CN113817354A - 包含含有聚氨酯的水分散体的层压印刷油墨 - Google Patents
包含含有聚氨酯的水分散体的层压印刷油墨 Download PDFInfo
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- CN113817354A CN113817354A CN202111141415.7A CN202111141415A CN113817354A CN 113817354 A CN113817354 A CN 113817354A CN 202111141415 A CN202111141415 A CN 202111141415A CN 113817354 A CN113817354 A CN 113817354A
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Abstract
本发明涉及一种包含聚氨酯水分散体粘结剂、颜料、水性载体和任选地添加剂的层压印刷油墨,其中聚氨酯由多异氰酸酯、特定的聚酯二醇、聚四氢呋喃二醇、单羟基聚氧化烯、二氨基酸化合物、多胺化合物和任选地一种或多种低分子量多元醇制备。
Description
本申请是申请号为201580004694.9、申请日为2015年1月14日、发明名称为“包含含有聚氨酯的水分散体的层压印刷油墨”的专利申请的分案申请。
本发明涉及一种包含聚氨酯水分散体粘结剂、颜料、水性载体和任选地添加剂的层压印刷油墨,其中聚氨酯由多异氰酸酯、特定的聚酯二醇、聚四氢呋喃二醇、单羟基聚氧化烯、二氨基酸化合物、多胺化合物和任选地一种或多种低分子量多元醇制备。本发明还涉及用所述油墨印刷的层压品以及制备所述层压品的方法。
包装如用于食品的包装通常包含由两个或更多个层压在一起且其中印刷油墨保留在两个层压膜之间的聚合物膜制备的印刷膜层压品。通常,当制备意欲用于包装食品产品的包装时,将膜印刷在一侧,将粘合剂施加于印刷品顶部以及围绕印刷品的透明区域上,且然后以层压针(laminated pin)将该膜层压到第二个膜。在联机印刷中,将粘合剂涂覆在新印刷的油墨或相对纸幅的顶部上,且其后立即层压。在很多情况下,层压是“脱机”完成的,这是指使印刷辊至另一层压位置。粘合剂必须结合到油墨和膜而不引起油墨渗出、流出、分层或产生不良结合强度。
适合用于经由辊印刷方法制造印刷层压品的印刷油墨(下文中称为“层压油墨”)面临各种希望的需求:
-在液体油墨中与颜料的高相容性
-印刷膜的粘接行为尽可能低
-膜层压品的高层压结合强度,以及还在多次印刷情况下
-已在印刷辊上临时干燥的油墨的高再溶解性
-无挥发性碱。
尤其应避免油墨成分的凝聚或絮凝。在其中“脱机”完成层压的情况下,重要的是印刷膜在层压之前抗粘接,即膜的印刷表面不是粘性的且不粘附到其他印刷或未印刷的膜表面区域。
高层压结合强度尤其关键且难以多次印刷层压品中实现,在多次印刷层压品中使第二印刷品或其他印刷品施加于第一印刷品上,例如将白色印刷品施加于之前彩色、非白色的印刷品上。
有意或无意中断可发生在辊印刷工艺过程期间。印刷辊滚筒上的油墨可在这些中断期间变为接触干燥。因此,重要的是当印刷工艺过程重新开始时,印刷设备上的干燥油墨在液体印刷油墨备料中快速再溶解。
由于卫生原因,希望提供不含氨且不含挥发性有机叔胺的印刷油墨。
WO 2009/023520公开了在各种基材上具有良好层压结合强度的包含含水聚氨酯粘结剂的层压油墨。
本发明的目的是对于一个或多个上述需求,特别是涉及改进的耐粘性和改进的再溶解行为,进一步优化层压印刷油墨而不过度损害一个或多个其他希望的需求。
本发明提供包含至少一种粘结剂、至少一种颜料、水性载体和任选地添加剂的层压印刷油墨,其中至少一种粘结剂为包含聚氨酯的水分散体,其中聚氨酯由包含以下化合物的组分制备:
a)至少一种具有至少两个异氰酸酯基团的多异氰酸酯,
b)二醇的组合,其中
b1)至少一种二醇为具有500-5000g/mol,优选约1000-3000g/mol的数均分子量的聚酯二醇,且
b2)至少一种二醇为具有500-5000g/mol,优选约1000-3000g/mol的数均分子量的聚四氢呋喃,
c)至少一种具有500-5000g/mol,优选约1000-3000g/mol的数均分子量的单羟基聚氧化烯化合物,
d)至少一种二氨基酸化合物,
e)至少一种具有至少两个氨基且不含酸基的多胺化合物,和
f)任选地一种或多种具有小于500g/mol,优选60-490g/mol的数均分子量的多元醇化合物。
优选聚氨酯由包含以下化合物的组分制备:
a)5-30重量%至少一种具有至少两个异氰酸酯基团的多异氰酸酯,
