CN103975107B - 具有阻挡涂层的纸和纸板包装 - Google Patents
具有阻挡涂层的纸和纸板包装 Download PDFInfo
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- CN103975107B CN103975107B CN201280060137.5A CN201280060137A CN103975107B CN 103975107 B CN103975107 B CN 103975107B CN 201280060137 A CN201280060137 A CN 201280060137A CN 103975107 B CN103975107 B CN 103975107B
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- monomer
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- 238000000576 coating method Methods 0.000 claims abstract description 42
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Abstract
本发明描述了由矿物油污染(例如再循环)纸生产的纸或纸板包装,其中该包装包含可通过施涂聚合物水分散体而得到的阻挡层,所述聚合物水分散体包含可通过(甲基)丙烯酸C1‑C4烷基酯、酸单体如丙烯酸或甲基丙烯酸、0‑20重量%丙烯腈和0‑10重量%其它单体在含水介质中在碳水化合物,优选降解淀粉形式的碳水化合物的存在下乳液聚合而得到的共聚物,其中共聚物的玻璃化转变温度为+10℃至+45℃。阻挡层可位于包装的一个表面上或者形成多层包装涂层的多层中的一层,或者作为涂层位于置于包装内的内袋的一侧上。
Description
本发明涉及由矿物油污染(例如再循环)纸生产且具有可通过施涂聚合物水分散体而得到的阻挡层的纸或纸板包装,所述聚合物水分散体包含可通过(甲基)丙烯酸C1-C4烷基酯、酸单体和任选其它单体在碳水化合物的存在下乳液聚合而得到的共聚物,其中共聚物的玻璃化转变温度为+10至+45℃。阻挡层可位于包装的一个表面上,或者形成多层包装涂层的多层中的一层,或者作为涂层位于置于包装内的内袋一侧上。本发明还涉及聚合物分散体在制备以防挥发性疏水有机物质的阻挡层中的用途。
纸板包装通常由再循环纸生产。在印刷纸,尤其是新闻纸的情况下,再循环纸可包含来自常用于印刷新闻纸的印刷油墨的矿物油残留物。甚至是室温下,挥发物从这些残留物中蒸发,并且在食品包装的情况下沉积在包装在盒子中的食品如意大利面制品、麦麸、米或脆玉米片上。甚至多数由聚合物膜构成的目前所用内袋不提供合适的保护。ZurichCantonal Laboratory进行的研究检测到包装在由再循环纸生产的包装中的食品中明显水平的矿物油残留物。挥发性矿物油组分主要是已知为健康顾虑的链烷烃和环烷烃,和芳族烃,尤其是具有15-25个碳原子的那些。
因此,需要降低食品被矿物油残留物或可能削弱包装产品质量的其它挥发性有机化合物污染的风险。这组包括例如目前争议的来自染料、增塑剂、光引发剂和其它来源的环境毒害和毒物,其可借助纸再循环方法而终止于包装中:例如异丙基硫杂蒽(ITX)、二苯甲酮、4-甲基二苯甲酮、邻苯二甲酸的酯、脂肪酸酯、脂肪酸酰胺(例如芥酸酰胺)。一个可能是省去辛烷值在生产食品包装中的再循环。这由于生态原因是不理想的且由于新纤维素的不充分可用性是不可行的。另一解决方法是省去新闻印刷用印刷油墨中的矿物油。但这遭遇工艺障碍,特别是关于纸表面上印迹的耐擦除性。油脂和油防水阻挡涂层是包装领域中已知的。WO2006/053849例如描述了用于纸和纸板的基于水基聚合物组合物的涂料。聚合物显示出良好的对液体多脂物质的屏障性能,但它显示出这未必还提供对以气体形式透过的物质的良好屏障效应,因为透过物质的传送机制是不同的。在液体油和油脂的情况下,传送经由纤维进行,为此毛细力和表面润湿起一份作用。在具有以气体形式传送的物质的问题的情况下,重要的不是毛细作用和润湿,而是吸着、扩散和孔隙率。
另外,还需要具有关于其它不关键但迁移性疏水物质如芳香的屏障性能的涂料。
公开号EP11168090.6和EP11168097.1的欧洲专利申请(美国公开号61/491248和61/491250)描述了具有阻挡涂层的纸和纸板包装。其中所述聚合物分散体提供对挥发性矿物油组分的良好屏障。然而,存在其中涂料组合物暴露于高剪切力,其中涂料组合物变得不稳定的某些应用技术,这在许多涂料应用中具有破坏效应。涂覆方法可例如导致在转辊和滚柱上形成凝结物,在刮板或刮刀上形成凝结物,或者在泵送操作中形成凝结物,或者在印刷方法(例如柔版印刷及其它)中在辊上形成碎片。
本发明的目的是提供尽管使用矿物油污染的再循环纸,但降低包装内容物被挥发性矿物油组分污染的风险,或者通常提供保护以防包装产品受通过包装的挥发性有机化合物削弱,或者赋予芳香屏障且还可使用非常剪切稳定的涂料组合物可靠地生产的包装。
该目的根据本发明通过至少部分由矿物油污染(例如再循环)纸生产的纸或纸板包装实现,其中包装包含至少一层可通过施涂聚合物水分散体而得到的阻挡层,所述聚合物水分散体包含至少一种可通过如下单体乳液聚合而得到的共聚物:
(a)一种或多种选自(甲基)丙烯酸C1-C4烷基酯的主要单体,
