CN113015772B - 分散体胶粘剂 - Google Patents
分散体胶粘剂 Download PDFInfo
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- CN113015772B CN113015772B CN201980063725.6A CN201980063725A CN113015772B CN 113015772 B CN113015772 B CN 113015772B CN 201980063725 A CN201980063725 A CN 201980063725A CN 113015772 B CN113015772 B CN 113015772B
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Abstract
本发明涉及基于水性聚氨酯或聚氨酯‑脲分散体的混合物的水性分散体胶粘剂用于通过喷雾凝聚法胶粘泡沫基底的用途。
Description
本发明涉及基于水性聚氨酯或聚氨酯-脲分散体的混合物的水性分散体胶粘剂用于通过喷雾凝聚法胶粘泡沫基底的用途。
当将泡沫基底胶粘到其它基底上时,例如对于泡沫-泡沫、泡沫-木材和泡沫-塑料的组合,主要在喷雾凝聚法中使用聚氯丁烯分散体胶粘剂。在这种方法中,将胶粘剂和凝聚剂分开传送到喷枪中,在喷雾射流中混合并凝聚。由于直到在喷雾射流中才发生混合,不需要考虑适用期。此外,凝聚的胶粘剂保留在待胶粘的基底表面上并且不扩散或仅少部分地扩散到泡沫基底的孔隙结构中。通常实现高的初始强度、足够长的开放时间和良好的耐热性。
重要应用领域是床垫和座椅家具的生产。特别在斯堪的纳维亚国家,需要聚氯丁烯分散体胶粘剂的无氯替代品,以例如能够满足北欧白天鹅环保图标(根据ISO 14024的I类环境标签)的要求。此外,它们应该具有高的初始强度和足够长的开放时间。
基于水性聚氨酯分散体的胶粘剂已在高要求的工业应用中在全世界获得认可,例如在制鞋、机动车内部部件的胶粘、膜层压或织物基底的胶粘的情况下。
在此类分散体用于胶粘基底的情况下,这通常在热活化过程后进行。在这种情况下,将分散体施加到基底上,并在水完全蒸发后,通过加热,例如使用红外辐射器来活化胶粘剂层,并转化成能胶粘的状态。胶粘剂膜变得发粘的温度被称为活化温度。
但是,当使用聚氨酯或聚氨酯-聚脲分散体时,也可使用湿胶粘法进行,即在施加胶粘剂后立即进行胶粘。必须机械固定待接合的部件直至胶粘剂凝固。这种方法常用于木材或织物基底的胶粘。
热活化法和湿胶粘法都较不适用于泡沫基底的胶粘。水的缓慢蒸发特别要求在胶粘剂的施加和胶粘过程之间的长等待时间,或适当的干燥装置。此外,该胶粘剂的并非微不足道的部分可在干燥前或在干燥过程中扩散到泡沫基底的孔隙中并随后不再可用于实际胶粘。
市场上已确立的基于水性聚氨酯分散体的胶粘剂通常不适合使用喷雾凝聚法,因为它们没有足够快地凝聚,没有足够的初始强度,或由于聚合物的结晶度而形成非常硬的胶粘接缝,这特别对于床垫生产是不可接受的。开放时间,即在胶粘剂的施加直至将待接合的部件接合在一起的时间(在此期间仍获得足够好的胶粘接合)通常仅为1分钟。但是,许多胶粘工艺需要至少两倍的时间。
WO 2013/053786 A1描述了水性聚氨酯分散体,其聚合物具有根据DIN 65467在20K/min的加热速率下通过差示扫描量热法测定的30℃至50℃的熔融温度,其中所述聚合物可由两种不同结晶的聚酯多元醇以预定用量比获得。这些聚氨酯分散体主要适合作为冷接触胶粘剂,但也可通过喷雾凝聚法使用。但是,在此可实现的初始强度对大多数泡沫胶粘应用而言不足。
来自BASF AG (德国Ludwigshafen)的Luphen® D DS 3548提供了环氧树脂改性的聚氨酯分散体,其尤其据报道也适用于喷雾凝聚法。此处所用的环氧树脂的基础是双酚A二缩水甘油醚。由于双酚A和由其形成的转化产物因其对内分泌系统的可能影响而特别令最终消费者极为不满并因此通常受到排斥,市场需要不含双酚A的胶粘剂和其它产品。
WO 2014/182170 A1描述了使用特定的无气喷涂法进行喷雾凝聚法。为此,使用聚氯丁烯分散体和增粘剂分散体的混合物以及聚氨酯分散体和增粘剂分散体的混合物。但是,这些在该文献中没有进一步规定。所提到的应用领域是在床垫和家具制造行业中的泡沫胶粘。但是,这一现有技术没有公开所用聚氨酯分散体的性质,也没有公开能采取何种措施来确保高的初始强度和足够长的开放时间。
本发明的目的因此是提供通过喷雾凝聚法胶粘泡沫基底的聚氯丁烯分散体胶粘剂的无氯且无双酚A的替代品,其没有表现出现有技术的缺点并具有高的初始强度和至少2分钟的足够长的开放时间。
EP 2 090 603 A2公开了含有以下组分的混合物的水性分散体
A) 水性聚氨酯或聚氨酯-脲分散体,其含有
I. 聚合物A),其由以下组分形成
I (i). 至少一种具有400至5000 g/mol的分子量的双官能脂族聚酯多元醇,
I (ii). 至少一种由六亚甲基二异氰酸酯(HDI)和1-异氰酸根合-3,3,5-三甲基-5-异氰酸根合甲基环己烷(IPDI)组成的混合物,和
I (iii). 至少一种由两种或更多种胺类扩链剂组成的混合物,其中至少一种化合物带有离子基团,
且聚合物A)在干燥后为半结晶或结晶的,在-65℃至-40℃的玻璃化转变温度Tg下发生玻璃化转变,
B) 不同于A)的水性聚氨酯或聚氨酯-脲分散体,其含有