b)10-80重量%二醇的组合,其中聚酯二醇(b1)和聚四氢呋喃二醇(b2)优选重量比为1∶2-2∶1,
c)1-20重量%至少一种具有500-5000g/mol的数均分子量的单羟基聚氧化烯化合物,
d)1-10重量%至少一种二氨基酸化合物,
e)0,1-10重量%至少一种具有至少两个氨基且不含酸基的多胺化合物,和
f)0-10重量%任选地一种或多种具有小于500g/mol,优选60-490g/mol的数均分子量的多元醇化合物。
多异氰酸酯(a)优选以5-30重量%,更优选10-25重量%的量使用。多异氰酸酯(a)尤其为二异氰酸酯X(NCO)2,其中X为具有4-12个碳的脂族烃基、具有6-15个碳的环脂族烃基或者具有6-15个碳的芳族烃基或者具有7-15个碳的芳脂族烃基。该类二异氰酸酯的实例为四亚甲基二异氰酸酯、六亚甲基二异氰酸酯(HDI)、十二亚甲基二异氰酸酯、1,4-二异氰酸酯基环己烷、1-异氰酸酯基-3,5,5-三甲基-5-异氰酸酯基甲基环己烷(IPDI)、2,2-双(4-异氰酸酯基环己基)丙烷、三甲基己烷二异氰酸酯、1,4-二异氰酸酯基苯、2,4-二异氰酸酯基甲苯、2,6-二异氰酸酯基甲苯、4,4′-二异氰酸酯基二苯基甲烷、2,4′-二异氰酸酯基二苯基甲烷、对苯二异氰酸酯、四甲代苯二异氰酸酯(TMXDI)、双(4-异氰酸酯基环己基)甲烷的异构体(HMDI,如反式/反式、顺式/顺式和顺式/反式异构体),以及这些化合物的混合物。这些异氰酸酯的特别重要的混合物为二异氰酸酯基甲苯和二异氰酸酯基二苯基甲烷的相应结构异构体的混合物,尤其是包含80摩尔%2,4-二异氰酸酯基甲苯和20摩尔%2,6-二异氰酸酯基甲苯的混合物。此外,芳族异氰酸酯如2,4-二异氰酸酯基甲苯和/或2,6-二异氰酸酯基甲苯与脂族或者环脂族异氰酸酯如六亚甲基二异氰酸酯或IPDI的混合物是特别有利的,其中脂族与芳族异氰酸酯的优选比例为4∶1-1∶4。除了上述异氰酸酯之外,其他可用作合成聚氨酯的化合物的异氰酸酯为不仅具有游离的异氰酸酯基团,还进一步具有异氰酸酯端基的那些,其中实例为二氮杂环丁二酮(uretdione)基团。尤其优选选自1-异氰酸酯基-3,5,5-三甲基-5-异氰酸酯基甲基环己烷(IPDI)、四甲代苯二异氰酸酯(TMXDI)、六亚甲基二异氰酸酯(HDI)、双(4-异氰酸酯基环己基)-甲烷(HMDI)或其混合物的多异氰酸酯(a)。
二醇(b)的组合优选以10-80重量%,更优选20-70重量%的量使用。聚酯二醇(b1)和聚四氢呋喃二醇(b2)的重量比优选为1∶3-3∶1,更优选1∶2-2∶1。聚酯二醇(b1)尤其为例如由Ullmann’sder technischen Chemie,第4版,第19卷,第62-65页已知的聚酯多元醇。优选使用由二羟醇与二元羧酸反应得到的聚酯多元醇。代替游离的多羧酸,还可使用相应的多酸酐或者相应的低级醇的多羧酸酯或其混合物以制备聚酯多元醇。多羧酸可为脂族、环脂族、芳脂族、芳族或杂环的,并且可为未取代的或(例如由卤原子)取代的和/或饱和的或不饱和的。实例为辛二酸、壬二酸、邻苯二甲酸和间苯二甲酸,邻苯二甲酸酐、四氢邻苯二甲酸酐、六氢邻苯二甲酸酐、四氯邻苯二甲酸酐、内亚甲基四氢邻苯二甲酸酐、戊二酸酐和马来酸酐,马来酸、富马酸和二聚脂肪酸。优选为式HOOC-(CH2)y-COOH的二羧酸,其中y为1-20的数,优选2-20的偶数,其中实例为琥珀酸、己二酸、癸二酸和十二烷基二甲酸。
用于制备聚酯二醇(b1)的合适多元醇的实例为乙二醇、1,2-丙二醇、1,3-丙二醇、1,3-丁二醇、1,4-丁二醇、1,4-丁烯二醇、1,4-丁炔二醇、1,5-戊二醇、新戊二醇、双(羟甲基)环己烷如1,4-双(羟甲基)环己烷、2-甲基-1,3-丙二醇、甲基戊二醇,以及二甘醇、三甘醇、四甘醇、聚乙二醇、二丙二醇、聚丙二醇、二丁二醇和聚丁二醇。优选为式HO-(CH2)x-OH的醇,其中x为1-20的数,优选2-20的偶数。该类醇的实例为乙二醇、1,4-丁二醇、1,6-己二醇、1,8-辛二醇和1,12-十二烷二醇。优选扩至新戊二醇。
还合适的是聚碳酸酯二醇,如可例如由光气与过量的上文作为用于聚酯多元醇的结构组分所述的低分子质量醇反应得到。内酯基聚酯二醇也是合适的,其为内酯的均聚物或共聚物,优选羟基封端的内酯与合适的双官能起始剂分子的加合物。合适的内酯优选为衍生自式HO-(CH2)z-COOH的化合物的那些,其中z为1-20且亚甲基单元的一个氢可由C1-C4烷基替换。实例为ε-己内酯、β-丙内酯、γ-丁内酯和/或甲基-ε-己内酯,及其混合物。合适的起始剂组分的实例为低分子质量的上文作为用于聚酯多元醇的结构组分所述的二羟醇。特别优选ε-己内酯的相应聚合物。低级聚酯二醇或聚醚二醇还可作为起始剂用于制备内酯聚合物。代替内酯的聚合物,还可使用对应于内酯的羟基羧酸的相应的、化学等价的缩聚物。