(b)0.1-5重量%的一种或多种例如选自丙烯酸和甲基丙烯酸的酸单体,
(c)0-20重量%丙烯腈,和
(d)0-10重量%的除单体(a)-(c)之外的其它单体,
其中共聚物的玻璃化转变温度为+10℃至+45℃,
其中乳液聚合在含水介质中在至少一种碳水化合物的存在下进行,
其中阻挡层可位于包装的一个或多个表面上,或者阻挡层可形成多层包装涂层的多层中的至少一层,或者阻挡层可作为涂层位于置于包装内的内袋的至少一侧上。包装特别适用于食品。
令人惊讶地发现聚合中碳水化合物的使用,尤其是降解多糖,即短链碳水化合物(例如麦芽糖糊精、葡萄糖浆)的使用导致所得聚合物分散体的剪切稳定性的明显改善,且出乎意料地,对屏障性能不具有不利影响。
矿物油污染应当理解意指纸包含不能通过常规分析方法检测到的量的具有至多25个碳原子的挥发性烃,尤其是挥发性链烷烃、挥发性环烷烃和/或挥发性芳族烃。挥发性烃为具有至多25个碳原子,例如5-22个碳原子的烃。在本发明一个实施方案中,矿物油污染来自印刷油墨,且包含挥发性链烷烃、挥发性环烷烃和/或挥发性芳族烃。
挥发性疏水有机化合物具有在20℃下在水中小于1重量%,优选小于0.1重量%的溶解度和小于500,优选小于350的分子量。
在下文中,名称“(甲基)丙烯…”和类似名称用作“丙烯…或甲基丙烯…”的缩写表示。
根据本发明使用的聚合物分散体是聚合物在含水介质中的分散体。含水介质可例如为完全无离子的水或者水与可溶混溶剂如甲醇、乙醇或四氢呋喃的混合物。优选不使用有机溶剂。分散体的固体含量优选为15-75重量%,更优选40-60重量%,更特别是50重量%以上。固体含量可例如通过乳液聚合中所用水量和/或单体量的适当调整而设置。分散在水分散体中的聚合物颗粒的中值粒度优选为400nm以下,更特别是300nm以下。中值粒度更优选为70-250nm或80-150nm。中值粒度在此处指粒度分布的d50值,即所有颗粒总质量的50重量%具有小于d50值的粒径。粒度分布可以以已知方式使用分析超速离心机测定(W.Makromolekulare Chemie185(1984),第1025-1039页)。聚合物分散体的pH可设置为pH4以上,尤其是5-9的pH。
根据本发明使用的共聚物为通过可自由基聚合单体乳液聚合而得到的乳液聚合物。共聚物由一种或多种选自(甲基)丙烯酸C1-C4烷基酯的主要单体(a)形成。主要单体(a)优选以基于100重量%所有单体的总和不小于70重量%,更优选不小于75重量%,例如79.5-99.5重量%使用。特别优选的主要单体(a)选自丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸乙酯和丙烯酸正丁酯。
共聚物由一种或多种酸单体(b)形成。酸单体为具有至少一个酸基团的烯属不饱和可自由基聚合单体,例如具有羧酸、磺酸或膦酸基团的单体。优选羧酸基团。丙烯酸、甲基丙烯酸、衣康酸、马来酸或富马酸例如是合适的。酸单体(b)优选选自丙烯酸和甲基丙烯酸。酸单体(b)以基于所有单体的总和0.1-5重量%,优选0.5-5重量%使用。
共聚物可任选由基于所有单体的总和0-20重量%的丙烯腈作为其它单体(c)形成。在本发明一个实施方案中,共聚物由1-20重量%,优选2-20重量%丙烯腈形成。
共聚物可任选由除单体(a)-(c)之外的其它单体(d)形成。其它单体(d)的量基于所有单体的总和为0-10重量%或0-5重量%。一个实施方案使用0.1-10重量%或0.1-5重量%其它单体(d)。另一实施方案不使用除单体(a)-(c)之外的其它单体。
其它单体(d)可选自(甲基)丙烯酸C5-C20烷基酯、包含至多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烃、除丙烯腈之外的烯属不饱和腈、乙烯基卤化物、包含1-10个碳原子的醇的乙烯基醚、具有2-8个碳原子和一个或两个双键的脂族烃或其混合物。(甲基)丙烯酸C5-C10烷基酯如丙烯酸2-乙基己酯例如是合适的。(甲基)丙烯酸烷基酯的混合物也是特别合适的。具有1-20个碳原子的羧酸的乙烯基酯例如为月桂酸乙烯酯、硬脂酸乙烯酯、丙酸乙烯酯、叔戊酸乙烯酯和乙酸乙烯酯。有用的乙烯基芳族化合物包括乙烯基甲苯、α-甲基苯乙烯、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,优选苯乙烯。甲基丙烯腈是腈的实例。乙烯基卤化物为氯-、氟-或溴-取代的烯属不饱和化合物,优选氯乙烯和偏二氯乙烯。乙烯基甲基醚和乙烯基异丁基醚是合适乙烯基醚的实例。优选包含1-4个碳原子的醇的乙烯基醚。作为具有4-8个碳原子和2个烯烃双键的烃,可提到丁二烯、异戊二烯和氯丁二烯。丙烯酸和甲基丙烯酸C5-C10烷基酯和乙烯基芳烃,尤其是苯乙烯及其混合物优选作为其它单体(d)。非常特别优选丙烯酸正己基酯、丙烯酸辛酯和丙烯酸2-乙基己酯、丙烯酸2-丙基庚酯、苯乙烯及其混合物。其它单体(d)还包括例如含羟基单体,尤其是(甲基)丙烯酸C1-C10羟基烷基酯以及(甲基)丙烯酰胺。有用的其它单体(d)进一步包括苯氧基乙二醇单(甲基)丙烯酸酯、丙烯酸缩水甘油酯、甲基丙烯酸缩水甘油酯、氨基(甲基)丙烯酸酯如(甲基)丙烯酸2-氨基乙酯。也可提到交联单体作为其它单体(d)。
在本发明一个实施方案中,共聚物可由如下单体得到:
(a)79.5-99.5重量%的一种或多种选自(甲基)丙烯酸C1-C4烷基酯的主要单体,
(b)0.5-5重量%的一种或多种选自丙烯酸和甲基丙烯酸的酸单体,
