CN103038270B - 可生物分解的复合箔 - Google Patents
可生物分解的复合箔 Download PDFInfo
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- CN103038270B CN103038270B CN201180037328.5A CN201180037328A CN103038270B CN 103038270 B CN103038270 B CN 103038270B CN 201180037328 A CN201180037328 A CN 201180037328A CN 103038270 B CN103038270 B CN 103038270B
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- 239000011888 foil Substances 0.000 title claims abstract description 45
- 239000002131 composite material Substances 0.000 title claims abstract description 36
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 120
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000000758 substrate Substances 0.000 claims abstract description 47
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- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 claims abstract description 32
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- 150000002762 monocarboxylic acid derivatives Chemical class 0.000 claims abstract description 7
- MMCOUVMKNAHQOY-UHFFFAOYSA-N carbonoperoxoic acid Chemical group OOC(O)=O MMCOUVMKNAHQOY-UHFFFAOYSA-N 0.000 claims abstract description 6
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Abstract
本发明涉及聚氨酯水分散体粘合剂用于制备可生物分解的复合箔的用途，其中使用聚氨酯分散体粘合剂使至少两个基底彼此粘合，其中至少一个基底为可生物分解的聚合物箔。至少60重量%的聚氨酯由二异氰酸酯、聚酯二醇和至少一种选自二羟基羧酸和二氨基羧酸的二官能羧酸构成。
Description
本发明涉及聚氨酯水分散体粘合剂用于制备可生物分解的复合箔的用途。本发明还涉及制备复合箔的方法并且涉及通过所述方法制备的复合箔。
柔性包装材料通常由通过合适的粘合剂彼此粘合的复合箔组成，其中至少一个彼此粘合的箔为聚合物箔。对可降解的复合箔包装材料有高需求，其中术语可降解材料还应理解为包括在生物条件下分解的材料即可分解的或可堆肥的材料。
主要的难题在于提供具有必要的功能和稳定性，但是当遭遇生物活性环境的刺激时将以最快速度和最大程度降解或分解的材料。降解方法过程的引发可以为在聚合物主链内的特定位置上微生物降解、水解降解或氧化降解。所有的降解产品应当表现出最大的安全性和最低的毒性并且不能在自然环境中积累，这是指降解产品应当进行完全的且最终的微生物降解。用于箔粘合的粘合剂还对生物分解性有作用。粘合剂首先旨在提供稳定的粘合，但是其次还促进降解性即箔复合物的分解。同时实现对这些根本上矛盾的需求并进行优化是相当困难的。
WO96/35733公开了包括片状结构的可降解且可堆肥的模塑体。其通过使用具有脲基的聚氨酯的水分散体制备。聚氨酯由二异氰酸酯组分、二醇组分、二氨基磺酸酯形式的二胺组分和任选地亲水聚醚醇构成。
生物可分解性的一些方面仍不令人满意。本发明的目的在于提供用于可降解的和可分解的复合箔——特别是用于柔性包装材料——的其他材料，其中所述复合箔可以被制备为具有最大便利性和粘合剂特性的最好品质，并且同时还具有最好的生物分解性品质。
已经发现该目的可以通过使用下述聚氨酯粘合剂分散体而实现。本发明提供聚氨酯水分散体粘合剂用于制备可生物分解的复合箔的用途，其中使用聚氨酯分散体粘合剂将至少一个第一基底粘合至至少一个第二基底，其中至少一个基底为可生物分解的聚合物箔，并且其中至少60重量%聚氨酯由以下物质构成：
(a)二异氰酸酯，
(b)聚酯二醇，和
(c)至少一种选自二羟基羧酸和二氨基羧酸的二官能羧酸。
本发明还提供制备复合箔的方法，所述方法包括提供基于本发明使用的聚氨酯的聚氨酯水分散体粘合剂，并且使用该聚氨酯水分散体粘合剂使至少两个基底彼此粘合，其中至少一个基底为可生物分解的聚合物箔。本发明还提供通过本发明方法制备的复合箔。
为了本发明的应用，如果例如最长12周的好氧堆肥后发现，受试材料原干重的最高10%以筛分粒级>2mm存在，则该材料具有生物分解性，其中测试根据标准EN13432(2000)进行。
