CN108473820B - 单组分层压胶粘剂用于复合膜层压的用途 - Google Patents
单组分层压胶粘剂用于复合膜层压的用途 Download PDFInfo
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- CN108473820B CN108473820B CN201780007024.1A CN201780007024A CN108473820B CN 108473820 B CN108473820 B CN 108473820B CN 201780007024 A CN201780007024 A CN 201780007024A CN 108473820 B CN108473820 B CN 108473820B
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/10—Homopolymers or copolymers of methacrylic acid esters
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
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- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- B32B15/085—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin comprising polyolefins
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- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
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- B32B15/088—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin comprising polyamides
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- B32B23/04—Layered products comprising a layer of cellulosic plastic substances, i.e. substances obtained by chemical modification of cellulose, e.g. cellulose ethers, cellulose esters, viscose comprising such cellulosic plastic substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
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- B32B23/04—Layered products comprising a layer of cellulosic plastic substances, i.e. substances obtained by chemical modification of cellulose, e.g. cellulose ethers, cellulose esters, viscose comprising such cellulosic plastic substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B23/042—Layered products comprising a layer of cellulosic plastic substances, i.e. substances obtained by chemical modification of cellulose, e.g. cellulose ethers, cellulose esters, viscose comprising such cellulosic plastic substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material of metal
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Abstract
本发明涉及单组分层压胶粘剂用于复合膜层压的用途，以及涉及一种用于复合膜层压的方法。该层压胶粘剂包含水性聚合物分散体，所述水性聚合物分散体可通过单体的自由基乳液聚合来制备，所述单体包含a)相对于单体的总量计，至少60重量％的至少一种选自以下的单体：丙烯酸C1至C20烷基酯、甲基丙烯酸C1至C20烷基酯、含有至多20个碳原子的羧酸的乙烯基酯、具有至多20个碳原子的乙烯基芳族化合物、乙烯基卤化物、含有至多10个碳原子的醇的乙烯基醚、具有2至8碳原子和一或两个双键的脂族烃，以及所述单体的混合物；和b)相对于单体的总量计，至少0.1重量％的至少一种具有至少一个酸基团的单体；和c)相对于单体的总量计，0.1至5重量％的至少一种具有至少一个选自酮基和醛基的官能团的烯键式不饱和化合物，其中水性聚合物分散体包含至少一种具有至少两个能与酮基或与醛基进行交联反应的官能团的化合物A；其中化合物A的对酮基或醛基呈反应性的基团与单体b)的酮基和醛基的摩尔比的值为1:10至2:1；并且其中对于复合膜层压，至少两个膜使用层压胶粘剂牢固地彼此粘着，以使得剥离强度为2.5N/15mm或更大，或者粘结在一起的膜仅可通过破坏至少一个膜才能分离。所述复合膜可以用于食品包装。
Description
本发明涉及特定的单组分层压胶粘剂用于复合膜层压的用途，以及涉及一种用于复合膜层压的方法。复合膜可特别有利地用于食品的包装。
例如，对用于柔性食品包装的具有良好的性能特性的复合膜层压，非常需要成本有效的胶粘剂。在该应用中广泛应用的是基于有机溶剂的胶粘剂体系。为了减少有机溶剂排放，水基胶粘剂体系代表了一种选择。丙烯酸酯聚合物分散体，也称为丙烯酸酯乳液具有特别重要的意义。基于丙烯酸酯的胶粘剂记载在例如WO 98/23656和在WO 00/50480中。
