CN114174367A - 杀菌胶粘剂组合物 - Google Patents
杀菌胶粘剂组合物 Download PDFInfo
- Publication number
- CN114174367A CN114174367A CN202080051154.7A CN202080051154A CN114174367A CN 114174367 A CN114174367 A CN 114174367A CN 202080051154 A CN202080051154 A CN 202080051154A CN 114174367 A CN114174367 A CN 114174367A
- Authority
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- China
- Prior art keywords
- component
- isocyanate
- adhesive
- layer
- polyol
- 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.)
- Pending
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- 239000000853 adhesive Substances 0.000 title claims abstract description 156
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- 229920005862 polyol Polymers 0.000 claims abstract description 131
- 150000003077 polyols Chemical class 0.000 claims abstract description 128
- -1 isocyanate compound Chemical class 0.000 claims abstract description 107
- 239000012948 isocyanate Substances 0.000 claims abstract description 88
- 150000002513 isocyanates Chemical class 0.000 claims abstract description 49
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- 229920000570 polyether Polymers 0.000 claims abstract description 35
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- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 description 5
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- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 4
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- 238000012546 transfer Methods 0.000 description 4
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- 239000004698 Polyethylene Substances 0.000 description 3
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- 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 3
- FKTHNVSLHLHISI-UHFFFAOYSA-N 1,2-bis(isocyanatomethyl)benzene Chemical compound O=C=NCC1=CC=CC=C1CN=C=O FKTHNVSLHLHISI-UHFFFAOYSA-N 0.000 description 2
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- SBJCUZQNHOLYMD-UHFFFAOYSA-N 1,5-Naphthalene diisocyanate Chemical compound C1=CC=C2C(N=C=O)=CC=CC2=C1N=C=O SBJCUZQNHOLYMD-UHFFFAOYSA-N 0.000 description 2
- LFSYUSUFCBOHGU-UHFFFAOYSA-N 1-isocyanato-2-[(4-isocyanatophenyl)methyl]benzene Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=CC=C1N=C=O LFSYUSUFCBOHGU-UHFFFAOYSA-N 0.000 description 2
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Abstract
一种用于产生层压物的基于溶剂的聚氨基甲酸酯杀菌胶粘剂系统,其包括:(A)至少一种异氰酸酯化合物,组分A,其包含:以下物质的掺合物:(i)至少一种脂肪族类异氰酸酯和(ii)至少一种芳香族类异氰酸酯;和(B)至少一种异氰酸酯反应性组分,组分B,其包含:(i)至少一种磷酸酯化合物和(ii)平均分子量小于1,500g mol的至少一种聚醚多元醇;一种用于产生上述胶粘剂的方法;一种包括上述胶粘剂的多层层压品;以及一种用于使用上述胶粘剂产生层压品的方法。
Description
技术领域
本发明涉及一种适用于层压方法中的杀菌胶粘剂组合物;和此类杀菌胶粘剂组合物的制备。更确切地说,本发明涉及一种供与层压膜一起使用的基于溶剂的杀菌胶粘剂组合物,所述胶粘剂组合物展现法规遵循性、快速固化和良好粘着性能;和其制得方法。
背景技术
胶粘剂组合物适用于多种目的。举例来说,使用一些胶粘剂将衬底的两个或更多个膜层粘附在一起由此形成复合膜,即,包含两个或更多个膜层的层压物。衬底的实例通常包括聚乙烯、聚丙烯、聚酯、聚酰胺、金属、纸或赛璐玢(cellophane)等。胶粘剂在不同的层压最终用途应用中的用途为通常已知的。举例来说,胶粘剂一般施用于层压膜之间,可用于制造用于柔性封装行业中以供封装食品、医药品和工业消费品,尤其食品封装的膜/膜和膜/箔层压物。层压胶粘剂通常可分为三个类别:(1)基于溶剂的层压胶粘剂,(2)无溶剂层压胶粘剂,以及(3)基于水的层压胶粘剂。胶粘剂的性能视所施加胶粘剂的类别和应用而改变。在基于溶剂的层压胶粘剂类别中,基于溶剂的聚氨基甲酸酯已广泛用于实现相对良好耐热性、耐湿性和耐化学性。
在基于溶剂的层压胶粘剂类别中,存在诸多种类;并且一个特定种类包括基于聚氨基甲酸酯的多组分层压胶粘剂;并且更确切地说,双组分胶粘剂。通常,基于聚氨基甲酸酯的双组分层压胶粘剂包括第一组分,其包含异氰酸酯和/或聚氨基甲酸酯预聚物,和包含一种或多种多元醇的第二组分。聚氨基甲酸酯预聚物可由聚异氰酸酯与聚醚多元醇和/或聚酯多元醇的反应而获得。第二组分包含聚醚多元醇和/或聚酯多元醇。每一组分可任选地包括一种或多种添加剂。此类系统中所常用的溶剂包括甲基乙基酮、乙酸乙酯、甲苯等,其皆必须为无水分的以防止聚氨基甲酸酯的异氰酸酯基过早反应。