(c)0-20重量%丙烯腈,且
不具有除单体(a)-(c)之外的其它单体。
根据类型和量调整共聚物的单体使得乳液聚合物的玻璃化转变温度为+10℃至+45℃,优选+15℃至+40℃。玻璃化转变温度可通过差示扫描量热法(ASTM D3418-08“中点温度”)测定。
乳液聚合在至少一种碳水化合物的存在下进行。碳水化合物可选自低聚糖(由2-10个糖单元构成)和多糖(由多于10个糖单元构成),尤其选自降解多糖,优选降解淀粉、降解半纤维素或降解脱乙酰壳多糖。特别优选麦芽糖糊精和葡萄糖浆。乳液聚合优选使用10-200重量份,更优选20-150重量份或30-150重量份碳水化合物每100重量份待聚合单体。
用于制备根据本发明使用的降解淀粉的有用起始淀粉包括所有天然淀粉,例如来自玉米(玉米)、小麦、燕麦、大麦、稻、小米、马铃薯、豆类、木薯、高粱或西米的淀粉。重要的还有具有高支链淀粉含量的那些天然淀粉,例如蜡玉米淀粉和蜡马铃薯淀粉。这些淀粉的支链淀粉含量为90%以上,通常95-100%。通过醚化或酯化化学改性的淀粉也可用于制备本发明聚合物分散体。这类产品是已知且市售的。它们例如通过将天然淀粉或降解天然淀粉用无机或有机酸、它们的酐或氯化物酯化而制备。特别重要的是磷酸化和乙酰化降解淀粉。将淀粉醚化的最常用方法是将淀粉在碱性水溶液中用有机卤化合物、环氧化物或硫酸盐处理。已知的淀粉醚为烷基醚、羟烷基醚、羧烷基醚和烯丙基醚。淀粉与2,3-环氧基丙基三甲基氯化铵的反应产物也是有用的。特别优选降解天然淀粉,更特别是降解成麦芽糖糊精或葡萄糖浆的天然淀粉。其它合适的淀粉包括阳离子改性淀粉,即具有氨基或铵基团的淀粉化合物。淀粉的降解可以通过酸或碱的作用酶、氧化或水解进行。降解淀粉是市售的。然而,也可首先将天然淀粉在含水介质中例如酶降解,在酶降解停止以后,在所得降解淀粉的水溶液或分散体中根据本发明进行单体的乳液聚合。碳水化合物,更特别是降解淀粉具有例如小于0.07dl/g或小于0.05dl/g的固有粘度ηi。固有粘度ηi优选为0.02-0.06dl/g。固有粘度ηi根据DIN EN1628在23℃的温度下测定。
DE值是表征多糖,更特别是本领域中非常常用的淀粉的降解度的可选方式。DE表示葡萄糖当量,并指干物质中还原糖的百分数含量。它相当于每100g干物质具有相同还原能力的葡萄糖(=葡萄糖)的量。DE值为聚合物降解进行至何种程度的度量;因此具有低DE值的所得产物保持高多糖含量和低的低分子量糖含量,而具有高DE值的产物主要仅由恰低分子量糖构成。合适降解淀粉的实例为麦芽糖糊精和葡萄糖浆。优选的麦芽糖糊精具有不小于约0.04至0.06dl/g的固有粘度、3-20的DE值和15000-20000g/mol的摩尔质量Mw。优选的葡萄糖浆具有0.02-0.04dl/g的固有粘度、20-30的DE值和3000-6000g/mol的摩尔质量Mw。由于它们的制备方法,这些产物以水溶液的形式得到,它们也直接商业化。这类麦芽糖糊精溶液具有50-70%的固体含量,而合适葡萄糖浆溶液具有70-95%的固体含量。然而,尤其是麦芽糖糊精也可以以喷雾干燥的形式作为粉末得到。
共聚物可以通过乳液聚合得到,在这种情况下考虑乳液聚合物。乳液聚合通常使用离子和/或非离子乳化剂和/或保护胶体/稳定剂作为表面活性化合物以增加含水介质中的单体分散体。保护胶体为在溶解时结合大量水且能够稳定水不溶性聚合物的分散体的聚合物。不同于乳化剂,它们通常不降低聚合物颗粒与水之间的表面张力。合适保护胶体的详细描述在Houben-Weyl,Methoden der organischen Chemie,第XIV/1卷,MakromolekulareStoffe,Georg-Thieme-Verlag,Stuttgart,1961,第411-420页中找到。有用的保护胶体包括例如两亲聚合物,即具有疏水和亲水基团的聚合物。可考虑天然聚合物如淀粉或合成聚合物。有用的乳化剂包括阴离子和非离子表面活性物质,其数均分子量通常为2000g/mol以下或者优选1500g/mol以下,而保护胶体的数均分子量通常为2000g/mol以上,例如2000-100000g/mol,更特别是5000-50000g/mol。阴离子和非离子乳化剂优选用作表面活性物质。合适的乳化剂为例如具有3-50的乙氧基化度的乙氧基化C8-C36脂肪醇,具有3-50的乙氧基化度的乙氧基化单-、二-和三-C4-C12烷基苯酚,磺基琥珀酸的二烷基酯的碱金属盐、C8-C12烷基硫酸酯的碱金属和铵盐,C12-C18烷基磺酸的碱金属和铵盐,以及C9-C18烷基芳基磺酸的碱金属和铵盐。当乳化剂和/或保护胶体(共同)用作用于分散单体的辅助剂时,其用量基于单体例如为0.1-5重量%。乳化剂的商品名例如为2A1、NP50、OC50、Emulgator825、Emulgator825S、OG、NSO、904S、I-RA、Lumiten E3065、ISC、NLS、Disponil LDBS20、Disponil FES77、Lutensol AT18、Steinapol VSL、Emulphor NPS25。表面活性物质通常以基于待聚合单体0.1-10重量%的量使用。
乳液聚合温度通常为30-130℃,优选50-90℃。聚合也可在压力下,例如在至多15巴,例如2-10巴的压力下进行。聚合介质可仅由水组成,但也可由水与溶混性液体如甲醇的混合物组成。优选仅使用水。乳液聚合不仅可以作为分批操作,而且以进料流添加方法的形式,包括分级或梯度模式进行。优选进料流添加方法,其中起初加入一部分聚合批料,加热至聚合温度,初始聚合,随后通常经由其中一种或多种包含纯或乳化形式的单体的两个或更多空间分离进料流与其余聚合批料连续或分阶段地混合。
