CN107532037A - 用于形成施加到金属上的弹性体组合物的体系 - Google Patents
用于形成施加到金属上的弹性体组合物的体系 Download PDFInfo
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- CN107532037A CN107532037A CN201680021700.6A CN201680021700A CN107532037A CN 107532037 A CN107532037 A CN 107532037A CN 201680021700 A CN201680021700 A CN 201680021700A CN 107532037 A CN107532037 A CN 107532037A
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Abstract
一种用于形成施加到基底上的弹性体组合物的体系包括异氰酸酯组分和异氰酸酯反应性组分。所述异氰酸酯组分包括聚合多异氰酸酯和任选异氰酸酯封端预聚物。所述异氰酸酯反应性组分可与所述异氰酸酯组分反应并包括多元醇组分和聚醚胺。所述多元醇组分是(a)疏水多元醇;(b)不同于所述疏水多元醇并具有大于500g/mol的重均分子量的聚醚多元醇;和(c)聚氨基多元醇的混合物。所述弹性体组合物作为所述异氰酸酯组分和所述异氰酸酯反应性组分的反应产物形成并可以作为弹性体涂层施加在基底如钢管上。具有施加的弹性体涂层的钢管满足如AWWA C222中阐述的用于供水工业的标准。
Description
对相关申请的交叉引用
本申请要求2015年2月16日提交的美国临时申请No.62/116,687的优先权,其内容经此引用并入本文。
发明背景
1.发明领域
本发明大体上涉及用于形成施加到金属上的弹性体组合物的体系。
2.相关技术描述
金属管道是每个城市的基础设施的基本组成部分。其用于各式各样的情形,包括室内和室外用途。金属管道可用于各式各样的用途,包括用于向住宅和企业输送饮用水。
为了保护这些管道免受腐蚀,通常在制造过程中向其暴露的外表面和内表面施加防腐蚀涂料组合物。这些涂料组合物因此必须能够保护金属管道免受安装之前和之后的腐蚀。另外,当用于输送饮用水的金属管道时,这些涂料组合物必须满足在供水工业中的使用安全性的社区标准。在美国对用于钢制水管和配件(fitting)的内部和外部的聚氨酯涂料组合物使用的一种标准是American Water Works Association Specification C222(ANSI/AWWA Standard C222,Standard for Polyurethane Coatings for the Interiorand Exterior of Steel Water Pipe,and Fittings,Revision Effective Date:December 1,2008),下文称作AWWA C222。AWWA C222提供对用于钢制水管的内部和外部的聚氨酯内衬和涂料体系的最低要求的指南,包括涂料、表面处理、测试、装卸和包装要求。
发明概述和优点
本申请提供一种用于形成施加到基底上的弹性体组合物的体系,其包括异氰酸酯组分和异氰酸酯反应性组分。
所述异氰酸酯组分包含聚合多异氰酸酯和任选异氰酸酯封端预聚物。所述异氰酸酯反应性组分包含多元醇组分和聚醚胺。所述多元醇组分是(a)疏水多元醇;(b)不同于所述疏水多元醇并具有大于500g/mol的重均分子量的聚醚多元醇;和(c)聚氨基多元醇的混合物。
本发明还公开了作为所述异氰酸酯组分和所述异氰酸酯反应性组分的反应产物形成的弹性体组合物。
本发明还公开了一种涂布基底的方法,其包括将所述弹性体组合物的层施加到基底上。
另外,本发明还公开了包括具有附着在其上的如上所述的弹性体涂层的基底的制品。在某些实施方案中,所述基底是具有外表面和内表面的金属管道,且所述弹性体组合物以层形式施加到外表面和内表面的至少一个上。
由本发明的体系形成的弹性体涂层理想地适用于保护金属管道免受腐蚀和磨损。特别地,由本发明的体系形成的弹性体涂层理想地适用于保护供水工业中所用的金属水管,因为用于钢管的该弹性体涂层满足如American Water Works AssociationSpecification C222中所述的对弹性体涂层的要求。
附图简述
联系附图考虑时容易理解本发明的其它优点,其参考下列详述更好地理解。
图1是具有在内表面和外表面上形成的弹性体涂层的金属管道的剖视图。
发明详述
该体系包含异氰酸酯组分和异氰酸酯反应性组分。术语“异氰酸酯反应性组分”在本发明的下列描述中也可与“树脂组分”互换使用。
在某些实施方案中,该异氰酸酯组分包含聚合异氰酸酯和任选异氰酸酯封端预聚物。该异氰酸酯反应性组分包括多元醇组分和聚醚胺。通常,该体系在两种或更多种分立组分,如异氰酸酯组分和异氰酸酯反应性组分中提供,即作为双组分(或2K)体系,其在下文中进一步描述。因此,本文所用的术语“体系”可与“双组分体系”互换使用和与“2K体系”互换使用。
要认识到,提到如本文所用的异氰酸酯和异氰酸酯反应性组分仅为了建立设置该体系的各组分的参考点和为了建立重量份基础。因此,不应解释为将本发明仅限于2K体系。例如,该体系的各组分可以都保持互相分开。
该体系还可包含附加组分,其可与异氰酸酯和/或异氰酸酯反应性组分包含在一起,或完全分立,如在下文进一步描述的第三组分中。
该体系用于形成弹性体组合物。在某些实施方案中,该弹性体组合物是该体系的异氰酸酯组分和异氰酸酯反应性组分的反应产物。
本申请还公开了这些弹性体组合物随后作为弹性体涂层施加在基底,特别是金属基底上。相关地,本申请公开了这些弹性体组合物作为涂层施加在制品,如金属管道上,其中这些制品上的涂层为这些制品提供所需的防腐蚀和外部机械应力的保护。特别地,该弹性体组合物形成理想地保护金属基底和金属制品免受腐蚀和磨损的硬质、坚韧和有弹性的弹性体涂层。该弹性体涂层在施加到这样的钢管道上时旨在满足American Water WorksAssociation Specification C222对用于供水工业的要求。