聚四氢呋喃二醇(b2)尤其可在例如BF3的存在下由四氢呋喃自身的加成聚合,或者由在包含反应性氢的起始剂组分如醇或胺(实例为水、乙二醇、1,2-丙二醇、1,3-丙二醇、1,2-双(4-羟基二苯基)丙烷或苯胺)上的加成反应得到。特别优选具有500-5000g/mol,特别是500-4500g/mol或者1000-3000g/mol的数均分子量的聚四氢呋喃。
至少一种单羟基聚氧化烯化合物(c)优选以1-20重量%,更优选以2-10重量%的量使用。合适的化合物(c)为烷醇起始的聚亚烷基二醇。这些化合物在聚合物的一个端基上具有烷基,且在另一端基上具有羟基。该烷醇优选具有2-8个或者2-5个碳原子,如乙醇、丙醇或丁醇,优选正丁醇。亚烷基例如为亚乙基、亚丙基或其混合物,优选亚乙基。通式可为HO-(A-O)n-R,其中A为上述亚烷基,R为上述烷基,且n为20-65的数。单羟基聚氧化烯化合物(c)的OH数优选为20-56mg KOH/g。
至少一种二氨基酸化合物(d)优选以1-10重量%,更优选以1-5重量%的量使用。合适的二氨基酸化合物可选自二氨基羧酸化合物和二氨基磺酸化合物。该类化合物例如符合式H2N-R1-NH-R2-X,其中R1和R2彼此独立为C1-C6链烷二基,优选亚乙基,且X为COOH或SO3H。特别优选的化合物(d)为N-(2-氨基乙基)-2-氨基乙烷羧酸和N-(2-氨基乙基)-2-氨基乙烷磺酸以及相应的碱金属盐,其中Na为特别优选的抗衡离子。
至少一种具有至少两个氨基且不含酸基的多胺化合物(e)优选以0,1-10重量%,更优选以0,1-2重量%的量使用。多胺化合物(e)通常可用于交联或者扩链,并且通常具有2个或更多个伯氨基和/或仲氨基。特别是当扩链和/或交联在水存在下进行时,使用具有2个或更多个伯氨基和/或仲氨基的多胺,因为胺通常与异氰酸酯反应比醇或者水更快。当希望用于经交联的聚氨酯或者高摩尔重量的聚氨酯的水分散体时,这在很多情况下是必需的。在该类情况下,随后进行如下程序,其中制备具有异氰酸酯基团的预聚物,将其快速分散在水中且然后通过加入具有两个或更多个异氰酸酯反应性氨基的化合物而经受扩链或者交联。适合于该目的的胺通常为具有32-500g/mol,优选60-300g/mol的摩尔重量的多官能胺,其具有至少两个选自伯氨基和仲氨基的氨基。实例为二胺如二氨基乙烷、二氨基丙烷、二氨基丁烷、二氨基己烷、哌嗪、2,5-二甲基哌嗪、氨基-3-氨基甲基-3,5,5-三甲基环己烷(异佛尔酮二胺,IPDA)、4,4-′-二氨基二环己基甲烷、1,4-二氨基环己烷、氨基乙基乙醇胺、肼、水合肼或者三胺如二亚乙基三胺或1,8-二氨基-4-氨基甲基辛烷。优选使用二胺和三胺的混合物,尤其是异佛尔酮二胺(IPDA)和二亚乙基三胺(DETA)的混合物。聚氨酯基于聚氨酯组分的总量,优选包含1-30摩尔%,尤其是4-25摩尔%的具有至少2个异氰酸酯反应性氨基作为单体(d)的多胺。优选多胺化合物选自异佛尔酮二胺、二亚乙基三胺及其混合物。
胺还可以封闭的形式使用,例如呈相应的酮亚胺、酮连氮或者胺盐形式。唑烷在使用时,例如在US专利号4,192,937中,还为封端的多胺,其可在制备聚氨酯中用于使预聚物扩链。当使用这种封端多胺时,它们通常在无水存在下与预聚物混合并且该类混合物随后与分散体的水或者与其一部分混合,以使相应的多胺通过水解而释放。
聚氨酯的硬度和弹性模量可通过使用具有小于500g/mol,例如约60-490g/mol,优选62-200g/mol的分子量的低分子质量的多元醇(f)(优选二醇)而提高。低分子量多元醇(f)的量优选为0-10重量%,更优选1-8重量%。作为多元醇(f)使用的化合物尤其为对制备聚酯二醇所述的短链链烷二醇的结构组分,其中优选具有2-12个碳的二醇、具有2-12个碳和偶数个碳的未支化二醇以及1,5-戊二醇、1,4-丁二醇和新戊二醇。
在本发明的一个方面中,聚氨酯仅由组分(a)-(e)或者仅由如上所述的组分(a)-(f)制备。
任选地聚氨酯可由一种或多种不同于组分(a)-(f)的具有至少一个异氰酸酯基团或具有至少一个异氰酸酯反应性基团的化合物制备。实例为可用于形成一定程度的支化或交联的具有超过2的官能度的醇,如三羟甲基丙烷、甘油和糖类。还合适的是除羟基之外还具有其他异氰酸酯反应性基团的一元醇,如具有一个或多个伯氨基和/或仲氨基的单醇;例如单乙醇胺。为了支化或者交联目的,还可使用具有超过2的官能度的异氰酸酯。市购化合物的实例为六亚甲基二异氰酸酯的异氰脲酸酯或缩二脲。
