CN103597045B - 包含具有脲基或脲基类似基团并具有缩水甘油基的聚合物的压敏粘合剂分散体 - Google Patents
包含具有脲基或脲基类似基团并具有缩水甘油基的聚合物的压敏粘合剂分散体 Download PDFInfo
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- CN103597045B CN103597045B CN201280028952.3A CN201280028952A CN103597045B CN 103597045 B CN103597045 B CN 103597045B CN 201280028952 A CN201280028952 A CN 201280028952A CN 103597045 B CN103597045 B CN 103597045B
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Abstract
本发明涉及一种含有聚合物P1的压敏粘合剂分散体。所述聚合物P1分散于水中并由乳液聚合形成。该聚合物P1由包含以下物质的单体混合物形成:(a)至少40重量%的(甲基)丙烯酸C4至C20烷基酯,其在聚合为均聚物时具有-30℃或更低的玻璃化转变温度;(b)至少0.05重量%的含有式(I)取代基的(甲基)丙烯酸酯单体,其中X代表CH2、O、NH或NR,并且R代表C1至C4烷基;和(c)至少0.1重量%的酸单体。
Description
本发明涉及一种包含水分散性聚合物P1的压敏粘合剂分散体,所述水分散性聚合物P1由含有以下物质的单体混合物通过乳液聚合形成:定义的(甲基)丙烯酸C4至C20烷基酯、定义的具有脲基或脲基类似基团的(甲基)丙烯酸酯单体、酸单体和任选地其他单体,或者所述单体混合物还包含(甲基)丙烯酸缩水甘油酯的单体混合物和/或所述压敏粘合剂分散体包含至少一种含有缩水甘油基的其他聚合物P2。
对于压敏粘合剂(PSAs),不仅需要对基材的有效粘合力(adhesion),而且需要粘合剂层内足够的内聚力(cohesion)(内部强度)。粘合力和内聚力是对立的性能特性。改善粘合力所采取的措施通常会同时导致内聚力的劣化,反之亦然。许多在室温下具有足够内聚力的PSAs,在高温下却不具有足够内聚力。然而,例如汽车行业或建筑行业中的很多应用——特别是在用于部件固定的胶带的情况下——即使在相对高的温度下也需要高内聚力而不产生粘合力的大幅劣化。
WO01/54896和EP822206描述了包含可通过乳液聚合获得且尤其是由具有脲基的(甲基)丙烯酸单体制备的聚合物的PSAs。与不具有脲基的聚合物相比,这些聚合物即使在高温下也产生改进的剪切强度(内聚力)和改进的粘合力。然而,需要实现在基于丙烯酸酯聚合物粘合产品的热稳定性方面的进一步改进。尽管EP710680还记载了尤其由具有脲基的(甲基)丙烯酸单体制备的水性聚合物分散体,但它们未构成压敏粘合剂。
本发明的一个目的是进一步改进PSAs的粘合特性,特别是用于部件固定的胶带的PSAs的粘合特性,并且实现粘合特性更好的温度稳定性。特别是所述PSAs即使在高温下也呈现出良好的内聚力,并且粘合力未受到严重的削弱或甚至得到提高。因此,已发现以下更详细地描述的PSA分散体。
本发明提供一种包含至少一种水分散性聚合物P1的压敏粘合剂分散体,所述水分散性聚合物P1由包含以下物质的单体混合物通过乳液聚合形成:
(a)至少60重量%的至少一种(甲基)丙烯酸C4至C20烷基酯,其在聚合为均聚物时具有-30℃或更低、优选-40℃或更低的玻璃化转变温度,
(b)至少0.05重量%的至少一种含有下式取代基的(甲基)丙烯酸酯单体
其中X为CH2、O、NH或NR,并且R为C1至C4烷基,
(c)至少0.1重量%的至少一种酸单体,
并且其中所述单体混合物或者包含至少0.05重量%的(甲基)丙烯酸缩水甘油酯和/或