有许多应用需要所使用的胶粘剂高度耐热，例如用于热扩散操作的膜层压制品或者用于可灭菌或可巴氏杀菌的食品包装。此外，许多层压制品需要对以下化学品具有高耐受性的胶粘剂：源自与胶粘剂直接接触的印刷油墨的化学品，或可由包装的内容物迁移通过内膜进入胶粘剂的化学品。在使用水性胶粘剂时，目前通常通过将外部化学交联剂引入分散体来产生这些耐热和耐化学品的要求。此处，特别使用水可乳化的异氰酸酯。此类双组分胶粘剂体系通常具有适用期有限，必须在适用期内加工胶粘剂的缺点。适用期通常为1小时至10小时。如果超过该适用期，则存在在胶粘剂中形成凝结物的风险和粘度增加的风险，这可能导致胶粘剂在膜载体上产生工业涂层时出现问题。此外，关于这类双组分胶粘剂，还存在在混合期间发生混合错误，反而影响胶粘剂的适当交联的危险。
作为对从水性环境施用到烯烃表面的胶粘剂层的粘着性的改进，从EP148386已知将二酰肼组分加入到分散体中。WO 2006/066761记载了酮官能化或醛官能化的乳液聚合物，其在成膜期间与存在于分散体液体中的第二组分发生交联反应，并且被用于自-粘着、易剥离的柔性-PVC膜。其中记载的乳液聚合物被用作压敏胶粘剂(PSAs)并且特征在于具有相当高的膜粘性。膜粘性可以以环形粘性的形式来描述。钢上的环形粘性通常远高于1.7N/25mm并且可最高达10N/25mm。用于复合膜层压中的层压胶粘剂和分散体不是压敏胶粘剂，并且仅具有非常小的粘性或没有粘性，特别地，在钢上具有优选小于1.7N/25mm的环形粘性。
本发明的目的是提供一种用于复合膜层压的单组分水性层压胶粘剂，其具有用于这些应用的常规双组分水性胶粘剂所达到的耐热性和耐化学性，并且产生了不易于再彼此移动的固态膜复合材料。
已发现，该目的可通过使用在下文中更详细阐述的层压胶粘剂而实现。本发明的主题是单组分层压胶粘剂用于复合膜层压的用途，
其中，层压胶粘剂以水性聚合物分散体的形式存在，并且水性聚合物分散体包含可通过单体的自由基乳液聚合制备的分散在水中的聚合物颗粒，所述单体包含
a)基于单体的总量计，至少60重量％的至少一种选自以下的单体：丙烯酸C1至C20烷基酯、甲基丙烯酸C1至C20烷基酯、含有至多20个碳原子的羧酸的乙烯基酯、具有至多20个碳原子的乙烯基芳族化合物、乙烯基卤化物、含有1至10个碳原子的醇的乙烯基醚、具有2至8碳原子和一或两个双键的脂族烃，以及这些单体的混合物，和
b)基于单体的总量计，至少0.1重量％的至少一种具有至少一个酸基团的单体，和
c)基于单体的总量计，0.1至5重量％、优选0.5至5重量％的至少一种具有至少一个选自酮基和醛基的官能团的烯键式不饱和化合物；
其中，水性聚合物分散体包含至少一种具有至少两个能与酮基或与醛基发生交联反应的官能团的化合物A；
其中，化合物A的对酮基或醛基呈反应性的基团与单体c)的酮基和醛基的摩尔比为1:10至2:1；
其中，在复合膜层压中，至少两个膜用层压胶粘剂牢固地彼此粘合，以使得剥离强度为2.5N/15mm或更大，或3N/15mm或更大，或者彼此粘合的膜仅可通过破坏至少一个膜才能分离。
本发明的水性聚合物分散体还包含这样一种化合物，即其含有至少两个能与酮基或醛基发生交联反应的官能团。为了最佳交联，选择该第二组分的量，使得第二组分的一个分子与第一组分的两个酮基或醛基官能团构成桥连化合物。
本发明的另一主题是一种通过使用单组分、非自粘着层压胶粘剂或使用水性聚合物分散体，优选施加压力和高温将至少两个膜彼此粘合来制备复合膜的方法。
本发明的另一主题是根据本发明可获得的复合膜用于食品包装、优选软包装的用途。
本发明的另一主题是水性聚合物分散体作为胶粘剂、更特别是作为层压胶粘剂用于制备例如食品包装的复合膜的用途。
本发明的另一主题是一种复合膜，其具有第一膜和至少一个第二膜，它们使用本文中所述的层压胶粘剂彼此粘合并且包含用于本发明的水性聚合物分散体。
下文偶尔使用命名“(甲基)丙烯酸……”和类似命名作为“丙烯酸……或甲基丙烯酸……”的缩写表示。在命名(甲基)丙烯酸Cx烷基酯和类似命名中，x表示烷基的碳原子的数目。
玻璃化转变温度可通过差示扫描量热法(ASTM D 3418-08，中点温度)测定。聚合物分散体中的聚合物的玻璃化转变温度是评估第二条加热曲线(加热速率20℃/min)时获得的玻璃化转变温度。
单组分胶粘剂是在其即将使用之前不添加外部交联剂(例如异氰酸酯交联剂)的胶粘剂。在复合膜制备的情况下，优选也没有UV交联，并且层压胶粘剂优选不包含可UV-交联的组分。
层压胶粘剂优选不是自粘着的。非自粘着胶粘剂是这样的胶粘剂，其与压敏胶粘剂相比，在室温下显示仅非常小的粘性，或无粘性，并且优选施加压力和/或高温来使用。粘性，测量为环形粘性，优选小于1.7N/25mm(胶粘剂以20μm的施用厚度，施用于12μm厚的聚酯膜，在钢上在室温(20℃)下以300mm/min的移动速度测量)。
根据本发明使用的聚合物分散体可通过烯键式不饱和的、可自由基聚合的化合物的自由基乳液聚合获得。
该聚合优选在没有乳化剂或有少许乳化剂的情况下进行以稳定本发明的聚合物分散体，就少许乳化剂而言，每100重量份单体加入小于1重量份的乳化剂，或小于0.8、优选小于或等于0.5重量份的乳化剂。乳化剂是在聚合之前或之后添加到聚合混合物中的非聚合两亲性表面活性物质。在本上下文中，例如源自使用乳化剂-稳定的聚合物种子的少量乳化剂是没有损害的。还可能的是，总共使用小于0.3重量份或小于0.2重量份的乳化剂，例如0.05至小于1重量份，0.05至小于0.8重量份，0.05至0.5重量份，或0.05至0.3重量份，基于100重量份的单体计，或没有乳化剂。
合适的保护胶体的综合性描述见于Houben-Weyl，Methoden der organischenChemie，卷XIV/1，Makromolekulare Stoffe，Georg-Thieme-Verlag，Stuttgart，1961，第411至420页。考虑的乳化剂包括阴离子、阳离子和非离子乳化剂。优选用作表面活性物质的是这样的乳化剂，与保护胶体相比，其分子量通常低于2000g/mol。在使用表面活性物质的混合物的情况下，单个组分当然必须彼此兼容，在有疑问时可通过一些预备试验来检验。优选使用阴离子和非离子乳化剂作为表面活性物质。常规的乳化剂是，例如，乙氧基化脂肪醇(EO水平：3至50，烷基：C8至C36)、乙氧基化的单-、二-和三烷基酚(EO水平：3至50，烷基：C4至C9)、磺基琥珀酸二烷基酯的碱金属盐，以及烷基硫酸酯的碱金属盐和铵盐(烷基：C8至C12)、乙氧基化烷醇的碱金属盐和铵盐(EO水平：4至30，烷基:C12至C18)、乙氧基化烷基酚的碱金属盐和铵盐(EO水平：3至50，烷基:C4至C9)、烷基磺酸的碱金属盐和铵盐(烷基：C12至C18)和烷基芳基磺酸的碱金属盐和铵盐(烷基：C9至C18)。