本发明使用的粘合剂基本由至少一种在水中分散的聚氨酯作为聚合物粘合剂、以及任选加入的物质例如填料、增稠剂、消泡剂等组成。聚合物粘合剂优选采取水中或由水和水溶性有机溶剂制备的混合物中的分散体形式，所述水溶性有机溶剂的沸点优选低于150℃（1巴）。特别优选水作为单一溶剂。水或其他溶剂不包括于涉及粘合剂组成的重量数据的计算中。
聚氨酯分散体粘合剂优选为可生物降解的。为了本发明的应用，如果根据标准ISO14855(2005)测定，例如20天后以CO2形式释放的气态碳与使用的材料的总碳含量的比例至少为30%，优选至少60%或至少80%，则该材料是可生物分解的。
聚氨酯优选主要由多异氰酸酯特别是二异氰酸酯、以及反应物聚酯二醇以及二官能羧酸构成。优选聚氨酯由至少40重量%，特别是至少60重量%，并且非常特别是至少80重量%的二异氰酸酯、聚酯二醇和二官能羧酸构成。
聚氨酯可以为非晶态的或半晶态的。如果聚氨酯为半晶态的，其熔点优选低于80℃。为此，优选聚氨酯包括多于10重量%，多于50重量%或至少80重量%的量的聚酯二醇，基于聚氨酯计。
全部聚氨酯优选由以下物质构成：
a)二异氰酸酯
b)二醇，其中，
b1)10至100mol%为摩尔质量为500至5000g/mol的聚酯二醇，基于二醇(b)的总量计，
b2)0至90mol%摩尔质量为60至500g/mol，基于二醇(b)的总量计，
c)至少一种二官能羧酸，其选自二羟基羧酸和二氨基羧酸，
d)任选的不同于单体(a)至单体(c)并且具有反应性基团的其他多官能化合物，其中所述反应性基团为醇羟基、伯氨基或仲氨基、或异氰酸酯基团，以及
e)任选的不同于单体(a)至单体(d)并且具有反应性基团的单官能化合物，所述反应性基团为醇羟基、伯氨基或仲氨基或异氰酸酯基团。
应特别提及的单体（a）为二异氰酸酯X(NCO)2，其中X为具有4至15个碳原子的脂族烃基、具有6至15个碳原子的脂环族或芳族烃基或具有7至15个碳原子的芳脂族（araliphatic）烃基。这些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、十二亚甲基二异氰酸酯、1,4-二异氰酰基环己烷、1-异氰酰基-3,5,5-三甲基-5-异氰酰基甲基环己烷（IPDI）、2,2-双(4-异氰酰基环己基)丙烷、三甲基己烷二异氰酸酯、1,4-二异氰酰基苯、2,4-二异氰酰基甲苯、2,6-二异氰酰基甲苯、4,4’-二异氰酰基二苯基甲烷、2,4’-二异氰酰基二苯基甲烷、对二甲苯二异氰酸酯、四甲基二甲苯二异氰酸酯(TMXDI)、双(4-异氰酰基环己基)甲烷(HMDI)的异构体例如反式/反式、顺式/顺式和顺式/反式异构体，以及由所述化合物组成的混合物。该类二异氰酸酯市售可得。所述异氰酸酯的重要的混合物特别是二异氰酰基甲苯和二异氰酰基二苯基甲烷各自的结构异构体的混合物，特别合适的混合物由80mol%的2,4–二异氰酰基甲苯和20mol%2,6–二异氰酰基甲苯制备。芳族异氰酸酯（例如2,4–二异氰酰基甲苯和/或2,6–二异氰酰基甲苯）与脂族或脂环族异氰酸酯（例如六亚甲基二异氰酸酯或IPDI）的混合物也是特别有利的，其中脂族异氰酸酯与芳族异氰酸酯优选的混合比例为4:1至1:4。除上述化合物外，可以用于聚氨酯结构的其他化合物为同时具有游离异氰酸酯基团和其他封端异氰酸酯基团例如脲二酮基团的聚氨酯。
为了良好的成膜和弹性，可以使用的二醇(b)主要为相对高分子量的二醇（b1），其具有约500至5000g/mol，优选约1000至3000g/mol的摩尔质量。这是数均摩尔质量Mn。Mn通过测定末端基团的数量（OH数量）而计算。二醇（b1）可以是聚酯多元醇，其中这些聚酯多元醇例如已知于UllmannsdertechnischenChemie[Ullmann’sencyclopediaofindustrialchemistry],第4版，第19卷，第62至65页。优选使用通过二官能醇与二官能羧酸反应而获得的聚酯多元醇。除游离多羧酸外，还可以使用相应的多羧酸酐或相应的低级醇的多羧酸酯或这些化合物的混合物来制备聚酯多元醇。多羧酸可以为脂族、脂环族、芳脂族、芳族或杂环的，并且可以任选地为不饱和的和/或例如被卤原子取代。所述多羧酸的可以提及的实例为：辛二酸、壬二酸、邻苯二甲酸、间苯二甲酸、邻苯二甲酸酐、四氢苯二甲酸酐、六氢苯二甲酸酐、四氯苯二甲酸酐、桥亚甲基四氢苯二甲酸酐、戊二酐、马来酸、马来酸酐、富马酸和二聚脂肪酸。优选为通式HOOC-(CH2)y-COOH的二羧酸，其中y为1至20的数字，优选2至20的偶数，实例为琥珀酸、己二酸、癸二酸和十二烷二羧酸。
可以使用的多官能醇的实例为乙二醇、丙-1,2-二醇、丙-1,3-二醇、丁-1,3-二醇、丁烯-1,4-二醇、丁炔-1,4-二醇、戊-1,5-二醇、新戊二醇、双(羟甲基)环己烷例如1,4-双(羟甲基)环己烷、2-甲基丙烷-1,3-二醇、甲基戊二醇以及二甘醇、三甘醇、四甘醇、聚乙二醇、双丙甘醇、聚丙二醇、二丁二醇和聚丁二醇。优选为通式为HO-(CH2)x-OH的醇，其中x为1至20的数字，优选地为2至20的偶数。其实例为二甘醇、丁-1,4-二醇、己-1,6-二醇、辛-1,8-二醇和十二烷-1,12-二醇。还优选为新戊二醇。
任选地还可以使用聚碳酸酯二醇，其例如可以通过光气与过量的作为聚酯多元醇的结构组分提及的低分子量醇反应而获得。