II. 聚合物B),其由以下组分形成
II (i). 至少一种具有400至5000 g/mol的分子量的双官能芳族聚酯多元醇,
II (ii). 至少一种具有62至399的分子量的双官能多元醇组分,
II (iii). 至少一种脂族二异氰酸酯和
II (iv). 至少一种具有离子基团的胺类扩链剂,
其中聚合物B)在干燥后为非晶的,在-15℃至+10℃的玻璃化转变温度Tg下发生玻璃化转变。
根据EP 2 090 603 A2,水性聚氨酯或聚氨酯-聚脲分散体的所述混合物适合作为根据热活化法和根据湿胶粘法的胶粘剂,并表现出好于单组分的胶粘强度。
现在已经令人惊讶地发现,EP 2 090 603 A2中描述的水性聚氨酯或聚氨酯-聚脲分散体的混合物也出色地适用于通过喷雾凝聚法胶粘泡沫基底,只要遵循特定的用量比。
本发明的主题因此是含有以下组分的混合物的水性分散体用于通过喷雾凝聚法胶粘泡沫基底的用途
A) 水性聚氨酯或聚氨酯-脲分散体,其含有
I. 聚合物A),其由以下组分形成
I (i). 至少一种具有400至5000 g/mol的分子量的双官能脂族聚酯多元醇,
I (ii). 至少一种由六亚甲基二异氰酸酯(HDI)和1-异氰酸根合-3,3,5-三甲基-5-异氰酸根合甲基环己烷(IPDI)组成的混合物,和
I (iii). 至少一种由两种或更多种胺类扩链剂组成的混合物,其中至少一种化合物带有离子基团,
且聚合物A)在干燥后为半结晶或结晶的,在-65℃至-40℃的玻璃化转变温度Tg下发生玻璃化转变,和
B) 不同于A)的水性聚氨酯或聚氨酯-脲分散体,其含有
II. 聚合物B),其由以下组分形成
II (i). 至少一种具有400至5000 g/mol的分子量的双官能芳族聚酯多元醇,
II (ii). 至少一种具有62至399的分子量的双官能多元醇组分,
II (iii). 至少一种脂族二异氰酸酯和
II (iv). 至少一种具有离子基团的胺类扩链剂,
其中聚合物B)在干燥后为非晶的,在-15℃至+10℃的玻璃化转变温度Tg下发生玻璃化转变;
并且其中所述混合物含有34.8重量%至90.2重量%的聚合物A)和9.8重量%至65.2重量%的聚合物B)。
关于本发明被称为聚氨酯分散体的分散体含有可为狭义上的聚氨酯的聚合物,即通过多元醇和多异氰酸酯的聚合获得的那些聚合物作为分散相,但它们也可以是其中使用单胺和/或二胺作为形成组分、任选作为扩链剂的那些。可根据本发明使用的分散体因此被称为水性聚氨酯或聚氨酯-脲分散体。
在喷雾凝聚法中,将水性胶粘剂分散体和凝聚剂分开传送到双组分喷枪中并在喷雾射流中混合。通常使用雾化器空气在0.1-5巴的压力下进行喷涂;但是,也可以如例如WO2015/137808中所述无气传送这两种组分的至少一种。在通往第一基底的表面的途中在喷雾射流中发生分散体的凝聚;在此,胶粘剂分散体中包含的一部分水在该过程中已蒸发。在碰撞时,胶粘剂聚合物在第一基底的表面上形成膜,其在仍湿状态下立即发粘。由于直到在喷雾射流中才发生胶粘剂分散体和凝聚剂的混合,不需要考虑适用期。由于聚合物膜在湿状态下的粘性,可立即接合第二表面,其中理想地例如在基底上对着胶粘剂面施加压力。通过将两个基底表面压在一起而施加压力是有利的,因为其提高胶粘的强度。同样有利的是,两个基底的至少一个是多孔的或透水的,以便从凝固的胶粘接头中带走水。
可考虑的凝聚剂包括优选周期表的第一、第二和第三主族的金属的盐的水溶液,特别是如果它们具有良好的水溶性。优选使用基于二价或三价阳离子的盐。特别优选使用氯化钙、硫酸锌或硫酸铝。非常特别优选使用氯化钙。也可作为水溶液使用根据上文描述的不同盐的混合物。
适合作为凝聚剂的盐水溶液中的盐浓度为1重量%至20重量%,优选2重量%至10重量%,特别优选3重量%至4重量%。基于胶粘剂溶液 + 凝聚剂溶液的总和计,凝聚剂的水溶液的比例为0.1重量%至50重量%,优选1重量%至30重量%,特别优选8重量%至20重量%重量,非常特别优选12重量%至18重量%。
或者,所用凝聚剂也可以是无机或有机酸,优选柠檬酸、磷酸或碳酸的水溶液,和一种或多种上述盐与一种或多种这些酸的混合物。
根据本发明使用的分散体在每种情况下通常含有30重量%至55重量%的固体,优选38重量%至52重量%。基于作为分散相包含在分散体中的聚合物A)和B),根据本发明的混合物含有34.8重量%至90.2重量%的聚合物A)和9.8重量%至65.2重量%的聚合物B),优选44.4重量%至87.8重量%的聚合物A)和12.2重量%至55.6重量%的聚合物B),特别优选54.5重量%至81.9重量%的聚合物A)和18.1重量%至45.5重量%的聚合物B),非常特别优选65.1重量%至81.9重量%的聚合物A)和18.1重量%至34.9重量%的聚合物B),基于聚合物固体A)和B)的总重量计。
可考虑的合适的双官能脂族聚酯多元醇A) I(i).特别包括如可由脂族或脂环族二羧酸,例如琥珀酸、甲基琥珀酸、戊二酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸、壬烷二甲酸、癸烷二甲酸、四氢邻苯二甲酸、六氢邻苯二甲酸、环己烷二甲酸、马来酸、富马酸、丙二酸或其混合物与多元醇,例如乙二醇、二-、三-或四乙二醇、丙-1,2-二醇、二-、三-或四丙二醇、丙-1,3-二醇、丁-1,4-二醇、丁-1,3-二醇、丁-2,3-二醇、戊-1,5-二醇、己-1,6-二醇、2,2-二甲基丙-1,3-二醇、1,4-二羟基环己烷、1,4-二羟甲基环己烷、辛-1,8-二醇、癸-1,10-二醇、十二烷-1,12-二醇或其混合物以已知方式制备的线性聚酯二醇。代替游离多羧酸,相应的多羧酸酐或相应的多羧酸低碳醇酯或其混合物也可用于生产聚酯。