其他合适的乳化剂为以下通式的化合物
其中R5和R6是氢或C4至C14烷基，并且不同时为氢，并且X和Y可以是碱金属离子和/或铵离子。优选R5和R6是具有6至18个碳原子的直链或支链的烷基，或者是氢，特别地，它们具有6、12和16个碳原子，其中R5和R6不同时为氢。X和Y优选为钠离子、钾离子或铵离子，其中特别优选钠。特别有利的化合物是这样的化合物，其中X和Y是钠，R5是具有12个碳原子的支链烷基，R6是氢或R5。通常使用含有50至90重量％分数的单烷基化产物的工业混合物。合适的乳化剂的商业产品为例如
2A1、
NP 50、
OC50、Emulgator 825、Emulgator 825S、
OG、
NSO、
904S、
I-RA、
E 3065、
FES 77、
AT 18、
VSL、
NPS 25。对于本发明，优选离子乳化剂或保护胶体。特别优选离子乳化剂，尤其是盐和酸，例如羧酸、磺酸和硫酸、磺酸盐或羧酸盐。特别地，也可以使用离子和非离子乳化剂的混合物。
聚合也可以在保护胶体的存在下进行。保护胶体是在溶剂化时结合大量的水并能够稳定水不溶性聚合物分散体的聚合物。与乳化剂相比，保护胶体通常不降低聚合物颗粒和水之间的界面张力。保护胶体的数均分子量位于例如1000g/mol以上。
单体a)
单体混合物包含基于单体的总量计至少60重量％、优选至少80重量％(例如60至99.8重量％或80至98重量％)、更优选至少90重量％的至少一种单体a)，所述单体a)选自丙烯酸C1至C20烷基酯、甲基丙烯酸C1至C20烷基酯、含有至多20个碳原子的羧酸的乙烯基酯、具有至多20个碳原子的乙烯基芳族化合物、乙烯基卤化物、含有1至10个碳原子的醇的乙烯基醚、具有2至8碳原子和一或两个双键的脂族烃，以及这些单体的混合物。
合适的单体a)为，例如，具有C1-C10烷基的(甲基)丙烯酸烷基酯，例如甲基丙烯酸甲酯、丙烯酸甲酯、丙烯酸正丁酯、丙烯酸乙酯和丙烯酸2-乙基己基酯，以及(甲基)丙烯酸山嵛酯、丙烯酸异丁酯、(甲基)丙烯酸叔丁酯和(甲基)丙烯酸环己酯。特别地，(甲基)丙烯酸烷基酯的混合物也是合适的。具有1至20个碳原子的羧酸的乙烯基酯为，例如，月桂酸乙烯酯、硬脂酸乙烯酯、丙酸乙烯酯、烷烃羧酸(Versatic acid)乙烯酯和丙烯酸乙烯酯。有用的乙烯基芳族化合物包括乙烯基甲苯、α-甲基苯乙烯和对-甲基苯乙烯、α-丁基苯乙烯、4-正丁基苯乙烯、4-正癸基苯乙烯，并且优选苯乙烯。乙烯基卤化物是被氯、氟或溴取代的烯键式不饱和化合物，优选氯乙烯和偏二氯乙烯。可提及的乙烯基醚的实例为乙烯基甲基醚或乙烯基异丁基醚。优选含有1至4个碳原子的醇的乙烯基醚。具有4至8个碳原子和两个烯烃双键的烃包括丁二烯、异戊二烯和氯丁二烯。作为单体a)，优选丙烯酸C1至C10烷基酯和甲基丙烯酸C1至C10烷基酯，更特别是丙烯酸C1至C8烷基酯和甲基丙烯酸C1至C8烷基酯，和苯乙烯，以及它们的混合物。特别优选丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸乙酯、丙烯酸正丁酯、甲基丙烯酸正丁酯、丙烯酸正己酯、丙烯酸辛酯、丙烯酸2-乙基己基酯、丙烯酸2-丙基庚基酯、苯乙烯，以及这些单体的混合物。
单体b)
单体混合物包含基于单体的总量计至少0.1重量％、更特别是0.1至5重量％或0.5至3重量％的至少一种具有至少一个酸基团的烯键式不饱和单体(酸单体)。该酸单体b)包含含有至少一个酸基团的单体，和其酸酐及其盐。单体b)包含α,β-单烯键式不饱和单羧酸和二羧酸、α,β-单烯键式不饱和二羧酸的单酯、上述α,β-单烯键式不饱和羧酸的酸酐，以及烯键式不饱和磺酸、膦酸或磷酸二氢盐以及它们的水溶性盐，例如它们的碱金属盐。其实例为丙烯酸、甲基丙烯酸、衣康酸、马来酸、富马酸、巴豆酸、乙烯基乙酸和乙烯基乳酸。合适的烯键式不饱和磺酸的实例包括乙烯基磺酸、苯乙烯磺酸、丙烯酰胺甲基丙磺酸、丙烯酸磺丙酯和甲基丙烯酸磺丙酯。优选的单体b)是α,β-单烯键式不饱和C3-C8羧酸和C4-C8二羧酸，例如，衣康酸、巴豆酸、乙烯基乙酸、丙烯酰胺基乙醇酸、丙烯酸和甲基丙烯酸，以及它们的酸酐。特别优选的单体b)是衣康酸、丙烯酸和甲基丙烯酸，以及它们的混合物。
单体c)
在本发明中，聚合物分散体含有酮基或醛基。该酮基或醛基可通过合适的单体c)的共聚合而键合至聚合物。单体混合物包含至少0.1重量％程度、或至少0.2重量％(例如0.1至5重量％，或0.2至5重量％)的具有至少一个选自酮基和醛基的官能团的烯键式不饱和单体。
单体c)的实例是丙烯醛；甲基丙烯醛；在烷基中具有1至20、优选1至10个碳原子的乙烯基烷基酮；甲酰苯乙烯；在烷基中具有一或两个酮基或一或两个醛基，或一个醛基和一个酮基的(甲基)丙烯酸烷基酯，其中烷基优选含有总共3至10个碳原子，实例为如例如DE-A2 722 097中所记载的(甲基)丙烯酰氧基烷基丙醛。此外，还合适的是例如由DE-A 2 061213或DE-A 2 207 209已知的那类N-氧代烷基(甲基)丙烯酰胺，实例为式R-C(＝O)-R’-NH-C(＝O)-CR”＝CH2的那些，其中R和R”彼此独立地为氢或具有1至10个碳原子的烃基(优选烷基)，并且R’是具有2至15个碳原子的烃基(优选亚烷基)。特别优选乙酰乙酰基(甲基)丙烯酸酯、(甲基)丙烯酸乙酰乙酰氧基乙酯，特别是双丙酮丙烯酰胺。
单体d)
单体混合物任选地包含至少一种另外的单体d)，其不同于单体a)至c)。单体d)用量可以是例如0至10重量％或0至5重量％，更特别是0.1至10重量％或0.1至5重量％或0.2至3重量％，基于单体的总量计。