特别是当所用的单体(a)基本仅包含脂族二异氰酸酯和/或环脂族二异氰酸酯时;以及当所用的单体(b1)基本仅包含由上述脂族二醇和二酸合成的聚酯二醇时;以及当组分(d)包含N-(2-氨基乙基)-2-氨基乙烷磺酸和/或N-(2-氨基乙基)-2-氨基乙烷羧酸的碱金属盐时;以及当组分(d)为DETA/IPDA的混合物时,得到具有特别好的性能特性的聚氨酯粘结剂。
在聚氨酯化学领域中,通常已知如何可通过选择共反应性单体的比例以及通过每分子反应性官能基团数的算术平均值调整聚氨酯的分子量。通常选择组分及其相应的摩尔量以使得比例A∶B为0.5∶1-2∶1,优选0.8∶1-1.5∶1,特别优选0.9∶1-1.2∶1,其中A为异氰酸酯基团的摩尔量且B为羟基的摩尔量和其他能够在加成反应中与异氰酸酯反应的官能基团的摩尔量的总和。非常特别优选比例A∶B尽可能接近1∶1。
所用的组分(a)-(f)通常平均具有1.5-2.5,优选1.9-2.1,特别优选2.0个异氰酸酯基团和/或能够在加成反应中与异氰酸酯反应的官能基团。
优选聚氨酯由包含以下化合物的组分制备:
a)5-30重量%至少一种具有至少两个异氰酸酯基团的多异氰酸酯,
b)10-80重量%二醇的组合,其中
b1)至少一种二醇为具有500-5000的分子量的聚酯二醇,以及
b2)至少一种二醇为具有500-5000g/mol的数均分子量的聚四氢呋喃,
其中聚酯二醇(b1)和聚四氢呋喃二醇(b2)优选重量比为1∶2-2∶1,
c)1-20重量%至少一种具有500-5000g/mol的数均分子量的单羟基聚氧化烯化合物,
d)1-10重量%至少一种二氨基酸化合物,
e)0,1-10重量%至少一种具有至少两个氨基且不含酸基的多胺化合物,和
f)0-10重量%任选地一种或多种具有小于500g/mol,优选60-490g/mol的数均分子量的多元醇化合物。
用于生产聚氨酯的结构组分的加成聚合优选在至多180℃,优选至多150℃,优选70-150℃的反应温度下在大气压力下或在自生压力下进行。聚氨酯和聚氨酯水分散体的生产对于本领域技术人员而言为已知的。聚氨酯优选呈水分散体形式并且以该形式使用。优选将聚合物分散体的pH调整到5以上,特别是在5.5-9.5之间。
PU分散体通常由一种以下方法制备。在丙酮方法中,离子性聚氨酯在大气压下在100℃以下沸腾的水可混溶的溶剂中由所述组分制备。加入水直到形成分散体,其中水为连续相。预聚物混合方法与丙酮方法的不同之处在于首先制备的具有异氰酸酯基团的预聚物并非完全反应(可能)的离子性聚氨酯。在这种情况下,选择组分以使得上述定义的比例A∶B为1.0-3,优选1.05-1.5。首先将预聚物在水中分散且然后可通过异氰酸酯基团与具有超过2个异氰酸酯反应性氨基的胺反应而交联,或者利用具有2个异氰酸酯反应性氨基的胺使其扩链。当不加入胺时还可进行扩链。在这种情况下,使异氰酸酯基团水解成氨基,其与预聚物剩余的异氰酸酯基团反应,且因此扩链。如果在制备聚氨酯中已使用溶剂,则通常例如通过减压蒸馏由分散体除去大部分溶剂。分散体优选具有少于10重量%溶剂含量,且特别优选不含溶剂。分散体通常具有10-75重量%,优选20-65重量%固体含量和10-500mPas的粘度(在20℃下和250s-1的剪切速率下测量)。
在本发明的一个方面中,层压印刷油墨不含氨和挥发性有机叔胺。术语挥发性意指沸点在100℃以下的化合物。
层压油墨优选包含8-60重量%,优选15-50重量%粘结剂,3-30重量%,优选6-30重量%颜料,15-60重量%,优选30-60重量%水和0,1-5重量%添加剂如表面活性剂、除沫剂和蜡。
粘结剂可仅为本发明聚氨酯粘结剂。还可使用本发明聚氨酯粘结剂与其他聚氨酯或非聚氨酯粘结剂树脂如丙烯酸系树脂的组合。当使用其他粘结剂树脂时,它们优选不超过粘结剂总量的约50%。油墨优选不含有氨;挥发性叔胺、残留的异氰酸酯和锡。
本发明的层压印刷油墨可通过简单地最小调整配制剂浓度而在柔性版或凹版印刷中使用。因此,可调整组分浓度以用于柔性版或凹版印刷中。例如,凹版油墨或者柔性版油墨优选包含约8-60重量%粘结剂,约3-30重量%颜料着色剂和约15-60重量%溶剂或水。如在a#2流杯中测量,油墨优选具有约15-30秒的粘度。流杯测量是用于测量油墨粘度的常用方法并且包括对校准量的油墨流动通过校准孔记时。较低粘度的油墨通常用于凹版印刷中,且较高粘度的油墨通常用于柔性版印刷中。因此,当油墨如在a#2流杯中测量的具有约28秒的粘度时,其适合用于柔性版印刷,并且当油墨如在a#2流杯中测量的具有约18秒的粘度时,其适合用于凹版印刷。