胶粘剂组合物的两种组分(即,异氰酸酯和多元醇组分)以预定比率组合,由此形成胶粘剂组合物。随后将溶剂中所携载的胶粘剂组合物施加于膜/箔衬底上。溶剂从所施加的胶粘剂组合物蒸发。随后使另一膜/箔衬底与另一衬底接触,形成可固化层压结构。层压结构随后经固化以将两个衬底粘结在一起。
基于溶剂的胶粘剂组合物可用于高性能层压物应用(例如杀菌、热充填、蒸煮袋等)中。举例来说,在杀菌柔性封装体应用中,杀菌柔性封装提供若干益处,如(1)消费者便利性,(2)封装于封装体中的食物的较长存放期,和(3)封装食物的原始风味的保持。如杀菌袋(retort pouch)的杀菌柔性封装通常用多层层压结构构建,如三层结构或四层结构。三层结构通常包括(例如)聚对苯二甲酸乙二酯(PET)的外层、金属箔(例如铝)的中间层以及浇铸聚丙烯(CPP)的内层;并且三层结构通常指示为PET//箔//CPP。四层结构通常包括(例如)PET的外层、金属箔的第一顶部中间层、尼龙的第二底部中间层和CPP的内层;并且四层结构通常指示为PET//箔//尼龙//CPP。将层压胶粘剂施加于结构以将不同层粘结在一起。用于杀菌柔性封装应用的层压胶粘剂不仅必须满足在高度酸性和脂肪食品存在下的高温下的极端性能要求,如在121摄氏度(℃)的温度下持续1小时(hr),或132℃的温度下持续30分钟(min);并且层压胶粘剂还必须满足极其严格的法规标准,如美国联邦管理局(FDA)和欧盟(EU)所颁布的法规。
基本上存在四种已知杀菌胶粘剂。两种胶粘剂是基于脂肪族异氰酸酯,其满足法规遵循性,但此类脂肪族类异氰酸酯胶粘剂的固化极为缓慢,并且胶粘剂具有性能问题。其它两种类型的胶粘剂含有芳香族异氰酸酯;并且此类芳香族类异氰酸酯胶粘剂固化快速,但此类胶粘剂不满足杀菌应用的法规遵循性并且胶粘剂还具有性能问题。现有技术未公开满足法规遵循性、具有快速固化特性并具有用于杀菌应用的良好粘着特性的“一体式”杀菌胶粘剂。
举例来说,用于杀菌应用的已知层压胶粘剂:(1)展现对广泛范围的杀菌衬底和结构的良好粘着性能,并且胶粘剂一般顺应于杀菌应用的全球食品法规;但胶粘剂展现缓慢固化特性,如在使用已知层压胶粘剂制得的封装体来封装食品之前在高于40℃下可固化至少10天;或(2)通常顺应于杀菌应用的全球食品法规;但胶粘剂展现缓慢固化特性,如在使用已知层压胶粘剂制得的封装体来封装食品之前在高于40℃下可固化至少10天;并且胶粘剂并未展现对广泛范围的杀菌衬底和结构的良好粘着性能;或(3)展现快速固化特性,如在10天内在环境条件下或在五天内在评估温度(例如大于或等于(≥)40℃)下可固化;并且胶粘剂对典型杀菌衬底和结构展现良好粘着性能;但胶粘剂一般不顺应于杀菌应用的全球食品法规,例如胶粘剂具有遵从FDA和EU法规的问题。还已知,基于芳香族的胶粘剂并未展现良好的粘着性能。
因此期望提供一种杀菌胶粘剂,其不仅展现极佳粘着性能、耐热性和耐化学性;而且还展现在环境固化条件下的快速固化特征(即固化时间小于[<]八天)及在评估温度(例如≥40℃)下<五天的固化时间。同时,期望提供一种满足法规遵循性的杀菌胶粘剂。举例来说,含有芳香族聚异氰酸酯(如,亚甲基二苯基二异氰酸酯(MDI)和甲苯二异氰酸酯(TDI))的胶粘剂可产生伯芳胺,如亚甲基二苯基二胺(MDA)和甲苯二胺(TDA),其为不合需要的并可潜在地从胶粘剂迁移到食品中。一般来说,为了顺应典型政府法规,所述法规要求芳胺迁移到以使用杀菌胶粘剂的封装体中所封装的食品中的芳胺总量需要为极低的,例如呈十亿分率(ppb)含量,以在胶粘剂经受严格杀菌测试条件之后,顺应FDA和EU食品法规。
发明内容
在本发明中,公开一种新颖的基于溶剂的胶粘剂,其展现所需性能属性并解决用于杀菌应用的先前已知胶粘剂的问题。在一个实施例中,本发明涉及一种用于产生层压物的多组分(例如二组分)、基于溶剂的聚氨基甲酸酯杀菌胶粘剂组合物,其包括异氰酸酯组分,组分A和异氰酸酯基(NCO)反应性组分,组分B。在一优选实施例中,胶粘剂组合物包括例如:(A)至少一种异氰酸酯化合物;其中所述至少一种异氰酸酯化合物,组分A包含以下物质的掺合物:(i)至少一种脂肪族类异氰酸酯和(ii)至少一种芳香族类异氰酸酯;和(B)至少一种异氰酸酯基(NCO)反应性组分;其中所述至少一种异氰酸酯反应性组分,组分B包含:(i)至少一种磷酸酯化合物和(ii)至少一种多元醇,其包含具有适当分子量分布,如平均分子量(Mw)<1,500克/摩尔(g/mol)的聚醚多元醇。
在其它实施例中,本发明包括用于产生上述胶粘剂的方法;包括上述胶粘剂的多层层压品;和使用上述胶粘剂产生层压品的方法。
附图说明
图1为显示在50℃的高温下固化3天后,本发明样品和比较样品的减弱全反射(ATR)的图示。
具体实施方式
本文中所公开的数值范围包括来自下限值和上限值的所有值,并包括下限值和上限值。对于含有确切值的范围(例如1或2或3至5或6或7的范围),包括任何两个确切值之间的任何子范围(例如以上范围1至7包括子范围1至2;2至6;5至7;3至7;5至6;等)。
术语“组合物”是指包含组合物的材料的混合物,以及由组合物的材料形成的反应产物和分解产物。
术语“包含”、“包括”、“具有”和其衍生词并不意图排除任何额外组分、步骤或程序的存在,无论其是否具体地公开。为避免任何疑问,除非相反陈述,否则通过使用术语“包含”所要求的所有组合物均可包括任何额外添加剂、佐剂或化合物,无论聚合或以其它方式。相比之下,术语“基本上由……组成”从任何随后列举的范围中排除任何其它组分、步骤或程序,除了对可操作性来说并非必不可少的那些之外。术语“由……组成”排除并未特定叙述或列出的任何组分、步骤或程序。除非另外陈述,否则术语“或”是指个别地以及呈任何组合形式的所列成员。单数的使用包括使用复数,并且反之亦然。
“异氰酸酯”为在其结构中含有至少一个异氰酸酯基的化学物质。异氰酸酯基由下式表示:-N=C=O或缩写为“NCO”。含有超过一个或至少两个异氰酸酯基的异氰酸酯为“聚异氰酸酯”。具有两个异氰酸酯基的异氰酸酯为二异氰酸酯,并且具有三个异氰酸酯基的异氰酸酯为三异氰酸酯等。异氰酸酯可为芳香族或脂肪族。
“聚异氰酸酯”为含有至少两个异氰酸酯基的分子。
“聚醚”为在相同原子直链中含有两个或更多个醚键的化合物。
“聚酯”为在相同原子直链中含有两个或更多个酯键的化合物。
“多元醇”为含有多个羟基(OH)的有机化合物。换句话说,多元醇含有至少两个OH基团。适合的多元醇的非限制性实例包括具有两个OH基团的二醇、具有三个OH基团的三醇和具有四个OH基团的四醇。
“聚酯多元醇”为在化合物的主链结构中含有聚酯和多元醇的化合物。
“聚醚多元醇”为在化合物的主链结构中含有聚醚和多元醇的化合物。
除非明确规定厚度,否则“膜”(包括在较厚制品中提及“膜层”时)包括在一个维度上具有约0.5毫米(mm)(20密耳)或更小的大体上一致并且均一厚度的任何薄、扁平的挤出或浇铸型热塑性制品。
“聚合物膜”为由聚合物或聚合物的混合物制成的膜。聚合物膜的组成通常为80重量%(wt%)的一种或多种聚合物。
“聚合物”为通过聚合相同或不同类型的单体来制备的聚合化合物。因此,通用术语聚合物涵盖术语“均聚物”(用于指代仅由一种类型的单体制备的聚合物,理解为可以将痕量的杂质并入聚合物结构中),以及术语“互聚物”,其包括共聚物(用于指代由两种不同类型的单体制备的聚合物)、三聚物(用于指代由三种不同类型的单体制备的聚合物),和由超过三种不同类型的单体制备的聚合物。痕量杂质,例如催化剂残余物,可并入聚合物之中和/或之内。其还涵盖共聚物的所有形式,例如无规、嵌段等。应注意,尽管聚合物通常称为“由”一种或多种指定单体“制得”、“基于”特定单体或单体类型、“含有”特定单体含量或类似说法,但在此情形下,术语“单体”应理解为指代特定单体的聚合残留物并且不指代未聚合物种。一般来说,本文中的聚合物称为基于作为对应单体的聚合形式的“单元”。