乳液聚合方法可使用惯常已知的助剂,例如水溶性引发剂和链转移剂。用于乳液聚合的水溶性引发剂为例如过二硫酸的铵盐或碱金属盐,例如过氧二硫酸钠、过氧化氢或有机过氧化物,例如叔丁基过氧化氢。氧化还原(还原-氧化)引发剂体系也是合适的。氧化还原引发剂体系由一种或多于一种通常无机还原剂和一种或多于一种有机或无机氧化剂组成。氧化组分包括例如用于乳液聚合的上述引发剂。还原组分为例如亚硫酸的碱金属盐,例如亚硫酸钠、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成化合物,例如丙酮亚硫酸氢盐,或还原剂,例如羟基甲烷亚磺酸及其盐,或抗坏血酸。氧化还原引发剂体系可以与可溶性金属化合物一起使用,其中金属组分可以两种或更多种价态存在。通常的氧化还原引发剂体系例如为抗坏血酸/硫酸铁(II)/过氧二硫酸钠、叔丁基过氧化氢/焦亚硫酸钠、叔丁基过氧化氢/羟基甲烷亚磺酸钠或叔丁基过氧化氢/抗坏血酸。各组分,例如还原组分也可以为混合物,例如羟基甲烷亚磺酸钠盐和焦亚硫酸钠的混合物。所述化合物通常以水溶液的形式使用,其中下限浓度由分散体中可容许的水量决定,上限浓度由所述化合物在水中的溶解度决定。通常,浓度基于溶液为0.1-30重量%,优选0.5-20重量%,更优选1.0-10重量%。引发剂的量基于待聚合单体通常为0.1-10重量%,优选0.5-5重量%。两种或更多种不同的引发剂也可用于乳液聚合中。为除去残留单体,引发剂还通常在实际乳液聚合结束以后加入。
在本发明方法的一个实施方案中,起初将至少15重量%引发剂与至少一些碳水化合物和任选种子胶乳一起装入含水介质中,并将单体和其余引发剂在聚合条件下计量加入该初始进料中。除引发剂和任选种子胶乳外,初始进料中还包含总待聚合单体的1-10重量%。然后在聚合开始以后,将其余单体、其余引发剂和任何碳水化合物在聚合条件下计量加入初始进料中,但单体和引发剂优选彼此分开地加入。在聚合条件下应当理解意指初始进料中的反应混合物已加热至进行聚合时的必需温度。
聚合在碳水化合物的存在下进行,所述碳水化合物可起初与单体一起装入或加入聚合容器中。任选可在聚合以后加入另一部分碳水化合物。
链转移剂可以例如基于100重量份待聚合单体0-0.8重量份的量用于聚合中,其降低摩尔质量。合适的链转移剂包括例如具有硫醇基团的化合物,例如叔丁基硫醇、丙酸巯基乙酯、巯基乙酸2-乙基己酯、巯基乙酸乙酯、巯基乙醇、巯基丙基三甲氧基硅烷、正十二烷基硫醇或叔十二烷基硫醇。另外可使用不具有硫醇基团的链转移剂,例如萜品油烯。在一个优选实施方案中,乳液聚合物使用基于单体量0.05-0.5重量%的至少一种链转移剂制备。
用于涂覆包装的聚合物分散体仅可由分散于水中的乳液聚合物组成以根据本发明使用。然而,所述聚合物分散体还可包含其它附加物质,例如填料、防粘剂、染料、流动调节剂、颜料、基料或增稠剂。
聚合物分散体也可以为纸涂料组合物的一部分,和/或与常用于纸涂层片中的颜料和基料组合,条件是屏障效应不因此过度受损。除水外,纸涂料组合物通常包含颜料、基料和用于设置必需流变性能的辅助剂如增稠剂。纸涂料组合物通常包含基于总固体含量优选至少80重量%,例如80-95重量%或80-90重量%的量的颜料。特别预期白色颜料。合适的颜料包括例如金属盐颜料,例如硫酸钙、铝酸硫酸钙、硫酸钡、碳酸镁和碳酸钙,其中优选碳酸盐颜料,更特别是碳酸钙。碳酸钙可以为天然粉碎碳酸钙(GCC)、沉淀碳酸钙(PCC)、石灰或白垩。合适的碳酸钙颜料可例如作为60、60或90ME得到。其它合适的颜料包括例如二氧化硅、氧化铝、铝水合物、硅酸盐、二氧化钛、氧化锌、高岭土、粘土、滑石或二氧化硅。合适的其它颜料可例如作为MP50(粘土)、90(粘土)或Talcum C10得到。
在本发明一个实施方案中,至少一种共聚物与基于1重量份共聚物例如至多1重量份颜料,优选片状颜料组合使用。片状颜料的实例为滑石、粘土或云母(云母)。优选滑石。优选的纵横比(长度:厚度比)为10以上。
根据本发明使用的聚合物分散体可与其它不同的聚合物基料组合使用,条件是屏障效应不会因而过度受损。优选其它基料以不大于20重量份、不大于10重量份、不大于5重量份的量使用,都基于100重量份碳水化合物,或者根本不使用。纸涂料组合物中记录的最重要功能是将颜料粘合在纸上并将颜料彼此粘合,并一定程度地填充颜料颗粒之间的空隙。对于每100重量份颜料,所用有机基料的量(根据基料固体,即不具有水或在21℃,1巴下为液体的其它溶剂)例如为1-50重量份,优选1-25重量份或5-20重量份。有用的其它基料包括天然基基料,更特别是基于淀粉的基料,以及合成基料,更特别是可通过乳液聚合得到的乳液聚合物。基于淀粉的基料在本文中应当理解指在聚合以后加入的任何天然、改性或降解淀粉。天然淀粉可由直链淀粉、支链淀粉或其混合物组成。改性淀粉可包括氧化淀粉、淀粉酯或淀粉醚。可使用水解降低淀粉(降解淀粉)的分子量。可能的降解产物包括低聚糖或糊精。优选的淀粉为谷类淀粉、玉米淀粉和马铃薯淀粉。特别优选谷类淀粉和玉米淀粉,非常特别优选谷类淀粉。