优选的是基于琥珀酸、甲基琥珀酸、戊二酸、己二酸或马来酸和丙-1,3-二醇、丁-1,4-二醇或己-1,6-二醇的双官能脂族聚酯多元醇A) I(i).。
特别优选的是基于己二酸和丁-1,4-二醇或己-1,6-二醇的双官能脂族聚酯多元醇A) I(i).。
非常特别优选的是基于己二酸和丁-1,4-二醇的双官能脂族聚酯多元醇A) I(i).。
双官能脂族聚酯多元醇A) I(i).的分子量为400至5000 g/mol,优选1500至3000g/mol,特别优选1900至2500 g/mol,非常特别优选2100至2300 g/mol。
所用异氰酸酯组分A) I(ii).是六亚甲基二异氰酸酯(HDI)和1-异氰酸根合-3,3,5-三甲基-5-异氰酸根合甲基环己烷(IPDI)的混合物。HDI:IPDI摩尔比优选为9:1至1:9,特别优选3:1至1:3,非常特别优选2:1。
组分A) I(iii).由两种或更多种胺类扩链剂的混合物组成,其中至少一种化合物带有离子基团。在本发明中,扩链剂也包括导致链终止的单胺。
单胺的实例是脂族和/或脂环族伯和/或仲单胺,如乙胺、二乙胺、异构丙基-和丁基胺、更高级的线性脂族单胺和脂环族单胺,如环己胺。进一步的实例是氨基醇,即在一个分子中含有氨基和羟基的化合物,例如乙醇胺、N-甲基乙醇胺、二乙醇胺或2-丙醇胺。进一步的实例是另外带有磺酸和/或羧基的单氨基化合物,例如牛磺酸、甘氨酸或丙氨酸。
二氨基化合物的实例是乙-1,2-二胺、己-1,6-二胺、1-氨基-3,3,5-三甲基-5-氨基甲基环己烷(异佛尔酮二胺)、哌嗪、1,4-二氨基环己烷或双(4-氨基环己基)甲烷。己二酸二酰肼、肼和水合肼也可考虑。多胺,如二亚乙基三胺也可代替二氨基化合物用作形成组分。
进一步的实例是氨基醇,即在一个分子中含有氨基和羟基的化合物,例如1,3-二氨基-2-丙醇、N-(2-羟乙基)乙二胺或N,N-双(2-羟乙基)乙二胺。
因此另外带有磺酸根和/或羧酸根基团的具有离子基团的二氨基化合物的实例包括例如N-(2-氨基乙基)-2-氨基乙磺酸/-羧酸的钠或钾盐、N-(3-氨基丙基)-2-氨基乙磺酸/-羧酸的钠或钾盐、N-(3-氨基丙基)-3-氨基丙磺酸/-羧酸的钠或钾盐或N-(2-氨基乙基)-3-氨基丙磺酸/-羧酸的钠或钾盐。优选的是N-(2-氨基乙基)-2-氨基乙磺酸的钠盐。
混合物A) I(iii).的优选成分是二乙醇胺、乙-1,2-二胺、1-氨基-3,3,5-三甲基-5-氨基甲基环己烷(异佛尔酮二胺)、哌嗪、N-(2-羟乙基)乙二胺和N-(2-氨基乙基)-2-氨基乙磺酸/-羧酸的钠盐。
特别优选的是二乙醇胺和N-(2-氨基乙基)-2-氨基乙磺酸的钠盐的混合物。
聚合物A)在干燥后为半结晶或结晶的,在-65℃至-40℃的玻璃化转变温度Tg,优选在-60℃至-45℃,特别优选在-55℃至-50℃的Tg下发生玻璃化转变。
当其在根据DIN 65467在20 K/min的加热速率下的DSC测量中具有与熔化焓> 5J/g,优选> 10 J/g,特别优选> 20 J/g,非常特别优选> 40 J/g对应的熔融峰时,聚合物A)被称为半结晶或结晶的。熔融峰由聚合物中的规则子结构的熔融造成。熔融温度在这种情况下优选为30℃至80℃,特别优选40℃至70℃,非常特别优选42℃至55℃。评估第一次加热,从而也检测缓慢结晶的聚合物。
当其在第一次加热的过程中没有熔融峰或只有熔化焓< 5 J/g,优选< 3 J/g,特别优选< 1 J/g的熔融峰时,聚合物B)被称为非晶。
在本发明的一个优选实施方案中,非晶聚合物B)没有熔融峰。
可考虑的双官能芳族聚酯多元醇B) II(i).特别包括如可由芳族二羧酸,例如对苯二甲酸、间苯二甲酸或邻苯二甲酸及其酸酐,例如邻苯二甲酸酐与多元醇,例如乙二醇、二-、三-或四乙二醇、丙-1,2-二醇、二-、三-或四丙二醇、丙-1,3-二醇、丁-1,4-二醇、丁-1,3-二醇、丁-2,3-二醇、戊-1,5-二醇、己-1,6-二醇、2,2-二甲基丙-1,3-二醇、1,4-二羟基环己烷、1,4-二羟甲基环己烷、辛-1,8-二醇、癸-1,10-二醇、十二烷-1,12-二醇或这些的混合物以已知方式制备的线性聚酯二醇。
优选的是基于邻苯二甲酸、邻苯二甲酸酐和丁-1,4-二醇或己-1,6-二醇的双官能芳族聚酯多元醇B) II(i).。
特别优选的是基于邻苯二甲酸或邻苯二甲酸酐和己-1,6-二醇的双官能芳族聚酯多元醇B) II(i).。
双官能芳族聚酯多元醇B) II(i).的分子量为400至5000 g/mol,优选1500至3000g/mol,特别优选1800至2300 g/mol,非常特别优选1900至2100 g/mol。
具有62至399的分子量并适合作为形成组分B) II(ii).的双官能多元醇组分的实例是在A) I(i).和B) II(i).下列举的产品,只要它们具有62至399道尔顿的分子量。进一步合适的组分是为聚酯多元醇的制备列举的多元醇,特别是二元醇,以及其它低分子量聚酯二醇,例如己二酸双(羟乙基)酯。短链双官能聚醚多元醇,例如环氧乙烷或环氧丙烷的均聚物、共聚物和接枝聚合物也可考虑。