如果使用,该异氰酸酯封端预聚物通常是异氰酸酯和多元醇和/或多胺的反应产物,通常异氰酸酯和多元醇的反应产物。该异氰酸酯封端预聚物可通过本领域技术人员理解的各种方法形成或可购自制造商、供应商等。
关于用于形成该异氰酸酯封端预聚物的异氰酸酯,该异氰酸酯包括一个或多个异氰酸酯(NCO)官能团,通常至少两个NCO官能团。对本发明而言,合适的异氰酸酯包括,但不限于,传统脂族、脂环族、芳基和芳族异氰酸酯。在某些实施方案中,该异氰酸酯选自二苯甲烷二异氰酸酯(MDI)、聚合二苯甲烷二异氰酸酯(PMDI)及其组合。聚合二苯甲烷二异氰酸酯在本领域中也被称作多亚甲基多亚苯基多异氰酸酯。对本发明而言,其它合适的异氰酸酯的实例包括,但不限于,甲苯二异氰酸酯(TDI)、己二异氰酸酯(HDI)、异佛尔酮二异氰酸酯(IPDI)、萘二异氰酸酯(NDI)及其组合。通常,用于形成该异氰酸酯封端预聚物的异氰酸酯包含二苯甲烷二异氰酸酯(MDI)。
如果用于形成该异氰酸酯封端预聚物,该多元醇包括一个或多个羟基(OH)官能团,通常至少两个OH官能团。该多元醇可以是本领域中已知的任何类型的多元醇。该多元醇通常选自乙二醇、二乙二醇、丙二醇、二丙二醇、丁二醇、甘油、三羟甲基丙烷、三乙醇胺、季戊四醇、山梨糖醇及其组合。对本发明而言,下面在附加的任选组分(辅助多元醇)的描述中描述了其它合适的多元醇。
多元醇可以相对于异氰酸酯以各种量使用,只要在反应前存在相对于OH官能团过量的NCO官能团以使形成后的异氰酸酯封端预聚物包括用于后续反应的NCO官能团。该异氰酸酯封端预聚物通常具有大约18至大约28,更通常大约20至大约25,再更通常大约22.9重量%的NCO含量。可以作为与1当量正二丁胺合并的异氰酸酯量测定NCO含量,其以重量%测量。
如果用于形成该异氰酸酯封端预聚物,该多胺包括一个或多个胺官能团,通常至少两个胺官能团。该多胺可以是本领域中已知的任何类型的多胺。该多胺通常选自乙二胺、甲苯二胺、二氨基二苯甲烷和多亚甲基多亚苯基多胺、氨基醇及其组合。合适的氨基醇的实例包括乙醇胺、二乙醇胺、三乙醇胺及其组合。
多胺可以相对于异氰酸酯以各种量使用,只要在反应前存在相对于胺官能团过量的NCO官能团以使形成后的异氰酸酯封端预聚物包括用于后续反应的NCO官能团。该异氰酸酯封端预聚物的NCO含量如上文描述和例举。
要认识到,该异氰酸酯封端预聚物可以由两种或更多种上述多元醇和/或两种或更多种上述多胺的组合形成。通常,该异氰酸酯封端预聚物是异氰酸酯和至少一种多元醇的反应产物以使该异氰酸酯封端预聚物在形成后包括氨酯键和NCO官能团。在本发明的一个具体实施方案中,该异氰酸酯封端预聚物包含聚合甲基二苯基二异氰酸酯和4,4’-甲基二苯基二异氰酸酯的半预聚物的共混物。对本发明而言,合适的异氰酸酯封端预聚物的具体实例可以商标如MP102购自BASF Corporation,Florham Park,NJ。要认识到,该体系可包括两种或更多种上述异氰酸酯封端预聚物的组合。
关于聚合异氰酸酯,该聚合异氰酸酯包括两个或更多个NCO官能团。该聚合异氰酸酯通常具有大约1.5至大约3.0,更通常大约2.0至大约2.8,再更通常大约2.7的平均官能度。该聚合异氰酸酯通常具有大约30至大约33,更通常大约30.5至大约32.5,再更通常大约31.5重量%的NCO含量。
对本发明而言,合适的聚合异氰酸酯包括,但不限于,上文在异氰酸酯封端预聚物的描述中描述和例举的异氰酸酯。通常,该聚合异氰酸酯包含聚合二苯甲烷二异氰酸酯(PMDI)。
对本发明而言,合适的聚合异氰酸酯的具体实例可以商标如M20Isocyanate购自BASF Corporation并以商标如R23000(具有2.7的标称或平均官能度)出售。要认识到,该体系可包括两种或更多种上述聚合异氰酸酯的组合。
该异氰酸酯封端预聚物通常以大约25至大约75,更通常大约50至大约75,再更通常大约55至大约65,再更通常大约60重量份的量存在于该异氰酸酯组分中,各自基于100重量份的异氰酸酯组分计。在某些实施方案中,该异氰酸酯封端预聚物通常以大约50至大约250,更通常大约100至大约200,再更通常大约125至大约175,再更通常大约150重量份的量存在于该体系中,各自相对于该体系中的每100重量份聚合异氰酸酯计。换言之,异氰酸酯封端预聚物和聚合异氰酸酯通常以大约1:2至大约2.5:1,更通常大约1:1至大约2:1,再更通常大约1.25:1至1.75:1,再更通常大约1.5:1的重量比存在于该体系中,例如存在于异氰酸酯组分中。
不受制于或受限于任何特定理论,但相信,如上文刚刚描述和例举的异氰酸酯封端预聚物和聚合异氰酸酯的组合和比率赋予该弹性体组合物提高的拉伸强度、伸长、硬度和玻璃化转变温度,以及相对于传统弹性体组合物改进的撕裂强度。
包含聚合异氰酸酯和任选异氰酸酯封端预聚物的异氰酸酯组分通常以基于100份该体系计35.5至40份的量存在。换言之,该异氰酸酯组分构成该体系的总重量的35.5至40重量%。
该体系如上所述还包括可与异氰酸酯组分反应以形成弹性体组合物的异氰酸酯反应性组分。在某些实施方案中,该异氰酸酯反应性组分包含多元醇组分和聚醚胺。
在某些实施方案中,该多元醇组分包括未反应的羟基并包含(a)疏水多元醇、(b)不同于疏水多元醇(a)并具有大于500的重均分子量的聚醚多元醇;和(c)聚氨基多元醇的混合物。
关于疏水多元醇(a),该疏水多元醇包括一个或多个OH官能团,通常至少两个OH官能团。疏水多元醇的疏水性可通过各种方法测定,如通过目视检查疏水多元醇与异氰酸酯的反应产物,其中该反应产物在混合这两种组分后立即脱气,然后引入水中,在此使反应产物固化。如果在该反应产物与水之间的界面(或表面)处没有沾污或起皱的迹象或如果没有气泡或泡沫形成的迹象,该疏水多元醇的疏水性被认为优异。