不同于根据本发明使用的聚合物的其它合成基料优选至少40重量%的程度,优选至少60重量%的程度,更优选至少80重量%的程度由所谓的主要单体组成。主要单体选自(甲基)丙烯酸C1-C20烷基酯、包含至多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烃、烯属不饱和腈、乙烯基卤化物、包含1-10个碳原子的醇的乙烯基醚、具有2-8个碳原子和一个或两个双键的脂族烃或其混合物。实例包括具有C1-C10烷基结构部分的(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-乙基己酯。(甲基)丙烯酸烷基酯的混合物也是特别合适的。具有1-20个碳原子的羧酸的乙烯基酯例如包括月桂酸乙烯酯、硬脂酸乙烯酯、丙酸乙烯酯、叔戊酸乙烯酯和乙酸乙烯酯。有用的乙烯基芳族化合物包括乙烯基甲苯、α-甲基苯乙烯、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,优选苯乙烯。腈的实例为丙烯腈和甲基丙烯腈。乙烯基卤化物为氯-、氟-或溴-取代的烯属不饱和化合物,优选氯乙烯和偏二氯乙烯。合适乙烯基醚的实例为乙烯基甲基醚和乙烯基异丁基醚。优选包含1-4个碳原子的醇的乙烯基醚。具有2-8个碳原子和一个或两个烯烃双键的烃的实例为乙烯、丙烯、丁二烯、异戊二烯和氯丁二烯。
优选的主要单体为(甲基)丙烯酸C1-C10烷基酯及其与乙烯基芳烃,更特别是苯乙烯或具有两个双键的烃,更特别是丁二烯的混合物,或者这类烃与乙烯芳烃,更特别是苯乙烯的混合物。在脂族烃(更特别是丁二烯)与乙烯基芳烃(更特别是苯乙烯)的混合物的情况下,比可例如为10:90-90:10,更特别是20:80-80:20。特别优选的主要单体为丁二烯和丁二烯与苯乙烯的上述混合物。除主要单体外,用作基料的乳液聚合物可包含其它单体,例如具有羧酸、磺酸或膦酸基团的单体。优选羧酸基团。具体实例为丙烯酸、甲基丙烯酸、衣康酸、马来酸和富马酸。乳液聚合物中烯属不饱和酸的含量通常为10重量%以下,优选8重量%以下,且至少0.1重量%或至少1重量%。其它单体包括例如含羟基单体,更特别是(甲基)丙烯酸C1-C10羟基烷基酯,或酰胺如(甲基)丙烯酰胺。
基质上的聚合物分散体涂层充当阻挡层。特别有效的阻挡层通过使用共聚物得到,由此具有共聚物的涂层具有在23℃下小于80g/m2d,优选小于50g/m2d,更优选小于10g/m2d,甚至更优选小于5g/m2d或小于1g/m2的气体正己烷渗透性,和在纸上5-30g/m2的涂布重量(参见下文所述实施例中的测量方法)。
用于涂覆的分散体中至少一种共聚物的含量优选为至少1重量%,更特别是至少5重量%且至多60或至多75重量%。优选水分散体中至少一种共聚物的含量为15-75重量%或40-60重量%。优选的共聚物水分散体具有在pH4和20℃下10-150000mPas或50-5000mPas(在20℃下用Brookfield粘度计测量,100rpm,心轴4)的粘度。分散于水分散体中的共聚物颗粒的中值粒度为例如0.02-100μm,优选0.05-10μm。它可使用例如光学显微术、光散射或冰冻断裂电子显微术测定。
颜料与屏障聚合物的重量比优选为0:100-75:25。当其它固体组分仍存在于整个体系中时,所有固体组分的总和与屏障聚合物的重量比优选为不大于90:10或80:20。
根据本发明,将载体基质用至少一种上述共聚物的水分散体涂覆。合适基质特别是纸、纸板和聚合物膜/板。用于涂覆的分散体可包含其它附加或辅助物质,例如增稠剂以设置流变,润湿辅助剂或基料。
为使用涂料组合物,将它例如在涂覆机上施涂于纸、纸板或聚合物载体膜/板上。当使用网时,聚合物分散体通常借助施涂辊从槽中施涂,并使用气刷变平。施涂涂层的其它方法包括例如反相凹版方法、喷雾方法或辊刮刀或本领域技术人员已知的其它涂覆方法。将载体基质在至少一侧上涂覆,即可将它一侧或两侧涂覆。用于纸和纸板的施涂方法的实例为幕涂、气刀、棒涂覆或刮板涂覆。用于膜/板涂覆的施涂方法的实例为刮刀、线绕杆、气刷、对向转辊施涂方法、对向转凹版涂覆、流延头或喷嘴。
在碳水化合物的存在下得到的聚合物分散体具有改善的剪切稳定性,所以特别用于其中涂料组合物暴露于高剪切负荷下的施涂方法。优选的施涂方法因此为刮板涂覆和柔版印刷。因此,本发明还提供生产上述本发明包装的方法,其中聚合物水分散体通过柔版印刷施涂于包装基质上。
施涂于板状材料上的量在聚合物膜/板的情况下优选为1-10g(聚合物固体)/m2,优选2-7g/m2,或者纸或纸板的情况下优选为5-30g/m2,优选5-15g/m2。在将涂料组合物施涂于载体基质上以后,将溶剂/水蒸发。为此,在连续方法的情况下,可引导材料通过可装配有例如红外线照射装置的干燥器导管。其后,引导涂覆且干燥的材料通过冷却辊,最后卷绕。干燥涂层的厚度优选为至少1μm,更特别是1-50μm,更优选2-30μm或5-30μm。
阻挡层可位于包装的至少一个表面上。它也可形成多层包装涂层的多层中的至少一层,或者它可作为涂层位于包装内的内袋的至少一侧上。阻挡涂层可直接施涂于载体材料的表面上;然而,仍另外的层可位于载体与阻挡涂层之间,例如底漆层、其它阻挡层或者有色或黑色和白色印刷油墨层。阻挡层优选位于包装的内侧上,所述侧面对包装内容物。
内袋优选由聚合物膜/板构成。内袋的材料优选选自聚烯烃,优选聚乙烯或定向聚丙烯,而聚乙烯不仅可通过乙烯的高压聚合方法,而且可通过低压聚合方法制备。为仍进一步改善在膜/板上的附着力,可首先使载体膜/板经受电晕处理。其它合适的载体膜/板例如为具有聚酯如聚对苯二甲酸乙二醇酯的膜/板,具有聚酰胺、聚苯乙烯和聚氯乙烯的膜/板。在一个实施方案中,载体材料包含可生物降解膜/板,例如可生物降解脂族-芳族共聚酯和/或聚乳酸的膜/板,例如或膜/板。合适的共聚酯例如由链烷二醇,尤其是C2-C8链烷二醇如1,4-丁二醇,脂族二羧酸,尤其是C2-C8二羧酸如己二酸,或芳族二羧酸如对苯二甲酸形成。载体膜/板的厚度通常为10-200μm。