其中所述压敏粘合剂分散体包含至少一种不同于聚合物P1且包含缩水甘油基的其他聚合物P2,
单体含量的数字各自基于所有单体的总和计。
本发明的PSA分散体包含由乳液聚合制备的聚合物作为关键组分;因此该分散聚合物为乳液聚合物。
在下文中,将术语“(甲基)丙烯酸酯”以及类似术语用作“丙烯酸酯或甲基丙烯酸酯”的缩写。
PSA是一种粘弹性粘合剂,其呈干态的固化膜在室温下(20℃)仍保持永久的粘性和粘合性。对基材的粘结通过温和施加压力而瞬间完成。PSA分散体是包含具有压敏粘合剂特性的聚合物——其在水中或水性介质中呈分散体——的组合物。
聚合物P1由第一单体类型(a)制备。单体类型(a)的存在量是至少60重量%,例如60%至95重量%,基于用于制备聚合物P1的单体的总量计。所述单体(a)选自(甲基)丙烯酸C4至C20烷基酯的那些,其在聚合成均聚物时具有-30℃或更低、或-40℃或更低、优选-45℃或更低的玻璃化转变温度。玻璃化转变温度可通过已知方法测定,实例为差热扫描量热法(参见,例如ASTM3418/82,“中点温度(Midpointtemperature)”)。优选的单体(a)为丙烯酸C4至C10烷基酯和甲基丙烯酸C4至C10烷基酯,更特别地为丙烯酸C4至C8烷基酯和甲基丙烯酸C4至C8烷基酯。特别优选的为丙烯酸正丁酯、丙烯酸正己酯、丙烯酸辛酯、丙烯酸2-乙基己酯或丁二烯,以及这些单体的混合物。
聚合物P1由第二单体类型(b)制备。单体类型(b)的存在量是至少0.05重量%,例如0.1%至5重量%,优选超过1重量%,例如1.5%至5重量%,基于用于制备聚合物P1的单体的总量计。
单体类型(b)为含有下式取代基的(甲基)丙烯酸酯单体
其中X为CH2、O、NH或NR,并且R为C1至C4烷基,且N原子上的箭头表示所述取代基与(甲基)丙烯酸酯单体的连接位置。当X为NH或NR时,该单体具有脲基。当X为O或CH2时,该单体被称为具有脲基类似基团的单体。单体(b)为例如以下式的那些
其中X定义如上,R为氢或甲基,并且A为二价连接基团,优选C1至C10烷基或C2至C4烷基。特别优选的是烷基中具有1至10个C原子、优选2至4个碳原子的(甲基)丙烯酸脲基烷基酯,更特别地为甲基丙烯酸脲基乙基酯(UMA)。
聚合物P1以至少0.1重量%、优选0.1%至5重量%、更优选0.2%至4重量%、非常优选0.5%至3重量%的量的酸单体形成,基于聚合物P1的单体总量计。酸单体为含有至少一个酸基团的烯键式不饱和、可自由基聚合的单体。酸单体为例如烯键式不饱和羧酸、烯键式不饱和磺酸以及乙烯基膦酸。所用的烯键式不饱和羧酸优选为分子中具有3至6个C原子的α,β-单烯键式不饱和的一元羧酸和二元羧酸。其实例有丙烯酸、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、丙烯酰胺基甲基丙磺酸、丙烯酸磺基丙酯和甲基丙烯酸磺基丙酯。优选丙烯酸和甲基丙烯酸及其混合物,特别优选丙烯酸。
用于形成聚合物P1的单体混合物可任选地包含其他单体(d),所述单体(d)不同于单体(a)-(c);换言之,单体(d)为在聚合成均聚物时具有超过-30℃、特别是超过-20℃、超过0℃或超过20℃的玻璃化转变温度的单体。受限于这些条件,所述单体(d)可选自:非(a)单体的(甲基)丙烯酸C1至C20烷基酯、(甲基)丙烯酸C1至C20羟基烷基酯、含有最高达20个碳原子的羧酸的乙烯酯、具有最高达20个碳原子的乙烯基芳族化合物、烯键式不饱和的腈、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个碳原子和一个或两个双键的脂族烃,或这些单体的混合物。所述单体(d)优选以1%至40重量%、更特别地以2%至30%的量使用,基于聚合物P1的单体总量计。实例包括具有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、丙烯酸乙酯、甲基丙烯酸乙酯。