还可以单独或与上述聚酯二醇结合使用基于内酯的聚酯二醇，其中所述基于内酯的聚酯二醇为内酯的均聚物或共聚物，优选地为具有末端羟基并且通过内酯加成至合适的二官能起始分子的加成反应而制备的加合物。可以使用的优选的内酯为衍生自通式HO-(CH2)z-COOH的化合物，其中z为1至20的数字并且亚甲基单元的H原子还可以被C1-C4-烷基替代。实例为ε-己内酯、β-丙内酯、γ-丁内酯和/或甲基-ε-己内酯以及这些化合物的混合物。合适的起始组分的实例为上述作为聚酯多元醇结构组分提及的低分子量二官能醇。特别优选ε-己内酯的相应的聚合物。低级聚酯二醇或聚醚二醇也可以作为起始材料用于制备内酯聚合物，除内酯聚合物外，还可以使用相应的相当于内酯的化学当量的羟基羧酸缩聚物。
除聚酯二醇外，还可以任选同时使用聚醚二醇。聚醚二醇具体可通过环氧乙烷、环氧丙烷、环氧丁烷、四氢呋喃、氧化苯乙烯或表氯醇例如在BF3存在下进行自身聚合而获得，或者通过所述化合物（任选地以混合物或相继）加成至具有活性氢原子的起始组分的加成反应而获得，所述具有活性氢原子的起始组分例如醇或胺，实例为水、乙二醇、丙-1,2-二醇、丙-1,3-二醇、2,2-双(4-羟基苯基)丙烷或苯胺。聚醚二醇的实例为聚环氧丙烷和聚四氢呋喃，其摩尔质量为240至5000g/mol，尤其是500至4500g/mol。然而，优选不将聚醚二醇作为结构组分用于聚氨酯。
还可以任选同时使用聚羟基烯烃，优选具有2个端羟基的那些，例如α,ω-二羟基聚丁二烯、α,ω–二羟基聚甲基丙烯酸酯或α,ω-二羟基聚丙烯酸酯。其他合适的多元醇为聚缩醛、聚硅氧烷和醇酸树脂。
优选至少95mol%或100mol%的二醇b1)为聚酯二醇。特别优选所用的二醇b1)仅包含聚酯二醇。
如果所用的二醇(b)同时包含二醇(b1)和摩尔质量为约60至500g/mol、优选62至200g/mol的低摩尔质量二醇(b2)，则可以提高聚氨酯的硬度和弹性模量。所用的单体(b2)特别是所述用于制备聚酯多元醇的短链烷二醇的结构组分，其中优选为具有2至12个碳原子和具有偶数个碳原子的未支化二醇，以及戊-1,5-二醇和新戊二醇。可以使用的二醇b2)的实例为乙二醇、丙-1,2-二醇、丙-1,3-二醇、丁-1,3-二醇、丁烯-1,4-二醇、丁炔-1,4-二醇、戊-1,5-二醇、新戊二醇、双(羟甲基)环己烷如1,4-双(羟甲基)环己烷、2-甲基丙-1,3-二醇、甲基戊二醇以及二甘醇、三甘醇、四甘醇、聚乙二醇、双丙甘醇、聚丙二醇、二丁二醇和聚丁二醇。优选通式HO-(CH2)x-OH的醇，其中x为1至20的数字，优选为2至20的偶数。其实例为乙二醇、丁-1,4-二醇、己-1,6-二醇、辛-1,8-二醇和十二烷-1,12-二醇。还优选为新戊二醇。
优选二醇(b1)的比例为10至100mol%或为60至100mol%，基于二醇(b)的总量计，并且单体(b2)的比例为0至90mol%或为0至40mol%，基于二醇(b)的总量计。
为实现聚氨酯的水分散性并且改进生物降解性，聚氨酯包含至少一种选自二羟基羧酸和二氨基羧酸的二官能羧酸。任选地还可以另外使用亲水结构组分，其提升分散性并且具有至少一个异氰酸酯基团或至少一个对异氰酸酯有反应性的基团，并且还具有至少一个亲水基团或一个可以转化为亲水基团的基团。在下文中，“亲水基团或潜在的亲水基团”简写为“(潜在)亲水基团”。当与用于构成聚合物主链的单体的官能团相比时，(潜在)亲水基团与异氰酸酯的反应要慢很多。
具有(潜在)亲水基团的组分的比例——基于组分(a)至(f)的总量计——通常以如下方式确定：(潜在)亲水基团的摩尔量为30至1000mmol/kg，优选50至500mmol/kg，并且特别优选80至300mmol/kg，基于所有单体(a)至(f)的总量计。(潜在)亲水基团可以为非离子型的或优选为(潜在)离子型亲水基团。可以使用的特定非离子型亲水基团为聚乙二醇醚的形式，其优选由5至100个重复环氧乙烷单元制成，优选10
至80个重复环氧乙烷单元。聚环氧乙烷单元的含量通常为0至10重量%，优选0至6重量%，基于所有单体(a)至(f)的总量计。具有非离子型亲水基团的单体的实例为使用至少20重量%环氧乙烷的聚环氧乙烷二醇、聚环氧乙烷一元醇、以及聚乙二醇和二异氰酸酯的反应产物，其中所述单体具有醚化的末端聚乙二醇基团。US-A3905929和US-A3920598的专利说明书中给出了该类二异氰酸酯以及它们的制备方法。
所用的二官能羧酸通常包括脂族、脂环族、芳脂族或芳族羧酸，其中这些二官能羧酸具有至少两个羟基或两个伯氨基或仲氨基。优选为二羟基烷基羧酸，特别是具有3至10个碳原子的那些，所述二羟基烷基羧酸还描述于US-A3412054中。特别优选为通式（c1）的化合物
其中R1和R2为C1-C4-烷二基(单元)，并且R3为C1-C4-烷基(单元)，特别是二羟甲基丙酸(DMPA)。
其他合适的化合物为具有高于500至10000g/mol的摩尔质量并且具有至少2个羧酸酯基团的二羟基化合物，其中这些化合物已知于DE-A3911827。所述化合物可以通过在加聚反应中二羟基化合物与四羧酸二酐例如苯均四酸二酐或环戊烷四酸二酐以摩尔比为2:1至1.05:1反应而获得。特别合适的二羟基化合物是作为扩链剂列出的单体(b2)以及二醇(b1)。
可以使用并且具有对异氰酸酯有反应性的氨基的单体(c)为二氨基羧酸，或DE-A2034479中提及并且衍生自脂族二伯二胺加成至α,β-不饱和羧酸的加成反应的加合物。该类化合物符合例如式(c2)
H2N-R4-NH-R5-X(c2)
其中R4和R5彼此独立地为C1-C6-烷二基单元，优选为亚乙基，并且X为COOH。特别优选的式(c2)化合物为N-(2-氨基乙基)-2-氨基乙烷甲酸和相应的碱金属盐，其中特别优选Na作为抗衡离子。