该疏水多元醇通常包含天然油多元醇(NOP)。换言之,该疏水多元醇通常不是基于石油的多元醇,即衍生自石油产品和/或石油副产品的的多元醇。一般而言,只有少数天然存在的植物油含有未反应的OH官能团,且蓖麻油通常是唯一具有足够OH官能团含量以使蓖麻油适合直接用作氨酯化学中的多元醇的直接由植物来源产生的市售NOP。大多数(即使不是所有)其它NOP需要可直接获自植物的油的化学改性。NOP通常衍生自本领域中已知的任何天然油,通常衍生自植物或坚果油。对本发明而言,合适的天然油的实例包括蓖麻油,和衍生自大豆油、菜籽油、椰子油、花生油、低芥酸菜籽油(canola oil)等的NOP。使用天然油有助于降低环境影响。
通常,如上文暗示,该疏水多元醇包含蓖麻油,在某些实施方案中已提纯以除去残留水的纯化蓖麻油。如下文提到,术语“蓖麻油”是指未纯化或纯化的蓖麻油。本领域技术人员会认识到,蓖麻油固有包括OH官能团,而其它NOP可能需要一个或多个附加加工步骤以获得OH官能团。一般而言,蓖麻油和经过加工以包括OH官能团的NOP都不包括醚基团。如果必要,此类加工步骤是本领域技术人员理解的。对本发明而言,合适的蓖麻油等级可购自各种供应商。例如,来自Eagle Specialty Products(ESP)Inc.,St.Louis,MO的CastorOil可用作疏水多元醇。对本发明而言,其它合适的疏水多元醇的具体实例可以商标如750、805、1005、1080和1102购自BASF Corporation。
在某些实施方案中,疏水多元醇,如纯化蓖麻油以该体系的总重量的大约27至大约35重量%,如29至30重量%的量存在于该体系中。
该多元醇组分还包括至少一种不同于疏水多元醇(a)的聚醚多元醇(b)。聚醚多元醇(b)具有至少500g/mol的重均分子量。本发明的聚醚多元醇(b)据信提高异氰酸酯反应性组分与异氰酸酯组分和其它附加组分或添加剂在该体系中的均匀性。
对本发明而言,合适的聚醚多元醇包括,但不限于,通过环氧化物,例如环氧乙烷(EO)、环氧丙烷(PO)、环氧丁烷(BO),或四氢呋喃在多官能引发剂存在下的聚合获得的产物。合适的引发剂化合物含有许多活性氢原子并包括水、丁二醇、乙二醇、丙二醇(PG)、二乙二醇、三乙二醇、二丙二醇、乙醇胺、二乙醇胺、三乙醇胺、甲苯二胺、二乙基甲苯二胺、苯二胺、二苯甲烷二胺、乙二胺、环己烷二胺、环己烷二甲醇、间苯二酚、双酚A、甘油、三羟甲基丙烷、1,2,6-己三醇、季戊四醇及其组合。
其它合适的聚醚多元醇包括聚醚二醇和三醇,如聚氧丙烯二醇和三醇和通过环氧乙烷和环氧丙烷同时或相继加成到二-或三官能引发剂上而得的聚(氧乙烯-氧丙烯)二醇和三醇。也可以使用具有该多元醇组分的重量的大约5至大约90重量%的氧乙烯含量的共聚物,其中该多元醇可以是嵌段共聚物、无规/嵌段共聚物或无规共聚物。另一些合适的聚醚多元醇包括通过四氢呋喃的聚合获得的聚四亚甲基醚二醇。
在某些实施方案中,聚醚多元醇(b)是在不存在或基本不存在环氧乙烷的情况下形成的产物,因为环氧乙烷据信提高使用其的弹性体组合物的亲水性。在某些实施方案中,聚醚多元醇(b)是通过环氧丙烷的聚合形成的产物。
另外,在某些实施方案中,本发明的聚醚多元醇(b)具有500至650g/mol,如569g/mol的重均分子量。
此外,在某些实施方案中,本发明的聚醚多元醇(b)具有3.5至4,如3.96的平均官能度。
另外,在某些实施方案中,聚醚多元醇(b)是通过环氧丙烷在不存在环氧乙烷的情况下的聚合获得的产物,具有500至650g/mol的重均分子量并具有3.5至4.0的平均官能度。
通过环氧丙烷的聚合获得并具有569g/mol的分子量和3.96的平均官能度的一种合适的聚醚多元醇(b)可作为P-736购自BASF Corporation。
在某些实施方案中,通过环氧丙烷的聚合获得的聚醚多元醇(b)以该体系的总重量的1.8至5重量%,如2至3重量%,如2.5重量%的量存在。
在另一些实施方案中,该异氰酸酯反应性组分还包括通过四氢呋喃的聚合获得的聚四亚甲基醚二醇或聚醚醇。
在某些实施方案中,该聚四亚甲基醚二醇具有650至2000g/mol的重均分子量,如1000g/mol的重均分子量,并据信由于其较高相对分子量而提供所得弹性体组合物的提高的耐冲击性。
一种合适的聚四亚甲基醚二醇可作为Polyether Diol 1000购自BASF Corporation。
另外,在某些实施方案中,该聚四亚甲基醚二醇以该体系的总重量的4至10重量%,如5至8重量%,如7.5重量%的量存在于该体系中。
本发明中所用的聚氨基多元醇(c)是包括羟基官能和胺官能的化合物并添加到该体系中以由于其较低的相对分子量而提供提高的硬度。
在某些实施方案中,该聚氨基多元醇是二胺。在再一些实施方案中,该聚氨基醇是基于乙二胺和环氧丙烷的聚醚多元醇四醇。
在某些实施方案中,该聚氨基多元醇具有280至310g/mol,如290至300g/mol的重均分子量。
在再一些实施方案中,该聚氨基多元醇以该体系的总重量的4至10重量%,如5至8重量%,如7.5重量%的量存在于该体系中。
用于本申请的一种合适的聚氨基多元醇(c)是可购自Carpenter并以商品名Carpol EDAP-770出售(也被称作Quadrol或POLY EDA 770)的具有大约290-295的重均分子量的基于乙二胺和环氧丙烷的聚醚多元醇四醇。
该异氰酸酯反应性组分还包括聚醚胺,其添加到该体系中以至少部分由于其较高的相对分子量而为形成的弹性体组合物提供提高的耐冲击性。
在某些实施方案中,聚醚胺(d)是聚醚二胺。
另外,在某些实施方案中,聚醚胺(d)具有1000至3000g/mol,如1500至2500g/mol,如2000g/mol的重均分子量。
在再一些实施方案中,聚醚二胺(d)以该体系的总重量的4至10重量%,如5至8重量%,如7.5重量%的量存在于该体系中。