优选的形成组分B) II(ii).是丁-1,4-二醇和己-1,6-二醇,特别优选己-1,6-二醇。
合适的形成组分B) II(iii).是每分子具有至少两个游离异氰酸酯基团的任意脂族化合物。优选使用二异氰酸酯Y(NCO)2,其中Y是具有4至12个碳原子的二价脂族烃基或具有6至15个碳原子的二价脂环族烃基。优选使用的此类二异氰酸酯的实例包括四亚甲基二异氰酸酯、甲基五亚甲基二异氰酸酯、六亚甲基二异氰酸酯、十二亚甲基二异氰酸酯、1,4-环己烷二异氰酸酯、1-异氰酸根合-3,3,5-三甲基-5-异氰酸根合甲基环己烷、4,4'-二环己基甲烷二异氰酸酯或4,4'-二异氰酸根合-2,2-二环己基丙烷或其混合物。
特别优选的是六亚甲基二异氰酸酯(HDI)、1-异氰酸根合-3,3,5-三甲基-5-异氰酸根合甲基环己烷(IPDI)和4,4'-二环己基甲烷二异氰酸酯及其混合物。但是,异氰酸酯优选独自使用。
非常特别优选的是六亚甲基二异氰酸酯(HDI)。
具有离子基团的胺类扩链剂B) II(vi).优选是另外带有磺酸根和/或羧酸根基团的二氨基化合物,例如N-(2-氨基乙基)-2-氨基乙磺酸的钠或钾盐、N-(3-氨基丙基)-2-氨基乙磺酸的钠或钾盐、N-(3-氨基丙基)-3-氨基丙磺酸的钠或钾盐、N-(2-氨基乙基)-3-氨基丙磺酸的钠或钾盐,或类似羧酸的钠或钾盐。
特别优选的是N-(2-氨基乙基)-2-氨基乙磺酸和类似羧酸的钠盐,非常特别优选的是N-(2-氨基乙基)-2-氨基乙磺酸的钠盐。
具有离子基团的胺类扩链剂B) II(iv).可独自或与如例如A) I(iii)下已描述的其它胺类扩链剂一起使用。它们优选独自使用。
聚合物B)在干燥后为非晶的,在-15℃至+10℃的玻璃化转变温度Tg,优选-10℃至+5℃,特别优选-5℃至0℃的Tg下发生玻璃化转变。
含有聚合物A)或B)的水性聚氨酯或聚氨酯-脲分散体具有10重量%至70重量%,优选25重量%至60重量%,特别优选35重量%至55重量%的固含量。
含有聚合物A)或B)的水性聚氨酯或聚氨酯-脲分散体优选通过丙酮法制备。为此,分别由组分A) I(i).和A) I(ii).,或B) II(i).、B) II(ii).和B) II(iii).制备预聚物,溶解在丙酮中并分别用组分A) I(iii).或B) II(iv).扩链。在用水分散后蒸馏出丙酮。丙酮法的应用和进行是现有技术并且是本领域技术人员已知的。
含有聚合物A)或B)的水性聚氨酯或聚氨酯-脲分散体和根据本发明的混合物优选不含外部乳化剂。
优选通过混合聚合物A)和B)的水性聚氨酯或聚氨酯或聚氨酯-脲分散体制备根据本发明的分散体。
用根据本发明的分散体通过喷雾凝聚法制成的胶粘部位在该材料立即撕裂前表现出足够的即时强度,其开放时间为至少3分钟。特别在将泡沫胶粘在泡沫上或将泡沫胶粘在具有三维结构并因此不平整的其它基底表面,例如木材、金属或塑料上时,通过根据本发明的方法制成的胶粘部位能够吸收泡沫的恢复力而无需等待时间,特别是无需完全除水。这样的应用的一个实例是通过折弯窄侧面和在喷涂施加根据本发明的胶粘剂分散体后在湿的情况下立即将它们压向彼此而胶粘长方体泡沫材料块以形成垫层。由于即时湿强度高,可立即再撤回外加的挤压力,而受到应力的泡沫材料没有回弹或位移。
特别地,通过根据本发明的分散体而生产胶粘剂组合物,其适用于生产胶粘复合体,其中该胶粘复合体包含基底、根据本发明的分散体和另一基底。在此,这两个基底可由相同或不同材料组成。按照定义,基底也可以是扁平结构。所述至少一个基底优选是泡沫基底。
泡沫基底被理解为是指由泡沫材料制成的基底,其中泡沫材料通常是具有泡孔结构和低密度的人造物质。在此可区分开孔、闭孔和混合泡孔的泡沫材料。根据硬度,将泡沫材料分成硬质泡沫和软质泡沫。几乎所有塑料都适用于发泡。
原则上,根据本发明的分散体适用于通过喷雾凝聚法胶粘所有泡沫基底。优选胶粘开孔和混合泡孔的泡沫基底。
在本发明的一个优选实施方案中,泡沫基底由聚氨酯(例如聚醚和聚酯泡沫)和/或橡胶,例如天然橡胶(NR)、苯乙烯-丁二烯橡胶(SBR)、乙烯-丙烯-二烯聚合物(EPDM)、丁二烯-丙烯腈橡胶(NBR)或氯丁橡胶(CR)组成。
在本发明的一个特别优选的实施方案中,所述一个或多个泡沫基底由聚氨酯组成。
根据本发明的分散体还以对非常多样化的其它基底,例如对木材、纸、皮革、纺织品、软木和塑料(热塑性塑料、弹性体、热固性材料、复合材料),如不同的聚氯乙烯等级、聚氨酯、聚乙酸乙烯酯、ABS、橡胶、聚(乙烯-乙酸乙烯酯)、聚碳酸酯或聚烯烃,例如填充或未填充的聚丙烯的良好附着力为特征。在极少数的情况下,必须预处理基底表面,例如通过上底漆、烧毛或电晕处理,特别是在非极性基底的情况下。
含有根据本发明的分散体的胶粘剂组合物因此适用于优选由上述材料形成的任意基底的胶粘。
根据本发明的胶粘剂特别适用于泡沫在泡沫上、泡沫在木材上、泡沫在各种塑料上和织物在各种基底上的胶粘。
包含用根据本发明使用的分散体胶粘的基底和扁平结构的胶粘复合体也是本申请的主题,例如通过根据本发明的用途获得的胶粘剂接合的泡沫基底。
实施例
下面基于实施例更详细阐释本发明。在此使用以下方法和试验方法:
A) 喷雾凝聚法:
用于双组分分散体胶粘剂的标准喷枪,即来自Walther Pilot公司的PILOT III2K用于施加。在此将胶粘剂和凝聚剂CaCl2(3重量%水溶液)分开传送到喷枪中,在喷雾射流中混合并使胶粘剂凝聚。由于直到在喷雾射流中才发生混合,不需要考虑适用期。选择86重量%胶粘剂分散体和14重量% CaCl2溶液的比率。