与二官能羧酸一起，还可以任选地使用具有亲水基团的其他单体，实例为合适的二羟基磺酸和二羟基膦酸，例如2,3-二羟基丙基膦酸或二氨基磺酸。然而，优选不使用任何二官能磺酸或膦酸。
离子型亲水基团特别是阴离子基团例如磺酸根基团、羧酸根基团和磷酸根基团（以其碱金属盐或铵盐形式），以及阳离子基团例如铵基团，特别是质子化的叔氨基基团，或季铵基团。潜在离子型亲水基团特别是那些可以通过简单的中和、水解或季铵化反应而转化为上述离子型亲水基团的基团，从而例如成为羧酸基团或叔氨基团。(潜在)离子型单体详细描述于例如UllmannsdertechnischenChemie[Ullmann’sencyclopediaofindustrialchemistry],第4版，第19卷，第311-313页以及例如DE-A1495745中。
实践上特别重要的(潜在)阳离子单体(c)特别是具有叔氨基团的单体，其实例为三(羟烷基)胺、N,N’-双(羟烷基)烷基胺、N-羟烷基二烷基胺、三(氨基烷基)胺、N,N’-双(氨基烷基)烷基胺和N-氨基烷基二烷基胺，其中所述叔胺的烷基和烷二基单元彼此独立地由1至6个碳原子组成。可以使用的其他化合物为具有叔氮原子并且优选具有两个端羟基的聚醚，例如可以本身常规的方式通过具有两个连接至胺上氮的氢原子的胺（例如甲胺、苯胺或N,N’-二甲肼）的烷氧基化而获得的那些。该类聚醚的摩尔质量通常为500至6000g/mol。所述叔胺用酸（优选强无机酸,例如磷酸、硫酸、氢卤酸或强有机酸）或通过与合适的季铵化试剂（例如C1-C6-烷基卤化物或苯甲基卤化物如溴化物或氯化物）反应而转化为铵盐。
只要使用具有潜在离子型基团的单体，则将这些单体转化为离子形式可以在异氰酸酯加聚（polyaddition）反应前、反应中或优选反应后进行，这是因为离子型单体通常在反应混合物中仅微溶。特别优选羧酸根基团以其与碱金属离子或铵离子作为抗衡离子的盐的形式存在。
与单体(a)至(c)不同并且任选地也作为聚氨酯组成部分的单体(d)通常用于交联或链扩展。这些单体通常为官能度大于2的非酚类醇、具有2个或更多个伯氨基和/或仲氨基的胺或不仅具有一个或更多醇羟基而且具有一个或更多伯氨基和/或仲氨基的化合物。具有高于2的官能度并且可以用于在一定程度上调节支化度或交联度的醇的实例为三羟甲基丙烷、甘油或糖。还可以使用不仅具有羟基而且具有对异氰酸酯有反应性的其他基团的一元醇，实例为具有一个或更多伯氨基和/或仲氨基的一元醇例如单乙醇胺。
特别是当链扩展和交联反应意欲在水的存在下进行时，使用具有2个或更多伯氨基和/或仲氨基的多胺，这是因为胺与异氰酸酯的反应速度通常大于醇或水与异氰酸酯的反应速度。当需要交联聚氨酯或高分子量的聚氨酯的水分散体时，这通常是一个必要条件。在这种情况下，方法是制备具有异氰酸酯基团的预聚物，使这些预聚物快速分散在水中，并且然后通过具有对异氰酸酯有反应性的多个氨基的化合物的加成而使其进行链扩展或交联。适于此目的的合适的胺通常为摩尔质量为32至500g/mol，优选60至300g/mol的多官能胺，其中这些胺包括至少两个选自伯氨基和仲氨基的氨基。其实例为二胺，例如二氨基乙烷、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、肼水合物、或三胺如二亚乙基三胺或1,8-二氨基-4-氨甲基辛烷。
这些胺还可以以封端形式使用，例如相应的酮亚胺（参见例如CA-A1129128）、酮连氮（参见例如US-A4269748）或胺盐（参见US-A4292226）形式。噁唑烷（例如US-A4192937中使用的那些）
也是可以用于制备本发明的聚氨酯的封端的多胺，从而使预聚物链扩展。当使用该类封端的多胺时，其通常在无水存在下与预聚物混合，然后该混合物与分散体水或与一部分分散体水混合，以通过水解释放相应的多胺。
优选使用二胺和三胺的混合物，特别优选使用异佛尔酮二胺（IPDA）和二亚乙基三胺（DETA）的混合物。
作为单体(d)，聚氨酯优选包含1至30mol%，特别是4至25mol%的具有至少2个对异氰酸酯有反应性的氨基的多胺，基于组分(b)和(d)的总量计。为相同目的，作为组分(d)，还可以使用官能度高于2的异氰酸酯。市售化合物的实例为异氰脲酸酯或六亚甲基二异氰酸酯的缩二脲。
可以任选同时使用的单体(e)为单异氰酸酯、一元醇和一元伯胺和一元仲胺。所述单体(e)的比例通常最高为10mol%，基于单体的总摩尔量计。所述的一元化合物通常具有其他官能团（实例为烯基或羰基）并且其被用于将官能团引入至聚氨酯，其中这些官能团使得聚氨酯分散以及进行交联或其他聚合物类反应。可以用于该目的的单体为例如异丙烯基-α,α-二甲基苄基异氰酸酯（TMI）和丙烯酸或甲基丙烯酸的酯例如丙烯酸羟乙酯或甲基丙烯酸羟乙酯。
如果使用的单体(a)基本上仅为脂族二异氰酸酯、脂环族二异氰酸酯或芳脂族二异氰酸酯，则特别获得具有特别良好的特性曲线的粘合剂。在优选的方法中，所述的单体结合物被二羟基单羧酸或二氨基单羧酸的碱金属盐作为组分(c)所补充；在本文中Na盐是最合适的。
通过选择互相具有反应性的单体比例，以及选择每个分子中反应性官能团的算术平均数而调节聚氨酯分子量的方法在聚氨酯化学领域是熟知的。一般方法选择组分(a)至(e)，以及这些组分各自的摩尔量，以使A:B的比例为0.5:1至2:1，特别是0.8:1至1.5，特别优选为0.9:1至1.2:1，A:B比例非常特别优选尽可能地接近1:1，其中
A为异氰酸酯基团的摩尔量并且
B为羟基的摩尔量和在加成反应中可以与异氰酸酯反应的官能团的摩尔量的总和。
所用的单体(a)至(e)通常具有平均1.5至2.5个，优选1.9至2.1个，特别优选2.0个异氰酸酯基团，还可具有在加成反应中可以与异氰酸酯反应的官能团。