为得到对膜/板和包装介质而言特异性的表面或涂层性能,例如良好的可印刷性,仍更好的屏障或阻挡行为、良好的防水性,可有利地将涂覆基质用还赋予这些所需性能的覆盖层再涂覆,或者使阻挡涂层经受电晕处理。根据本发明预涂覆的基质显示出良好的再涂性。再涂覆也可使用以上所述方法中的一种进行,或者同时多重涂覆可例如通过使用幕涂机以连续操作进行而不中间卷绕和展开膜/板或纸。本发明阻挡层因此位于体系内部,覆盖层然后决定表面性能。覆盖层具有在阻挡层上良好的附着力。
本发明还提供生产包装的方法,所述方法包括提供上述聚合物水分散体形式的组合物,施涂于包装基质或内袋表面上并干燥,其中聚合物水分散体包含上述共聚物中的至少一种。
本发明还提供包含上述共聚物中的至少一种的聚合物水分散体在制备芳香阻挡层或以防挥发性疏水有机化合物的阻挡层,优选以防挥发性矿物油组分的阻挡层,更特别是在生产包装,更特别是食品包装中的用途。
根据本发明涂覆的基质显示出以防挥发性疏水有机化合物,更特别是以防挥发性矿物油组分的显著屏障性能。涂覆基质本身可用作包装介质。涂层例如具有非常好的机械性能并显示出良好的阻挡行为。用于涂覆的聚合物分散体显示出高剪切稳定性。
实施例
除非上下文中另外提出,百分数为重量计。所报告的含量涉及水溶液或分散体中的含量。
使用以下输入材料:
MMA 甲基丙烯酸甲酯
MA 丙烯酸甲酯
AS 丙烯酸
S 苯乙烯
nBA 丙烯酸正丁酯
AN 丙烯腈
C Dry MD01915:麦芽糖糊精(Cargill)
C Sweet01403:葡萄糖浆(Cargill)
C Plus10998:液体麦芽糖糊精(Cargill)
S505用于纸和纸板涂覆的基料,苯乙烯/丙烯酸酯/丙烯腈共聚物,约50%浓度
Finntalc 滑石粉,片状颜料
HG90 90碳酸钙颜料
实施例1-3:聚合物分散体的制备(对比分散体)
将反应器用氮气清洗并加入450.0g软化水和3.0g乳化剂(LDBS20,在水中20%)作为初始进料。将初始进料中的混合物加热至70-90℃。然后加入21.43g过氧二硫酸钠(7%浓度),然后搅拌50分钟。将由240.0g水、26.67g乳化剂(Dowfax2A1,在水中45%)和600.0g根据表1的单体混合物组成的乳液进料经2小时计量加入反应器中。在乳液进料结束以后使体系聚合45分钟。然后将反应器冷却至室温。固体含量:约45%
实施例4-7:碳水化合物稳定化聚合物分散体的制备
将反应器用氮气清洗并以表1的量加入427.1g软化水和C Dry MD01915(94.7%浓度)。将初始进料中的混合物加热至86℃。然后加入3.2g过氧二硫酸钠(7%浓度),然后搅拌5分钟。将由180.0g水、20.0g乳化剂(2A1,45%浓度)和450.0g根据表1的单体混合物组成的乳液进料计量经2小时加入反应器中。与乳液进料同时,开始引发剂进料(12.9g过氧二硫酸钠,7%浓度)并同样经2小时计量加入。在乳液进料结束以后使体系聚合45分钟。然后将反应器冷却至室温。固体含量:根据表1。
实施例8:用葡萄糖浆稳定化的聚合物分散体的制备
将反应器用氮气清洗并加入351.8g软化水和312.5g C Sweet01403葡萄糖浆(72%浓度)。将初始进料中的混合物加热至86℃。然后加入3.2g过氧二硫酸钠(7%浓度),然后搅拌5分钟。将由180.0g水、20.0g乳化剂(Dowfax2A1,45%浓度)和450.0g的根据表1的单体混合物组成的乳液进料经2小时加入反应器中。与乳液进料同时,开始引发剂进料(12.9g过氧二硫酸钠,7%浓度)并同样经2小时计量加入。在乳液进料结束以后使体系聚合45分钟。然后将反应器冷却至室温。固体含量:根据表1。
表1:共聚物组成,量以重量%表示
实施例 | 单体 | 降解淀粉[pphm]1) | Tg | 固体含量(%) |
1 | 55MA/44MMA/1AS | - | 约50℃ | 45 |
2 | 14S/69nBA/14AN/3AS | - | 约5℃ | 45 |
3 | 55EA,44MMA,1AS | - | 30℃ | 45 |
4 | 55EA,44MMA,1AS | 30 | 30℃ | 47 |
5 | 55EA,44MMA,1AS | 50 | 30℃ | 50 |
6 | 55EA,44MMA,1AS | 75 | 30℃ | 54 |
7 | 55EA,44MMA,1AS | 100 | 30℃ | 57 |
8 | 55EA,44MMA,1AS | 50 | 30℃ | 50 |
1)重量份每100重量份单体
实施例9-14:碳水化合物稳定化聚合物分散体的制备
将反应器用氮气清洗并以表2的量加入软化水和C Plus10998麦芽糖糊精(94.7%浓度)。将初始进料中的混合物加热至86℃。然后加入3.2g过氧二硫酸钠(7%浓度),然后搅拌5分钟。将由180.0g水、20.0g乳化剂(Dowfax2A1,45%浓度)和450.0g单体混合物(4.5g丙烯酸、198.0g甲基丙烯酸甲酯和247.5g丙烯酸乙酯)组成的乳液进料经2小时计量加入反应器中。与乳液进料同时,开始引发剂进料(12.9g过氧二硫酸钠,7%浓度)并同样经2小时计量加入。在乳液进料结束以后使体系聚合45分钟。然后将反应器冷却至室温。