用于本申请的一种合适的聚醚胺是α-(2-氨基甲基乙基)-ω-(2-氨基甲基乙氧基)-聚(氧(甲基-1,2-乙烷二基)),其具有53.3至58.9mg KOH/g的胺值并由BASFCorporation以商品名Polyetheramine D 2000出售。
该体系可包括一种或多种附加组分,如添加剂组分。该添加剂组分可包含本领域中已知的任何传统添加剂。对本发明而言,合适的添加剂包括,但不限于,扩链剂、交联剂、链终止剂、加工添加剂、增粘剂、阻燃剂、抗氧化剂、消泡剂、防沫剂、水清除剂、分子筛、热解法二氧化硅、紫外线稳定剂、填料、触变剂、聚硅氧烷、表面活性剂、催化剂、着色剂、惰性稀释剂及其组合。如果使用,该添加剂组分可以以任何量,如基于该体系的100重量份异氰酸酯反应性组分计大约0.05至10重量份的量包含在该体系中。
在某些实施方案中,该添加剂组分包含防沫剂。在一个实施方案中,该防沫剂包含包括分散在其中的粉状二氧化硅的硅树脂流体(silicone fluid)。该硅树脂流体可用于降低和/或消除该弹性体组合物的发泡。应该认识到,该硅树脂流体可以预置于溶剂中。防沫剂的实例包括可购自Dow Corning,Midland,MI的Antifoam MSA和Antifoam A。
如果使用,该防沫剂通常以大约0.01至大约0.10,更通常大约0.025至大约0.075,再更通常大约0.05重量份的量存在于该体系中,各自基于该体系的100重量份的异氰酸酯反应性组分计。要认识到,该体系可包括两种或更多种上述防沫剂的任何组合。
在某些实施方案中,该添加剂组分包含分子筛。分子筛是可用于保持或增加干燥,即干燥态的吸湿剂。该分子筛通常包含具有大量小孔隙的分子。小孔隙使得尺寸小于该孔隙的分子,如水分子能被吸附,而更大分子,如异氰酸酯和异氰酸酯反应性组分中存在的那些分子无法被吸附。通常,该分子筛可吸附高达和超过分子筛重量的20%的水。因此,该分子筛可与疏水多元醇协同和配合工作以在水有机会与该体系的异氰酸酯组分反应之前通过吸附水将水对该弹性体组合物的影响减至最低。
如果使用,应该认识到,可以使用本领域中已知的任何分子筛,如铝硅酸盐矿物、粘土、多孔玻璃、微孔木炭、沸石、活性炭或具有例如水的小分子可经其扩散的开放结构的合成化合物。合适的分子筛的实例包括Baylith Paste和分子筛3A,可获自各种供应商,如Zeochem,Louisville,KY。
如果使用,分子筛通常以该体系的总重量的大约0.01至大约5.0,更通常大约0.10至大约2.5,再更通常大约1.25重量%的量存在于该体系中。要认识到,该体系可包括两种或更多种上述分子筛的任何组合。
在某些实施方案中,该添加剂组分包含可购自各种供应商的热解法二氧化硅。合适的热解法二氧化硅的一个实例是可购自Evonik Industries Inc.,Essen,Germany的R-972。热解法二氧化硅通常充当流变控制剂,并且如果该热解法二氧化硅是疏水的,其赋予该弹性体组合物额外的疏水性。
如果使用,该热解法二氧化硅通常以该体系的总重量%的大约0.10至大约10.0,更通常大约0.5至大约2.5,再更通常大约1.25重量%的量存在于该体系中。要认识到,该体系可包括两种或更多种热解法二氧化硅的任何组合。
在包括分子筛和热解法二氧化硅的某些实施方案中,在将疏水多元醇与异氰酸酯反应性组分的其余部分混合之前,将这些组分与疏水多元醇合并以形成混合在一起的糊。
在某些实施方案中,该添加剂组分包含着色剂。该着色剂可选自颜料、染料及其组合。该着色剂可以是液体或粉末形式的。如果使用,该着色剂通常是颜料,或两种或更多种颜料的颜料混合物。该颜料或颜料混合物用于赋予该弹性体组合物所需颜色,如果该颜料是无机的,该颜料也可赋予该弹性体组合物紫外线防护。
不同类型的颜料可用于本发明。例如,二氧化钛可用于为该弹性体组合物提供白色且炭黑可用于提供黑色,而二氧化钛和炭黑的各种混合物可用于为该弹性体组合物提供各种色调的灰色。
用于本发明的炭黑和二氧化钛的合适等级的实例可分别购自ColumbianChemicals Company,Marietta,GA,Titanium Technologies,Wilmington,DE和Repi S.p.A。除炭黑和/或二氧化钛外或替代炭黑和/或二氧化钛,也可以使用其它颜料,包括但不限于红色、绿色、蓝色、黄色、绿色和棕色,和它们的颜料混合物,以赋予该弹性体组合物颜色。
基于一种或多种着色剂的颜料的更具体实例包括宝石蓝、玉绿色、Sedona红、琥珀棕和黄玉棕。用于本发明的颜料的合适等级的实例可购自各种公司,如BASF Corporation和Penn Color,Inc.,Hatfield,PA。要认识到,可以使用上述着色剂,例如颜料的各种混合物以赋予该弹性体组合物各种颜色、强度和色调。
如果使用,该着色剂通常以该体系的总重量的大约0.10至大约5.0,更通常大约0.5至2.0,再更通常大约0.6重量%的量存在于该体系中。要认识到,该体系可包括两种或更多种上述着色剂的任何组合。
在某些实施方案中,该添加剂组分包含催化剂组分。在一个实施方案中,该催化剂组分包含锡催化剂。对本发明而言,合适的锡催化剂包括有机羧酸的锡(II)盐,例如乙酸锡(II)、辛酸锡(II)、乙基己酸锡(II)和月桂酸锡(II)。在一个实施方案中,该有机金属催化剂包含二丁基二月桂酸锡,其是有机羧酸的二烷基锡(IV)盐。对本发明而言,合适的有机金属催化剂,例如二丁基二月桂酸锡的具体实例可以商品名购自Air Productsand Chemicals,Inc.,Allentown,PA。该有机金属催化剂还可包含有机羧酸的其它二烷基锡(IV)盐,如二丁基二乙酸锡、二丁基马来酸锡和二辛基二乙酸锡。
对本发明而言,其它合适的催化剂的实例包括胺基催化剂、铋基催化剂、镍基催化剂、锆基催化剂、锌基催化剂、铝基催化剂、锂基催化剂、氯化铁(II);氯化锌;辛酸铅;三(二烷基氨基烷基)-s-六氢三嗪,包括三(N,N-二甲基氨基丙基)-s-六氢三嗪;四烷基氢氧化铵,包括四甲基氢氧化铵;碱金属氢氧化物,包括氢氧化钠和氢氧化钾;碱金属醇盐,包括甲醇钠和异丙醇钾;和具有10至20个碳原子和/或OH侧基的长链脂肪酸的碱金属盐。