单体d)是，例如，在水中具有增加的溶解性的中性单体和/或非离子单体，实例为上述羧酸的酰胺或N-羟烷基酰胺，例如丙烯酰胺、甲基丙烯酰胺、N-羟甲基丙烯酰胺和N-羟甲基甲基丙烯酰胺，或苯氧基乙基乙二醇单(甲基)丙烯酸酯。其他单体d)还有，例如，含有羟基的单体，更特别是上述α,β-单烯键式不饱和羧酸的羟烷基酯，优选(甲基)丙烯酸C1-C10羟烷基酯，例如，丙烯酸羟乙酯、甲基丙烯酸羟乙酯、丙烯酸羟丙酯或甲基丙烯酸羟丙酯，以及丙烯酸4-羟丁基酯。其他单体d)还有，例如，含有氨基的单体，更特别是上述α,β-单烯键式不饱和羧酸的氨基烷基酯，优选(甲基)丙烯酸C1-C10氨基烷基酯，例如，(甲基)丙烯酸2-氨基乙基酯或甲基丙烯酸叔丁基氨基乙基酯。作为单体d)，另外考虑的是α,β-单烯键式不饱和C3-C8羧酸的腈，例如丙烯腈或甲基丙烯腈。其他合适的单体d)是除烯键式不饱和双键外还具有至少一个缩水甘油基、噁唑啉基、脲基或类似脲的基团的双官能单体。缩水甘油基单体的实例为烯键式不饱和缩水甘油醚和缩水甘油酯，例如，乙烯基缩水甘油醚、烯丙基缩水甘油醚和甲代烯丙基缩水甘油醚，以及(甲基)丙烯酸缩水甘油酯。单体d)的实例还有具有多于一个可自由基聚合的基团，更特别是两个或更多个(甲基)丙烯酸酯基团的交联单体，例如二(甲基)丙烯酸丁二醇酯或甲基丙烯酸烯丙酯。特别优选的单体d)是在烷基中具有1至10个碳原子的(甲基)丙烯酸羟烷基酯。
化合物A
用于本发明的分散体还包含至少一种具有至少2个官能团、更特别是2至5个官能团的化合物A，所述官能团与酮基或醛基发生交联反应。能够与酮基或醛基发生交联反应的化合物的实例是具有酰肼基团、羟胺基团、肟醚基团或氨基基团的化合物。具有酰肼基团的合适的化合物是，例如，具有优选至多500g/mol的摩尔重量的多羧酸酰肼。优选的酰肼化合物是具有优选2至10个碳原子的二羧基二酰肼。实例包括草酸二酰肼、丙二酸二酰肼、琥珀酸二酰肼、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、衣康酸二酰肼和/或间苯二甲酸二酰肼。特别优选己二酸二酰肼、癸二酸二酰肼和间苯二甲酸二酰肼。具有氨基的合适的化合物的实例是乙二胺、丙二胺、四亚甲基二胺、五亚甲基二胺、六亚甲基二胺、二亚乙基三胺、三亚乙基四胺、聚乙烯亚胺、部分水解的聚乙烯基甲酰胺、环氧乙烷和环氧丙烷加合物如“Jeffamines”、环己烷二胺和苯二甲胺。具有所述官能团的化合物可以在任何时间点添加至组合物，或添加至聚合物分散体。在水性分散体中，尚不存在与酮基或醛基的交联。交联仅在干燥过程中在涂布的衬底上发生。
优选地，化合物A是己二酸二酰肼，并且单体c)是双丙酮丙烯酰胺。
具有所述官能团的化合物的量优选使得对酮基和/或醛基呈反应性的官能团与聚合物的酮基和/或醛基的摩尔比为1:10至2:1，更特别为1:5至2:1，更优选为1:2至2:1，且非常优选为1:1.3至1.3:1。特别优选等摩尔量的官能团和酮基和/或醛基。
优选地，用于本发明的聚合物分散体的聚合物颗粒是由包含以下的单体制备：
a)基于单体的总量计，90至99.4重量％或90至98重量％的至少一种选自以下的单体：丙烯酸C1至C8烷基酯、甲基丙烯酸C1至C8烷基酯和苯乙烯，以及这些单体的混合物，和
b)基于单体的总量计，0.5至3重量％的至少一种选自丙烯酸、甲基丙烯酸和衣康酸的单体，和
c)基于单体的总量计，0.1至5重量％的至少一种具有至少一个酮基的烯键式不饱和化合物，其选自(甲基)丙烯酸乙酰乙酰基酯、(甲基)丙烯酸乙酰乙酰氧基乙酯和双丙酮丙烯酰胺；
d)基于单体的总量计，0至5重量％的不同于单体a)至c)的其他单体，其选自丙烯酰胺、甲基丙烯酰胺、N-羟甲基丙烯酰胺和N-羟甲基甲基丙烯酰胺、单(甲基)丙烯酸苯氧基乙基乙二醇酯、含有羟基的单体、含有氨基的单体、α,β-单烯键式不饱和C3-C8羧酸的腈，除烯键式不饱和双键外还具有至少一个缩水甘油基、噁唑啉基、脲基或类似脲基的基团的双官能单体，以及具有多于一个可自由基聚合的基团的交联单体，
并且其中化合物A是具有2至10个碳原子的二羧基二酰肼。
优选这样选择聚合的单体，使得玻璃化转变温度范围为-40℃至+15℃，更特别是-35℃至+10℃或-10℃至+10℃。根据本发明，通过有目的地改变单体类型和数量，本领域技术人员能够制备聚合物具有所需范围的玻璃化转变温度的水性聚合物组合物。可借助Fox方程指引。根据Fox(T.G.Fox，Bull.Am.Phys.Soc.1956[Ser.II]1，第123页；以及根据Ullmann's 
der technischen Chemie，卷19，第18页，第4版，VerlagChemie，Weinheim，1980)，共聚物的玻璃化转变温度通过以下方式良好近似地计算：
1/Tg＝x1/Tg 1+x2/Tg 2+....xn/Tg n，
其中x1、x2....xn是单体1、2....n的质量分数，Tg 1、Tg 2....Tg n是一次仅由单体1、2....n之一合成的聚合物的玻璃化转变温度(以开尔文为单位)。多数单体的均聚物的Tg值是已知的，并且列于例如Ullmann's Encyclopedia of Industrial Chemistry，卷A21，第5版，第169页，VCH Weinheim，1992中；均聚物的玻璃化转变温度的其他来源为，例如，J.Brandrup，E.H.Immergut，Polymer Handbook，第1版；J.Wiley，New York 1966，第2版；J.Wiley，New York 1975，第3版；J.Wiley，New York 1989。
在本发明的一个实施方案中，聚合使用至少一种链转移剂来进行。以此方式，可通过链终止反应降低乳液聚合物的摩尔质量。在此过程中，链转移剂与聚合物键合，通常键合至链端。链转移剂的量特别是每100重量份待聚合的单体0.05至4重量份，更优选0.05至0.8重量份，且非常优选0.1至0.6重量份。合适的链转移剂为，例如，具有巯基的化合物，例如叔丁基硫醇、巯基乙醇酸乙基己酯、巯基乙醇、巯基丙基三甲氧基硅烷或叔十二烷基硫醇。链转移剂通常为低分子量化合物，即分子量小于2000、更特别小于1000g/mol。优选巯基乙酸2-乙基己基酯(EHTG)、异辛基3-巯基丙酸酯(IOMPA)和叔十二烷基硫醇(tDMK)。
聚合优选在晶种控制下，即在聚合物晶种的存在下进行(晶种胶乳)。晶种胶乳是平均粒径为优选20至40nm的细分聚合物颗粒的水性分散体。晶种胶乳的用量为每100重量份的单体优选0.01至0.5重量份，更优选0.03至0.3重量份。例如基于聚苯乙烯或基于聚甲基丙烯酸甲酯的胶乳是合适的。优选的晶种胶乳是聚苯乙烯晶种。
本发明的聚合物分散体通过乳液聚合制备。乳液聚合包括在水中使用常规的离子和/或非离子乳化剂和/或保护胶体或稳定剂作为表面活性化合物来稳定单体液滴，并随后由单体形成的聚合物颗粒来使烯键式不饱和化合物(单体)聚合。然而，优选地，聚合在具有少许乳化剂并且不添加或形成保护胶体的情况下进行。所得聚合物分散体可通过特定方式来稳定。该方式基于在非常少量的聚合物晶种存在下(晶种控制)慢的初始单体进料，随后将在聚合期间或之后使用的酸单体中和。