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、叔碳酸乙烯酯(Versatic acidvinyl esters)和乙酸乙烯酯。合适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。腈的实例有丙烯腈和甲基丙烯腈。所述乙烯基卤化物为被氯、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。乙烯基醚包括例如乙烯基甲醚和乙烯基异丁基醚。优选包含1至4个碳原子的醇的乙烯基醚。具有2至8个碳原子和一个或两个烯属双键的烃包括乙烯、丙烯、异戊二烯和氯丁二烯。特别优选作为其他单体的有丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸乙酯、苯乙烯、(甲基)丙烯酸C1-C10羟烷基酯和(甲基)丙烯酰胺,以及这些单体的混合物。一个实施方案使用0%-5重量%、优选0.05%至5重量%的(甲基)丙烯酸C1-C10羟烷基酯。
本发明的PSA分散体包含至少一种由以下单体形成的聚合物:所述单体包括至少一种具有至少一个缩水甘油基的单体。在本发明的一个实施方案中,聚合物P1由至少一种具有至少一个缩水甘油基的单体(e)形成。在本发明的另一个实施方案中,存在由至少一种聚合物P1和至少一种聚合物P2组成的聚合物共混物,所述聚合物P1不是由单体(e)形成,并且聚合物P2由至少一种单体(e)和任选的其他单体形成,但不是由类型(b)的单体形成。当然也可以是聚合物P1和P2的聚合物共混物,其中P1和P2均由单体(e)形成。
优选的具有缩水甘油基的单体(e)为(甲基)丙烯酸缩水甘油酯((甲基)丙烯酸2,3-环氧丙基酯)。特别优选的为甲基丙烯酸缩水甘油酯(GMA)。如果单体(e)为用于形成聚合物P1的单体混合物的部分,则其优选以0.1%至5重量%、更特别0.5%至3重量%的量存在,基于聚合物P1的单体的总量计。如果单体(e)为用于形成聚合物P2的单体混合物的部分,则其优选以1%至20重量%、更特别5%至15重量%的量存在,基于聚合物P2的单体的总量计。
一个优选的聚合物P1例如由以下物质合成:
60%至95重量%的单体(a)
0.1%至5重量%的单体(b)
0.1%至5重量%的酸单体(c)
2%至30重量%的其他单体(d)以及
0.1%至5重量%的(甲基)丙烯酸缩水甘油酯。
一个特别优选的聚合物P1例如由以下物质合成:
75%至90重量%的单体(a)
0.5%至3重量%的单体(b)
0.5%至2重量%的酸单体(c)
2%至20重量%的其他单体(d)以及
0.5%至3重量%的(甲基)丙烯酸缩水甘油酯。
聚合物P1的玻璃化转变温度优选-60至0℃,更优选-60至-10℃,以及非常优选-60℃-20℃。
玻璃化转变温度可通过常规方法例如差热扫描量热法(ASTM3418/82,“中点温度”)测定。
一个优选的聚合物P2例如由以下物质合成:
80%至99重量%的单体(a)和(d)
0.1%至5重量%的酸单体(c)
1%至20重量%的(甲基)丙烯酸缩水甘油酯。
在本发明的一个实施方案中,聚合物P2通过单体(a)、单体(c)、(甲基)丙烯酸缩水甘油酯和任选的单体(d)的单体混合物以对于聚合物P1指定的量聚合形成。
单体(b)(例如UMA)与单体(e)(例如GMA)的量或与用于P1和P2的单体(e)的总和的重量比优选地为0.1至10,更优选地为0.2至5。
聚合物P1和P2可通过乳液聚合制备,并且随着具有上述定义的烯键式不饱和可自由基聚合的单体通过自由基在水中引发的乳液聚合而聚合,然后其为乳液聚合物。为了支持单体在水性介质中的分散,可以使用通常用作分散剂的保护胶体和/或乳化剂。