对本发明而言,其它合适的催化剂,尤其是三聚催化剂的另一些实例包括N,N,N-二甲基氨基丙基六氢三嗪、钾、乙酸钾、N,N,N-三甲基异丙基胺/甲酸酯,及其组合。合适的三聚催化剂的一个具体实例可以商品名购自Air Products andChemicals,Inc.。
对本发明而言,其它合适的催化剂,尤其是叔胺催化剂的再一些实例包括1-甲基immidazol、DABCO 33-LV、二甲基氨基乙醇、二甲基氨基乙氧基乙醇、三乙胺、N,N,N',N'-四甲基乙二胺、N,N-二甲基氨基丙基胺、N,N,N',N',N"-五甲基二亚丙基三胺、三(二甲基氨基丙基)胺、N,N-二甲基哌嗪、四甲基亚氨基-双(丙基胺)、二甲基苄基胺、三甲基胺、三乙醇胺、N,N-二乙基乙醇胺、N-甲基吡咯烷酮、N-甲基吗啉、N-乙基吗啉、双(2-二甲基氨基-乙基)醚、N,N-二甲基环己基胺(DMCHA)、N,N,N',N',N"-五甲基二亚乙基三胺、1,2-二甲基咪唑、3-(二甲基氨基)丙基咪唑及其组合。合适的叔胺催化剂的具体实例可以商品名例如41购自Air Products and Chemicals,Inc.。
如果使用,该催化剂组分可以以各种量使用。通常,该催化剂组分以确保足够的开放/工作时间的量使用。要认识到,该催化剂组分可包括上述催化剂的任何组合。
如上所述,在某些实施方案中,该弹性体组合物包含异氰酸酯封端预聚物、聚合异氰酸酯和异氰酸酯反应性组分的反应产物。
本发明进一步提供一种形成弹性体组合物的方法。该方法包含提供异氰酸酯封端预聚物、聚合异氰酸酯和异氰酸酯反应性组分和作为其反应产物形成弹性体涂层的步骤。
本发明的所得弹性体组合物的异氰酸酯指数(NCO指数)为大约98至115,如100至大约110,更通常大约100至大约107,如103。换言之,在该体系中通常相对于该异氰酸酯反应性组分中存在的羟基和胺基团贡献的活性氢原子的摩尔量设定异氰酸酯组分中的未反应NCO基团的摩尔量,以使异氰酸酯组分中的未反应NCO基团相对于多元醇组分中的未反应羟基轻微化学计算过量(即该体系的NCO:OH摩尔比为0.98:1至1.15:1,如1:1至1.10:1,如1:1至1.07:1,如1.03:1)。在该典型实施方案中,这种轻微NCO过量能使形成的弹性体组合物中的残留未反应NCO基团与水分反应以促进该弹性体组合物在作为弹性体涂层施加到其预期金属基底上时或之后的进一步固化。此处1.15:1的上限防止弹性体涂层变得太脆。
该弹性体组合物在本领域中可被称作2K弹性体聚氨酯组合物。混合异氰酸酯和异氰酸酯反应性组分以形成该弹性体组合物的反应产物。本文所用的术语“反应产物”旨在涵盖异氰酸酯和异氰酸酯反应性组分之间的相互作用和/或反应的所有阶段。通常,在异氰酸酯和异氰酸酯反应性组分开始互相接触时开始形成该反应产物。
当喷涂该弹性体组合物时,应该认识到,异氰酸酯组分和异氰酸酯反应性组分可以在离开喷雾器的喷嘴之前或之后混合。在一个实施方案中,该树脂和异氰酸酯组分在离开喷雾器的喷嘴时是分开的料流并在涂布基底之前混合。在另一些实施方案中,该树脂和异氰酸酯组分在离开喷雾器的喷嘴之前预混。
本发明的弹性体组合物理想地保护金属管道免受腐蚀和磨损。特别地,本发明的弹性体组合物理想地保护供水工业中所用的钢制水管,因为根据本发明的实施方案形成并施加到钢制水管的内侧和外侧的弹性体涂料组合物满足AWWA C222对用于供水工业的钢管和配件上所用的弹性体涂层的要求。
因此,例如,如图1中所示,本发明的弹性体组合物可作为弹性体涂层22施加在金属管道20的内表面24和/或外表面26上。通常,涂层22的弹性体组合物在施加到内表面24和/或外表面上后基本或完全固化以形成基本不粘表面。该弹性体涂料组合物中的如上所述的任何残留NCO含量可能与金属管道20的环境中的残留水分反应以进一步固化各自的弹性体层22。
特别地,本发明的弹性体涂料组合物在根据AWWA C222的Section4.3和4.4施加到钢管的预处理表面上时,在钢管上形成满足如Section 4.2中对阴极剥离(如根据ASTM G95测得的12mm的最大剥离半径)、挠性(根据ASTM D522在77mm心轴上挠性180°弯曲中无开裂或层离)、耐冲击性(根据ASTM G14最少8.5N·m(牛顿米))、耐磨性(根据ASTM D4060使用CS17轮最多100-mg涂层损失/1000转)、耐化学性(根据ASTM D543Practice A,Procedure 1在各试剂中浸渍30天后长度或宽度的总质量损失不大于5%)、介电强度(根据ASTM D149(在20mil下)最低250V/mil)、吸水性(如通过ASTM D570测得2.0%的最大吸水)、拉开粘合力(根据ASTM D4541大于1500psi(10,342千帕斯卡))和硬度(根据ASTM D2240在肖氏D标度上65的最低Durometer硬度)阐述的AWWA C222标准的弹性体涂层。
下列实施例旨在例示本发明而非以任何方式被视为限制本发明的范围。
实施例
该体系的异氰酸酯反应性组分和异氰酸酯组分的一个实例显示在下表1中,所有值是基于100重量份该体系计的重量份(pbw)并以基于该体系的总重量%计的重量%表示。
表1:用于形成弹性体组合物的体系
1Pluracol P-736;2Polyetheramine D-2000;3PolyPolyether Diol1000;R-972,可获自Evonik Specialty Chemicals;5Quadrol;6Lupragen N201,可获自BASF Corporation;7Dabco T-12催化剂,可获自Air Products and Chemicals,Inc.;8Bright White 18361,可获自Repi,S.p.A;9Ethacure 100,可获自Albemarle;10Elastoflex R23000T,可购自BASF Corporation.