表2:共聚物组成/淀粉,量以重量%表示
实施例 | 降解淀粉[pphm]1) | 初始进料中的水量[g] | 固体含量(%) |
9 | 30 | 180 | 50 |
10 | 50 | 180 | 50 |
11 | 75 | 180 | 51 |
12 | 100 | 180 | 51 |
13 | 150 | 158 | 51 |
14 | 200 | 135 | 51 |
1)重量份每100重量份单体
实施例15(对比例)
类似于实施例3,不同之处在于在聚合以后混入C Plus10998麦芽糖糊精(30pphm)。
实施例16(对比例)
C Plus10998液体麦芽糖糊精
涂覆纸通过使用手动涂布器或实验室涂布器将试验组合物以25-28g/m2涂布重量施涂于亚光标准纸上总共两次涂覆和干燥而生产。
对气体矿物油组分的屏障试验
将9ml己烷倒入包含海绵的容器中并用具有开口和密封环(内径63mm)的盖密封。将开口用待测试屏障材料紧紧地密封,同时屏障材料不与己烷浸润的海绵接触。测量容器的重量降低。重量降低是经由气相通过屏障材料离开的己烷的度量,因此为对气体矿物油组分的屏障性能的度量。将以g表示的重量降低转化成1m2纸面积,然后作为g/m2d报告。
剪切稳定性试验
将100g试验组合物在1升方形瓶中用具有锯齿状搅拌盘的Pentraulik搅拌器以8000rpm的速度搅拌5分钟。在剪切以后,将试验组合物通过125μ筛过滤,在70℃下干燥2小时,将滤渣算术地投射到1kg试验组合物上,并作为剪切稳定性的度量评估。得到的滤渣越少,在剪切过程中形成的凝结物越少,且剪切稳定性越大。
孔试验
将具有蓝色染料的试验油(具有2%苏丹蓝的松节油或油酸)用脱脂棉球擦在涂有试验组合物的基质表面上,并立即用脱脂棉球的干净区域除去。孔和未涂覆的位置立刻变色,完整涂层上的油可除去而不引起任何着色。通过目测检查评估试验面积。变色越小,涂覆表面上孔的不存在性越大。
试验结果汇总于表3和4中。
表3:实施例1-7的试验结果
1)重量份每100重量份单体
结果显示本发明实施例4-7显示出在剪切稳定性、己烷渗透性和孔形成方面有利性能的最好组合。
表4:实施例9-16的试验结果
1)重量份每100重量份单体
结果显示碳水化合物的最佳量为30-150pphm且当碳水化合物在聚合期间已经存在时剪切稳定性有利。
实施例17-21:有色纸涂层片
制备具有根据表5的组成的纸涂层片。将涂层片用增稠剂(HT)调整至约1500-2000mPas(Brookfield100/min)的粘度并用NaOH调整至约8.2-8.3的pH。屏障试验结果汇总于表5中。
表5:实施例17-21的组合物,量以基于固体含量的重量份表示
Claims (26)
1.至少部分地由矿物油污染纸生产的纸或纸板包装,其中所述包装包含至少一层可通过施涂聚合物水分散体而得到的阻挡层,所述聚合物水分散体包含至少一种可通过如下单体的乳液聚合而得到的共聚物:
(a)一种或多种选自(甲基)丙烯酸C1-C4烷基酯的主要单体,
(b)0.1-5重量%一种或多种酸单体,
(c)0-20重量%丙烯腈,和
(d)0-10重量%的除单体(a)-(c)之外的其它单体,
其中共聚物的玻璃化转变温度为+10℃至+45℃,
其中乳液聚合在含水介质中在至少一种碳水化合物的存在下进行,
其中阻挡层可位于包装的一个或多个表面上,或者阻挡层可形成多层包装涂层的多层中的至少一层,或者阻挡层可作为涂层位于置于包装内的内袋的至少一侧上,
其中共聚物至少70重量%的程度由主要单体(a)构成,矿物油污染包括挥发性链烷烃、挥发性环烷烃和/或挥发性芳族烃。
2.根据权利要求1的包装,其中碳水化合物选自降解多糖。
3.根据权利要求1的包装,其中碳水化合物选自降解淀粉、降解半纤维素或降解脱乙酰壳多糖。
4.根据权利要求1或2的包装,其中碳水化合物选自具有小于0.07dl/g的固有粘度ηi的降解多糖。
5.根据权利要求1或2的包装,其中碳水化合物选自具有0.02-0.06dl/g的固有粘度ηi的降解多糖。
6.根据权利要求1-3中任一项的包装,其中乳液聚合使用10-200重量份碳水化合物每100重量份单体。
7.根据权利要求1-3中任一项的包装,其中乳液聚合使用20-150重量份碳水化合物每100重量份单体。
8.根据权利要求1-3中任一项的包装,其中主要单体(a)选自丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸乙酯和丙烯酸正丁酯。
9.根据权利要求1-3中任一项的包装,其中共聚物可由如下单体得到:
(a)79.5-99.5重量%的一种或多种选自(甲基)丙烯酸C1-C4烷基酯的主要单体,
(b)0.5-5重量%的一种或多种选自丙烯酸和甲基丙烯酸的酸单体,
(c)0-20重量%丙烯腈,且
不具有除单体(a)-(c)之外的其它单体。
10.根据权利要求1-3中任一项的包装,其中共聚物的玻璃化转变温度为+15℃至+40℃。
11.根据权利要求1-3中任一项的包装,其中其它单体(d)选自(甲基)丙烯酸C5-C20烷基酯、包含至多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烃、除丙烯腈之外的烯属不饱和腈、乙烯基卤化物、包含1-10个碳原子的醇的乙烯基醚、具有2-8个碳原子和一个或两个双键的脂族烃及其混合物。