在胶粘剂领域已公认,制得两部分胶粘剂系统包括:提供包含含异氰酸酯组分的第一部分(本文中为组分A);提供包含NCO反应性组分的第二部分,如多元醇组分(本文中为组分B);并且接着合并或混合组分A与组分B以形成两部分胶粘剂系统或组合物。
在一个广泛实施例中,本发明涉及一种用于产生层压物的至少一种基于溶剂的聚氨基甲酸酯杀菌胶粘剂,所述胶粘剂包括组分A,其包含至少一种含异氰酸酯化合物;和组分B,其包含至少一种NCO反应性组分;其中所述至少一种NCO反应性组分含有(i)至少一种磷酸酯化合物和(ii)至少一种多元醇,其包含平均Mw<1,500g/mol的聚醚多元醇。在一个实施例中,至少一种NCO反应性组分中的磷酸酯多元醇可以例如0.1wt%至30wt%的浓度存在。在第一优选实施例中,胶粘剂的至少一种异氰酸酯化合物为例如至少一种脂肪族类异氰酸酯。在第二优选实施例中,至少一种异氰酸酯化合物为(i)至少一种芳香族类异氰酸酯与(ii)至少一种脂肪族类异氰酸酯的掺合物。在第二优选实施例中,至少一种芳香族类异氰酸酯可为包含以下的反应产物的异氰酸酯预聚物:(i)至少一种聚异氰酸酯和(ii)Mw>1,500g/mol的至少一种聚醚多元醇。
本发明的独特胶粘剂具有优于迄今为止已知的基于溶剂的聚氨基甲酸酯杀菌胶粘剂系统的若干优点,包括例如(1)良好粘着性能;(2)快速固化特性;和(3)(a)无芳胺迁移量或(b)极低的芳胺迁移量。独特的基于溶剂的聚氨基甲酸酯杀菌胶粘剂系统继而适用于制得具有良好耐热性和良好耐化学性的层压物的方法中,所述层压物用于制得杀菌封装制品。
如前述,在另一实施例中,用于制得本发明的基于溶剂的聚氨基甲酸酯杀菌胶粘剂的至少一种含异氰酸酯化合物,组分A为例如以下物质的掺合物:(i)至少一种脂肪族类异氰酸酯和(ii)至少一种芳香族类异氰酸酯。适用于本发明的含异氰酸酯化合物可选自例如由以下组成的组:异氰酸酯单体、聚异氰酸酯(例如二聚体、三聚体等)、异氰酸酯预聚物和其两种或更多种的混合物。如本文所用,“聚异氰酸酯”为含有两个或更多个异氰酸酯基的任何化合物。
此外,含异氰酸酯的化合物可选自由以下组成的组:脂肪族聚异氰酸酯、环脂肪族聚异氰酸酯、芳香族聚异氰酸酯和其两种或更多种的组合。“脂肪族聚异氰酸酯”为不含有芳环的聚异氰酸酯。“环脂肪族聚异氰酸酯”为脂肪族聚异氰酸酯的子组,其中化学链呈环状结构。“芳香族聚异氰酸酯”为含有一个或多个芳环的聚异氰酸酯。
适用于本发明的脂肪族类异氰酸酯组分,组分A的组分(i)可包括一种或多种化合物,其包括例如在直链或分支链亚烷基残基中在一个实施例中具有3个碳原子(C)至16个C和在另一实施例中具有4个C至12个C的脂肪族聚异氰酸酯。环脂肪族聚异氰酸酯也适用于本发明,其包括例如在亚环烷基残基中在一个实施例中具有4个C至18个C和另一实施例中具有6个C至15个C的环脂肪族聚异氰酸酯。环脂肪族二异氰酸酯是指以环与脂肪族方式键结的NCO基团,如异佛尔酮二异氰酸酯和二异氰酸酯基二环己基甲烷(H12MDI)。
适用于本发明的适合脂肪族聚异氰酸酯和环脂肪族聚异氰酸酯的实例包括但不限于环己烷二异氰酸酯、甲基环己烷二异氰酸酯、乙基环己烷二异氰酸酯、丙基环己烷二异氰酸酯、甲基二乙基环己烷二异氰酸酯、丙烷二异氰酸酯、丁烷二异氰酸酯、戊烷二异氰酸酯、己烷二异氰酸酯、庚烷二异氰酸酯、辛烷二异氰酸酯、壬烷二异氰酸酯,壬烷三异氰酸酯,如4-异氰酸酯基甲基-1,8-辛烷二异氰酸酯(TIN)、癸烷二异氰酸酯和三异氰酸酯、十一烷二异氰酸酯和三异氰酸酯以及十二烷二异氰酸酯和三异氰酸酯、六亚甲基二异氰酸酯(HDI)、二异氰酸酯基二环己基甲烷(H12MDI)、2-甲基戊烷二异氰酸酯(MPDI)、2,2,4-三甲基六亚甲基二异氰酸酯/2,4,4-三甲基六亚甲基二异氰酸酯(TMDI)、降冰片烷二异氰酸酯(NBDI)、二甲苯二异氰酸酯(XDI)、1,4-或1,3-双(异氰酸酯基甲基)环己烷(H6XDI)、四甲基二甲苯二异氰酸酯和其两种或更多种的二聚体,三聚体,衍生物和混合物。适用于本发明的合适脂肪族聚异氰酸酯和环脂肪族聚异氰酸酯还包括例如基于XDI的聚异氰酸酯、基于H6XDI的聚异氰酸酯、XDI异氰尿酸酯、基于HDI的聚异氰酸酯、基于H12MDI的聚异氰酸酯、HDI异氰尿酸酯和其两种或更多种的混合物。
在一个优选实施例中,适用于本发明的脂肪族类组分包括例如基于XDI的聚异氰酸酯、基于HDI的聚异氰酸酯和其混合物。
适用于本发明的脂肪族类组分的示例性商业产品中的一些包括例如可购自三井化学(Mitsui Chemical)的TAKENATE D-110N和TAKENATE D-120N;可购自科思创公司(Coverstro Company)的Desmodur N 3200和Desmodur Quix175;和其混合物。
根据本公开适用的额外含异氰酸酯化合物包括但不限于4-甲基-环己烷1,3-二异氰酸酯、2-丁基-2-乙基五亚甲基二异氰酸酯、3(4)-异氰酸酯基甲基-1-甲基环己基异氰酸酯、2-异氰酸酯基丙基环己基异氰酸酯、2,4'-亚甲基双(环己基)二异氰酸酯、1,4-二异氰酸酯基-4-甲基-戊烷和其两种或更多种的混合物。
另外,适用作根据本公开的组分A的组分(i)的含异氰酸酯化合物包括例如异氰酸酯预聚物。“异氰酸酯预聚物”为聚异氰酸酯与异氰酸酯反应性组分的反应产物,其化学计量比(NCO/OH)在一个实施例中大于(>)2.0,在另一实施例中为3.0至10.0,并且在再另一实施例中为4.0至7.0。如上所述,聚异氰酸酯选自例如芳香族聚异氰酸酯、脂肪族聚异氰酸酯、环脂肪族聚异氰酸酯和其混合物。可与聚异氰酸酯反应以形成异氰酸酯预聚物(也称为“聚氨基甲酸酯预聚物”)的适合异氰酸酯反应性组分包括例如具有羟基、氨基和硫基的化合物。可与聚异氰酸酯反应以形成适用于本发明的异氰酸酯预聚物的异氰酸酯反应性组分包括例如聚醚多元醇、聚酯多元醇、聚己内酯多元醇、聚丙烯酸酯、聚碳酸酯多元醇、基于天然油的多元醇和其两种或更多种的混合物。
可与聚异氰酸酯反应以形成适用于本发明的异氰酸酯预聚物的异氰酸酯反应性组分还可通过异氰酸酯反应性组分的羟基数和其羟基官能度表征。“羟基数(hydroxylnumber)”或“羟值(hydroxyl value)”为化学物质中的游离羟基含量的量度。羟基数为中和在对一克含有游离羟基的化学物质进行乙酰化时吸收的乙酸所需的氢氧化钾(KOH)的毫克数。羟基数(OHN)通常表示为氢氧化钾毫克数/每克化学物质(mg KOH/g)。羟基数是根据DIN53240测定。
“羟基官能度”为化合物的一个分子中存在的羟基的数目。羟基官能团是根据ASTMD4274-16测量,其中结果在一个实施例中报告为1或更大的整数,并且在另一实施例中报告为1至6。
在一些实施例中,异氰酸酯反应性组分的平均羟基数可为例如在一个实施例中1mg KOH/g至2,000mg KOH/g,在另一实施例中5mg KOH/g至2,000mg KOH/g,在再另一实施例中14mg KOH/g至850mg KOH/g,在又另一实施例中28mg KOH/g至500mg KOH/g,并且在甚至再另一实施例中,35mg KOH/g至450KOH/g。在一些实施例中,异氰酸酯反应性组分的平均摩尔质量在一个实施例中为例如62g/mol至20,000g/mol,在另一实施例中为250g/mol至12,000g/mol,在再另一实施例中为500g/mol至6,000g/mol,并且在又另一实施例中为800g/mol至3,000g/mol。
在一些实施例中,异氰酸酯反应性组分的平均羟基官能度在一个实施例中可为例如1.0至6.0,在另一实施例中,1.8至4.0,并且在再另一实施例中,2.0至3.0。由本发明的脂肪族类组分所展现的有利特性之一包括例如提供可顺应广泛政府法规的胶粘剂。