混合表1的组分并作为弹性体组合物以38.9ft2/gal(3.61平方米/3.79升,或0.95平方米/升)的理论覆盖率以35密尔厚度根据如下文概括的下列表面预处理、材料制备、施加设备和指南施加到各种基底上(包括可获自ACT in Hillsdale,Michigan的1/16英寸(0.16厘米)镀锌钢基底板;可获自Lake Shore Service,Inc.in Wyandotte,Michigan的1/4英寸(0.64厘米)碳钢板;schedule 40管段,测得为12英寸(30.48厘米)长和2英寸(5.08厘米)内径和2 3/8”(6.03厘米)外径,可获自KTA-Tator,Inc.,Pittsburgh,Pennsylvania;和可获自Grainger in Romulus,Michigan的3/8英寸(0.95厘米)厚的高密度聚乙烯片)。这些板在评估前在环境条件下风干7天。
表面预处理:
·在喷砂清洁前目视检查所有部件。
·将所有粗糙焊缝或尖锐突起磨光滑。
·使用溶剂洗涤除去油、油脂或其它有机污染物的任何沉积物。
·待涂布的所有表面根据SSPC-SP1完全干燥,无潮湿、粉尘、砂粒、油、油脂或任何其它污染物。
·基底温度比露点温度高至少5°F(3℃)。
·使用接近白色的喷砂,SSPC-SP10/NACE No.2和3-4mil profile。该喷砂介质干净,无尘,坚硬、尖锐和有角。
·在涂布前将清洁过的表面喷气,刷拭或真空处理以除去任何粉尘和碎片,并在生锈前涂布。在涂布前表现出锈迹的任何清洁过的钢再喷砂。
材料制备:
·在使用前,各树脂材料在其原始容器中借助批准的混合器搅拌不少于30分钟。
·防止打开的树脂和异氰酸酯的桶受到水分污染。
施加设备和指南:
·通过2:1体积的多组分高压计量机施加该弹性体涂料组合物。该机器保持喷枪处至少150°F(66℃)的组分温度,以及高达3000psi的操作压力。使用具有可变喷嘴梢(其能够优化喷雾型式)的撞击混合型无气喷枪施加该弹性体组合物。
·机器:GlasCraft MHR-VR
·喷枪:GlasCraft Probler 2
·混合室:01
·Fan Tip:36/40
·混合比–体积份:200树脂比100异氰酸酯
·组分温度:150°F(66℃)树脂/异氰酸酯
·组分压力:2,000psi(13790千帕斯卡)树脂/2,100psi(14479千帕斯卡)异氰酸酯
基本根据AWWA C222中详述的测试程序评估在适当的基底上制备的弹性体组合物的阴极剥离、拉开粘合力、挠性、耐冲击性、耐磨性、吸水性、硬度、耐化学性、介电强度和拉伸强度,下面进一步概括各试验并且这些试验的结果概括在下表2中。
阴极剥离
在如上提供的镀锌钢基底板上根据标题为“Standard Test Method forCathodic Disbondment Test of Pipeline Coatings(Attached Cell Method)”的ASTMG-95-07(13)的修改版本在环境试验条件(大约23℃)下进行涂布板的阴极剥离测试。修改包括外加电压和试验持续时间。使用DeFelsko6000非破坏性电子涂层测厚仪在样品上获得涂层厚度测量。
测试样品的程序包括在用于阴极结合测试的涂布钢板的中心穿过涂层钻出1/8英寸(.3173cm)直径的露白(holiday)至金属表面。用聚硅氧烷粘合剂(silicone adhesive)将直径4英寸(10.16厘米)的管段粘合到各板上以使露白位点在该管道的内径内。用电解质溶液(在去离子水中的3质量%氯化钠)填充管道内部(即孔隙)以使露白位点浸在电解质溶液中。使用铂线作为外加电流阳极,并在样品上施加-1.5V电位28天。
在28天后,通过以“X”形状穿过涂层到基底切割45°径向切口并用美工刀片手动剥开涂层以测定粘合损失程度,在之前浸渍的露白位点和在涂布板上的一个未浸渍的位点评估涂层粘附。从原始露白位点到暴露基底的最远点测量涂层剥离量。
一旦移除涂层,在与之前浸渍的露白位点对应的钢板表面上目视观察染污。视觉上显而易见在之前浸渍的露白位点周围明显一圈染污。测量这一圆圈并与归因于阴极剥离试验的阴极剥离量相关联。从原始露白位点到染污的更远径向点测量染污量。对许多样品重复该试验且平均径向染污概括在下表2中。
拉开粘合力
根据标题为“Pull-Off Strength of Coatings Using Portable AdhesionTesters,Test Method E,‘Self Aligning Adhesion Tester Type V”的评估拉开粘合力。
在根据上列表面预处理准备的4英寸x 8英寸x 0.25英寸(10.16厘米x 20.32厘米x 0.635厘米)钢板上进行拉开粘合力(Pull off adhesion)。使用DeFelsko6000非破坏性电子涂层测厚仪在各板上的五个点测定涂层厚度。用60grit砂纸打磨受试表面并擦干净。使用氰基丙烯酸酯或双组分环氧胶将20毫米直径dollies(其表面用80grit砂纸打磨)粘贴到打磨过的样品表面上,在拉开前使其在环境实验室条件下干燥24小时。在使用DeFelsko PosiTest AT-A Automatic Adhesion Tester拉开前围绕至金属表面的拉开根部(pull stub)对样品表面评分。
挠性
根据ASTM D522/D522M-13,“Standard Test Methods for Mandrel Bend Testof Attached Organic Coatings,”Method B进行挠性测试。试验板是冷轧钢1/32英寸x 4英寸x 12英寸(0.081厘米x 10.16厘米x 30.5厘米)-ACT CRS 04x12x026 B1000 P99XDIW;UNP并通过上述方法施加涂层。使用DeFelsko6000非破坏性电子涂层测厚仪在样品上获得涂层厚度测量。
在这一试验中,各样品在3英寸(7.62厘米)心轴上弯曲180°,然后用8X比较器透镜检查裂纹。对许多样品重复该试验且结果概括在下表2中。