聚合物中的酸基团优选通过在聚合期间或之后加入中和剂来中和，其中酸基团通过加入碱被全部或部分中和。中和剂可以例如在与单体混合物进料平行的单独进料中加入。在所有单体进料之后，聚合容器优选包含中和至少10％且优选10％至100％或25％至90％酸当量所需量的中和剂。特别优选的中和剂是氨。
乳液聚合可使用水溶性引发剂来引发。水溶性引发剂的实例是过二硫酸的铵盐和碱金属盐，例如过二硫酸钠；过氧化氢；或有机过氧化物，例如叔丁基氢过氧化物。还适合作为引发剂的是还原-氧化(氧化还原)引发剂体系。氧化还原引发剂体系由至少一种通常的无机还原剂和一种无机或有机氧化剂组成。氧化组分是，例如上文已经提及的乳液聚合引发剂。还原组分是，例如亚硫酸的碱金属盐，如亚硫酸钠、亚硫酸氢钠；焦亚硫酸的碱金属盐，例如焦亚硫酸钠；脂族醛和酮的亚硫酸氢盐加合化合物，例如丙酮亚硫酸氢盐；或还原剂，例如羟基甲烷亚磺酸和其盐；或抗坏血酸。氧化还原引发剂体系可与其金属组分能够以多种价态存在的可溶性金属化合物一起使用。常规的氧化还原引发剂体系为，例如抗坏血酸/硫酸亚铁(II)/过二硫酸钠、叔丁基氢过氧化物/焦亚硫酸钠、叔丁基氢过氧化物/羟基甲烷亚磺酸钠。各组分，如还原组分，也可为混合物，例如羟基甲烷亚磺酸的钠盐和焦亚硫酸钠的混合物。
所述引发剂通常以水溶液的形式使用，其浓度下限由分散体中可接受的水量确定，上限由特定化合物在水中的溶解度确定。引发剂的浓度通常为0.1-30重量％、优选0.5-20重量％且更优选1.0-10重量％，基于待聚合的单体计。在乳液聚合中也可使用两种或更多种不同的引发剂。
乳液聚合优选在30至130℃、优选50至90℃下进行。聚合介质可仅由水组成或者由水和与水混溶的液体(例如甲醇、乙醇或四氢呋喃)的混合物组成。优选仅使用水。乳液聚合可以以进料方法的形式进行，包括分阶段或梯度的方式。在聚合中，可以开始就引入聚合物晶种，以便更有效地构建粒度。
在自由基水乳液聚合的过程中，将引发剂加入到聚合容器中的方式是本领域普通技术人员已知的。其可以全部包括在聚合容器的初始进料中，或者连续地或以分阶段的方式以其在自由基水乳液聚合过程中消耗的速率使用。这具体取决于引发剂体系的化学性质和聚合温度。优选初始加入一部分并将剩余的以其消耗的速率进料至聚合区。为了除去残余单体，通常在乳液聚合结束之后，即在单体转化至少95％之后，适当地再加入引发剂。在进料过程中，各组分可以从上面、侧面或下面通过反应器基板加入到反应器中。
乳液聚合通常提供固含量为15至75重量％、优选40至60重量％且更优选不少于50重量％的聚合物的水性分散体。
优选将聚合物分散体的pH调节至pH大于5，更特别至pH在5.5至8之间。
本发明的聚合物分散体可用在用于制备例如层压体的水性胶粘剂的制备中，即用在用于粘合大表面积的衬底、更特别是用于制备复合膜的水性层压胶粘剂的制备中。
本发明还涉及一种通过使用上述单组分层压胶粘剂将至少两个膜彼此粘合来制备复合膜的方法。
在该方法中，水性聚合物分散体可以其本身使用或者以与常规助剂配制后使用。常规助剂的实例是润湿剂、增稠剂、光稳定剂、杀菌剂、消泡剂等。
在制备复合膜的方法中，使用水性聚合物分散体将至少两个膜彼此粘合。在该方法中，本发明的聚合物分散体或适当配制的制剂通过例如刮涂、铺展等施用于待粘合的大表面积的衬底上，优选层厚度为0.1至20g/m2，更优选1至7g/m2。可采用常规的涂布技术，例如辊涂、反向辊涂、凹版辊涂、反向凹版辊涂、刷涂、棒涂、喷涂、喷枪涂布、凹面涂布、幕帘式涂布或浸涂。在蒸发掉分散体的水一段短时间后(优选1-60秒后)，即可将经涂布的衬底层压至第二衬底，温度可为例如20至200℃，优选20至100℃，压力可为例如100至3000kN/m2，优选300至2000kN/m2。
在本发明的复合膜层压中，用层压胶粘剂将至少两个膜彼此粘合，优选地使得剥离强度(24h后，在23℃下/50％相对湿度)优选为2.5N/15mm或更大或者3N/15mm或更大，或者彼此粘合的膜仅可通过破坏至少一个膜而分离。
本发明的聚合物分散体被用作单组分组合物，即不含额外的交联剂，更特别地不含异氰酸酯交联剂。至少一个膜可以金属化或印刷在涂有胶粘剂的一侧。合适的衬底的实例包括聚合物膜，更特别是聚乙烯(PE)、定向聚丙烯(OPP)、未拉伸的聚丙烯(CPP)、聚酰胺(PA)、聚对苯二甲酸乙二醇酯(PET)、聚乙酸酯、赛璐酚、涂覆(蒸汽涂覆)有金属如铝的聚合物膜(简称金属化膜)；或者由铝构成的金属箔。所述箔和膜可以彼此粘合或粘合至另一类型的膜或箔，例如聚合物膜粘合至金属箔、不同的聚合物膜彼此粘合等。所述箔和膜也可以例如已经用印刷油墨印刷。
衬底膜的厚度可总计为例如5至100μm，优选5至40μm。
本发明的一个实施方案是一种使用上述本发明的水性聚合物分散体之一制备的复合膜，第一膜的材料选自OPP、CPP、PE、PET和PA，第二膜或箔的材料选自OPP、CPP、PE，PET，PA和金属箔。在本发明的一个实施方案中，第一膜或箔和/或第二膜或箔被印刷或金属化在涂布有本发明的聚合物分散体的相应侧。
在涂布有本发明的聚合物分散体之前，箔或膜衬底的表面处理不是绝对必须的。但是，如果在涂布前将膜或箔衬底的表面改性，则可以获得更好的结果。在此情况下，可以采取常规表面处理，例如电晕处理，以增强粘附力。电晕处理或其他表面处理进行至足以用涂布组合物润湿的程度。通常，约10瓦每平方米每分钟的电晕处理足以用于该目的。或者或此外，任选地，也可以在箔或膜衬底和粘合剂涂层之间使用底漆或夹层。此外，复合膜上可存在额外的功能层，实例为阻隔层、印刷层、着色层或清漆层、或保护层。这些功能层可位于外侧，即背对胶粘剂涂布侧的箔或膜衬底的一侧；或在内侧，在箔或膜衬底和胶粘剂层之间。
特别地，根据本发明可获得的膜/箔层压体的特定的优点为以下：
-刚刚层压后，复合膜层压中良好的剥离强度(即时强度)
-在高温下，复合膜层压中良好的剥离强度(热稳定性)
-在胶粘剂暴露于可迁移的化学品的情况下，复合膜层压中良好的剥离强度
实施例
缩写
IA 衣康酸
AA 丙烯酸
S 苯乙烯
MA 丙烯酸甲酯
nBA 丙烯酸正丁酯
HPA 丙烯酸羟丙酯
DAAM 双丙酮丙烯酰胺
ADDH 己二酸二酰肼
EHTG 巯基乙酸2-乙基己基酯(链转移剂)
pphm 每百份单体的份数(每100重量份单体的重量份)
SC 固含量