具有异氰酸酯基的化合物还通过以化合物的总重量计的异氰酸酯基的重量百分比表征。异氰酸酯基的重量百分比被称为“%NCO”并根据ASTM D2572-97测量。
按组分A中的组分的总量计,本发明方法中所用的脂肪族类组分的量包括例如在一个实施例中为30wt%至100wt%,在另一实施例中为40wt%至90wt%并且在再另一实施例中为50wt%至80wt%。
适用于本发明的芳香族类异氰酸酯组分,组分A的组分(ii)可包括例如一种或多种聚异氰酸酯化合物,其包括但不限于例如1,3-和1,4-亚苯基二异氰酸酯;1,5-亚萘基二异氰酸酯;2,6-甲苯二异氰酸酯(2,6-TDI);2,4-甲苯二异氰酸酯(2,4-TDI);2,4'-二苯基甲烷二异氰酸酯(2,4'-MDI);4,4'-二苯基甲烷二异氰酸酯(4,4'-MDI);3,3'-二甲基-4,4'-联苯二异氰酸酯(TODI)和其异构体;聚合异氰酸酯;以及其两种或更多种的混合物。
适用于本发明的示例性商业芳香族类组分中一些可包括例如可购自陶氏化学公司(Dow Chemical Company)的Isonate 125M、ADCOTTE L76-204、共反应物CT(CoreactantCT)和催化剂F(Catalyst F);可购自科思创公司的E 2200/76;和其混合物。由本发明的芳香族类组分展现的有利特性之一包括例如提供可快速固化的胶粘剂。
本发明方法中所用的芳香族类异氰酸酯组分的量按组分A中的组分的总量计,例如在一个实施例中为5wt%至95wt%,在另一实施例中为20wt%至90wt%,并且在再另一实施例中为30wt%至90wt%。
如前述,用于制得胶粘剂的至少一种NCO反应性组分,组分B为例如至少一种NCO反应性组分,其含有(i)至少一种磷酸酯化合物和(ii)至少一种多元醇,其包含平均Mw<1,500g/mol的聚醚多元醇。如本文所用,“多元醇”是指每分子具有两个或更多个羟基(即,-OH)的化合物。如本文所用,“醚”是指含有醚键的化合物。如本文所用,“聚醚”是指每分子含有两个或更多个醚键的化合物。为聚醚和多元醇两者的化合物在本文中称为“聚醚多元醇”。“脂肪族聚醚多元醇”为在其分子中不含有芳环的聚醚多元醇。“芳香族聚醚多元醇”为在其分子中含有一个或多个芳环的聚醚多元醇。
在一个实施例中,适用于本发明的磷酸酯化合物,组分B的组分(i)可选自例如具有以下化学结构(I)的磷酸酯化合物:
其中R1为任何有机基团。除结构(I)中所显示的侧基之外,R1可或可不具有一个或多个额外侧接-OH基团,并且R1可或可不具有一个或多个结构(I)的额外侧基。-OH基团和结构(I)的一个或多个基团中的任何两个或更多个可或可不连接于R1的同一原子。在一优选实施例中,每一-OH基团和结构(I)的每一基团连接于R1的单独原子。
表征R1的适宜方式为描述具有以下结构(II)的化合物:
其中R1与结构(I)中相同。具有结构(II)的化合物在本文中称为“前体多元醇”。
在一些实施例中,适合的前体多元醇的数均Mw在一个实施例中为90g/mol或更高,在另一实施例中为200g/mol或更高,并且在再另一实施例中为400g/mol或更高。在一些实施例中,适合的前体多元醇的数均Mw在一个实施例中为4,000g/mol或更低,在另一实施例中为2,000g/mol或更低,在再另一实施例中为1,200g/mol或更低,在又另一实施例中为900g/mol或更低,并且在甚至再另一实施例中为500g/mol或更低。在一些实施例中,适合的前体多元醇的数均Mw在一个实施例中为200g/mol至4,000g/mol,在另一实施例中为400g/mol至2,000g/mol,在再另一实施例中为400g/mol至1,200g/mol,并且在又另一实施例中为400g/mol至900g/mol。
在一些实施例中,适合的前体多元醇为烷基高碳多元醇、单醣、双醣和具有以下结构(III)的化合物:
其中R2、R3、R4和R5中的每一个相互独立地为任何有机基团;n1、n2和n3中的每一个相互独立地为0至10的整数。除了结构(III)中所显示的侧基之外,R2可或可不具有一个或多个额外侧基。进一步理解,侧基中的任何两个或更多个可或可不连接于R2的同一原子。在一些实施例中,存在具有结构(III)的化合物的混合物,其中结构(III)的化合物的n1、n2和n3中的一个或多个的值彼此不同。本文中通过阐述参数n1、n2或n3的非整数值来描述此类混合物,其中非整数值表示所述参数的数均值。当需要评估此类混合物的分子量时,使用数均分子量。
在具有结构(III)的前体多元醇中,在一个优选实施例中,每一侧基连接于R2的单独原子。在具有结构(III)的前体多元醇中,在另一优选实施例中,R3、R4和R5中的一个或多个为在一个实施例中具有1个C至4个C,在另一实施例中具有2个C至3个C和在再另一实施例中具有3个C的烃基。在具有结构(III)的前体多元醇中,在再另一优选实施例中,R3、R4和R5中的一个或多个为烷基,其可为直链或环状或分支链或其组合;在又另一优选实施例中,R3、R4和R5中的一个或多个为直链或分支链烷基;并且在甚至再另一优选实施例中,R3、R4和R5中的一个或多个为分支链烷基。在甚至又另一优选实施例中,R3、R4和R5彼此相同。
在具有结构(III)的前体多元醇中,在一个优选实施例中,n1、n2和n3中的一个或多个为0至8。在具有结构(III)的前体多元醇中,在另一优选实施例中,n1、n2和n3中的一个或多个为1或更大。在具有结构(III)的前体多元醇中,在再另一优选实施例中,n1、n2和n3中的一个或多个为6或更小。在具有结构(III)的前体多元醇中,在又另一优选实施例中,n1、n2和n3彼此相同。
在一个实施例中,具有结构(III)的前体多元醇的群为其中R2、R3、R4和R5中的每一个为烷基的化合物;此类前体多元醇在本文中称为烷氧基化烷基三醇。在三醇中,当n1、n2和n3中的至少一个为1或更大并且R2具有以下结构(IV)时:
则三醇在本文中已知为烷氧基化甘油。在烷氧基化三醇中,当R3、R4和R5中的每一个为恰好具有3个C的分支链烷基时,烷氧基化三醇在本文中已知为丙氧基化三醇。丙氧基化三醇(其中R2具有结构(IV))在本文中已知为丙氧基化甘油。
在为烷基高碳多元醇的前体多元醇中,在一个实施例中,为具有10个C或更少碳原子的化合物;在另一实施例中,为具有6个C或更少碳原子的化合物;在再另一实施例中,为具有3个或更少碳原子的化合物;并且在又另一实施例中,化合物为甘油。
在甚至再另一实施例中,前体多元醇为烷基高碳多元醇和具有结构(III)的化合物。应注意,如果n1等于(=)n2=n3=0,并且如果R2为烷基或具有羟基的烷基,那么具有结构(IV)的化合物为烷基高碳多元醇。
在一个实施例中,前体多元醇的群为烷基三醇和烷氧基化烷基三醇。在这些化合物中,在一个实施例中为甘油和烷氧基化甘油;并且在另一实施例中为烷氧基化甘油。在烷氧基化甘油中,在一个优选实施例中,为丙氧基化甘油。
适用于本发明的另一类别的适合的磷酸酯化合物包括含有氨基甲酸酯键的化合物。通过使一种或多种适合的磷酸酯官能多元醇与一种或多种聚异氰酸酯,并且在一优选实施例中包括一种或多种二异氰酸酯反应来制得含有氨基甲酸酯键的磷酸酯化合物。在一优选实施例中,聚异氰酸酯的量保持足够低以使得反应产物中的一些或全部为磷酸酯官能多元醇。或者,多元醇可首先与聚异氰酸酯反应以制得随后与聚磷酸反应的-OH封端的预聚物。具有氨基甲酸酯键的磷酸酯化合物包括在一个通用实施例中数均Mw在1,000g/mol至6,000g/mol范围内,在另一实施例中在1,200g/mol至4,000g/mol范围内并且在再另一实施例中在1,400g/mol至3,000g/mol范围内的化合物。