聚氨酯可为在除去溶剂或水时形成的膜,或者可为可辐射固化的。除非配制成可电子束固化的,可辐射固化的组合物通常包含光引发剂。油墨除粘结剂和溶剂之外还包含着色剂。着色剂为一种或多种颜料,或者可能的话,颜料和一种或多种染料的组合。着色剂可为有机或无机的。最常用的颜料包含偶氮染料(例如溶剂黄14、分散黄23和间胺黄)、蒽醌染料(例如溶剂红1 11、分散紫1、溶剂蓝56和溶剂橙3)、呫吨染料(溶剂绿4、酸性红52、碱性红1和溶剂橙63)、吖嗪染料(例如烟黑)等。主要的可用有机颜料包括联苯胺黄AAOT(例如颜料黄14CI#21095)、联苯胺黄AAOA(例如颜料黄12CI#21090)、酞菁蓝(例如颜料蓝15)、立索红(例如颜料红52∶1CI#15860∶1)、甲苯胺红(例如颜料红22CI#12315)、二嗪紫(例如颜料紫23CI#51319)、酞菁绿(例如颜料绿7CI#74260)、酞菁蓝(例如颜料蓝15CI#74160)、萘甲酸红(例如颜料红48∶2CI#15865∶2)。无机颜料包括二氧化钛(例如颜料白6CI#77891)、碳黑(例如颜料黑7CI#77266)、铁氧化物(例如红、黄和棕)、氧化铁黑(例如颜料黑11CI#77499)、氧化铬(例如绿)、亚铁氰化铁铵(例如蓝)等。着色剂不限制于前述。因此,着色剂可为任何常见有机或无机颜料如硫化锌、颜料白6、颜料黄1、颜料黄3、颜料黄12、颜料黄13、颜料黄14、颜料黄17、颜料黄63、颜料黄65、颜料黄73、颜料黄74、颜料黄75、颜料黄83、颜料黄97、颜料黄98、颜料黄106、颜料黄114、颜料黄121、颜料黄126、颜料黄127、颜料黄136、颜料黄174、颜料黄176、颜料黄188、颜料橙5、颜料橙13、颜料橙16、颜料橙34、颜料红2、颜料红9、颜料红14、颜料红17、颜料红22、颜料红23、颜料红37、颜料红38、颜料红41、颜料红42、颜料红57、颜料红112、颜料红122、颜料红170、颜料红210、颜料红238、颜料蓝15、颜料蓝15∶1、颜料蓝15∶2、颜料蓝15∶3、颜料蓝15∶4、颜料绿7、颜料绿36、颜料紫19、颜料紫23、颜料黑7等。
层压印刷油墨还可包含常见油墨添加剂以调整印刷油墨的流动、表面张力和光泽度。该类添加剂通常为聚合物分散剂、表面活性剂、蜡或其组合。这些添加剂可起流平剂、润湿剂、填料、分散剂、消泡剂或脱气剂的作用,或者可加入额外的助剂以提供特定功能。当着色剂为颜料时,层压印刷油墨可包含聚合物分散剂,以在混合和研磨操作期间使颜料分散在溶剂中。油墨的所有组分可一起共混并研磨以使颜料颗粒降低到希望的尺寸分布,通常10微米或更少,或者作为选择,可使颜料和聚合物分散剂在溶剂中预混并研磨以形成“基体”,其随后与油墨组合物的其余组分共混。油墨组分可在高速混合器中混合,直至达到淤浆稠度,且然后通过介质研磨机直至颜料降低到10微米或更小。本发明油墨广泛的多功能性容许其不用聚合物分散剂制备,但优选利用聚合物分散剂制备它们,以用于在例如聚乙烯醇缩丁醛中研磨或者与例如硝化纤维基体共混。因此本发明油墨可包含0重量份至约12重量份的聚合物分散剂。其他有用的着色剂、溶剂和助剂可通过查阅The Printing InkManual而确定。
本发明进一步涉及通过将本发明油墨用于在层压品的至少一部分表面上印刷而得到或可得到的印刷层压品。该印刷层压品优选由至少两个聚合物膜通过利用层压粘合剂层压膜而制备,其中油墨保留在层压膜之间。至少一个在其表面上留有油墨的聚合物膜优选包含选自聚丙烯、聚对苯二甲酸乙二醇酯、聚酰胺和低密度聚乙烯的材料。
本发明进一步涉及制备印刷层压品的方法,该方法包括:
将至少一种本发明层压油墨通过辊印刷方法(如凹版印刷或柔性版印刷)施加到第一个聚合物膜的至少一部分表面,并且通过使用粘合剂将印刷或未印刷的第二个聚合物膜层压到第一个聚合物膜的含有油墨的表面。第一个和/或第二个聚合物膜的材料优选选自聚丙烯、聚对苯二甲酸乙二醇酯、聚酰胺和低密度聚乙烯。
此外,本发明还涉及本发明聚氨酯分散体在用于将经印刷的(第一个)基材层压到(第二个)柔性膜的水基油墨中的用途。这些层压品在热封之前和之后具有优选>1.5N/15mm,最优选>2N/15mm的高层压结合强度。
通过本领域技术人员熟知的程序进行层压。通常层压品例如通过将本发明油墨置于塑料基材表面而得到。干燥后,得到经涂覆的基材。随后,使用层压粘合剂以使第二塑料表面固定到经涂覆的基材。塑料基材优选为聚合物膜,尤其是透明的聚合物膜或者其中至少一个聚合物膜为透明的。
本发明不同彩色的油墨尤其适用于多次印刷,即:将第一彩色印刷油墨层覆盖有至少一个其他的白色或非白色油墨层。
本发明油墨的优点是粘结剂与颜料的高相容性;层压前印刷膜的良好的粘接行为;膜层压品的高层压结合强度,以及还有在多次印刷的情况下;已在印刷辊上临时干燥的油墨的高再溶解性;无需挥发性碱。