用于制备聚氨酯的结构组分的加聚反应在最高达180℃的反应温度（优选最高达150℃）、在大气压力或自生压力下进行。聚氨酯和聚氨酯水分散体的制备分别为本领域技术人员所已知。聚氨酯优选为水分散体形式并且以该形式使用。聚合物分散体的pH优选被调节至pH为高于5，特别是pH为5.5至8.5。
本发明使用的粘合剂包含羧酸基团并且优选包含其他反应性基团，其中这些基团可以互相或与外交联剂进行交联反应。优选存在的所述反应性基团的量为0.0001至0.5mol/100g粘合剂，特别优选为0.0005至0.5mol/100g粘合剂。羧基还可以通过水解反应形成，并且因此还可以在聚氨酯中不含任何初始的羧基时进行交联。
在本发明一个实施方案中，聚氨酯分散体粘合剂包括至少有一种外交联剂。合适的交联剂的实例为具有至少2个异氰酸酯基团的多异氰酸酯例如由二异氰酸酯形成的异氰脲酸酯、具有至少1个碳二亚胺基团的化合物、化学封端的异氰酸酯、被包覆的异氰酸酯、被包覆的脲二酮、缩二脲或脲基甲酸酯。氮丙啶、噁唑啉和环氧化物也是合适的。所用的外交联剂的量优选为0.5至10重量%，基于分散体的固含量计。外交联剂为在交联反应前没有键合至聚氨酯而是分散或溶解于聚氨酯分散体中的化合物。然而，也可以使用已经键合至聚氨酯的交联剂（内交联剂）。
在本发明中，本发明的聚氨酯分散体以水性粘合剂制剂的形式用于制备层压材料，即以水性层压粘合剂制剂的形式用于粘合大表面积基底；所述聚氨酯分散体可以特别用于制备复合箔。
因此，本发明还提供通过使用包含至少一种本发明的聚合物分散体的水性粘合剂制剂来制备复合箔的方法。本文中的聚合物水分散体可以以其自身使用或在用常规助剂进一步加工后使用。常规助剂的实例为润湿剂、增稠剂、保护胶体、光稳定剂、杀生物剂、消泡剂等。本发明的粘合剂制剂不需要加入塑化树脂（增粘剂）或其他增塑剂。在制备复合箔的方法中，至少两个基底用聚合物水分散体彼此粘合。所述基底为大面积的柔性组件，其中至少一个基底为并且优选两个基底均为一个或多个聚合物箔。
在本发明制备复合箔的方法中，本发明的聚合物分散体或相应的经进一步加工的制剂优选使用0.1至20g/m2，特别优选1至7g/m2的层厚通过例如刮除（doctoring）、铺展等施用于待粘合的基底。可以使用常规的涂覆方法例如辊涂、反向辊涂、凹版辊涂(gravure-rollcoating)、反向凹版辊涂、刷涂、杆涂、喷涂、气刷涂、面涂(meniscuscoating)、幕涂或浸涂。短时间空气干燥分散体的水后（优选1至60秒），将涂覆的基底层压至第二基底，其温度可以为例如20至200℃，优选20至100℃，并且其压力为例如100至3000kN/m2，优选300至2000kN/m2。
在一个实施方案中，本发明的聚合物分散体作为单组分组合物施用，即没有另外的交联手段，特别是不含异氰酸酯交联剂。然而，本发明的聚合物分散体还可以作为二组分粘合剂施用，其中加入交联组分例如可水乳化的异氰酸酯。至少一个基底可以被金属化或印刷在涂覆有粘合剂的面上。至少一个基底、优选两个基底为可生物分解的。
有利的是通过挤出涂覆方法将可生物分解的聚合物（第一基底）施用于第二基底。上述水性层压粘合剂制剂（聚合物分散体）作为中间层施用。在挤出涂覆方法中使用层压粘合剂制剂的优点源于可以降低挤出温度。所用的温和条件节约能量并且防止可分解聚合物的任何分解。
为了本发明的目的，当物质或物质组合物根据DINEN13432的生物降解的百分比为至少90%时，所述物质或物质混合物符合“可生物分解或可降解”的特征。
生物降解通常导致聚酯（混合物）在合适的和可能的时间段内分解。降解可以为酶解、水解、氧化降解和/或通过接触电磁辐射例如UV辐射而进行降解，并且大多数时主要由于接触微生物例如细菌、酵母菌、真菌和藻类而进行降解。生物降解性可以通过例如使聚酯与堆肥混合并且使其储存特定的时间而量化。例如在DINEN13432中，不含CO2的空气在堆肥过程中通过熟肥，并且使堆肥经历限定的温度曲线。本文中的生物降解度定义为生物降解的百分比，其为由样品释放的CO2净量（减去由不含样品的堆肥释放的CO2量）与可以由样品释放的CO2最大量（由样品的碳含量计算）的比例。可生物降解的聚酯（混合物）通常在堆肥仅数天后即显示出明显的降解标志，例如真菌生长、破裂和穿孔。
测定生物降解度的其他方法记载于例如ASTMD5338和ASTMD6400-4中。
合适的基底的实例为由下列制成的箔：木素、淀粉、纤维素材料、聚乳酸（PLA）、聚乳酸立构复合物（PLLA-PDLA）、聚乙醇酸（PGA）、脂族聚酯、脂族-芳族共聚酯和聚羟基烷酸酯、玻璃纸、聚碳酸丙烯酯（PPC）和上述材料的混合物。脂族聚酯的实例为聚丁二酸丁二醇酯（PBS）、聚丁二酸丁二醇酯-共聚-己二酸丁二醇酯（PBSA）、聚丁二酸丁二醇酯-共聚-癸二酸丁二醇酯（PBSSe）、聚己内酯（PCL）和聚环十五烷内酯。脂族-芳族共聚酯的实例为聚己二酸丁二醇酯-共聚-对苯二酸丁二醇酯（PBAT）、聚癸二酸丁二醇酯-共聚-对苯二酸丁二醇酯（PBSeT）、聚壬二酸丁二醇酯-共聚-对苯二酸丁二醇酯（PBAzeT）、聚十三烷二酸丁二醇酯-共聚-对苯二酸丁二醇酯（PBBrasT）。特别合适的材料的实例为箔，例如F或FS。聚羟基烷酸酯的实例为聚-3-羟基丁酸酯(PHB)、聚-3-羟基丁酸酯-共聚-3-羟基戊酸酯(P(3HB)-共聚-P(3HV))、聚-3-羟基丁酸酯-共聚-4-羟基丁酸酯(P(3HB)-共聚-P(4HB))、聚-3-羟基丁酸酯-共聚-3-羟基己酸酯(P(3HB)-共聚-P(3HH))。特别合适的混合物为脂族-芳族共聚酯与PLA的混合物（例如箔）或脂族聚酯、脂族-芳族共聚酯或聚乙烯醇与淀粉的混合物（例如箔）。