在一些实施例中,磷酸酯化合物为包括前体多元醇和磷酸类型酸的反应物的反应产物,并且所得磷酸酯化合物具有结构(I)的化学结构。
在一个优选实施例中,选择磷酸型酸和前体多元醇的量以如下测定Mp:Mx的比:Mhy=前体多元醇的每分子羟基数;Nx=Mhy-2;Mx=(前体多元醇摩尔数)×(Nx);并且Mp=含于磷酸型酸中的磷原子摩尔数。
一般来说,Mp:Mx的比在一个实施例中为0.1:1或更高,在另一实施例中为0.2:1或更高,在再另一实施例中为0.5:1或更高,并且在又另一实施例中为0.75:1或更高。在一些实施例中,Mp:Mx的比为1.1:1或更低。
通常,磷酸型酸与前体多元醇的重量比在一个实施例中为0.005:1或更高,在另一实施例中为0.01:1或更高,并且在再另一实施例中为0.02:1或更高。在一些实施例中,磷酸型酸与前体多元醇的重量比为0.3:1或更低,或0.2:1或更低,或0.12:1或更低。
在一些实施例中,磷酸型酸含有聚磷酸。并且,一般来说,磷酸型酸中的聚磷酸的量按磷酸型酸的重量计,在一个实施例中为75wt%或更多,在另一实施例中为80wt%或更多,并且在再另一实施例中为90wt%或更多。可购得各种等级的聚磷酸;每一等级通过百分比表征。为了测定等级,首先认识到,对于纯单体正磷酸,五氧化二磷的含量视为72.4%。也可分析任何等级的聚磷酸以考虑一摩尔聚磷酸(分子量标记为“Fppa”)含有标记为“Nppo”的五氧化二磷摩尔数,并且五氧化二磷百分比(“PCppo”)由PCppo=(Nppo×142)/Fppa给出,表示为百分比。则聚磷酸的等级即为比率(表示为百分比):等级=PCppo/72.4。
在一些实施例中,所使用的聚磷酸在一个实施例中具有100%或更高,并且在另一实施例中具有110%或更高的等级。在一些实施例中,所使用的聚磷酸在一个实施例中具有150%或更低,并且在另一实施例中具有125%或更低的等级。
在一些实施例中,除了一种或多种磷酸酯官能多元醇之外,所公开的基于溶剂的胶粘剂组合物还含有一种或多种无磷多元醇。
关于适合磷酸酯和此类适合磷酸酯的制备的其它信息可见于例如PCT公开第WO/2015/168670号中。
通常,本发明中所用的磷酸酯化合物,组分B的组分(i)的量按多元醇组分,组分B的干重计,在一个实施例中为0.1wt%至80wt%,在另一实施例中为1wt%至70wt%,在再另一实施例中为5wt%至60wt%,在又另一实施例中为10wt%至60wt%,在甚至再另一实施例中为20wt%至60wt%。
适用于本发明的多元醇组分,组分B的组分(ii)包含至少一种聚醚多元醇。一般来说,聚醚多元醇的分子量在一个实施例中<1,500g/mol,在另一实施例中<1,000g/mol,并且在再另一实施例中为50g/mol至1,500g/mol。在另一实施例中,并入于本发明的多元醇组分(组分B)中的聚醚多元醇的分子量为150g/mol至1,500g/mol并且官能度为2.0至6.0。
适用于本发明的示例性适合聚醚多元醇包括但不限于例如聚丙二醇、聚四亚甲基醚二醇、基于聚环氧丁烷的多元醇和其共聚物;以及其混合物。
适用于本发明的示例性适合聚丙二醇包括但不限于例如基于环氧丙烷、环氧乙烷的多元醇,或其与选自以下引发剂的混合物:丙二醇、二丙二醇、山梨糖醇、蔗糖、甘油和/或其混合物。举例来说,聚丙二醇可包括可购自陶氏化学公司的VORANOLTM;可购自巴斯夫(BASF)公司的PLURACOLTM;可购自龙沙(Lonza)的POLY-GTM、POLY-LTM和POLY-QTM;和可购自科思创的ACCLAIMTM;以及其混合物。在一个优选实施例中,使用官能度在2至6之间并且Mw为250g/mol至1,500g/mol的聚丙二醇。
适用于本发明的示例性适合聚四亚甲基醚二醇包括但不限于例如可购自巴斯夫公司的POLYTHFTM;可购自英威达(Invista)的TERTHANETM;可购自三菱(Mitsubishi)的PTMGTM;和可购自达里(Dairen)的PTGTM;以及其混合物。在一个优选实施例中,使用官能度在2至6之间并且Mw为250g/mol至1,500g/mol的聚四亚甲基醚二醇。
适用于本发明的示例性适合基于聚环氧丁烷的多元醇包括但不限于例如聚环氧丁烷均聚物多元醇、聚环氧丁烷-聚环氧丙烷共聚物多元醇和聚环氧丁烷-聚环氧乙烷共聚物多元醇;以及其混合物。在一个优选实施例中,使用官能度为2.0至4.0并且Mw为150g/mol至1,500g/mol的基于聚环氧丁烷的多元醇。
在其它实施例中,适用于本发明的聚醚多元醇包括但不限于例如低分子量二醇,包括但不限于例如乙二醇、二乙二醇、三乙二醇、丙二醇、1,3-丙二醇、1,3-丁二醇、1,4-丁二醇、1,6-己二醇、三羟甲基丙烷、三异丙醇胺、新戊二醇;和其混合物。
通常,本发明中所用的组分,聚醚多元醇,组分B的组分(ii)的量按多元醇组分,组分B的干重计,在一个实施例中为20wt%至99.9wt%,在另一实施例中为30wt%至99wt%,并且在再另一实施例中为40wt%至95wt%。
除了聚醚多元醇(组分B的组分(ii))以外,多元醇组分B可任选地包括(iii)至少一种聚酯多元醇。通常,当使用时,聚酯多元醇(组分B的组分(iii))的分子量在一个实施例中为<3,000g/mol,在另一实施例中<3,500g/mol,并且在再另一实施例中为500g/mol至3,000g/mol。
适用于本发明的适合聚酯多元醇包括但不限于例如脂肪族聚酯多元醇;芳香族聚酯多元醇;脂肪族聚酯多元醇与芳香族聚酯多元醇的共聚物;聚碳酸酯多元醇;聚己内酯多元醇;和其混合物。这些聚酯多元醇:为多元酸与多元醇的反应产物;或光气或碳酸酯单体与多元醇的反应物;或经由环酯化合物的开环聚合产生。
适用于本发明的示例性适合多元酸包括丁二酸、己二酸、壬二酸、癸二酸、十二烷二甲酸、顺丁烯二酸酐、反丁烯二酸、1,3-环戊烷-二甲酸、1,4-环己烷二甲酸、对苯二甲酸、间苯二甲酸、邻苯二甲酸、1,4-萘二甲酸、2,5-萘二甲酸、2,6-萘二甲酸、萘二甲酸、二苯二甲酸、1,2-双(苯氧基)乙烷-p,p'-二甲酸,以及这些二甲酸的酸酐或酯形成衍生物;以及对羟基苯甲酸、对(2-羟基乙氧基)苯甲酸,和这些二羟基甲酸的酯形成衍生物或二聚酸;以及其混合物。这些多元酸可单独或以两种或更多种多元酸的组合形式使用。
根据本公开,可使用任何已知的多元醇。适用于本发明的适合多元醇的非限制性实例包括:二醇,如乙二醇、丙二醇、1,3-丙二醇、1,4-丁二醇、1,5-戊二醇、3-甲基-1,5-戊二醇、1,6-己二醇、新戊二醇、甲基戊二醇、二甲基丁二醇、丁基乙基丙二醇、二乙二醇、三乙二醇、四乙二醇、二丙二醇、三丙二醇、双羟基乙氧基苯、1,4-环己二醇、1,4-环己烷-二甲醇、三乙二醇、聚己内酯二醇、二聚二醇、双酚A和氢化双酚A;经由环酯化合物(如丙内酯、丁内酯、ε-己内酯、8-戊内酯和β-甲基-δ-戊内酯)的开环聚合而产生的聚酯;和由一种或多种单体以常用方式借助于作为引发剂的一种或多种含有两个活性氢原子的化合物进行加成聚合而产生的聚醚,单体包括环氧乙烷、环氧丙烷、环氧丁烷、氧化苯乙烯、表氯醇、四氢呋喃和亚环己基,一种或多种化合物为如,乙二醇、二乙二醇、三乙二醇、丙二醇、1,3-丙二醇、1,3-丁二醇、1,4-丁二醇、1,6-己二醇和新戊二醇;以及其混合物。这些多元醇可单独或以两种或更多种多元醇的组合形式使用。
通常,聚酯多元醇,组分B的任选的组分(iii)(当使用时可添加到多元醇组分,组分B中)的量可包括例如按多元醇组分,组分B的干重计,在一个实施例中为0wt%至多20wt%,在另一实施例中为0.01wt%至15wt%,并且在再另一实施例中为0.1wt%至10wt%。
一般来说,本发明的胶粘剂组合物包括(C)至少一种溶剂作为组分C。举例来说,但不限于,溶剂可选自由以下组成的组:乙酸乙酯、甲基醚酮、甲苯和其混合物。