对合适的保护胶体的全面描述见于Houben-Weyl,Methoden derorganischen Chemie,卷XIV/1,Makromolekulare Stoffe[Macromolecular Compounds],Georg-Thieme-Verlag,Stuttgart,1961,第411-420页。合适的乳化剂包括阴离子、阳离子和非离子界面活性物质,其数均分子量通常低于2000g/mol或优选低于1500g/mol,而保护胶体的数均分子量大于2000g/mol,例如2000至100000g/mol,更特别为5000至50000g/mol。对于界面活性物质,优选使用阴离子和非离子乳化剂。合适的乳化剂为例如乙氧基化度为3至50的乙氧基化C8-C36脂肪醇;乙氧基化度为3至50的乙氧基化单-烷基苯酚、双烷基苯酚-和三烷基苯酚;磺基琥珀酸二烷基酯的碱金属盐;C8至C12烷基硫酸酯的碱金属盐和铵盐;C12至C18烷基磺酸的碱金属盐和铵盐以及C9至C18烷基芳基磺酸的碱金属盐和铵盐。阳离子乳化剂为例如具有至少一个氨基或铵基以及至少一个C8-C22烷基的化合物。如果将乳化剂和/或保护胶体用作用于分散单体的助剂,则其使用量例如为0.1%至5重量%,基于单体计。乳化剂的商品名为例如A1、NP50、OC50、Emulgator825、Emulgator825S、OG、NSO、904S、I-RA、Lumiten E3065、Disponil FES77、Lutensol AT18、Steinapol VSL、Emulphor NPS25。界面活性物质通常以0.1%至10重量%的量使用,基于待聚合的单体计。
在乳液聚合中,通常使用用于单体的自由基聚合的水溶性引发剂。用于乳液聚合的水溶性引发剂为例如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,例如叔丁基过氧化氢。同样合适的有所谓的还原氧化(氧化还原)引发剂体系。所述氧化还原引发剂体系由至少一种常规的无机还原剂和有机或无机氧化剂组成。所述氧化组分包含例如上文已经定义的乳液聚合引发剂。所述还原组分包括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(如焦亚硫酸钠),脂族醛和酮的亚硫酸氢盐加成化合物(如丙酮亚硫酸氢盐),或诸如羟基甲烷亚磺酸及其盐的还原剂,或抗坏血酸。所述氧化还原引发剂体系可与金属组分能以多个价态存在的可溶性金属化合物一起使用。典型的氧化还原体系为例如抗坏血酸/硫酸亚铁(II)/过二硫酸钠、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。所述各个组分——例如还原组分——也可以是混合物,一个实例是羟基甲烷亚磺酸的钠盐与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,所述水溶液的较低浓度由分散体中可接受的水量确定,且较高浓度由各化合物在水中的溶解度决定。一般而言,该浓度为0.1重量%至30重量%,优选0.5重量%至20重量%,更优选1.0重量%至10重量%,基于溶液计。所述引发剂的量通常为0.1%至10重量%,优选0.5%至5重量%,基于待聚合的单体计。还可以将两种或更多不同引发剂用在乳液聚合中。
在聚合过程中,还可以使用聚合调节剂——已知为链转移剂。链转移剂导致链终止反应,并且由此降低聚合物的摩尔量。在这一过程中,链转移剂连接至聚合物,通常连接至链末端。链转移剂的量可具体达到每100重量份的待聚合单体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重量份的量。合适的链转移剂特别是含有巯基的化合物,例如叔丁基硫醇、巯基乙酸乙酯、巯基乙醇、巯基丙基三甲氧基硅烷或叔十二烷基硫醇。一般而言,链转移剂为分子量小于2000、更特别地小于1000g/mol的低分子量化合物。
乳液聚合通常在30至130℃,优选在50至90℃下发生。聚合介质可仅由水组成或由水和可与水混溶的液体(如甲醇、乙醇或四氢呋喃)的混合物组成。优选仅使用水。