耐冲击性
根据标题为“Standard Test Method for Impact Resistance of PipelineCoatings(Falling Weight Test)”的ASTM G14-04(10)e1测定涂布基底上的涂层的耐冲击性。在这一试验中,以如上所述的方式涂布5个测得为12英寸长(30.48厘米)的管段。使用DeFelsko6000非破坏性电子涂层测厚仪在各板上的五个点上测定涂层厚度。将管固定到该方法中概述的装置上,并如该方法中概述从24至48英寸(60.96至121.92厘米)的各种高度投落3.2磅(1.45千克)锤体(落锤)。观察各管段上的20个冲击位置并使用高度、重量和涂层失效频率数据计算冲击强度。结果概括在下表2中。
耐磨性
根据标题为“Standard Test Method for Abrasion Resistance of OrganicCoatings by the Taber Abraser”的ASTM D4060-14测定Taber耐磨性。将一式双份的1/32英寸x 4英寸x 4英寸涂布冷轧钢板(0.081厘米x10.16厘米x 10.16厘米)(ACT CRS04x12x026 B1000 P99X DIW;UNP板)称重,然后使用1000克负荷和Cs-17磨轮施以1000个周期。使用DeFelsko6000非破坏性电子涂层测厚仪在各板上的五个点上测定涂层厚度。在100周期试验后获取研磨后重量,并记录以毫克计的重量损失。对许多样品重复该试验且结果概括在下表2中。
吸水性
根据标题为“Standard Test Method for Water Absorption of Plastics”withProcedure 7.4,“Long Term Immersion”的ASTM D570-98(10)e1测量自由膜样品的吸水性。在这一试验中,根据上述表面预处理、材料制备、施加设备和施加指南(将钢基底换成HDPE板)将涂层施加到高密度聚乙烯(HDPE)片(至少3/8英寸(至少0.95厘米)厚)上。从HDPE片上取下的自由膜上切割3个测得为3英寸x 1英寸(7.72厘米x 2.54厘米)的条并使用Mitutoyo Digimatic Calipers测量各条的厚度。样品在保持在50℃的炉中调节24小时。在调节后,样品在干燥器中冷却并立即称重。然后将样品浸在保持在大约70°F(大约21℃)、50%相对湿度的实验室条件下的去离子水中。在24小时、一周和两周后从水中取出样品并再称重。然后根据公式计算重量增加百分比:[重量增加%=(湿重量-调节后重量)/调节后重量]x100%]。
肖氏D硬度
根据ASTM D2240-05(10),“Standard Test Method for Rubber Property-Durometer Hardness”评估涂层的硬度。使用肖氏D硬度计(使用校准硬度块检验),由从3/8英寸(0.95厘米)厚的高密度聚乙烯片上取下的自由膜样品(根据如上述吸水性试验中描述的方法制备)获得五个读数。平均结果概括在下表2中。
耐化学性
根据AWWA C222-08,“Polyurethane Coatings for the Interior and Exteriorof Steel Water and Pipe Fittings,”(其参考ASTM D543-14,“Standard Practices forEvaluating the Resistance of Plastics to Chemical Reagents”)评估耐化学性。用于此试验的化学溶液包括10%氯化钠、30%氯化钠、30%氢氧化钠、No.2柴油燃料和去离子水。在环境温度(大约23℃)下浸渍30天后计算三个重复涂布板的质量和尺寸的平均变化。使用Mitutoyo Digimatic Calipers在各样品的五个点上获得涂层尺寸测量。对许多样品重复该试验且结果概括在下表2中。
介电强度
根据ASTM D199-09(13),“Standard Test Method for Dielectric BreakdownVoltage and Dielectric Strength of Solid Electrical Insulating Materials atCommercial Power Frequencies”,Method A进行介电强度测试。在许多样品板上的测试平均结果概括在下表2中。
拉伸强度
根据标题为“Standard Test Method for Tensile Properties of Plastics”的ASTM D638type IV评估涂层的拉伸强度。在这一试验中,样品获自从3/8英寸(0.95厘米)厚的高密度聚乙烯片上取下的自由膜样品(根据如上述吸水性章节中描述的方法制备涂布片材)。用液压冲切机冲出ASTM D638Type IV试样,并用机械厚度计测量厚度。样品在23℃和50%RH(相对湿度)的标准环境条件下预调节最少24小时。所有测试在MTS通用测试机上使用Testworks 4软件在相同的标准环境条件下进行。
结果
根据上述方法进行的阴极剥离、拉开粘合力、挠性、耐冲击性、耐磨性、吸水性、硬度、耐化学性、介电强度和拉伸强度的测试结果提供在下表2中。
表2:弹性体涂料组合物的评估(AWWA C222 Standard)
要理解的是,所附权利要求书不限于表示详述中描述的任何特定化合物、表面处理材料或方法,它们在落在所附权利要求书范围内的特定实施方案之间可变。关于本文中赖以描述各种实施方案的特定特征或方面的任何马库什群组,可以由各马库什群组的各成员独立于所有其它马库什成员获得不同、特殊和/或出乎意料的结果。可以独立和/或组合依赖马库什群组的各成员并为所附权利要求书范围内的具体实施方案提供足够的支持。