本发明现在通过以下非限制性实施例说明。
实施例
颜料相容性的测试方法:
在使30重量%树脂基颜料浓缩物与70%本发明聚氨酯分散体共混后,制得层压彩色油墨。
树脂基颜料浓缩物的典型配制剂:
40%有机颜料(例如PY13、PR57.1、PB15.3、PB7)/10%树脂/1%表面活性剂/0.5%除沫剂/48.5%水。
在制备油墨后直接、1天后和7天后测量油墨粘度。记录粘度稳定性。将油墨稀释到印刷粘度(25秒DIN4杯)并在OPP(取向聚丙烯)膜上印刷。评判视觉外观(颜色强度、光泽度、透明度)。
在使40%不含树脂的颜料浓缩物与60%本发明聚氨酯分散体共混后制得层压白色油墨。
不含树脂的白色颜料浓缩物的典型配制剂:
75%二氧化钛/3%表面活性剂/0.5%除沫剂/21.5%水。
在制备油墨后,直接、1天后和7天后测量油墨粘度。记录粘度稳定性并评判颜料沉降。将油墨稀释到印刷粘度(25秒DIN4杯)并在OPP膜上印刷。评判视觉外观(不透明度、光泽度)。
对于粘度测量的测试方法:
在20℃的油墨温度下,根据测试油墨配制剂制备120g彩色(或150g白色)油墨。将油墨置于流杯(例如DIN4杯)中并记录使杯变空的运行(直到来自杯的流动不再是连续流动的)所需要的时间。粘度以“秒DIN4”记录。对于再溶解性的测试方法:
将油墨稀释到印刷机粘度(25秒DIN4杯)并且在实验室印刷机上凹版印刷在基材(例如LDPE)上。
使印刷机停止并将印压辊由基材上提起。使印刷机停止5分钟,以容许油墨干燥至凹印滚筒单元。5分钟后,使印刷机再次启动并计数在印刷基材上恢复原始图像的滚筒旋转量。印刷图像恢复得越快,油墨的再溶解性(=本身再溶解的能力)越好。
典型油墨制备:
通过使30份(树脂基或不含树脂的)颜料糊(例如PB15.3)与70份粘结剂测试分散体共混制备彩色油墨。可采用DIN4杯测量油墨粘度。使用30/70的颜料糊/水共混物可使油墨粘度减少到20s DIN4。
通过使40份不含树脂的颜料糊(例如PW6)与60份粘结剂测试分散体共混制备白色油墨。可采用DIN4杯测量油墨粘度。使用40/60的颜料糊/水共混物,可将油墨粘度降低到20s DIN4。
典型油墨施用:
使用绕线棒0(4μm湿油墨)将油墨施加到coex-OPP(30MB400-取向聚丙烯膜,其可由ExxonMobil Chemical得到)的经处理侧上以及经化学处理的聚酯(813,其可由DuPont Teijin Films得到)上。将油墨作为100%颜色(1层),200%颜色(2层)和100%颜色加上100%白色(2层)施用。在制备层压品之前,使得到的印刷品在烘箱中在60℃下干燥60s,随后在室温下进一步干燥约1小时的时间。
典型的层压程序:
为了测试层压结合强度,利用双组分聚氨酯层压粘合剂将在coex-OPP和经化学处理的聚酯上的印刷品层压到coex-OPP和标准LDPE(低密度聚乙烯),分别得到OPP//OPP和PET//LDPE层压品。
双组分聚氨酯层压粘合剂的制备:
层压品的制备:
将新制备的粘合剂以2.5g/m2的涂覆重量(干燥)施加到第二个(未印刷的)膜,且随后在烘箱中在60℃下干燥10s以蒸发溶剂。然后将经印刷的膜(coex-OPP和经化学处理的PET)的印刷侧小心施加到第二个膜(分别coex-OPP和LDPE)的粘合剂侧,从而避免在层压品中产生气泡,以得到OPP//OPP和PET//LDPE层压品结构。将得到的层压品在压力(约0.25kg/cm2)下储存3天,以容许粘合剂固化。
实施例1:聚氨酯分散体
表1:聚氨酯分散体组分
pTHF2000:分子量约2000(1950-2050)的聚四氢呋喃
将预装料的各组分装入反应器容器,随后加入异氰酸酯混合物(进料1)。将丙酮(进料2)加入混合物并将混合物加热到回流直至达到理论NCO值。加入1,4-丁二醇(进料3)并使反应在回流下进一步搅拌直至达到希望的NCO值。将混合物用丙酮(进料4)稀释。在50℃的内部温度下,加入进料5。通过加入水(进料6),随后加入胺混合物和水(进料7)使混合物分散。在真空下蒸馏丙酮。
产物表征:
固体含量:45%
pH:9.5
粘度:约130mPa.s(25℃)
实施例2:印刷油墨以及印刷和层压应用
彩色油墨:
聚氨酯分散体(实施例1) 70重量%
白色油墨:
T750W颜料浓缩物PW6 40重量%
聚氨酯分散体(实施例1) 60重量%
直接在制备油墨之后,使用DIN4杯测量油墨粘度。对相同油墨测量1天后和7天后的粘度以作为油墨稳定性的度量。结果在表2中给出。
表2:粘度(秒DIN4杯)
直接的粘度 | 1天后的粘度 | 7天后的粘度 | |