单体进料可以间歇、连续或分段进行。进料过程可以分段法或梯度法进行。优选的进料方法是,其中将一部分聚合反应批料作为初始进料引入,加热至聚合温度,且其聚合开始,随后将余下的聚合批料通常经两次或多次空间上分离的进料流——其中一个或多个进料流包含纯物质形式或乳化形式的单体——连续、分段或以浓度梯度供给至聚合区域,在该供料过程中维持聚合反应。在聚合反应中,还可以在初始进料中包括聚合种子用于例如更有效地设定粒度。
在自由基水性乳液聚合过程中将引发剂加入聚合容器的方式对于本领域普通技术人员而言是已知的。引发剂可以整体包括在加入至聚合容器的初始进料中,或根据在自由基水性乳液聚合过程中消耗的速率连续或分段加入。在各个情况下这将取决于引发剂体系的化学性质和聚合温度。优选将一部分引发剂包括在初始进料中,并以其消耗速率将剩余的部分提供至聚合区域。如果使用分子量调节剂,则所述调节剂或链转移剂也可部分地包括在初始进料中或在聚合过程中或接近聚合结束时全部或部分地加入。
为了实现反应器的高空/时收率,优选具有尽可能高的固含量的分散体。为了能达到>60重量%的固含量,应该设置双峰或多峰粒度,这是因为否则粘度太高,且分散体不能再处理。制备新一代的颗粒可通过例如加入种子(EP81083)、加入过量乳化剂、或加入微粒乳状液进行。与低粘度和高固含量结合相关的另一优势是涂布性能的在高固含量下得到改善。制备一代或多代新的颗粒可在任何需要的时间点进行。所述时间点通过低粘度所需的粒度分布确定。
在聚合过程中,优选至少部分连续地加入所述单体。在某种程度上,所述单体还可以在聚合开始之前作为初始进料引入聚合容器中。优选在加入聚合容器的初始进料中包括不超过单体总量30重量%、更优选不超过20重量%、非常优选不超过10重量%的单体。剩余单体——即优选至少70重量%、更优选至少80重量%、非常优选至少90%的单体——在聚合过程中连续加入。在一个具体的实施方案中,初始进料中不包括单体;换言之,全部单体在聚合过程中加入。对于进料过程,各个组分可通过反应器底座(reactor base)由上部、侧部或由下部加入反应器。
在一个实施方案中,聚合物P1在至少两个阶段制备,在第一聚合阶段中单体(b)的量高于甲基丙烯酸缩水甘油酯的量,并且在后续聚合阶段中单体(b)的量低于甲基丙烯酸缩水甘油酯的量;换言之,仅仅在第二聚合阶段才主要使用(即,超过一半)或全部地使用缩水甘油基单体(e)。在另一个实施方案中,聚合物P1在一个阶段中制备,其中单体(a)和(e)同时聚合。
为了除去剩余单体,还可以——在乳液聚合完全结束后,即在全部单体转化后——另外加入引发剂(化学除臭)。对于乳液聚合而言,通常得到固含量为15至75重量%、优选40至75重量%的聚合物水性分散体。由此制备的聚合物优选以其水性分散体形式使用。
分散体颗粒的粒度分布可为单峰、双峰或多峰的。对于单峰粒度分布而言,分散于水性分散体中的聚合物颗粒的平均粒度优选低于400nm,更特别地低于200nm。特别优选平均粒径介于140和200nm之间。本文中的平均粒径意指粒度分布的d50,即所有颗粒总质量的50重量%具有小于d50的粒度。粒度分布可以已知方式使用分析超速离心机测定(W.Makromolekulare Chemie185(1984),第1025-1039页)。对于双峰或多峰粒径分布而言,粒径可最高达1000nm。聚合物分散体的pH优选设定为大于4.5的pH,更特别地为介于5和8之间的pH。
本发明的PSA分散体可以包含添加剂。所述添加剂选自例如填料、染料、流动控制助剂、增稠剂(优选缔合增稠剂(associative thickeners))、消泡剂、增塑剂、颜料、润湿剂、UV保护剂和增粘剂。为了改进表面润湿性,PSAs可特别包含润湿助剂,实例为脂肪醇乙氧基化物、烷基酚乙氧基化物、磺基琥珀酸酯、壬基酚乙氧基化物、聚氧乙烯/聚氧丙烯或十二烷基磺酸钠。用量通常为每100重量份聚合物(固体)0.05至5重量份、更特别为0.1至3重量份。