按胶粘剂组合物中的组分的总量计,本发明方法中所用的溶剂,组分C的量可为例如在一个实施例中20wt%至90wt%,在另一实施例中30wt%至80wt%,并且在再另一实施例中40wt%至70wt%。
在一些实施例中,本发明的胶粘剂组合物可包括(D)一种或多种额外任选的常规成分或添加剂作为组分D,包括但不限于例如催化剂、增粘剂、塑化剂、流变改质剂、助粘剂、抗氧化剂、填充剂、着色剂、颜料、表面活性剂、溶剂、聚合物(包括例如除上文所论述以外的热塑性树脂)、脱水试剂(包括例如硅烷)、苯甲酰氯、其它多元醇(包括例如脂肪多元醇)、紫外线指示剂和其两种或更多种的组合。
作为说明性实施例,胶粘剂组合物可包括例如助粘剂。适合助粘剂的非限制性实例包括偶联剂,如硅烷偶联剂、钛酸酯偶联剂和铝酸酯偶联剂;环氧树脂;磷酸;聚磷酸和磷酸酯。
适用于本发明的硅烷偶联剂的实例包括但不限于氨基硅烷,如γ-氨丙基三乙氧基硅烷、γ-氨丙基-三甲氧基硅烷、N-β(氨乙基)-γ-氨丙基三甲氧基硅烷、N-β(氨乙基)-γ-氨丙基三甲基二甲氧基硅烷,和N-苯基-γ-氨丙基三甲氧基硅烷、环氧硅烷,如β-(3,4-环氧环己基)-乙基三甲氧基硅烷、γ-缩水甘油氧基丙基-三甲氧基硅烷和γ-缩水甘油氧基丙基三乙氧基硅烷;乙烯基硅烷,如乙烯基三(β-甲氧基乙氧基)硅烷、乙烯基三乙氧基硅烷、乙烯基三甲氧基硅烷和γ-甲基丙烯酰氧基丙基三甲氧基硅烷;六甲基二硅氮烷;γ-巯基丙基-三甲氧基硅烷;以及其混合物。
适用于本发明的钛酸酯偶联剂的实例包括但不限于四异丙氧基钛、四-正丁氧基钛、钛酸丁酯二聚体、钛酸四硬脂酰酯、乙酰基丙酮酸钛、乳酸钛、四辛二醇钛酸酯、乳酸钛、四硬脂氧基钛和其混合物。
环氧树脂的实例包括但不限于多种易于购得的环氧树脂,如双酚A-表氯醇(epi-bis)型环氧树脂、酚醛清漆型环氧树脂、β-甲基表氯醇型环氧树脂、环状环氧乙烷型环氧树脂、缩水甘油醚型环氧树脂、缩水甘油酯型环氧树脂、聚二醇醚型环氧树脂、二醇醚型环氧树脂、环氧化脂肪酸酯型环氧树脂、聚羧酸酯型环氧树脂、氨基缩水甘油基型环氧树脂、间苯二酚型环氧树脂;以及其混合物。
在一些实施例中,助粘剂可为磷酸酯化合物。在其它实施例中,助粘剂为环氧硅烷((3-缩水甘油基氧基丙基)-三甲氧基硅烷)。在一些实施例中,磷酸可并入多元醇组分中,而环氧硅烷可并入异氰酸酯组分中。在一些实施例中,环氧硅烷与磷酸均并入多元醇组分中。
在一些实施例中,不包括非反应性组分(如溶剂)的胶粘剂组合物(即,异氰酸酯组分与多元醇组分一起)的平均官能度为2至2.5。
当使用时,任选的组分D的量按胶粘剂组合物中的组分的总量计,可为例如在一个实施例中0wt%至15wt%,在另一实施例中0.01wt%至10wt%,并且在再另一实施例中0.1wt%至5wt%。
在一个广泛实施例中,产生胶粘剂组合物的方法包括混合上文所述的异氰酸酯和多元醇组分以形成可固化胶粘剂组合物。预期在本发明中使用两个部分,异氰酸酯部分和多元醇组分部分。还预期所公开胶粘剂组合物的异氰酸酯组分和多元醇组分可分开制得并且必要时储存直到需要使用胶粘剂组合物为止。在一些实施例中,异氰酸酯组分和多元醇组分在25℃下各自为液体。当需要使用胶粘剂组合物时,通常以1与2.5之间的化学计量比(NCO/OH)使异氰酸酯组分与多元醇组分彼此接触并混合在一起。预期当使这些两种组分接触时,开始固化反应,其中异氰酸酯基与羟基反应以形成氨基甲酸酯键联。通过使两种组分接触形成的胶粘剂组合物可称作“可固化混合物”。
为形成胶粘剂组合物,两种组分的混合可在形成胶粘剂组合物的过程中的任何适合的时间进行并将胶粘剂施加于衬底上,如在施加过程之前、期间或作为其结果。所有本发明步骤均可在环境室温条件下进行。按需要可采用加热或冷却。并且混合可使用适合常规混合器进行,如使用电动、气动或以其它方式提供动力的机械混合器。
在一通用实施例中,制备本发明的基于溶剂的胶粘剂组合物的方法包括例如步骤(1)提供异氰酸酯组分;(2)提供多元醇组分;(3)混合两种组分以形成树脂混合物;(4)在溶剂中稀释树脂混合物以形成按经稀释树脂混合物的总重量计,施加固体含量在一个实施例中为25wt%至55wt%,在另一实施例中为30wt%至45wt%,并且在再另一实施例中为35wt%至40wt%的经稀释树脂混合物;和(5)从组合物去除溶剂以形成胶粘剂组合物,随后将所述组合物施加于衬底上并随后固化组合物。
在固化树脂混合物之前,异氰酸酯组分与多元醇组分的混合比在一个实施例中为100:1至100:12,并且在另一实施例中为100:4至100:10。
由本发明的基于溶剂的胶粘剂组合物展现的一些有利特性包括例如(1)良好粘着性能;(2)快速固化;和(3)迁移到使用胶粘剂的封装体中所封装的食品中的(a)非所需芳胺(如MDA和TDA)量不存在,或(b)非所需芳胺(如MDA和TDA)含量较低。
举例来说,在杀菌测试之前胶粘剂的干燥粘结力在一个实施例中可大于500g/25mm,在另一实施例中为500g/25mm至2,500g/25mm,在再另一实施例中为700g/25mm至2000g/25mm并且在又另一实施例中为800g/25mm至1,800g/25mm。
举例来说,在121℃下的1小时杀菌测试之后的胶粘剂的粘结力在一个实施例中可大于200g/25mm,在另一实施例中为200g/25mm至2,500g/25mm,并且在再另一实施例中为300g/25mm至2,000g/25mm。粘结力可取决于所用膜衬底的类型,并且在一些实施例中,当测试衬底之后,在粘结之前发生失效模式时,膜可粘结。
胶粘剂的固化时间在一个实施例中可为1天至8天,在另一实施例中为1天至7天并且在再另一实施例中为2天至7天。
本文还公开一种使用本发明的胶粘剂组合物形成层压物的方法。在一些实施例中,胶粘剂组合物,如上文所论述的胶粘剂组合物在25℃下呈液态。即使组合物在25℃下为固体,视需要可接受加热组合物以将组合物转化成液态。溶剂添加到经混合的胶粘剂组合物中直到达到所需固体含量为止。一般来说,在一个实施例中使用50%或更大的固体含量。
本发明的胶粘剂组合物适用于将衬底粘结在一起;并且胶粘剂组合物可用于广泛多种单一适合的衬底或多个适合的衬底上。衬底可为类似材料或不同材料。举例来说,在一些实施例中,衬底可选自高、低或中等密度塑料(例如选自以下的类型:聚苯乙烯、聚乙烯、ABS、聚氨基甲酸酯、聚对苯二甲酸乙二酯、聚对苯二甲酸丁二酯、聚丙烯、聚苯、聚碳酸酯、聚丙烯酸酯、聚氯乙烯、聚砜和其混合物)、纸、木材和再造木材产品、经聚合物涂布的衬底、经蜡涂布的纸板、卡纸板、粒子板、纺织物、皮革和金属(例如铝、铁以及其它非铁金属)、金属化塑料(例如金属化塑料膜)等。
多个衬底层的湿式和干式粘结层压为可能的。胶粘剂组合物可使用常规施加技术施加于所需衬底,所述施加技术如轮转凹版印刷、弹性凸版印刷、常规或无空气喷涂、滚涂、刷涂、绕线棒涂、刮涂或,如幕涂、覆涂(flood-coating)、旋杯喷涂(bell-coating)、盘涂(disc-coating)和浸涂法的涂布方法。用胶粘剂组合物涂布衬底可在衬底的整个表面上或衬底的表面的一部分上进行,如沿边缘或在间断的位置。施加于衬底后,如通过施加热和空气流,或用于去除胶粘剂组合物中所存在的大体上所有剩余溶剂的一些其它适合常规方法来干燥胶粘剂组合物。
包含本发明的基于溶剂的胶粘剂组合物的层压物可通过以下而形成:将胶粘剂施加于两个不同衬底中的至少一个并将衬底组合在一起,以使得胶粘剂安置于两个衬底的表面之间;并且随后固化胶粘剂以在两个衬底之间形成粘结。衬底可包括例如两个单独的膜;并且所述膜中的每一个可由不同材料或相同材料制成。一般来说,将胶粘剂组合物的一层施加于膜表面。在一个实施例中,施加于膜表面的可固化胶粘剂组合物混合物的层的厚度为1微米(μm)至5μm。如本文所用,“膜”为在结构的一个维度中为0.5mm或更小;以及在结构的其它两个维度中均为1厘米(cm)或更长的任何结构。