彩色 | 35秒 | 37秒 | 37秒 |
白色 | 21秒 | 22秒 | 22秒 |
在能够在基材上印刷油墨之前,必须将油墨稀释到印刷机粘度。
·对于彩色油墨,使用30%HPD96 PB15.3/70%水的共混物,降低粘度至20秒DIN4。
·对于白色油墨,使用40%T750W PW6/60%水的共混物,降低粘度至20秒DIN4。
表3:稀释到印刷粘度的典型实施例:
直接的粘度 | 稀释(油墨∶水) | 印刷粘度 | |
彩色 | 37秒 | 100∶5 | 20秒 |
白色 | 22秒 | 100∶2 | 20秒 |
油墨施用:
使用K-棒0(施加4微米湿涂覆重量),在共挤出的OPP(MB400,ExxonMobil公司)和聚酯膜(Mylar 813,Teijin-DuPont公司)上印刷油墨。
对于双层(彩色+白色):印刷第一彩色层并将印刷品在烘箱中干燥,然后在第一层顶部印刷第二白色油墨层并再次将印刷品在烘箱中干燥。
干燥:
对于单层印刷:将经印刷的基材放置于60℃空气温度下的空气循环烘箱中10秒,然后将印刷品在室温下放置1小时,然后将其层压到第二个膜。
对于双层印刷:印刷第一彩色层,在空气循环烘箱中在60℃下干燥10秒,印刷第二白色油墨层,在60℃下干燥10秒并在室温下留置印刷品1小时,然后将其层压到第二个膜。
层压:
使用双组分层压粘合剂,将经印刷的膜(OPP或PET)层压到第二个膜(OPP或LDPE),以得到OPP//OPP或PET//LDPE层压品:
·使用K棒1(6微米湿涂覆重量)将层压粘合剂施加到第二个膜上,随后干燥(在60℃下在烘箱中10秒)
·将经印刷的膜施加到第二个膜上,其中印刷侧面对粘合剂
·通过使用10kg的辊,稳固地挤压层压结构
·将层压品放置于压力(10kg块状物)下并在室温下储存3天
层压结合强度:
为了测量层压结合强度(=将层压品剥开所需要的力),由经固化的层压品切下15mm宽的条,并且使用Lloyd Instruments张力测试仪测量结合强度。在150mm/min的速度下进行测量。在测量期间,应使层压条保持相对于膜夹片(film clamp)在90°角下。在层压条在140℃/400N/1s下使用Brugger热封机热封之后,重复该测试,以模拟热封结合强度。以N/15mm记录层压结合强度。
表4:层压结合强度测量结果的典型实施例
耐粘性:
将稀释的油墨(稀释到20秒DIN4杯的粘度)印刷到相关基材(例如LDPE、OPP、PET、尼龙)上。施加的涂覆重量:对于彩色,1.0g/m2且对于白色,1.5g/m2。印刷品将在烘箱中干燥:在60℃下10秒。干燥后,将第二个层膜(相同规格)置于印刷膜的顶部,其中第二个膜的背面面对印刷膜的印刷侧。将膜置于Specac实验室印刷机中并在5吨/30℃/24小时(表示65kg/cm2)下粘接。在由粘接测试仪取出样品后,将未印刷层膜由印刷层移除,并评判未印刷的膜粘附到印刷膜(“粘接”)的趋势并作为“剥离”(粘性)和“破坏”(油墨转印到未经印刷膜)记录。耐粘性测量结果的典型实施例在下文中记录。值从1(坏,粘接油墨)至5(好,非粘接油墨)。
表5:耐粘性测量结果
Claims (15)
1.一种制备印刷层压品的方法,其包括:
通过辊印刷方法将至少一种层压油墨施加到第一个聚合物膜的至少一部分表面,并且通过使用粘合剂将未经印刷的第二个聚合物膜层压到第一个聚合物膜的含有油墨的表面,
其中层压印刷油墨包含至少一种粘结剂、至少一种颜料、水性载体和任选地添加剂,其中至少一种粘结剂为包含聚氨酯的水分散体,其中聚氨酯由包含以下化合物的组分制备:
a)至少一种具有至少两个异氰酸酯基团的多异氰酸酯,
b)二醇的组合,其中
b1)至少一种二醇为具有500-5000的分子量的聚酯二醇,且
b2)至少一种二醇为具有500-5000g/mol,优选1000-3000g/mol的数均分子量的聚四氢呋喃,
其中聚酯二醇b1)和聚四氢呋喃二醇b2)的重量比为1:2-2:1,
c)至少一种具有500-5000g/mol的数均分子量的单羟基聚氧化烯化合物,
d)至少一种二氨基酸化合物,
e)至少一种具有至少两个氨基且不含酸基的多胺化合物,以及
f)任选地一种或多种具有小于500g/mol,优选60-490g/mol的数均分子量的多元醇化合物;
其中层压印刷油墨为包含8-60重量%的至少一种粘结剂,3-30重量%至少一种颜料和15-60重量%水的凹版油墨或者柔性版油墨,和
其中油墨具有适合用于柔性版印刷或凹版印刷的粘度,
其中粘度根据在a#2流杯中测量为15-30秒。