增粘剂为本领域技术人员本身已知的。所述增粘剂为用于粘合剂或弹性体的改善这些体系的自粘性(粘着性、固有粘结、自粘合)的添加剂。其通常具有相对低的摩尔质量(Mn为约200–2000g/mol),高于弹性体的玻璃化转变温度,以及与弹性体足够的相容性;换言之,增粘剂至少部分地溶解在由弹性体形成的聚合物膜中。增粘剂的用量优选为每100重量份聚合物(固体/固体)5至100重量份、更优选10至50重量份。合适的增粘剂为例如基于天然树脂的那些,如松香。基于天然树脂的增粘剂包括天然树脂本身以及其例如通过歧化或异构化、聚合、二聚或加氢形成的衍生物。它们可以其盐(具有例如单价或多价抗衡离子(阴离子))的形式或优选以其酯化形式存在。用于酯化的醇可以为单羟基的或多羟基的。实例为甲醇、乙二醇、二乙二醇、三乙二醇、1,2,3-丙三醇和季戊四醇。此外还发现用作增粘剂的为酚醛树脂;烃类树脂,例如苯并呋喃-茚树脂、聚萜烯树脂、萜烯低聚物;基于不饱和CH化合物的烃类树脂,如丁二烯、戊烯、甲基丁烯、异戊二烯、戊间二烯、二乙烯基甲烷、戊二烯、环戊烯、环戊二烯、环己二烯、苯乙烯、α-甲基苯乙烯、乙烯基甲苯。同样越来越多被用作增粘剂的为具有低分子量的聚丙烯酸酯。这些聚丙烯酸酯优选具有低于30000的重均分子量Mw。聚丙烯酸酯优选由至少60重量%、更特别至少80重量%的(甲基)丙烯酸C1-C8烷基酯组成。优选的增粘剂为天然或化学改性的松香。松香主要由松香酸或其衍生物组成。
本发明的PSA分散体可用于制备粘性制品,或已经赋予自粘性的制品。该粘性制品可以为标签。优选的标签为自粘纸标签或膜标签,其中粘合剂施用加至作为载体材料的纸或膜上。所述粘性制品还可以为胶带,其中粘合剂施用至胶带类载体材料。所述胶带的载体材料可包含织造或非织造织物、薄膜、纸、毛毡、泡沫和共挤出物,或这些的结合物。应用领域为无载体的单面和双面胶带、医用胶带、粘性包装带、电缆包装带、地毯铺设带、粘性装配带、用于固定屋顶毡片的胶带、已经呈现出自粘性的载体材料例如泡沫,例如沥青板等。因此,本发明还提供本发明的PSA分散体用于制备自粘制品的用途,更具体为用于制备用于组件固定的胶带的用途,更具体地为在汽车建造中、用于电子制品或在建筑应用中的用途。
对于粘性制品的制备,粘合剂层可以常规方式例如辊涂、刮刀涂布或喷涂等施用至载体材料。当使用水性粘合剂分散体时,水可通过例如在50至150℃下干燥除去。由此得到的经涂布的基材用作例如自粘制品,如标签、胶带或薄片。为此,在粘合剂施用之前或之后,可切割载体以形成胶带、标签或薄片。为后续使用,基材涂布有PSA的一侧可以衬上防粘纸,例如硅化纸。
本发明还提供一种胶带,所述胶带具有至少一层载体层且其一面或两面涂有至少一种本发明的PSA分散体。用于制备胶带的优选载体材料为聚乙烯(PE)、定向聚丙烯(oPP)、聚对苯二甲酸乙二醇酯(PET)、PE泡沫和聚氨酯泡沫(PU泡沫)。
为制备胶带,PSA分散体的施用量基于固含量计优选为至少20g/m2或至少30g/m2,例如60至80g/m2。
本发明的一个实施方案为一种胶带,其中载体层材料选自PE、oPP、PET、PE泡沫和PU泡沫的胶带和/或所述胶带具有至少一层加衬(lining)所述粘合剂层的可剥离保护层。
本发明的粘性制品具有非常好的粘合性能,特别是良好的热稳定性。
实施例
使用的材料
实施例1
通过由表1所列的单体组合物的乳液聚合制备非本发明的PSA分散体D1至D3。
表1:用于制备PSA分散体D1至D3的单体组合物,其用量以重量份计,
D1 | D2 | D3 | |
种子 | 0.4 | 0.4 | 0.4 |
nBA | 87.75 | 87.75 | 87.75 |
MMA | 7.8 | 6.8 | 5.85 |
UMA | - | 1.0 | 1.95 |
AA | 1.5 | 1.5 | 1.5 |
苯乙烯 | 1.0 | 1.0 | 1.0 |
HPA | 1.95 | 1.95 | 1.95 |
性能测试:
将PSAs以75g/m2的涂布重量涂布在作为载体的RN36PET膜上,并在90℃下干燥5分钟。切开涂布有PSA的载体以得到25mm宽的测试带。
a)剪切强度
为测定剪切强度,将测试带以25x25mm的粘合面积粘附至钢板上,用重1kg的轧辊辊压1次,并随后悬挂负载1kg的重物。在标准条件下(23℃;50%相对湿度)和70℃下测定剪切强度(内聚力)。剪切强度的测量是该重物掉落所花的时间,以小时计;每种情况下,由5次测量计算平均值。
b)S.A.F.T.测试
将测试带以25x25mm的粘合面积粘附至AFERA钢上,使用重2kg的轧辊辊压4次,在至少16小时的接触时间后,悬挂负载1kg的重物。在负载过程中,由23℃开始、以0.5℃/min的速率进行连续加热。该重物掉落时所达到的加热温度是粘合剂热稳定性的量度。每种情况下由3次测量计算平均值。
测试结果汇总于表2中。
表2:D1-D3的测试结果
pphm:份每一百份单体;重量份每100重量份单体。
结果示出了使用单体类型b)得到了具有改善的但仍未最优化的热稳定性的粘合剂。增加单体b)的使用量未提供任何进一步的改善。
实施例2
制备分散体D4至D13。全部组合物汇总于表3和表4中。
分散体D4:
具有单峰粒度分布的非本发明的分散体D4由表3中所示的单体组合物通过乳液聚合制备。
分散体D5:
具有单峰度径分布的本发明的PSA分散体D5在两个阶段中通过乳液聚合制备,首先聚合80重量份的单体乳液1并随后聚合20重量份的单体乳液2。
单体乳液1:87.5重量份的n-BA、2重量份的UMA、6重量份的MMA、2重量份的HPA、1重量份的苯乙烯、1.5重量份的AA
单体乳液2:51重量份的n-BA、10重量份的GMA、37重量份的MMA、2重量份的AA
分散体D6:
如对于分散体D5,首先聚合90重量份的单体乳液1并随后聚合10重量份的单体乳液2。
分散体D7:
具有双峰粒度分布的非本发明的PSA分散体D7类似于D4制备,其不同在于,在60%的单体乳液进料后加入1.6pphm额外的种子。
分散体D8:
具有双峰粒度分布的本发明的PSA分散体D8类似于D5制备,其不同在于,在60%的单体乳液进料后加入1.6pphm额外的种子。
分散体D9:
具有双峰粒度分布的本发明的PSA分散体D9类似于D6制备,其不同在于,在60%的单体乳液进料后加入1.6pphm额外的种子。
分散体D10:
类似于分散体D5,
单体乳液2:86.5重量份的n-BA、10重量份的GMA、2重量份的HPA、1.5重量份的AA
分散体D11:
类似于分散体D6,
单体乳液2:86.5重量份的n-BA、10重量份的GMA、2重量份的HPA、1.5重量份的AA
分散体D12:
类似于分散体D8,
单体乳液2:86.5重量份的n-BA、10重量份的GMA、2重量份的HPA、1.5重量份的AA
分散体D13:
类似于分散体D9,
单体乳液2:86.5重量份的n-BA、10重量份的GMA、2重量份的HPA、1.5重量份的AA
表3:用于制备PSA分散体D4至D13的单体组合物,其用量以重量份计
PSD:粒度分布方式
表4:用于制备PSA分散体D4至D13的单体组合物,其用量以重量份计
D10 | D11 | D12 | D13 | |
PSD | 单峰 | 单峰 | 双峰 | 双峰 |
种子 | 0.4 | 0.4 | 2 | 2 |
nBA | 87.5 | 87.6 | 87.5 | 87.6 |
MMA | 4.7 | 5.3 | 4.7 | 5.3 |
UMA | 1.56 | 1.76 | 1.56 | 1.76 |
AA | 1.5 | 1.5 | 1.5 | 1.5 |
苯乙烯 | 0.8 | 0.9 | 0.8 | 0.9 |
HPA | 1.96 | 1.96 | 1.96 | 1.96 |
GMA | 2 | 1 | 2 | 1 |
PSD:粒度分布方式
应用测试的结果汇总于表5中。
表5:测试结果,D4-D13