LT 透光性；用于确定粒度差异的参数。在此情况下，将聚合物分散体稀释至固含量为0.01％，并相对于纯水而测量透光性。
Tg(计算) 通过Fox方程由存在于共聚物中的单体的均聚物的玻璃化转变温度及其重量分数计算的玻璃化转变温度：
1/Tg＝xA/TgA+xB/TgB+xC/TgC+........
Tg：计算的共聚物的玻璃化转变温度
TgA：单体A的均聚物的玻璃化转变温度
TgB、TgC：单体B、C等相应的Tg
xA：单体A的质量/共聚物的总质量，
xB、xC：相应地，对于单体B、C等。
实施例1和2
| 单体 | 实施例1(重量份) | 实施例2(重量份) |
| MA | 65.1 | 63.1 |
| nBA | 29.8 | 29.8 |
| HPA | 2 | 2 |
| IA | 1 | 1 |
| AA | 0.1 | 0.1 |
| DAAM | 2 | 4 |
所列单体在于水中存在0.1pphm聚苯乙烯晶种和0.1pphm乳化剂(
FES 27)的情况下在85℃的温度下进行聚合。所使用的引发剂是过氧二硫酸钠。为了进一步稳定聚合物颗粒，在聚合过程中加入总共0.35pphm的碱(氨)。为了使聚合物分散体中的单体减少，在聚合之后采用借助雕白粉C和叔丁基过氧化氢的化学除臭。在冷却至室温后，将聚合物分散体与ADDH混合。
实施例3(对比实施例)
| 实施例3(重量份) | |
| MA | 67.1 |
| nBA | 29.8 |
| HPA | 2 |
| IA | 1 |
| AA | 0.1 |
| DAAM | -- |
所列单体在于水中存在0.3pphm聚苯乙烯晶种和0.25pphm乳化剂(
FES 27)的情况下在80℃的温度下进行聚合。所使用的引发剂是过氧二硫酸钠。为了进一步稳定聚合物颗粒，在聚合过程中加入总共0.3pphm的碱(氨)。为了使聚合物分散体中的单体减少，在聚合之后采用借助丙酮亚硫酸氢盐和叔丁基过氧化氢的化学除臭。
实施例4和5
所列单体在于水中存在0.1(实施例4)或0.3(实施例5)pphm聚苯乙烯晶种和0.1(实施例4)或0.5(实施例5)pphm乳化剂的情况下在85℃的温度下进行聚合。所使用的引发剂是过氧二硫酸钠。为了进一步稳定聚合物颗粒，在聚合过程中加入总共0.35pphm的碱(氨)。为了使聚合物分散体中的单体减少，在聚合之后采用借助丙酮亚硫酸氢盐和叔丁基过氧化氢的化学除臭。在冷却至室温后，将聚合物分散体与ADDH混合。
实施例6(对比实施例)
| 实施例6(重量份) | |
| n-BA | 63 |
| S | 35.5 |
| AA | 1.5 |
| EHTG | 1 |
| DAAM | -- |
所列单体在于水中存在0.1pphm聚苯乙烯晶种和0.1pphm乳化剂(
LDBS 20)的情况下在85℃的温度下进行聚合。所使用的引发剂是过氧二硫酸钠。为了进一步稳定聚合物颗粒，在聚合过程中加入总共0.35pphm的碱(氨)。为了使聚合物分散体中的单体减少，在聚合之后采用借助丙酮亚硫酸氢盐和叔丁基过氧化氢的化学除臭。
实施例7(对比)
表1：实施例1-7的湿样本值
相关应用的测试
衬底，层压膜：
聚酯膜，12μm厚，电晕预处理，表面张力>38mN/m；
PE膜60μm厚，电晕预处理，表面张力>38mN/m
胶粘剂施用：
直接施用至基底膜的电晕预处理侧，施用重量为2.5-3.0g/m2(干的)。
环形粘性:
将胶粘剂以20μm(干的)的施用厚度施用于12μm厚的聚酯膜，并在90℃下进行干燥，持续3分钟。将涂布的聚酯膜切割为25mm宽和200mm长的条，并使该条形成环。使该环胶粘剂向外，在两端夹入拉伸试验机的钳口。使环以300mm/min的速度移动到剖光的不锈钢表面，以产生40×25mm的接触面积。然后，将环以300mm/min的速度与钢表面拉离，在此过程中环形粘性测定为最大力(在室温下；20℃)，以N/25mm为单位。
在23℃下的动态剥离阻力：
将基膜预处理侧向上地固定在实验室涂布装置上，并将待测试的胶粘剂直接刮涂到膜上。用热空气鼓风机将胶粘剂干燥2分钟，然后在层压膜上放上手动辊，并在辊层压状态下在70℃下以5m/min的辊速度和6.5bar的层压压力进行按压。之后，使用切割模板将层压体切割成15毫米宽的条，并进行各种储存周期。储存之后，在拉伸试验机上撕断层压条，并记录达到这样所需的力。测试在拉伸试验机上以90度角和100mm/min的移除速度进行。将测试条一侧打开，其中一端夹入拉伸试验机的上夹爪，另一端夹入拉伸试验机的下夹爪，并着手测试。所记录的结果是3次单独测量的平均值，以N/15mm为单位。
可以在不同的储存条件之后对样本进行测试：
1.层压后立即测试(<3min)
2. 24h(在23℃下/50％的相对湿度)之后
3. 24h(在23℃下/50％的相对湿度)+在50℃下在番茄酱中7天之后
在90℃下的动态剥离阻力：
将基膜预处理侧向上地固定在实验室涂布单元上，并将待测试的胶粘剂直接刮涂到膜上。用热空气鼓风机将胶粘剂干燥2分钟，然后在层压膜上放上手动辊，并在辊层压状态下在70℃下以5m/min的辊速度和6.5bar的层压压力进行按压。然后使用切割模板将层压体切割成15毫米宽的条，并在23℃/50％相对湿度下储存24小时。储存之后，在90℃温度下在具有气压室的拉伸试验机上拉开层压条，并记录达到这样所需的力。测试在具有气压室的拉伸试验机上以100mm/min的移除速度进行。将测试条一侧打开，其中一个结果端夹入拉伸试验机的上夹爪，另一个夹入拉伸试验机的下夹爪，并着手测试。测试在1分钟的等待时间之后开始，以调节测试条。评价：所记录的结果是3次单独测量的力的平均值，以N/15mm为单位。
破裂模式的评估：
A＝胶粘剂层仍然完全在基底膜上(胶粘剂破裂)
K＝胶粘剂层分离而不从材料上脱落(粘合破裂)
MB＝膜部分或完全破裂
表2：胶粘剂分散体的粘着值
该表显示出，根据本发明的实施例可以非常有效地用作复合膜层压中的单组分胶粘剂，特别是如果需要高温稳定性和对可迁移化学品的耐受性时。
优选的<1pphm的乳化剂的量使得使用本发明的分散体制备的层压体(实施例5对比于实施例5a)产生特别高的即时强度。
Claims (18)
1.单组分层压胶粘剂用于复合膜层压的用途，该层压胶粘剂以水性聚合物分散体的形式存在并且不包含可UV-交联的组分，所述水性聚合物分散体包含通过单体的自由基乳液聚合可制备的分散在水中的聚合物颗粒，所述单体包含
a)基于单体的总量计，90至99.4重量％的丙烯酸C1至C8烷基酯和苯乙烯的混合物，和