2.根据权利要求1的方法,其中多异氰酸酯(a)选自1-异氰酸酯基-3,5,5-三甲基-5-异氰酸酯基甲基环己烷(IPDI)、四甲代苯二亚甲基二异氰酸酯(TMXDI)、六亚甲基二异氰酸酯(HDI)、双(4-异氰酸酯基环己基)甲烷(HMDI)或其混合物。
3.根据前述权利要求中任一项的方法,其中聚酯二醇由至少一种其中y为1-20的数,优选2-20的偶数的式HOOC-(CH2)y-COOH的二羧酸与至少一种选自其中x为1-20的数的式HO-(CH2)x-OH的化合物和新戊二醇及其混合物的多元醇制备。
4.根据前述权利要求中任一项的方法,其中在至少一种单羟基聚氧化烯化合物中的亚烷基为亚乙基和/或亚丙基。
5.根据前述权利要求中任一项的方法,其中至少一种二氨基酸化合物选自二氨基羧酸化合物和二氨基磺酸化合物,优选N-(2-氨基乙基)-2-氨基乙烷磺酸、N-(2-氨基乙基)-2-氨基乙烷羧酸及其相应的碱金属盐。
6.根据前述权利要求中任一项的方法,其中至少一种多胺化合物选自异佛尔酮二胺、二亚乙基三胺及其混合物。
7.根据前述权利要求中任一项的方法,其中聚氨酯由包含以下化合物的组分制备:
a)5-30重量%至少一种具有至少两个异氰酸酯基的多异氰酸酯,
b)10-80重量%二醇的组合,
c)1-20重量%至少一种具有500-5000g/mol数均分子量的单羟基聚氧化烯化合物,
d)1-10重量%至少一种二氨基酸化合物,
e)0.1-10重量%至少一种具有至少两个氨基且不含酸基的多胺化合物,以及
f)0-10重量%任选地一种或多种具有小于500g/mol,优选60-490g/mol的数均分子量的多元醇化合物。
8.根据前述权利要求中任一项的方法,其中油墨不含氨,且不含挥发性有机叔胺。
9.根据前述权利要求中任一项的方法,其中层压印刷油墨包含8-60重量%粘结剂,3-30重量%颜料,15-60%的水和0.1-5重量%添加剂如表面活性剂、除沫剂和蜡。
10.根据前述权利要求中任一项的方法,其中所用单体(a)基本仅包含脂族二异氰酸酯和/或环脂族二异氰酸酯;且所用单体(b1)基本仅包含由脂族二醇和二酸合成的聚酯二醇;且组分(d)包含N-(2-氨基乙基)-2-氨基乙烷磺酸和/或N-(2-氨基乙基)-2-氨基乙烷羧酸的碱金属盐;且组分(d)为DETA/IPDA的混合物。
11.根据前述权利要求中任一项的方法,其中辊印刷方法为凹版印刷或者柔性版印刷。
12.根据前述权利要求中任一项的方法,其中第一个和/或第二个聚合物膜的材料选自聚丙烯、聚对苯二甲酸乙二醇酯、聚酰胺和低密度聚乙烯。
13.一种根据权利要求1-12中任一项的方法制备的印刷层压品,在其至少一部分表面上具有前述权利要求中任一项的油墨。
14.根据前述权利要求的印刷层压品,其中层压品由至少两个聚合物膜通过使用层压粘合剂层压膜而制备,其中油墨保留在层压膜之间。
15.根据前两个权利要求的印刷层压品,其中至少一个在其表面上保留有油墨的聚合物膜包含选自聚丙烯、聚对苯二甲酸乙二醇酯、聚酰胺和低密度聚乙烯的材料。
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- 2015-01-14 WO PCT/EP2015/050590 patent/WO2015107078A1/en active Application Filing
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KR20160110471A (ko) | 2016-09-21 |
US20160326389A1 (en) | 2016-11-10 |
JP2017507205A (ja) | 2017-03-16 |
BR112016016298B8 (pt) | 2022-10-25 |
KR102231319B1 (ko) | 2021-03-24 |
US10280320B2 (en) | 2019-05-07 |
WO2015107078A1 (en) | 2015-07-23 |
ES2866630T3 (es) | 2021-10-19 |
EP3094692B1 (en) | 2021-02-24 |
BR112016016298B1 (pt) | 2022-03-15 |
MX2016009292A (es) | 2016-10-07 |
EP3094692A1 (en) | 2016-11-23 |
JP6534672B2 (ja) | 2019-06-26 |
BR112016016298A2 (zh) | 2017-08-08 |
CN105916947A (zh) | 2016-08-31 |
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