm的方格,胶带剥离)。
○: 剩余方格数100/100
△: 剩余方格数95-99/100
×: 剩余方格数小于95/100。
表3概括评估试验的各自结果(除非另行规定,表中的值代表重量份)。
由表3中的结果可以看出,本发明的水性涂装组合物具有良好成品外观、对电沉积膜的良好附着力和优异的耐冲击性。
工业适用性
由于本发明的水性聚氨酯树脂组合物甚至在该组合物具有高固含量时也具有良好流动性,使用该组合物的涂料具有良好的成品外观。此外,使用该组合物的涂膜对基底的附着力,特别是对电沉积涂膜的附着力良好,并且甚至在单个涂层(单涂层)体系和多层涂层体系中也可提供优异的耐冲击性。相应地,本发明的水性聚氨酯树脂组合物适合作为水性涂料的原料以涂覆电沉积膜。
根据本发明,有可能获得具有优异的成品外观和对电沉积膜的附着力和耐冲击性的水性聚氨酯树脂组合物,这些是相互矛盾的所需性质。本发明的水性聚氨酯树脂组合物可广泛用作涂装组合物、涂料组合物、墨水组合物、胶粘剂组合物等的原料。
Claims (14)
1.水性聚氨酯树脂组合物,其包含由至少以下组分(a)至(d)获得的聚氨酯树脂:
(a) 彼此不同的至少两种类型的有机二异氰酸酯化合物和/或多异氰酸酯化合物;
(b) 多元醇化合物;
(c) 含酸性基团的化合物,其包含至少两种类型的化合物,它们是含有羧基作为酸基的化合物(含羧基的化合物)和含有磺基作为酸基的化合物(含磺基的化合物);和
(d) 选自多胺化合物、二胺化合物、多元醇化合物和烷醇胺化合物的扩链剂,所述扩链剂具有不大于400的分子量,
其中所述水性聚氨酯树脂组合物在聚氨酯树脂的含量为65重量%时具有不小于500Pa·s且不大于50000 Pa·s的粘度。
2.根据权利要求1的水性聚氨酯树脂组合物,其中组分(c)的含酸性基团的化合物是具有两个或更多个羟基或氨基的化合物。
3.根据权利要求1或2的水性聚氨酯树脂组合物,其中作为组分(a)包括彼此不同的至少两种类型的有机二异氰酸酯化合物。
4.根据权利要求1至3任一项的水性聚氨酯树脂组合物,其中所述有机二异氰酸酯化合物包括至少一种类型的脂环族二异氰酸酯化合物。
5.根据权利要求1至4任一项的水性聚氨酯树脂组合物,其中至少一种类型的有机二异氰酸酯化合物是选自4,4'-二环己基甲烷二异氰酸酯和异佛尔酮二异氰酸酯的脂环族二异氰酸酯化合物,且所述脂环族二异氰酸酯化合物的含量百分比为基于100摩尔%的组分(a)的有机二异氰酸酯化合物计不大于80摩尔%。
6.根据权利要求1至5任一项的水性聚氨酯树脂组合物,其中组分(b)的多元醇化合物含有聚醚多元醇。
7.根据权利要求1至6任一项的水性聚氨酯树脂组合物,其中组分(b)是聚四亚甲基二醇多元醇。
8.根据权利要求1至7任一项的水性聚氨酯树脂组合物,其中组分(b)具有大于400 g/mol且不大于6000 g/mol的平均分子量。
9.根据权利要求1至8任一项的水性聚氨酯树脂组合物,其中聚氨酯树脂中所含的组分(b)的百分比为不小于60重量%。
10.根据权利要求1至9任一项的水性聚氨酯树脂组合物,其中组分(c)在聚氨酯树脂中的存在量使得含羧基的化合物和含磺基的化合物的总重量为0.2至10重量%。
11.根据权利要求1至10任一项的水性聚氨酯树脂组合物,其中羧基的酸值与组分(c)中的总酸值的比率为0.20至0.95。
12.根据权利要求1至11任一项的水性聚氨酯树脂组合物,其中所述聚氨酯树脂中的羧基的酸值在4.5至30 mgKOH/g的范围内。
13.根据权利要求1至12任一项的水性聚氨酯树脂组合物,其中所述聚氨酯树脂的含量百分比为20至65重量%。
14.涂装组合物、涂料组合物、墨水组合物或胶粘剂组合物,其含有根据权利要求1至13任一项的水性聚氨酯树脂组合物。
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EP20152018.6A EP3851468A1 (en) | 2020-01-15 | 2020-01-15 | Aqueous polyurethane resin composition and coating material using the composition |
EP20152018.6 | 2020-01-15 | ||
PCT/EP2020/087651 WO2021136727A1 (en) | 2019-12-30 | 2020-12-22 | Aqueous polyurethane resin composition and coating material using the composition |
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CN115368533A (zh) * | 2022-09-08 | 2022-11-22 | 大余松瀛化工有限公司 | 一种水性聚氨酯树脂制备方法及其应用 |
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JP2023509021A (ja) | 2023-03-06 |
US20230048853A1 (en) | 2023-02-16 |
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