喷枪的精确设定原则上是本领域技术人员已知的,可为具体情况定制而没有过分高的支出,并可通过简单的预备实验确定。可通过将储器和基底重新称重来测定用量比和施加重量。
使用以下设定:
a.) 胶粘剂组分: 传送压力1.3巴
b.) 凝聚剂组分: 传送压力0.3巴
c.) 雾化器空气压力: 2.8巴
d.) 用于胶粘剂组分的孔(喷嘴): 1.0 mm
e.) 用于凝聚剂组分的孔(喷嘴): 0.4 mm
f.) 施加重量: 130 - 150 g/m²(湿)
B) 初始强度的测定:
作为试验材料,使用具有10 x 5 x 3 cm的尺寸和40 kg/m³的单位体积重量的来自STN Schaumstoff-Technik-Nürnberg GmbH公司的ST 5540 (1) PU泡沫材料试样(见图1)。为了评估初始强度,在通过喷雾凝聚法将胶粘剂施加到泡沫材料体(1)的上侧(2)(施加量130 - 150 g/m²湿)后立即用木棒(3)(D = 7 mm圆木棒或7 x 7 mm矩形)将试样中间对折(4)并借助试验装置(5)进给经过2个钢辊(6)(直径40 mm,长度64 mm),使用螺纹轴(8)将钢辊的切向间距(7)预先设定为10 mm。如果尽管在试样中存在恢复力、但试样或胶粘接缝(9)没有打开,初始强度足够。
C) 开放时间的测定
作为试验材料,使用具有10 x 5 x 3 cm的尺寸和20 kg/m³的单位体积重量的来自Recticel公司的Recticel T 20120聚醚泡沫材料体。为了评估开放时间,在借助喷雾凝聚法施加胶粘剂(施加量130 - 150 g/m²湿)后立即每60秒或如果必要时以特定时间间隔,将试样中间对折并用轻掌压接合在一起。强度不再足够且试样由于出现恢复力而打开表明开放时间结束。
D) 胶粘接缝的硬度的确定:
在室温下储存24小时后通过触摸在感官上与参考样品直接比较地评估在B)下制成的试样的胶粘接缝。使用具有不同肖氏A硬度的市售聚氯丁烯胶乳(CovestroDeutschland AG)制造参考样品。由Dispercoll® C 84(纯的干燥聚合物的肖氏A硬度= 88)形成的试样的胶粘接缝作为硬的胶粘接缝的参考,由Dispercoll® C 74(纯的干燥聚合物的肖氏A硬度= 55)形成的试样的胶粘接缝作为中等硬度的胶粘接缝的参考,且由Dispercoll® C 2372(纯的干燥聚合物的肖氏A硬度= 40)形成的试样的胶粘接缝作为软的胶粘接缝的参考。
E) 借助DSC确定玻璃化转变温度、熔融温度和熔化焓:
使用来自Perkin-Elmer公司的Pyris Diamond DSC量热计借助差示扫描量热法(DSC)测定玻璃化转变温度以及熔融温度和熔化焓。为此,通过将分散体以100 µm湿膜厚度刮涂到玻璃板上,制造膜,通风2小时,然后将该膜与玻璃板一起在干燥箱中在室温和0%相对室内湿度下干燥3天。然后,使用10毫克来自该膜的样品材料,在下列测量条件下记录DSC曲线:迅速冷却到起始温度-100℃、然后开始在氦气气氛下以20 K/min的加热速率和320K/min的冷却速率从-100℃至+150℃加热三次,并用液氮冷却。玻璃化转变温度对应于在玻璃化转变的一半高度处的温度,其中评估第三次加热。对于熔融温度和熔化焓的测定,评估第一次加热。
F) 原料:
聚酯I: 由丁-1,4-二醇和己二酸形成的聚酯二醇,OH值 = 50
聚酯II: 由己-1,6-二醇和邻苯二甲酸酐形成的聚酯二醇,OH值 = 56
Desmodur® H: 六亚甲基1,6-二异氰酸酯(德国Leverkusen的CovestroDeutschland AG)
Desmodur® I: 异佛尔酮二异氰酸酯(德国Leverkusen的Covestro DeutschlandAG)。
实施例1(根据本发明):
含有聚合物A)的水性聚氨酯或聚氨酯-脲分散体的制备:
450克聚酯I在110℃和15毫巴下脱水1小时。在80℃下,加入30.11克Desmodur® H,然后20.14克Desmodur® I。该混合物在80至90℃下搅拌,直至达到1.15%的恒定异氰酸酯含量。将反应混合物溶解在750克丙酮中并在此冷却到48℃。在剧烈搅拌下向该均匀溶液中加入5.95克N-(2-氨基乙基)-2-氨基乙磺酸的钠盐和2.57克二乙醇胺在65克水中的溶液。在30分钟后,通过加入700克水进行分散。在丙酮的蒸馏脱除后获得具有40.0重量%的固含量的水性聚氨酯-聚脲分散体。
包含的聚合物在干燥后为半结晶的,具有在-54℃的玻璃化转变温度Tg下的玻璃化转变、48℃的熔融温度和50.4 J/g的熔化焓。
实施例2(根据本发明):
含有聚合物B)的水性聚氨酯或聚氨酯-脲分散体的制备:
1215克聚酯II在110℃和15毫巴下脱水1小时。在80℃下,加入4.6克己-1,6-二醇和179.0克Desmodur® H并在90℃下搅拌该混合物,直至达到2.28%的恒定异氰酸酯含量。将反应混合物溶解在2490克丙酮中并在此冷却到48℃。在剧烈搅拌下向该均匀溶液中加入31.9克N-(2-氨基乙基)-2-氨基乙磺酸的钠盐在300克水中的溶液。在30分钟后,通过加入1150克水进行分散。在丙酮的蒸馏脱除后获得具有50.0重量%的固含量的水性聚氨酯-聚脲分散体。
包含的聚合物在干燥后为非晶的(在DSC中没有熔融峰)并在-1.5℃的玻璃化转变温度Tg下具有玻璃化转变。
