CN114045143B - 高透明反应型聚氨酯热熔胶及其制备方法 - Google Patents
高透明反应型聚氨酯热熔胶及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种高透明反应型聚氨酯热熔胶及其制备方法。该高透明反应型聚氨酯热熔胶由以下重量份的原料制备而成：无定形聚酯多元醇20～45份，聚醚多元醇10～50份，异氰酸酯10～40份，丙烯酸树脂10～30份，粘合促进剂0.2～2.5份，潜固化剂0.5～3份，催化剂0.01～0.2份，紫外光吸收剂0.5～2份，抗氧剂0.5～2份；所述异氰酸酯为环己基甲烷二异氰酸酯、异佛尔酮二异氰酸酯和六亚甲基二异氰酸酯中的一种或多种；所述丙烯酸树脂的玻璃化转变温度大于50℃。该反应型聚氨酯热熔胶透明性优异，耐黄变性好，初粘力大，固化速度快，且固化时胶层不会产生明显气泡，粘接性能优良，最终粘结强度高。
Description
技术领域
本发明涉及密封胶领域，特别是涉及一种高透明反应型聚氨酯热熔胶及其制备方法。
背景技术
反应型聚氨酯热熔胶(PUR)一般以端异氰酸酯基(-NCO)聚氨酯预聚体为基料，配以其他助剂制备而成，该胶粘剂在室温下为固体，热熔施胶后能和水以及含有活泼氢的物质发生化学反应，产生化学交联固化。PUR因具有操作简单、性能优异、环境友好等特点，近年来在诸多行业得到了快速发展。
近年来，随着人们生活水平的提高，对物品的美观要求越来越高，透明材料在化妆品、电子电器、运动器材等领域应用越来越广泛，相应透明胶粘剂需求也与日俱增，PUR因其优异的性能在透明材料粘接领域占据了重要地位。但目前，市售透明PUR大多存在如下几个问题:①透明性不佳，且容易黄变；②初粘力低，固化速度较慢；③固化过程中胶层容易产生较多气泡，导致粘接缺陷。
发明内容
针对上述技术问题，本发明提供了一种高透明反应型聚氨酯热熔胶。该反应型聚氨酯热熔胶透明性优异，耐黄变性好，初粘力大，固化速度快，且固化时胶层不会产生明显气泡，粘接性能优良，最终粘结强度高。
具体的技术方案如下：
一种高透明反应型聚氨酯热熔胶，由以下重量份的原料制备而成：无定形聚酯多元醇20～45份，聚醚多元醇10～50份，异氰酸酯10～40份，丙烯酸树脂10～30份，粘合促进剂0.2～2.5份，潜固化剂0.5～3份，催化剂0.01～0.2份，紫外光吸收剂0.5～2份，抗氧剂0.5～2份；
所述异氰酸酯为环己基甲烷二异氰酸酯(HMDI)、异佛尔酮二异氰酸酯(IPDI)和六亚甲基二异氰酸酯(HDI)中的一种或多种；
所述丙烯酸树脂的玻璃化转变温度大于50℃；
所述粘合促进剂为3-异氰酸酯丙基三乙氧基硅烷、3-异氰酸酯丙基三甲氧基硅烷、3-巯丙基三甲氧基硅烷和3-巯丙基三乙氧基硅烷中的一种或多种；
所述潜固化剂为3-羟乙基-1,3-恶唑烷、2-异丙基-3-羟乙基-1,3-恶唑烷、2-苯基-3-羟乙基-1,3-恶唑烷、(S)-N-Boc-2,2-二甲基-4-(2-羟乙基)恶唑烷、2-异丙基-N-羟乙基-恶唑烷和2,2-二甲基-N-羟乙基-1,3-恶唑烷中的一种或多种。
在其中一些实施例中，所述高透明反应型聚氨酯热熔胶由以下重量份的原料制备而成：无定形聚酯多元醇38～42份，聚醚多元醇25～30份，异氰酸酯12～16份，丙烯酸树脂15～20份，粘合促进剂1.8～2.2份，潜固化剂1.8～2.2份，催化剂0.05～0.15份，紫外光吸收剂0.7～1.0份，抗氧剂1.0～1.4份。
在其中一些实施例中，所述丙烯酸树脂的玻璃化转变温度大于55℃。高玻璃化转变温度的丙烯酸树脂更有利于提高热熔胶的初粘力，同时也可以缩短热熔胶的开放时间。
在其中一些实施例中，所述丙烯酸树脂的玻璃化转变温度为55℃-80℃。
在其中一些实施例中，所述丙烯酸树脂为2013和/或/>2016。
在其中一些实施例中，所述无定形聚酯多元醇的羟值为10mgKOH/g-112mgKOH/g。