在一些实施例中,使另一膜的表面与可固化混合物的层接触以形成未固化的层压物。可固化混合物随后经固化或使其固化。未固化的层压物可经受压力,例如通过穿过轧辊,其可经或可不经加热。可加热未固化的层压物以加速固化反应。
用于形成层压结构的适合衬底包括膜,如纸、编织和非编织物、聚合物膜、金属箔、经金属涂布的(金属化)聚合物膜和其组合。衬底经分层以形成层压结构,其中根据本发明的胶粘剂组合物将衬底中的一个或多个粘附在一起。膜可任选地具有在其上用油墨印刷图像的表面。油墨可与胶粘剂组合物接触。在一些实施例中,膜为聚合物膜和经金属涂布的聚合物膜,并且在一优选实施例中,膜为聚合物膜。“聚合物膜”为由聚合物或聚合物的混合物制成的膜。聚合物膜的组成通常为80wt%或更大的一种或多种聚合物。
胶粘剂组合物对于封装和密封应用尤其具有吸引力。举例来说,塑料膜、金属膜或金属化塑料膜可用本发明的胶粘剂组合物层压(例如在其整个表面或其表面的至少一部分上,如沿其边缘或在间断的位置)以形成层压物。在一个优选实施例中,使用层压物例如以形成由至少两层膜制成的小袋,其中胶粘剂粘结在两个膜层之间。在一些实施例中,食品可经封装用于蒸煮袋制备,或所得层压物可用于密封或封装一些其它制品。
实例
呈现以下实例以进一步详细说明本发明,但不应将其理解为限制权利要求书的范围。除非相反陈述、由上下文暗示或在本领域中惯用,否则所有份数和百分比均按重量计,并且截至本公开的申请日为止,所有测试方法均为现行的。
本发明实例(Inv.Ex.)和比较实例(Comp.Ex.)中所用的各种原材料或成分阐述于如下表I中:
表I-原材料
实例1和2以及比较实例A和B-胶粘剂
实例中所用的胶粘剂调配物的成分描述于表II中;并且胶粘剂调配物根据以下程序制备:
用于制备磷酸酯化合物的一般程序
在烘箱中干燥1升(L)多颈圆底烧瓶,用干燥氮气(N2)冲洗30分钟,随后馈入150克(g)VORANOLTM CP 450聚醚多元醇并置于70毫升/分钟(mL/min)的N2吹扫下。注射器装载有4g 115%聚磷酸20酸(PPA)。在激烈搅动下将PPA逐滴添加到聚醚多元醇中。观察到极小温度升高。将反应器内含物加热到100℃持续1小时,随后冷却到45℃。随后,将40g乙酸乙酯添加到反应器,随后缓慢添加50g ISONATETM 125M二异氰酸酯。通过施加冰批料控制显著放热以使反应罐保持低于75℃,并观察到由黄色25变成琥珀色。随后将反应器维持在65℃下1小时,此时将内含物冷却并封装。产物具有以下特性:76.0%固体,羟基数(OHN)为112mg KOH/g,酸值(AV)为19.0mg KOH/g,并且在25℃下粘度为1,665毫帕斯卡(millipascal)-秒(mPa·s)。
用于制备异氰酸酯组分(组分A)的一般程序
用于制备本发明实例1和本发明实例2的异氰酸酯反应性组分的相关成分描述于表II中。使用本发明实例1的异氰酸酯组分作为样品制备的典型实例,将约450g ADCOTETM577和约50g MOR-FREETM C33馈入玻璃反应器中。将反应器加热到约40℃并且所得混合物在40℃下搅拌约30分钟。随后,将所得样品混合物封装并置放于储存器中以供随后使用。
用于制备异氰酸酯反应性组分(组分B)的一般程序
用于制备本发明实例1和本发明实例2的异氰酸酯反应性组分的相关成分描述于表II中。使用实例1的异氰酸酯反应性组分作为样品制备的典型实例,将约400g VORANOLTMCP450、约40g POLYGTM 30-112和约360g磷酸酯化合物馈入玻璃反应器中。将反应器加热到约40℃并且所得混合物在40℃下搅拌约30分钟。随后,将所得样品混合物封装并置放于储存器中以供随后使用。
用于制备胶粘剂调配物的一般程序
用于制备包括异氰酸酯反应性组分、异氰酸酯组分和溶剂的胶粘剂调配物的相关成分描述于表II中。使用本发明实例1的胶粘剂作为胶粘剂调配物样品制备的典型实例,将约1,000g异氰酸酯组分(组分A)、约160g异氰酸酯反应性组分(组分B)和约1,460g乙酸乙酯装载于塑料容器中。使用机械混合器在室温(约25℃)下将材料混合30分钟,获得本发明实例1的调配胶粘剂。
表II-胶粘剂调配物
*“Ad”代表“胶粘剂”。
实例3和4以及比较实例C和D-层压物
用于制备层压物的一般程序
表III描述用于实例以使用以上表II中描述的胶粘剂制备层压物和层压物样品的各种膜。基于基于溶剂的胶粘剂的层压物在室温(约25℃)下经由诺德美克(Nordmeccanica)Labo Combi 400中试涂布机产生。在层压之前电晕处理聚合物膜,并在无电晕处理的情况下使用铝(Al)箔。每一层压物的涂布重量维持在约4.9克/平方米(g/m2)下。随后在受控环境中(例如在25℃和50%相对湿度下,在50℃下)固化所制备的层压物。
使用各膜制备各实例,所述膜包括“Prelam”,其为12μm(48规格)聚酯(“PET”)膜,以3.26g/m2(2.00lbs/令)层压于具有ADCOTETM/共反应物F的0.00035mil Al箔,可购自陶氏化学公司;和厚度为3mil(75μm)的浇铸聚丙烯(“CPP”)膜。
表III-膜层压物
*“Ad”代表“胶粘剂”。
膜的测试和测量方法
粘结强度测量
在切割成15mm宽并且1英寸(25.4mm)长条带的层压物样品上进行90°T剥离测试,并在配备有50牛顿(N)荷重计(loading cell)的Thwing AlbertTM QC-3A剥离测试仪上在1英寸(25.4mm)条带上以4英寸/分钟(101.6mm/min)的速率拉动。测试三个单独样品条带并对三个条带的结果值求平均值。当层压物中的两个膜经分离(剥离)时,记录在拉动期间力的平均值。如果膜中的一个拉伸或破裂,那么记录最大力或断裂时的力。根据以下名称记录失效模式(FM)或失效的模式(MOF):
“FS”代表“膜拉伸”。
“FT”表示“膜撕裂”(或断裂)。
“DL”代表“剥离”,其表示次膜与主膜分离。
“AT”代表“胶粘剂转移”,其表示胶粘剂不能粘附于主膜并且转移到次膜。
“AS”代表胶粘剂分开(或内聚失效),其表示在主膜和次膜两者上都发现有胶粘剂。
“MT”代表“金属转移”,其表示发生金属从金属化膜转移到次膜。
“PMT”代表“部分金属转移”。
在制得层压物的后尽快测试初始或“湿”粘结力。在以下所指示的时间间隔下进行额外T剥离测试。
固化时间
ATR用于监测箔//CPP结构中的本发明和比较胶粘剂的固化,并在异氰酸酯峰从ATR光谱消失时测定所用每一胶粘剂的固化时间。
用于制备小袋的一般程序
层压物由如上所述的Prelam//CPP制成。将9英寸×12英寸(23cm×30.5cm)的层压物薄片中的一个折叠,以得到约9英寸×6英寸(23cm×15.3cm)的双层,以使得一个层的CPP膜与另一层的CPP膜接触。在切纸机上修整折叠层压物的边缘,得到约5英寸×7英寸(12.7cm×17.8cm)的折叠片。将折叠片的两个长侧和一个短侧在边缘处热密封,得到内部尺寸为4英寸×6英寸(10.2cm×15.2cm)的成品小袋。热密封在400℉(204℃)下在40磅/平方英寸(psi)(276千帕斯卡[kPa])的液压下进行1秒(s)。针对每一测试制得两个或三个小袋。
小袋的测试和测量方法
杀菌性能测试
经由开口边缘用100毫升(mL)±5mL蒸馏水(DI水)或1:1:1酱(等重量份番茄酱、醋和植物油的掺合物)填充如上文所述制备的小袋。避免将填充物溅到热密封区域,因为这可能导致热密封在测试期间失效。在填充之后,以使小袋内部滞留的空气减到最少的方式将小袋顶部密封。检查小袋的所有四侧上的密封完整性以确保在密封时没有会导致小袋在测试期间泄漏的缺陷。丢弃并替换任何有缺陷的小袋。在一些情况下,标记层压物中的缺陷以鉴别在测试期间是否会产生新的额外缺陷。