b)基于单体的总量计，至少0.1重量％的至少一种具有至少一个酸基团的单体，和
c)基于单体的总量计，0.1至5重量％的至少一种具有至少一个选自酮基和醛基的官能团的烯键式不饱和化合物；
其中在乳液聚合中，每100重量份的单体使用少于1重量份的乳化剂，
其中，水性聚合物分散体包含至少一种具有至少两个能与酮基或与醛基发生交联反应的官能团的化合物A；
其中，化合物A的对酮基或醛基呈反应性的基团与单体c)的酮基和醛基的摩尔比为1:10至2:1；
其中，在复合膜层压中，至少两个聚合物膜用层压胶粘剂牢固地彼此粘合，以使得在层压制备之后24h在23℃下测量的剥离强度为2.5N/15mm或更大，或者彼此粘合的聚合物膜仅可通过破坏至少一个膜而分离。
2.根据权利要求1所述的用途，其中所述单体包含0.5至5重量％的至少一种具有至少一个选自酮基和醛基的官能团的烯键式不饱和化合物，基于单体的总量计。
3.根据权利要求1所述的用途，其中层压胶粘剂的粘性小于1.7N/25mm，作为环形粘性测量，以20μm的施用厚度施用于12μm厚的聚酯膜，并在钢上在室温20℃以300mm/min的移动速度测量。
4.根据权利要求1或2所述的用途，其中聚合物颗粒由包括以下的单体制备
a)基于单体的总量计，90至99.4重量％的丙烯酸C1至C8烷基酯和苯乙烯的混合物，和
b)基于单体的总量计，0.1至5重量％的至少一种具有至少一个酸基团的单体，和
c)基于单体的总量计，0.1至5重量％的至少一种具有至少一个选自酮基和醛基的官能团的烯键式不饱和化合物；
d)基于单体的总量计，0至10重量％的不同于单体a)至c)的其他单体。
5.根据权利要求1或2所述的用途，其中单体d)选自丙烯酰胺、甲基丙烯酰胺、N-羟甲基丙烯酰胺、N-羟甲基甲基丙烯酰胺、单(甲基)丙烯酸苯氧基乙基乙二醇酯、含有羟基的单体、含有氨基的单体、α,β-单烯键式不饱和C3-C8羧酸的腈，除烯键式不饱和双键之外还具有至少一个缩水甘油基、噁唑啉基或脲基的双官能单体，以及具有多于一个可自由基聚合的基团的交联单体。
6.根据权利要求1或2所述的用途，其中单体b)选自丙烯酸、甲基丙烯酸和衣康酸，以及单体d)选自在烷基中具有1至10个碳原子的(甲基)丙烯酸羟烷基酯。
7.根据权利要求1或2所述的用途，其中单体c)选自丙烯醛、甲基丙烯醛、在烷基中具有1至20个碳原子的乙烯基烷基酮、甲酰苯乙烯、在烷基中具有一个或两个酮基或醛基或者具有一个醛基和一个酮基的(甲基)丙烯酸烷基酯、N-氧代烷基(甲基)丙烯酰胺、(甲基)丙烯酸乙酰乙酰基酯、(甲基)丙烯酸乙酰乙酰氧基乙酯和双丙酮丙烯酰胺。
8.根据权利要求1或2所述的用途，其中化合物A选自具有酰肼基团、羟胺基团、肟醚基团或氨基的化合物。
9.根据权利要求1或2所述的用途，其中化合物A是具有2至10碳原子的二羧基二酰肼，以及单体c)选自(甲基)丙烯酸乙酰乙酰基酯、(甲基)丙烯酸乙酰乙酰氧基乙酯和双丙酮丙烯酰胺。
10.根据权利要求1或2所述的用途，其中化合物A是己二酸二酰肼，以及单体c)是双丙酮丙烯酰胺。
11.根据权利要求1或2所述的用途，其中聚合物颗粒由包含以下的单体制备：
a)基于单体的总量计，90至99.4重量％的丙烯酸C1至C8烷基酯和苯乙烯的混合物，和
b)基于单体的总量计，0.5至3重量％的至少一种选自丙烯酸、甲基丙烯酸和衣康酸的单体，和
c)基于单体的总量计，0.1至5重量％的至少一种具有至少一个酮基的烯键式不饱和化合物，其选自(甲基)丙烯酸乙酰乙酰基酯、(甲基)丙烯酸乙酰乙酰氧基乙酯和双丙酮丙烯酰胺；
d)基于单体的总量计，0至5重量％的不同于单体a)至c)的其他单体，其选自丙烯酰胺、甲基丙烯酰胺、N-羟甲基丙烯酰胺和N-羟甲基甲基丙烯酰胺、单(甲基)丙烯酸苯氧基乙基乙二醇酯、含有羟基的单体、含有氨基的单体、α,β-单烯键式不饱和C3-C8羧酸的腈，除烯键式不饱和双键之外还具有至少一个缩水甘油基、噁唑啉基或脲基的双官能单体，以及具有多于一个可自由基聚合的基团的交联单体，
并且其中化合物A是具有2至10个碳原子的二羧基二酰肼。
12.根据权利要求1或2所述的用途，其中化合物A的对酮基或醛基呈反应性的基团与单体c)的酮基和醛基的摩尔比为1:1.3至1.3:1。
13.根据权利要求1或2所述的用途，其中待粘合的膜的材料选自聚乙烯、定向聚丙烯、未拉伸聚丙烯、聚酰胺、聚对苯二甲酸乙二醇酯、聚乙酸酯、赛璐酚、金属化膜和金属箔。
14.根据权利要求1或2所述的用途，其中聚合物颗粒的玻璃化转变温度为-40至+15℃。
15.根据权利要求14所述的用途，其中聚合物颗粒的玻璃化转变温度为-10至+10℃。
16.一种通过使用根据权利要求1至15的任一项中的单组分层压胶粘剂将至少两个膜彼此粘合来制备复合膜的方法。
17.根据前述权利要求1至16中任一项可获得的复合膜用于食品包装的用途。
18.一种复合膜，其具有使用根据权利要求1至15的任一项中的层压胶粘剂彼此粘合的第一膜和至少一个第二膜。
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| EP16151707 | 2016-01-18 | ||
| EP16151707.3 | 2016-01-18 | ||
| PCT/EP2017/050365 WO2017125277A1 (de) | 2016-01-18 | 2017-01-10 | Verwendung eines einkomponentigen laminierklebstoffs zur verbundfolienkaschierung |
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| EP3781622B1 (de) | 2018-04-20 | 2022-10-12 | Basf Se | Haftklebstoffzusammensetzung mit auf vernetzung über keto- oder aldehydgruppen beruhendem gelgehalt |
| CN111989377B (zh) * | 2018-04-20 | 2022-07-19 | 巴斯夫欧洲公司 | 用于疏水性聚合物的水性分散体的添加剂组合物 |
| GB2577308A (en) * | 2018-09-21 | 2020-03-25 | Synthomer Deutschland Gmbh | Contact adhesives |