实施例3(对比):
使用来自实施例1的分散体(含有100%聚合物A)。从表中可以看出,尽管初始强度良好,但获得太硬的胶粘接缝且1分钟的开放时间不够。
实施例4(对比):
实施例1和2的分散体的根据本发明的混合物的制备和用途:
将95重量份来自实施例1的分散体(半结晶)和5重量份来自实施例2的分散体(非晶)在搅拌下混合并均化。将固含量计入考虑,根据本发明的混合物含有93.8重量%的聚合物A和6.2重量%的聚合物B。
从表中可以看出,尽管初始强度良好,但获得太硬的胶粘接缝且1分钟的开放时间不够。
实施例5(根据本发明):
实施例1和2的分散体的根据本发明的混合物的制备和用途:
将92重量份来自实施例1的分散体(半结晶)和8重量份来自实施例2的分散体(非晶)在搅拌下混合并均化。将固含量计入考虑,根据本发明的混合物含有90.2重量%的聚合物A和9.8重量%的聚合物B。
从表中可以看出,初始强度良好,胶粘接缝为中等硬度且3分钟的开放时间满足要求。
实施例6(根据本发明):
实施例1和2的分散体的根据本发明的混合物的制备和用途:
将90重量份来自实施例1的分散体(半结晶)和10重量份来自实施例2的分散体(非晶)在搅拌下混合并均化。将固含量计入考虑,根据本发明的混合物含有87.8重量%的聚合物A和12.2重量%的聚合物B。
从表中可以看出,初始强度良好,胶粘接缝为中等硬度且4分钟的开放时间满足要求。
实施例7(根据本发明):
实施例1和2的分散体的根据本发明的混合物的制备和用途:
将85重量份来自实施例1的分散体(半结晶)和15重量份来自实施例2的分散体(非晶)在搅拌下混合并均化。将固含量计入考虑,根据本发明的混合物含有81.9重量%的聚合物A和18.1重量%的聚合物B。
从表中可以看出,初始强度良好,胶粘接缝为中等硬度且7分钟的开放时间满足要求。
实施例8(根据本发明):
实施例1和2的分散体的根据本发明的混合物的制备和用途:
将80重量份来自实施例1的分散体(半结晶)和20重量份来自实施例2的分散体(非晶)在搅拌下混合并均化。将固含量计入考虑,根据本发明的混合物含有76.2重量%的聚合物A和23.8重量%的聚合物B。
从表中可以看出,初始强度良好,胶粘接缝为中等硬度且7分钟的开放时间满足要求。
实施例9(根据本发明):
实施例1和2的分散体的根据本发明的混合物的制备和用途:
将75重量份来自实施例1的分散体(半结晶)和25重量份来自实施例2的分散体(非晶)在搅拌下混合并均化。将固含量计入考虑,根据本发明的混合物含有70.6重量%的聚合物A和29.4重量%的聚合物B。
从表中可以看出,初始强度良好,胶粘接缝为中等硬度且7分钟的开放时间满足要求。
实施例10(根据本发明):
实施例1和2的分散体的根据本发明的混合物的制备和用途:
将70重量份来自实施例1的分散体(半结晶)和30重量份来自实施例2的分散体(非晶)在搅拌下混合并均化。将固含量计入考虑,根据本发明的混合物含有65.1重量%的聚合物A和34.9重量%的聚合物B。
从表中可以看出,初始强度良好,胶粘接缝为中等硬度且7分钟的开放时间满足要求。
实施例11(根据本发明):
实施例1和2的分散体的根据本发明的混合物的制备和用途:
将60重量份来自实施例1的分散体(半结晶)和40重量份来自实施例2的分散体(非晶)在搅拌下混合并均化。将固含量计入考虑,根据本发明的混合物含有54.5重量%的聚合物A和45.5重量%的聚合物B。
从表中可以看出,初始强度良好,胶粘接缝为中等硬度且7分钟的开放时间满足要求。
实施例12(根据本发明):
实施例1和2的分散体的根据本发明的混合物的制备和用途:
将50重量份来自实施例1的分散体(半结晶)和50重量份来自实施例2的分散体(非晶)在搅拌下混合并均化。将固含量计入考虑,根据本发明的混合物含有44.4重量%的聚合物A和55.6重量%的聚合物B。
从表中可以看出,初始强度良好,胶粘接缝为中等硬度且4分钟的开放时间满足要求。
实施例13(根据本发明):
实施例1和2的分散体的根据本发明的混合物的制备和用途:
将40重量份来自实施例1的分散体(半结晶)和60重量份来自实施例2的分散体(非晶)在搅拌下混合并均化。将固含量计入考虑,根据本发明的混合物含有34.8重量%的聚合物A和65.2重量%的聚合物B。
从表中可以看出,初始强度良好,胶粘接缝柔软且3分钟的开放时间满足要求。
实施例14(对比):
实施例1和2的分散体的根据本发明的混合物的制备和用途:
将30重量份来自实施例1的分散体(半结晶)和70重量份来自实施例2的分散体(非晶)在搅拌下混合并均化。将固含量计入考虑,根据本发明的混合物含有25.5重量%的聚合物A和74.5重量%的聚合物B。
从表中可以看出,不存在初始强度。
实施例15(对比):
使用来自实施例2的分散体(含有100%聚合物B)。
从下表中可以看出,不存在初始强度。
表: 根据本发明的实验和对比实验的结果
实施例 | 聚合物A / B[重量%] | 初始强度 | 接缝的硬度 | 开放时间[分钟] |
3(对比) | 100 / 0 | 是 | 硬 | 1 |
4(对比) | 93.8 / 6.2 | 是 | 硬 | 1 |
5(根据本发明) | 90.2 / 9.8 | 是 | 中等 | 3 |
6(根据本发明) | 87.8 / 12.2 | 是 | 中等 | 4 |
7(根据本发明) | 81.9 / 18.1 | 是 | 中等 | 7 |