在其中一些实施例中，所述无定形聚酯多元醇的羟值为18mgKOH/g-60mgKOH/g。
在其中一些实施例中，所述无定形聚酯多元醇的羟值为30mgKOH/g-50mgKOH/g。
在其中一些实施例中，所述无定形聚酯多元醇为7100系列的无定形聚酯多元醇。
在其中一些实施例中，所述无定形聚酯多元醇为7130和/或/>7150。
在其中一些实施例中，所述聚醚多元醇为聚氧化丙烯二醇。
在其中一些实施例中，所述聚氧化丙烯二醇的数均分子量为1800-2200。
在其中一些实施例中，所述高透明反应型聚氨酯热熔胶由以下重量份的原料制备而成：无定形聚酯多元醇713039～41份，数均分子量为2000的聚氧化丙烯二醇26～28份，异佛尔酮二异氰酸酯13～15份，丙烯酸树脂/>201317～19份，3-异氰酸酯丙基三甲氧基硅烷1.9～2份，3-羟乙基-1,3-恶唑烷1.9～2份，催化剂0.05～0.15份，紫外光吸收剂0.7～1.0份，抗氧剂1.0～1.4份。
在其中一些实施例中，所述催化剂为二月桂酸二丁基锡(DBTDL)、三亚乙基二胺和二吗啉基二乙基醚(DMDEE)中的至少一种。
在其中一些实施例中，所述抗氧剂为四[β-(3,5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯(抗氧剂1010)和2,6-二叔丁基对甲基苯酚(抗氧剂264)中的至少一种。
在其中一些实施例中，所述紫外光吸收剂为UV-123、UV-328、UV-770、UV-928和UV-1130中的至少一种。
本发明还提供了上述高透明反应型聚氨酯热熔胶的制备方法。
具体技术方案如下：
一种耐热反应型聚氨酯热熔胶的制备方法，包括以下步骤：
(1)将所述无定形聚酯多元醇、聚醚多元醇、丙烯酸树脂投入反应容器中，加热至100℃～130℃，在搅拌下真空脱水60分钟～180分钟，真空度为-0.095MPa～-0.05MPa；
(2)投入所述异氰酸酯，在氮气或者惰性气体的保护下于100℃～120℃搅拌反应60分钟～120分钟；
(3)投入所述潜固化剂，在氮气或者惰性气体保护下于100℃～120℃搅拌反应10分钟～30分钟；
(4)依次投入所述粘合促进剂、催化剂、抗氧剂、紫外吸收剂，在氮气或者惰性气体保护下于100℃～120℃搅拌混合20分钟～40分钟；
(5)于100℃～120℃下抽真空至无气泡出现，出料，即得。
本发明的高透明反应型聚氨酯热熔胶，选择无定形聚酯多元醇，不仅能缩短热熔胶的开放时间，提高初粘力，并且利用无定形聚酯多元醇制备的聚氨酯热熔胶冷却后为无色透明固体，相比于冷却后为白色固体的结晶聚酯多元醇，采用无定形聚酯多元醇制备的PUR固化后胶层透明性更高；选择添加适量丙烯酸树脂，在热熔胶冷却时，可以加速热熔胶凝聚，有利于提高热熔胶的初粘力；选择带有活性基团异氰酸基或巯基的偶联剂作为粘合促进剂，带巯基的偶联剂可以与NCO发生化学反应，而带异氰酸基的偶联剂在PUR湿固化反应时可以参与湿固化反应，二者均可引入交联固化体系，同时其附带的烷氧基与粘接基材表面形成氢键或发生化学反应，可以提高热熔胶对粘接基材的附着力；选择带羟基的恶唑烷作为潜固化剂，其羟基可与PUR体系的NCO发生化学反应，而恶唑烷基可以在PUR湿固化时，优先与空气中的湿气发生反应，减少CO2气体的产生，可以防止PUR在粘接时产生气泡，导致粘接缺陷，同时因为恶唑烷基与湿气反应迅速，可以大大提高PUR体系的固化速度。因此，与现有技术相比，本发明具有以下有益效果：
1、本发明的反应型聚氨酯热熔胶通过添加玻璃化转变温度较高的丙烯酸树脂、特定种类的粘合促进剂和潜固化剂，配合特定的异氰酸酯，按照特定配比与无定形聚酯多元醇和聚醚多元醇等组分相互配合制备得到，从而使其具有高透明、初粘力强、固化速度快、最终粘接强度高等综合性能优异的优点，特别适合于对透明性要求较高的领域使用，具有良好的市场前景。