12.根据权利要求1-3中任一项的包装,其中共聚物与每1重量份共聚物至多1重量份颜料组合使用。
13.根据权利要求1-3中任一项的包装,其中共聚物与每1重量份共聚物至多1重量份具有10以上的纵横比的片状颜料组合使用。
14.根据权利要求1-3中任一项的包装,其中共聚物以15-75重量%的量包含在用于制备阻挡涂层的聚合物水分散体中。
15.根据权利要求1-3中任一项的包装,其中共聚物以40-60重量%的量包含在用于制备阻挡涂层的聚合物水分散体中。
16.根据权利要求1-3中任一项的包装,其中具有共聚物的涂层具有在23℃下小于50g/m2d的气体正己烷渗透性和在纸上5-30g/m2的涂布重量。
17.根据权利要求1-3中任一项的包装,其中阻挡层作为涂层位于置于包装内的内袋的至少一侧上,且内袋的材料选自聚烯烃。
18.根据权利要求1-3中任一项的包装,其中阻挡层作为涂层位于置于包装内的内袋的至少一侧上,且内袋的材料选自聚乙烯或定向聚丙烯。
19.根据权利要求1-3中任一项的包装,其中阻挡层厚度为2-30μm。
20.生产根据权利要求1的包装的方法,所述方法包括提供聚合物水分散体形式的组合物且施涂于包装基质或内袋表面上并干燥,其中聚合物水分散体包含至少一种共聚物,所述共聚物具有基于根据权利要求1-15中任一项的聚合物分散体的特征。
21.根据权利要求20的生产包装的方法,其中聚合物水分散体通过印刷方法施涂于包装基质上。
22.根据权利要求20的生产包装的方法,其中聚合物水分散体通过柔版印刷施涂于包装基质上。
23.包含至少一种具有基于根据权利要求1-15中任一项的聚合物分散体的特征的共聚物的聚合物水分散体在制备以防挥发性疏水有机化合物的阻挡层中的用途。
24.根据权利要求23的用途,其中挥发性疏水有机化合物具有在20℃下在水中小于1重量%的溶解度和小于500的分子量。
25.根据权利要求23的用途,其中挥发性疏水有机化合物具有在20℃下在水中小于0.1重量%的溶解度和小于350的分子量。
26.根据权利要求23-25中任一项的用途,其中阻挡层为芳香阻挡层或者以防挥发性矿物油组分的阻挡层。
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- 2012-12-03 KR KR1020147018225A patent/KR20140106644A/ko not_active Application Discontinuation
- 2012-12-03 ES ES12794343.9T patent/ES2658896T3/es active Active
- 2012-12-03 JP JP2014545193A patent/JP6272774B2/ja not_active Expired - Fee Related
- 2012-12-03 CA CA2857715A patent/CA2857715A1/en not_active Abandoned
- 2012-12-03 US US14/360,803 patent/US9950502B2/en active Active
- 2012-12-03 BR BR112014013066A patent/BR112014013066A2/pt not_active Application Discontinuation
- 2012-12-03 CN CN201280060137.5A patent/CN103975107B/zh active Active
- 2012-12-03 EP EP12794343.9A patent/EP2788549B1/en active Active
- 2012-12-03 PL PL12794343T patent/PL2788549T3/pl unknown
- 2012-12-03 WO PCT/EP2012/074189 patent/WO2013083504A1/en active Application Filing
- 2012-12-03 PT PT127943439T patent/PT2788549T/pt unknown
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CA2857715A1 (en) | 2013-06-13 |
BR112014013066A2 (pt) | 2017-06-13 |
KR20140106644A (ko) | 2014-09-03 |
JP2015500927A (ja) | 2015-01-08 |
EP2788549A1 (en) | 2014-10-15 |
US20150274350A1 (en) | 2015-10-01 |
EP2788549B1 (en) | 2017-11-08 |
PL2788549T3 (pl) | 2018-05-30 |
PT2788549T (pt) | 2018-01-12 |
ES2658896T3 (es) | 2018-03-12 |
US9950502B2 (en) | 2018-04-24 |
JP6272774B2 (ja) | 2018-01-31 |
WO2013083504A1 (en) | 2013-06-13 |
CN103975107A (zh) | 2014-08-06 |
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