箔还可以是金属涂覆的，例如铝涂覆的（金属化的）聚合物箔（简称为：金属化箔）。上述箔可以例如已用印刷油墨印刷。第一基底的材料优选选自木素、淀粉、纤维素材料、聚乳酸、聚乙醇酸、脂族聚酯、脂族-芳族共聚酯、聚羟基烷酸酯、聚碳酸丙烯酯、以及上述材料的混合物，并且第二基底的材料优选选自纸、木素、淀粉、纤维素材料、聚乳酸、聚乙醇酸、脂族聚酯、脂族-芳族共聚酯、聚羟基烷酸酯、聚碳酸丙烯酯、以及上述材料的混合物。
在本发明的一个实施方案中，第一箔和/或第二箔在各自用本发明的聚合物分散体涂覆的面上金属化或印刷。基底膜的厚度可以为例如5至100μm，优选5至40μm。
特别优选复合箔，其中第一基底的材料为纸并且第二基底的材料为聚乳酸或包含聚乳酸并且包含脂族-芳族共聚酯的混合物。
如上所述，这些复合箔可以通过层压方法或挤出方法制备。WO
2010/034712描述了用于纸涂覆的有利的挤出方法，以及优选用于此目的的可生物分解的聚合物，并且所述文件明确地通过引用的方式并入本文。WO2010/034712中的挤出方法通过第一基底和第二基底之间的本发明的层压粘合剂层而补充。
分散体涂料在施用前不需要加热。如果涉及片状涂层，则施用技术与热熔粘合剂的施用技术类似。纸幅速度非常高：最高达3000m/min。因此分散体涂覆方法还可以在造纸机流水线上进行。
对于薄层，还可以以热熔体形式将可生物分解的聚合物以挤出涂覆方法或分散体施用方法的具体形式施用至某种程度。所述方法描述于Ullmann,TSETrollerCoating。热熔粘合剂（热熔体）由预加热至约150至200℃的进料罐泵入喷嘴，通过该喷嘴将材料施用于表面。
挤出涂覆方法已进行了开发从而将薄聚合物层以100至600m/min的高纸幅速度施用于柔性基底例如纸、纸板或具有金属层的多层箔。可生物分解的聚合物可以在现有用于聚乙烯的挤出涂覆系统中加工(J.Nentwig:Kunststofffolien[Plasticsfoils],HanserVerlag,Munich2006,p.195;H.J.Saechtling:KunststoffTaschenbuch[Plasticshandbook],HanserVerlag,Munich2007,p.256;C.Rauwendaal:PolymerExtrusion,HanserVerlag,Munich2004,p.547)。
“纸产品”用作基底。为本发明的目的，术语“纸产品”包括所有类型的纸，特别是纸板。
适于制备纸产品的纤维为常规使用的任何类型，例如机械纸浆、漂白和未漂白的化学纸浆、由任何一年生植物和废纸而得的纸浆（包括碎解形式的涂覆或未涂覆的纸浆）。所述纤维可以单独使用或以任何需要的这些纤维的混合物形式使用以制备纸浆，由纸浆可制备纸产品。术语机械纸浆包括例如磨木浆、热机械纸浆（TMP）、化学热机械纸浆（CTMP）、压力磨木浆、半化学纸浆、高产量化学纸浆和盘磨机械浆（RMP）。例如硫酸盐纸浆、亚硫酸盐纸桨和碱法纸浆为合适的化学纸浆。适于制备纸浆的一年生植物的实例为稻、小麦、甘蔗和红麻。
在每种情况下就固体而言，通常将0.01至3重量%，优选0.05至1重量%用量的胶料(size)加入化学纸浆，基于干纸物质计，并且所述用量根据所需待抛光的纸的上胶程度改变。纸可以另外包含其他物质，例如淀粉、颜料、染料、荧光增白剂、杀生物剂、纸张增强剂、固色剂、消泡剂、助留剂和/或助滤剂。
所制备的牛皮纸衬板（复合箔）优选具有以下结构：
i)30至600g/m2，优选40至400g/m2，并且特别优选50至
150g/m2克重的纸，
ii)厚度为1至100μm，优选5至80μm，并且特别优选10至60μm的可生物分解的聚合物层。
可以将非常宽范围的材料用于纸层，例如白色或棕色牛皮纸衬板、纸浆、废纸、瓦楞状材料或筛屑。
纸箔复合物的总厚度一般为31至1000g/m2。优选可以将层压用于制备80-500μm的纸箔复合物，并且挤出涂覆可以特别优选地用于制备50-300μm的纸箔复合物。
在用本发明聚合物分散体涂覆之前不是必须进行表面涂覆箔基底。然而，如果在涂覆工序前对箔基底的表面进行改性则可以获得更好的结果。本文中可以使用常规的表面处理（实例为电晕处理）以增强粘合效果。进行电晕处理或其他的表面处理至涂料组合物充分润湿所需的程度。使用约10瓦特/(米2·分钟)的电晕处理对于所述目的通常是足够的。作为替代方案或此外还可以在箔基底和粘合剂涂层之间任选地使用底层涂料或中间层。复合箔还可以具有其他额外的功能层例如阻挡层、印刷层、色彩层、漆层或保护层。其中功能层的位置可以在外部，即在背对粘合剂涂覆面的箔基底的面，或在内部，即箔基底和粘合剂层之间。
本发明的复合箔内，第二基底（例如纸）受到保护以抵御矿物油和其他类型的油，以及抵御脂肪和水分，这是因为第一基底（例如可生物分解的聚合物箔）发挥了合适的阻挡效果。另一方面，当复合箔用于食品包装时，食物受保护以抵御例如废纸中存在的矿物油和矿物质，这是因为第一基底（例如可生物降解的聚合物箔）发挥了所述的阻挡效果。此外，因为复合箔可以与自身紧密结合以及紧密结合至纸、纸板和金属，其可以制备例如咖啡杯、饮料纸盒或冷冻产品的纸盒。