此外,赖以描述本发明的各种实施方案的任何范围和子范围独立地并共同地落在所附权利要求书的范围内,并被理解为描述和考虑了包括其内的整数和/或分数值的所有范围,即使在本文中没有明确写出这些值。本领域技术人员容易认识到,所列举的范围和子范围足以描述和实现本发明的各种实施方案,且这样的范围和子范围可进一步描绘成相关的1/2、1/3、1/4、1/5诸如此类。仅举一例,“0.1至0.9”的范围可进一步描绘成下1/3,即0.1至0.3,中间1/3,即0.4至0.6,和上1/3,即0.7至0.9,它们独立地并共同地在所附权利要求书的范围内并可独立地和/或共同地赖以为所附权利要求书范围内的具体实施方案提供足够的支持。此外,对于界定或修饰范围的词语,如“至少”、“大于”、“小于”、“不大于”等,要理解的是,这样的词语包括子范围和/或上限或下限。作为另一实例,“至少10”的范围固有地包括至少10至35的子范围、至少10至25的子范围、25至35的子范围,诸如此类,并且可以独立地和/或共同地依赖各子范围并为所附权利要求书范围内的具体实施方案提供足够的支持。最后,可以依赖所公开的范围内的独立数值并为所附权利要求书范围内的具体实施方案提供足够的支持。例如,“1至9”的范围包括各种独立整数,如3,以及含小数点的独立数值(或分数),如4.1,可以依赖它们为所附权利要求书范围内的具体实施方案提供足够的支持。
已经以示例性方式描述了本发明,并且要理解的是,所用术语意为描述性而非限制性的。明显地,可以根据上述教导作出本发明的许多修改和变动。可以与具体描述不同地实施本发明。
Claims (23)
1.一种用于形成施加到基底上的弹性体组合物的体系,所述体系包含:
异氰酸酯组分,其包含聚合多异氰酸酯;和
异氰酸酯反应性组分,其包含多元醇组分和聚醚胺,所述多元醇组分包含下列成分的混合物:
(a)疏水多元醇;
(b)不同于所述疏水多元醇的聚醚多元醇,所述聚醚多元醇具有大于500g/mol的重均分子量;和
(c)聚氨基多元醇。
2.根据权利要求1的体系,其中所述聚合多异氰酸酯包含聚合二苯甲烷二异氰酸酯。
3.根据前述权利要求任一项的体系,其中所述异氰酸酯组分进一步包含基于100重量份的所述异氰酸酯组分计以大约25至大约75份的量存在于所述异氰酸酯组分中的异氰酸酯封端预聚物。
4.根据前述权利要求任一项的体系,其中所述异氰酸酯组分构成所述体系的总重量的35.5至40重量%。
5.根据前述权利要求任一项的体系,其中所述疏水多元醇包含天然油多元醇。
6.根据权利要求5的体系,其中所述天然油多元醇包含蓖麻油。
7.根据前述权利要求任一项的体系,其中所述聚醚多元醇具有500至650g/mol的重均分子量。
8.根据权利要求7的体系,其中所述聚醚多元醇衍生自环氧丙烷在不存在环氧乙烷的情况下的催化加成反应。
9.根据权利要求7或权利要求8的体系,其中所述聚醚多元醇具有3.5至4.0的平均官能度。
10.根据权利要求7至9任一项的体系,其中所述聚醚多元醇构成所述体系的总重量的1.8至5重量%。
11.根据前述权利要求任一项的体系,其中所述异氰酸酯反应性组分进一步包含通过四氢呋喃的聚合获得的聚四亚甲基醚二醇。
12.根据前述权利要求任一项的体系,其中所述异氰酸酯反应性组分进一步包含通过四氢呋喃的聚合获得并具有650至2000g/mol的重均分子量的聚四亚甲基醚二醇。
13.根据权利要求11或权利要求12的体系,其中所述聚四亚甲基醚二醇构成所述体系的总重量的4至10重量%。
14.根据前述权利要求任一项的体系,其中所述聚氨基多元醇包含基于乙二胺和环氧丙烷的聚醚多元醇四醇。
15.根据前述权利要求任一项的体系,其中所述聚氨基多元醇构成所述体系的总重量的4至10重量%。
16.根据前述权利要求任一项的体系,其中所述聚醚胺构成所述体系的总重量的4至10重量%。
17.根据前述权利要求之一的体系,其包含,基于100重量份的所述体系计:
35.5至40重量份的所述异氰酸酯组分;
25至37重量份的蓖麻油作为所述天然油多元醇;
1.8至5重量份的衍生自环氧丙烷的催化加成反应的聚醚多元醇,所述聚醚多元醇具有500至650的重均分子量和3.5至4.0的平均官能度;和
4至10重量份的通过四氢呋喃的聚合获得并具有650至2000g/mol的重均分子量的聚四亚甲基醚二醇;
4至10重量份的所述聚氨基多元醇;和
4至10重量份的所述聚醚胺。
18.根据前述权利要求任一项的体系,其中所述异氰酸酯组分中的NCO基团与所述异氰酸酯反应性组分中的活性氢的摩尔比为1:1至1.10:1。
19.通过使根据前述权利要求任一项的所述体系的所述异氰酸酯组分与所述异氰酸酯反应性组分反应而得的弹性体组合物。
20.一种制品,其包含基底和附着在其上的弹性体涂层,所述弹性体涂层包含根据权利要求19的弹性体组合物。
21.根据权利要求20的制品,其中所述基底包含具有外表面和内表面的金属管道,并且其中将所述弹性体涂料组合物施加到所述外表面和所述内表面的至少一个上以形成附着在其上的弹性体涂层,并且其中具有所述施加的弹性体涂层的所述钢管满足如AWWA C222中阐述的用于供水工业的标准。
22.一种涂布基底的方法,其包括将根据权利要求19的所述弹性体组合物的层施加到基底表面上以形成弹性体涂层。
23.一种形成弹性体组合物的方法,其包括:
将根据权利要求1至18任一项的所述体系的所述异氰酸酯组分与所述异氰酸酯反应性组分混合在一起;和
使所述异氰酸酯组分与所述异氰酸酯反应性组分反应以形成所述弹性体组合物。
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CN113677763A (zh) * | 2019-04-30 | 2021-11-19 | 巴斯夫欧洲公司 | 管道配重涂料 |
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EP3259296A1 (en) | 2017-12-27 |
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