| US20220111626A1 (en) * | 2019-01-11 | 2022-04-14 | Basf Se | Film coating method using engraving roller system |
| CN110511700A (zh) * | 2019-09-18 | 2019-11-29 | 湖北航天化学技术研究所 | 一种单组份丙烯酸酯乳液复膜胶及其制备方法 |
| CN113524843A (zh) * | 2021-08-03 | 2021-10-22 | 海南赛诺实业有限公司 | 一种高阻隔复合膜及其制备方法 |
| WO2023114625A1 (en) * | 2021-12-16 | 2023-06-22 | Dow Global Technologies Llc | Polymer dispersion composition |
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| WO2006066761A1 (de) * | 2004-12-17 | 2006-06-29 | Basf Aktiengesellschaft | Vernetzbarer haftklebstoff für wiederablösbare weich-pvc-träger |
| CN102939310A (zh) * | 2010-06-11 | 2013-02-20 | 巴斯夫欧洲公司 | 用于生产复合膜的聚合物水性分散体的多步制备方法 |
| EP2636714A1 (de) * | 2012-03-09 | 2013-09-11 | Basf Se | Mehrstufige herstellung wässriger haftklebstoffdispersionen für die herstellung von selbstkle-benden artikeln |
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| GB1329126A (en) | 1969-12-11 | 1973-09-05 | Mitsubishi Rayon Co | Acrylic fibre and a method for manufacturing the same |
| JPS5033767B1 (zh) | 1971-03-11 | 1975-11-04 | ||
| DE2722097C3 (de) | 1977-05-16 | 1981-09-17 | Basf Ag, 6700 Ludwigshafen | (Meth)acryloxy-alkylpropanale, Verfahren zu dessen Herstellung und Verwendung derselben |
| DE3343779A1 (de) | 1983-12-03 | 1985-06-13 | Basf Ag, 6700 Ludwigshafen | Verfahren zur verbesserung der haftung von klebstoffschichten, die aus waessriger dispersion auf polyolefinoberflaechen aufgebracht werden |
| JPH082538A (ja) | 1994-06-22 | 1996-01-09 | Toppan Printing Co Ltd | 包装袋 |
| DE19649383A1 (de) | 1996-11-29 | 1998-06-04 | Basf Ag | Kaschierklebstoffe |
| DE19908183A1 (de) | 1999-02-25 | 2000-08-31 | Basf Ag | Wässrige Polymerdispersionen |
| DE10135379A1 (de) * | 2001-07-25 | 2003-02-06 | Basf Ag | UV-vernetzbare Kaschierklebstoffe |
| DE10253332A1 (de) * | 2002-11-14 | 2004-05-27 | Basf Ag | UV-vernetzbare Kaschierklebstoffe |
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| WO2006066761A1 (de) * | 2004-12-17 | 2006-06-29 | Basf Aktiengesellschaft | Vernetzbarer haftklebstoff für wiederablösbare weich-pvc-träger |
| CN102939310A (zh) * | 2010-06-11 | 2013-02-20 | 巴斯夫欧洲公司 | 用于生产复合膜的聚合物水性分散体的多步制备方法 |
| EP2636714A1 (de) * | 2012-03-09 | 2013-09-11 | Basf Se | Mehrstufige herstellung wässriger haftklebstoffdispersionen für die herstellung von selbstkle-benden artikeln |
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| EP3405540A1 (de) | 2018-11-28 |
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| JP2019509357A (ja) | 2019-04-04 |
| US11015091B2 (en) | 2021-05-25 |
| BR112018014569A2 (pt) | 2018-12-11 |
| EP3405540B1 (de) | 2020-04-22 |
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| WO2017125277A1 (de) | 2017-07-27 |
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