8(根据本发明) | 76.2 / 23.8 | 是 | 中等 | 7 |
9(根据本发明) | 70.6 / 29.4 | 是 | 中等 | 7 |
10(根据本发明) | 65.1 / 34.9 | 是 | 中等 | 7 |
11(根据本发明) | 54.5 / 45.5 | 是 | 中等 | 6 |
12(根据本发明) | 44.4 / 55.6 | 是 | 中等 | 4 |
13(根据本发明) | 34.8 / 65.2 | 是 | 软 | 3 |
14(对比) | 25.5 / 74.5 | 否 | 不可测定 | 0 |
15(对比) | 0 / 100 | 否 | 不可测定 | 0 |
Claims (8)
1.含有以下组分的混合物的水性分散体用于通过喷雾凝聚法胶粘泡沫基底的用途
A) 水性聚氨酯或聚氨酯-脲分散体,其含有
I. 聚合物A),其由以下组分形成
I (i). 至少一种具有400至5000 g/mol的分子量的双官能脂族聚酯多元醇,
I (ii). 至少一种由六亚甲基二异氰酸酯(HDI)和1-异氰酸根合-3,3,5-三甲基-5-异氰酸根合甲基环己烷(IPDI)组成的混合物,和
I (iii). 至少一种由两种或更多种胺类扩链剂组成的混合物,其中至少一种化合物带有离子基团,
且聚合物A)在干燥后为半结晶或结晶的,在-65℃至-40℃的玻璃化转变温度Tg下发生玻璃化转变,和
B) 不同于A)的水性聚氨酯或聚氨酯-脲分散体,其含有
II. 聚合物B),其由以下组分形成
II (i). 至少一种具有400至5000 g/mol的分子量的双官能芳族聚酯多元醇,
II (ii). 至少一种具有62至399的分子量的双官能多元醇组分,
II (iii). 至少一种脂族二异氰酸酯和
II (iv). 至少一种具有离子基团的胺类扩链剂,
其中聚合物B)在干燥后为非晶的,在-15℃至+10℃的玻璃化转变温度Tg下发生玻璃化转变;
并且其中所述混合物含有基于聚合物A)和B)的总和计34.8重量%至90.2重量%的聚合物A)和9.8重量%至65.2重量%的聚合物B)。
2.如权利要求1中所述的水性分散体的用途,其特征在于所述混合物含有44.4重量%至87.8重量%的聚合物A)和12.2重量%至55.6重量%的聚合物B)。
3.如权利要求1中所述的水性分散体的用途,其特征在于所述混合物含有54.5重量%至81.9重量%的聚合物A)和18.1重量%至45.5重量%的聚合物B)。
4.如权利要求1至3中任一项所述的水性分散体的用途,其特征在于HDI:IPDI摩尔比为9:1至1:9。
5.如权利要求1至3中任一项所述的水性分散体的用途,其特征在于HDI:IPDI摩尔比为3:1至1:3。
6.如权利要求1至3中任一项所述的水性分散体的用途,其特征在于组分A) I(iii).是二乙醇胺和N-(2-氨基乙基)-2-氨基乙磺酸的钠盐的混合物。
7.如权利要求1至3中任一项所述的水性分散体的用途,其特征在于组分B) II(i).是基于邻苯二甲酸、邻苯二甲酸酐和1,4-丁二醇或1,6-己二醇的聚酯多元醇。
8.通过如权利要求1中所述的用途获得的经胶粘剂接合的泡沫基底。
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Application Number | Priority Date | Filing Date | Title |
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EP18197309.0 | 2018-09-27 | ||
EP18197309.0A EP3628711A1 (de) | 2018-09-27 | 2018-09-27 | Dispersionsklebstoffe |
PCT/EP2019/075842 WO2020064826A1 (de) | 2018-09-27 | 2019-09-25 | Dispersionsklebstoffe |
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CN113015772A CN113015772A (zh) | 2021-06-22 |
CN113015772B true CN113015772B (zh) | 2022-08-02 |
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US (2) | US11198786B2 (zh) |
EP (2) | EP3628711A1 (zh) |
CN (1) | CN113015772B (zh) |
WO (1) | WO2020064826A1 (zh) |
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EP3628711A1 (de) * | 2018-09-27 | 2020-04-01 | Covestro Deutschland AG | Dispersionsklebstoffe |
US20240101879A1 (en) | 2021-01-19 | 2024-03-28 | Covestro Deutschland Ag | Storage-Stable 1K Spray Adhesives Based on Polyurethane Dispersions |