随后将含有1:1:1酱的小袋置放于设定在121℃下的STERIS高压釜中1小时。在杀菌之后移出小袋并将开孔、起泡、脱层或漏泄的程度与经标记的先前存在的缺陷中的任一个进行比较。记录观察结果。将小袋切开,倒空,并用肥皂和水冲洗。从小袋切下一个或多个一英寸(2.54cm)条带,并根据上文所述的标准粘结强度测试来测量层压物粘结强度。其在去除小袋内含物之后尽快完成。目视检查小袋的内部并记录任何可见缺陷。
杀菌法规样品制备
由30.8平方英寸(in2)(198.7平方厘米(cm2)层压物组成的小袋各填充有100mL3%乙酸/样品。随后将小袋转移到杀菌釜腔室中,其中将小袋在121℃下储存2小时。在测试之后并且在冷却到环境温度后,将乙酸转移到聚乙烯瓶中。
提取乙酸样品并且制备以在制备数天内进行分析,并在制备24小时内经由液相色谱/质谱分析(LC/MS)进行分析。
对如上文所述制备的各种样品进行以上测试和测量程序。表IV描述此类样品的性能。
表IV-膜样品的性能
*“Ad”代表“胶粘剂”。
对于基于溶剂的胶粘剂,Inv.Ex.1和Inv.Ex.2展现良好耐化学性和耐温性。另外,Inv.Ex.1和Inv.Ex.2展现快速固化特性(例如在50℃下3天以固化)。Inv.Ex.1和Inv.Ex.2还展示低MDA含量(例如在50℃下仅固化3天之后,<20ppb)。
其它实施例
在一个实施例中,本发明包括一种基于溶剂的杀菌胶粘剂组合物,其包含:(A)至少一种异氰酸酯化合物,组分A,其中所述至少一种异氰酸酯化合物,组分A包含:以下物质的掺合物:(i)至少一种脂肪族类异氰酸酯和(ii)至少一种芳香族类异氰酸酯;和(B)至少一种异氰酸酯反应性组分,组分B,其中所述至少一种异氰酸酯反应性组分,组分B包含:(i)至少一种磷酸酯化合物和(ii)平均分子量小于1,500g/mol的至少一种聚醚多元醇。
在另一实施例中,至少一种脂肪族类异氰酸酯,胶粘剂的组分A的组分(i)选自由以下组成的组:基于二甲苯二异氰酸酯的聚异氰酸酯、基于1,4-或1,3-双(异氰酸酯基甲基)环己烷的聚异氰酸酯、二甲苯二异氰酸酯异氰尿酸酯、基于六亚甲基二异氰酸酯的聚异氰酸酯、基于二异氰酸酯基二环己基甲烷的聚异氰酸酯、六亚甲基二异氰酸酯异氰尿酸酯和其混合物。
在另一实施例中,至少一种芳香族类异氰酸酯,胶粘剂的组分A的组分(ii)选自由以下组成的组:1,3-和1,4-亚苯基二异氰酸酯、1,5-亚萘基二异氰酸酯、2,6-甲苯二异氰酸酯、2,4-甲苯二异氰酸酯、2,4'-二苯基甲烷二异氰酸酯、4,4'-二苯基甲烷二异氰酸酯、3,3'-二甲基-4,4'-联苯二异氰酸酯、聚合异氰酸酯和其混合物。
在另一实施例中,至少一种芳香族类异氰酸酯,胶粘剂的组分A的组分(ii)为包含(α)至少一种异氰酸酯化合物和(β)至少一种多元醇化合物的反应产物的异氰酸酯预聚物。并且在另一实施例中,至少一种异氰酸酯化合物,组分(α)选自由以下组成的组:芳香族聚异氰酸酯、脂肪族聚异氰酸酯、环脂肪族聚异氰酸酯和其混合物。并且在另一实施例中,多元醇化合物,组分(β﹞选自由以下组成的组:聚醚多元醇、聚酯多元醇、聚己内酯多元醇、聚丙烯酸酯、聚碳酸酯多元醇、基于天然油的多元醇和其混合物。
在另一实施例中,聚醚多元醇,组分(β)的分子量小于5,000g/mol。并且在另一实施例中,聚酯多元醇,组分(β)的分子量大于1,500g/mol。
在另一实施例中,不具有溶剂的至少一种异氰酸酯化合物,组分A的异氰酸酯含量为1重量%至25重量%。
在另一实施例中,至少一种磷酸酯化合物,胶粘剂的组分B的组分(i)选自由以下组成的组:具有以下结构(I)的磷酸酯化合物:
其中R1为有机基团,其中R1可或可不具有一个或多个额外侧接-OH基团,其中R1可或可不具有一个或多个结构(I)的额外侧基,并且其中所述-OH基团和结构(I)的一个或多个基团中的两个或更多个可或可不连接于R1的同一原子;含有氨基甲酸酯键的磷酸酯化合物;以及其混合物。并且在另一实施例中,至少一种磷酸酯化合物,胶粘剂的组分B的组分(i)的含量为0.1重量%至30重量%。
在另一实施例中,至少一种聚醚多元醇,胶粘剂的组分B的组分(ii)选自由以下组成的组:聚丙二醇、聚四亚甲基醚二醇、基于聚环氧丁烷的多元醇、其混合物和其共聚物。
在另一实施例中,至少一种异氰酸酯反应性组分,胶粘剂的组分B进一步包括(iii)平均分子量小于1,500g/mol的至少一种聚酯多元醇。
在另一实施例中,至少一种聚酯多元醇,胶粘剂的组分B的组分(iii)选自由以下组成的组:脂肪族聚酯多元醇、芳香族聚酯多元醇、脂肪族聚酯多元醇和芳香族聚酯多元醇的共聚物、聚碳酸酯多元醇、聚己内酯多元醇和其混合物。
在另一实施例中,至少一种聚酯多元醇,胶粘剂的组分B的组分(iii)为:(1)多元酸与多元醇的反应产物,(2)光气或碳酸酯单体与多元醇的反应产物;或(3)经由环酯化合物的开环聚合产生。
在另一实施例中,本发明的胶粘剂进一步包含:(C)选自由以下组成的组的溶剂:乙酸乙酯、甲基醚酮、甲苯和其混合物。
在另一实施例中,本发明的胶粘剂进一步包含:(D)选自由以下组成的组的添加剂:催化剂、表面活性剂、调平剂、消泡剂、流变改质剂、有色颜料和其混合物。
Claims (10)
1.一种基于溶剂的杀菌胶粘剂组合物,其包含:
(A)至少一种异氰酸酯化合物,组分A,其包含:以下物质的掺合物:(i)至少一种脂肪族类异氰酸酯和(ii)至少一种芳香族类异氰酸酯;和
(B)至少一种异氰酸酯反应性组分,组分B,其包含:(i)至少一种磷酸酯化合物和(ii)平均分子量小于1,500g/mol的至少一种聚醚多元醇。
2.根据权利要求1所述的胶粘剂,其中所述至少一种芳香族类异氰酸酯,组分A的组分(ii)为包含以下的反应产物的异氰酸酯预聚物:(α)至少一种异氰酸酯化合物和(β)至少一种多元醇化合物。
4.根据权利要求1所述的胶粘剂,其中所述至少一种聚醚多元醇,组分B的组分(ii)选自由以下组成的组:聚丙二醇、聚四亚甲基醚二醇、基于聚环氧丁烷的多元醇、其混合物和其共聚物。
5.根据权利要求1所述的胶粘剂,其中所述至少一种异氰酸酯反应性组分,组分B进一步包括(iii)平均分子量小于1,500g/mol的至少一种聚酯多元醇。
6.根据权利要求1所述的胶粘剂,其中所述至少一种聚酯多元醇,组分B的组分(iii)选自由以下组成的组:脂肪族聚酯多元醇、芳香族聚酯多元醇、脂肪族聚酯多元醇与芳香族聚酯多元醇的共聚物、聚碳酸酯多元醇、聚己内酯多元醇和其混合物。
7.一种用于产生基于溶剂的聚氨基甲酸酯杀菌胶粘剂组合物以用于产生层压物的方法,其包含掺合:
(A)至少一种异氰酸酯化合物;组分A,其包含:以下物质的掺合物:(i)至少一种脂肪族类异氰酸酯和(ii)至少一种芳香族类异氰酸酯;和
(B)至少一种异氰酸酯反应性组分,组分B,其包含:(i)至少一种磷酸酯化合物和(ii)至少一种多元醇,其包含平均分子量小于1,500g/mol的至少一种聚醚多元醇。
8.一种多层层压品,其包含:
(a)至少第一层;
(b)至少第二层;和
(c)安置于所述第一层与所述第二层之间的根据权利要求1所述的杀菌胶粘剂;其中所述胶粘剂经固化以将所述第一层粘结于所述第二层。
9.一种用于产生层压品的方法,其包含以下步骤:
(I)将根据权利要求1所述的杀菌胶粘剂施加于所述第一层和/或所述第二层的表面的至少一部分;
(II)接触所述第一层和所述第二层使得所述胶粘剂安置于所述第一层与所述第二层之间;和
(III)固化所述胶粘剂以形成层压物,其包含经由所述固化胶粘剂粘结于所述第二层的所述第一层。
10.一种用于杀菌封装的容器,其包含根据权利要求8所述的层压物。
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