复合箔特别适于制备干燥食物例如咖啡、茶、汤粉、粉末酱的纸袋；液体例如化妆品、清洁组合物、饮料的纸袋；管状层压物；纸运输袋、纸层压物和用于冰淇淋、甜食（例如巧克力棒和穆兹利(muesli)棒）的共挤出物和纸粘合胶带；纸杯、酸奶罐；即用餐托盘；弯曲纸板容器（罐、卷筒）、外包装（酒瓶、食物）的湿强度纸盒；由涂覆的纸板制成的水果盒；快餐盘；夹壳（clampshells）；饮料纸盒和液体（例如洗涤剂和清洗组合物）用纸盒、冷冻产品的纸盒、冰包装材料（例如冰杯、圆锥形冰淇淋威化饼的包装材料）；纸标签；花盆和植物盆。
本发明制备的复合箔特别适于制备柔性包装材料，特别是用于食品包装。
本发明的优点在于本发明使用的聚氨酯粘合剂分散体可以提供各种基底彼此的良好粘合，赋予粘合的复合物以高强度。本发明制备的复合箔的特征还有良好的生物降解性。
实施例
实施例1
将996.77g由己二酸和1,4-丁二醇制备的聚酯二醇（OH数=43.9）和0.13g四丁基钛酸酯（TBOT）溶解于260g的丙酮然后加热至60℃，在65℃下与46.2g甲苯二异氰酸酯反应1小时；然后混合物在66℃下再与44.6g的六亚甲基二异氰酸酯反应3.5小时。然后混合物用1040g丙酮稀释并冷却至50℃。此时NCO含量为0.5%。然后使用51.2g40%强度的氨基乙基氨基丙酸的钠盐的水溶液15分钟以进行链扩展，并且混合物使用1638g去离子水分散。真空中在最高达43℃的温度下蒸馏移除丙酮，并且将固含量调节至40%。
分析值：LD:87.5；粘度：32mPas；K值51；pH:8.0
实施例2
将400g由己二酸和间苯二甲酸1:1的混合物与1,6-己二醇制备的聚酯二醇（OH数=56）与20.1g二羟甲基丙酸和150g丙酮在40℃下搅拌，并且在外部温度为90℃下与112g六亚甲基二异氰酸酯反应3小时。然后混合物用550g丙酮稀释并冷却至30℃。NCO含量为2%。使用12g三乙胺以进行中和并且使用34g异佛尔酮二胺以进行链扩展。然后混合物使用650g去离子水分散，然后立即用溶于100g去离子水的8.2g二亚乙基三胺交联。真空中在最高达42℃的温度下通过蒸馏移除丙酮。
分析值：固含量44%；LD:80；粘度：21mPas
实施例3（对比实施例，不可降解）
在100℃下，801g聚环氧丙烷二醇（OH数为56）与64.4g二羟甲基丙酸和溶于70g丙酮中的153.3g甲苯二异氰酸酯反应6小时。然后混合物用800g丙酮稀释并冷却至30℃。NCO含量<0.2%。使用与50g去离子水混合的8.64gNaOH（50%强度）以进行中和，然后混合物使用650g去离子水分散。真空中在最高达42℃的温度下通过蒸馏移除丙酮，并且将分散体的固含量调节至60%。
分析值：LD:42；粘度：185mPas；K值：42;pH:6.4
实施例4（根据WO96/35733实施例3的对比）
将510g由己二酸和2:1的1,6–己二醇/新戊二醇制备的聚酯二醇（OH数=57）在真空中和外部温度120℃下脱水，氮气下加入0.6g的苯甲酰氯和90.3g的六亚甲基二异氰酸酯，并且混合物在内部温度115℃下反应30分钟。使用1500g丙酮进行稀释并冷却至50℃。此时NCO含量为1%。使用由29.08g50%强度的氨基乙基氨基乙磺酸的钠盐的水溶液、4.5g乙二胺和60g去离子水制备的混合物15分钟以进行链扩展，并且通过使用900g去离子水15分钟以制备分散体。真空中在最高达51℃的温度下通过蒸馏移除丙酮。
分析值：固含量：46%；LD:44；粘度16.4mPas；K值：77；pH6.4
实施例5（含有交联剂）
将基于六亚甲基二异氰酸酯计3重量%用量（相当于使用7.5重量%的固体）的异氰脲酸酯加入至实施例1的分散体中。
堆肥测试
通过在玻璃皿中于60℃下干燥本发明实施例1和4的分散体来制备箔。箔的直径为4.5cm并且厚度为1mm。将箔埋在堆肥中并且在58℃下培育。定期对箔进行视觉评价和称重。
起始：
实施例1：重量：100%
实施例4：重量：100%
3周后：
实施例1：重量：约90%，表面粗糙、不平、几乎穿孔、降解显著
实施例4：重量：约96%；表面粗糙、降解非常少
6周后：
实施例1：重量：约70%，表面非常不平且具有许多大小最大为5mm的穿孔；降解非常显著
实施例4：重量：约93%；与3周后的评价视觉上无差别
聚氨酯分散体的生物降解性：
根据ISO14855(2005)通过分析释放的二氧化碳而对实施例1、2、3和5的水分散体进行生物降解性测试。以百分比测定的生物降解度定义为以CO2形式释放的气态碳与所用材料的总碳含量的比例。表1对该结果进行了整理。
表1：聚氨酯分散体的生物降解度
| 实施例 | 20天后的降解度[%] | 28天后的降解度[%] |
| 实施例1 | 70 | 79 |
| 实施例2 | 34 | 39 |
| 实施例3 | 0 | 0 |
| 实施例5 | 90 | 95 |
复合箔的分解：
根据标准EN13432(2000)，如果最长12周的好氧堆肥后发现，受试材料的干重为原干重的最多10%并以>2mm的筛分粒级存在，则该包装材料具有足够的通过分解而降解的特性（degradabilitybydisintegration）。
通过用实施例1的聚氨酯分散体涂覆由聚乳酸制备的箔并且使其粘合至由聚乳酸制备的第二箔来制备复合箔。复合箔总厚度为49μm。根据EN13432(2000)测定分解度。
最长12周后发现2mm筛分粒级的复合箔的残留量为8.2%。因此，该箔通过堆肥的分解度符合EN13432标准的条件，因此具有良好的降解性。
Claims (12)
1.聚氨酯水分散体粘合剂用于制备可生物分解的复合箔的用途，其中使用聚氨酯分散体粘合剂将至少一个第一基底粘合至至少一个第二基底，其中至少一个所述基底为根据标准EN13432(2000)可生物分解的聚合物箔，其中至少60重量％的聚氨酯由以下物质构成：