结果示出,使用类型b)的单体结合含有缩水甘油基的单体在粘合剂部件上得到了显著改善的热稳定性。
Claims (13)
1.一种压敏粘合剂分散体,其包含至少一种由单体混合物通过乳液聚合形成的水分散聚合物P1,所述单体混合物包括:
(a)至少60重量%的至少一种(甲基)丙烯酸C4至C20烷基酯,其在聚合为均聚物时具有-30℃或更低的玻璃化转变温度,
(b)至少0.05重量%的至少一种含有下式取代基的(甲基)丙烯酸酯单体
其中X为CH2、O、NH或NR,并且R为C1至C4烷基,
(c)至少0.1重量%的至少一种酸单体,
(d)0.05至5重量%的至少一种(甲基)丙烯酸C1-C10羟烷基酯,
并且其中所述单体混合物或者包含0.1至5重量%的甲基丙烯酸缩水甘油酯(e)和/或
其中所述压敏粘合剂分散体包含至少一种不同于聚合物P1并且包含缩水甘油基的其他聚合物P2,所述聚合物P2由包含对于聚合物P1指定的量的单体(a)、单体(c)、甲基丙烯酸缩水甘油酯(e)和任选地单体(d)的单体混合物通过聚合形成,
其中单体(b)与单体(e)的重量比为0.1至10,
单体含量的数字各自基于所有单体的总和计。
2.权利要求1的压敏粘合剂分散体,其中所述单体(a)选自丙烯酸正丁酯、丙烯酸正己酯、丙烯酸辛酯和丙烯酸2-乙基己酯,以及这些单体的混合物。
3.前述权利要求中任一项的压敏粘合剂分散体,其中单体(b)为甲基丙烯酸脲基乙酯。
4.权利要求1的压敏粘合剂分散体,其中酸单体(c)选自丙烯酸和甲基丙烯酸。
5.权利要求1的压敏粘合剂分散体,其中单体(a)以60重量%至95重量%的量存在,单体(b)以0.1重量%至5重量%的量存在,单体(c)以0.1重量%至5重量%的量存在,其他单体(d)以0.05重量%至5重量%的量存在,且甲基丙烯酸缩水甘油酯以0.1重量%至5重量%的量存在。
6.权利要求1的压敏粘合剂分散体,其中所述分散体包含选自以下的添加剂:填料、染料、流动控制助剂、增稠剂、消泡剂、增塑剂、颜料、润湿剂、UV保护剂和增粘剂。
7.权利要求1的压敏粘合剂分散体,其中聚合物P1的制备以至少两个阶段进行,在第一聚合阶段中单体(b)的量高于(甲基)丙烯酸缩水甘油酯的量,并且在后续聚合阶段中单体(b)的量低于(甲基)丙烯酸缩水甘油酯的量。
8.一种胶带,其具有至少一层载体层且其一面或两面涂有至少一种前述权利要求中任一项的压敏粘合剂分散体。
9.前述权利要求的胶带,其中所述压敏粘合剂分散体的施用量基于固含量计为至少30g/m2。
10.前述两项权利要求任一项的胶带,其中所述载体层的材料选自聚乙烯、定向聚丙烯、聚对苯二甲酸乙二醇酯、PE泡沫和聚氨酯泡沫,和/或所述胶带具有至少一层加衬粘合剂层的可剥离保护层。
11.权利要求1至7中任一项的压敏粘合剂分散体用于制造自粘制品的用途。
12.权利要求1至7中任一项的压敏粘合剂分散体或权利要求8至10中任一项的胶带用于固定组件的用途。
13.权利要求12的用途,其中所述用途为在汽车建造中、用于电子制品或在建筑应用中。
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WO2012139941A1 (de) | 2012-10-18 |
EP2697324B1 (de) | 2018-06-13 |
ES2683721T3 (es) | 2018-09-27 |
CN103597045A (zh) | 2014-02-19 |
BR112013026344B1 (pt) | 2021-02-09 |
US20120263950A1 (en) | 2012-10-18 |
EP2697324A1 (de) | 2014-02-19 |
BR112013026344A2 (pt) | 2020-04-14 |
US9587144B2 (en) | 2017-03-07 |
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