EP4029891A1 (de) | 2021-01-19 | 2022-07-20 | Covestro Deutschland AG | Lagerstabile 1k-sprühklebstoffe auf basis von polyurethandispersionen |
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EP2110395A1 (de) * | 2008-04-18 | 2009-10-21 | Bayer MaterialScience AG | Wässrige Polyurethanlösungen für Polyurethan-Systeme |
ES2674926T3 (es) | 2011-10-14 | 2018-07-05 | Covestro Deutschland Ag | Adhesivos de contacto en frío |
NL2010773C2 (en) | 2013-05-08 | 2014-11-13 | Saba Dinxperlo B V | A method of applying adhesive. |
NL2012409B1 (en) | 2014-03-12 | 2015-11-26 | Saba Dinxperlo B V | Improved low pressure 2-K handheld spray gun. |
EP3628711A1 (de) * | 2018-09-27 | 2020-04-01 | Covestro Deutschland AG | Dispersionsklebstoffe |
-
2018
- 2018-09-27 EP EP18197309.0A patent/EP3628711A1/de not_active Ceased
-
2019
- 2019-09-25 US US17/274,821 patent/US11198786B2/en active Active
- 2019-09-25 CN CN201980063725.6A patent/CN113015772B/zh active Active
- 2019-09-25 EP EP19772751.4A patent/EP3856863A1/de active Pending
- 2019-09-25 WO PCT/EP2019/075842 patent/WO2020064826A1/de unknown
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2021
- 2021-11-05 US US17/519,661 patent/US20220056265A1/en not_active Abandoned
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US4386992A (en) * | 1979-05-11 | 1983-06-07 | Sunstar Chemical Ind. Co., Ltd. | Two-part adhesive and bonding method employing same |
US5624758A (en) * | 1995-06-07 | 1997-04-29 | H.B. Fuller Licensing & Financing, Inc. | Water-based adhesive formulation having enhanced characteristics |
US6290803B1 (en) * | 1995-06-07 | 2001-09-18 | H. B. Fuller Licensing & Financing Inc. | Bonding method for water-based formulations having enhanced characteristics |
CN101784601A (zh) * | 2007-08-24 | 2010-07-21 | 拜尔材料科学股份公司 | 低粘度含水粘合剂聚合物分散体 |
CN101508785A (zh) * | 2008-02-15 | 2009-08-19 | 拜尔材料科学股份公司 | 分散体粘合剂 |
CN107406724A (zh) * | 2015-04-07 | 2017-11-28 | 科思创德国股份有限公司 | 用粘合剂粘合基材的方法 |
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US20210317307A1 (en) | 2021-10-14 |
US11198786B2 (en) | 2021-12-14 |
EP3856863A1 (de) | 2021-08-04 |
US20220056265A1 (en) | 2022-02-24 |
EP3628711A1 (de) | 2020-04-01 |
CN113015772A (zh) | 2021-06-22 |
WO2020064826A1 (de) | 2020-04-02 |
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