(a)至少一种二异氰酸酯，
(b)至少一种聚酯二醇，和
(c)至少一种选自二羟基羧酸和二氨基羧酸的二官能羧酸，
其中所述聚氨酯分散体粘合剂为根据ISO14855(2005)可生物降解的。
2.前述权利要求的用途，其中至少80重量％的聚氨酯由至少一种聚酯二醇(b)构成。
3.权利要求1或2的用途，其中至少80重量％的至少一种聚酯二醇(b)由至少一种脂族二羧酸和至少一种脂族二醇构成。
4.权利要求1或2的用途，其中聚氨酯由以下物质构成：
a)至少一种二异氰酸酯，
b)至少一种二醇，其中所述二醇中
b1)10至100mol％为摩尔质量为500至5000g/mol的聚酯二醇，基于二醇(b)的总量计，
b2)0至90mol％的摩尔质量为60至500g/mol，基于二醇(b)的总量计，
c)至少一种二官能羧酸，其选自二羟基羧酸和二氨基羧酸，
d)任选的不同于单体(a)至单体(c)并且具有反应性基团的其他多官能化合物，其中所述反应性基团为醇羟基、伯氨基或仲氨基、或异氰酸酯基团，以及
e)任选的不同于单体(a)至单体(d)并且具有反应性基团的单官能化合物，所述反应性基团为醇羟基、伯氨基或仲氨基或异氰酸酯基团。
5.权利要求1或2的用途，其中所述聚氨酯分散体粘合剂包含至少一种外交联剂。
6.权利要求5的用途，其中所述交联剂选自由二异氰酸酯形成并且具有至少2个异氰酸酯基团的异氰脲酸酯、具有至少一个碳二亚胺基团的化合物、化学封端的异氰酸酯、被包覆的异氰酸酯、被包覆的脲二酮、缩二脲、脲基甲酸酯、氮丙啶、噁唑啉、环氧化物以及所述物质的混合物。
7.权利要求1或2的用途，其中第一基底的材料选自木素、淀粉、纤维素材料、聚乳酸、聚乙醇酸、脂族聚酯、脂族-芳族共聚酯、聚羟基烷酸酯、聚碳酸丙烯酯以及所述材料的混合物，并且第二基底的材料选自纸、木素、淀粉、纤维素材料、聚乳酸、聚乙醇酸、脂族聚酯、脂族-芳族共聚酯、聚羟基烷酸酯、聚碳酸丙烯酯以及所述材料的混合物。
8.权利要求1或2的用途，其中第一基底的材料为纸并且第二基底的材料为聚乳酸或包含聚乳酸且包含脂族-芳族共聚酯的混合物。
9.权利要求1或2的用途，用于制备柔性包装材料。
10.一种制备复合箔的方法，包括提供具有权利要求1至6任一项中的基于聚氨酯的特征的聚氨酯水分散体粘合剂，和使用所述聚氨酯水分散体粘合剂使至少两个基底彼此粘合，其中至少一个基底为可生物分解的聚合物箔。
11.一种制备复合箔的方法，包括通过挤出涂覆将第一基底——一种可生物分解的聚合物——施用至第二基底，并施用具有权利要求1至6任一项中的基于聚氨酯的特征的聚氨酯水分散体粘合剂作为中间层。
12.权利要求10或11制备的复合箔。
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| US8698036B1 (en) | 2013-07-25 | 2014-04-15 | Hypertherm, Inc. | Devices for gas cooling plasma arc torches and related systems and methods |
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| CN115697689A (zh) | 2020-06-09 | 2023-02-03 | 巴斯夫欧洲公司 | 回收粘接制品的方法 |
| EP4237247A1 (en) | 2020-07-28 | 2023-09-06 | Société des Produits Nestlé S.A. | A container for beverage preparation |
| US20230390167A1 (en) | 2020-10-30 | 2023-12-07 | Basf Se | Process for producing microparticles laden with an aroma chemical |
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| TW202338038A (zh) * | 2021-09-28 | 2023-10-01 | 瑞士商雀巢製品股份有限公司 | 可生物降解層壓膜及由其製成之容器 |
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| WO2024074562A1 (en) | 2022-10-06 | 2024-04-11 | Basf Se | Thermoplastic polymer blend and use thereof |
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| WO2012013506A1 (de) | 2012-02-02 |
| EP2598546B1 (de) | 2019-04-10 |
| JP2013537574A (ja) | 2013-10-03 |
| CN103038270A (zh) | 2013-04-10 |
| JP6029584B2 (ja) | 2016-11-24 |
| ES2734266T3 (es) | 2019-12-05 |
| EP2598546A1 (de) | 2013-06-05 |
| BR112013001530A2 (pt) | 2016-05-24 |
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