2、本发明的反应型聚氨酯热熔胶为单组分湿气固化聚氨酯胶黏剂，属于无溶剂环保型胶黏剂行业，可用于塑料、玻璃、金属、纺织等基材的粘接。
3、本发明的反应型聚氨酯热熔胶的制备工艺简单，容易操作，易于工业化。
具体实施方式
下面通过具体实施例来进一步说明本发明的技术方案。本领域技术人员应该明了，所述实施例仅仅是帮助理解本发明，不应视为对本发明的具体限制。
除非另有定义，本发明所使用的所有的技术和科学术语与属于本发明的技术领域的技术人员通常理解的含义相同。本发明的说明书中所使用的术语只是为了描述具体的实施例的目的，不用于限制本发明。
本发明的术语“包括”和“具有”以及它们任何变形，意图在于覆盖不排他的包含。例如包含了一系列步骤的过程、方法、装置、产品或设备没有限定于已列出的步骤或模块，而是可选地还包括没有列出的步骤，或可选地还包括对于这些过程、方法、产品或设备固有的其它步骤。
在本发明中提及的“多个”是指两个或两个以上。“和/或”，描述关联对象的关联关系，表示可以存在三种关系，例如，A和/或B，可以表示：单独存在A，同时存在A和B，单独存在B这三种情况。字符“/”一般表示前后关联对象是一种“或”的关系。
本发明实施例和对比例中中采用的无定形聚酯多元醇购自赢创公司的7100系列，具体如下：
7130，羟值为31mgKOH/g～39mgKOH/g；
7150，羟值在38mgKOH/g～46mgKOH/g。
聚氧化丙烯二醇(PPG)购自江苏钟山化工有限公司，Mn＝2000，羟值为54mgKOH/g～58mgKOH/g。
丙烯酸树脂2013、/>2016购自英国璐彩特化工有限公司，其中，
2013的玻璃化转变温度(Tg)为76℃，Mn＝34000；
2016的玻璃化转变温度(Tg)为59℃，Mn＝60000。
丙烯酸树脂AC1420，购自赢创公司，其玻璃化转变温度(Tg)为44℃，Mn＝30000。
松香树脂RE 100L和萜烯树脂/>TR 105购自美国亚利桑那化学公司。
碳化二亚胺改性4,4’-二苯基甲烷二异氰酸酯(MDI)购自美国亨斯迈公司。
其他原料组分均为普通市售产品。
以下为具体实施例。
本发明实施例和对比例所用原料如下表1所示：
表1各实施例和对比例中各原料组分及其配比(重量份)
实施例和对比例提供的反应型聚氨酯热熔胶的制备方法包括以下步骤：
(1)将无定形聚酯多元醇、聚醚多元醇、丙烯酸树脂投入反应釜中，加热至120℃，在搅拌下真空脱水120分钟，真空度为-0.09MPa；
(2)投入异氰酸酯，在N2保护下于110℃搅拌反应90分钟；
(3)投入潜固化剂，在N2保护下于110℃搅拌反应20分钟；
(4)依次投入粘合促进剂、催化剂、抗氧剂、紫外吸收剂，在N2保护下于110℃搅拌混合30分钟；
(5)恒温110℃，抽真空至无气泡出现，出料，即得。
效果测试：
取实施例1-3和对比例1-9制得的反应型聚氨酯热熔胶，按GB/T 7124-2008测试热熔胶的初粘力(试样在25℃/50％RH的条件下进行固化3min后测试的拉伸剪切强度)、固化速度(试样在25℃/50％RH的条件下分别进行固化2h、6h、12h和24h后测试的拉伸剪切强度与最终粘接度的百分比)、最终粘接强度(试样在25℃/50％RH的条件下进行固化7d后测试的拉伸剪切强度)；按GB/T 2410-2008，测试热熔胶的透光率和雾度；按HG/T 3862-2006，测试热熔胶的黄变指数(PUR固化物在氙灯老化仪上照射480h)。测试结果如表2所示。
表2实施例1-3和对比例1-9的反应型聚氨酯热熔胶相关性能测试结果
由表2的实验数据可见，本发明实施例1-3制备的高透明聚氨酯热熔胶具有透明度高、耐黄变性好、初粘力大、固化速度快和最终粘接强度高的优点，可应用于透明材料的粘结应用。其中，实施例3的反应型聚氨酯热熔胶在其优选的原料和特定配比下，获得了最为优异的综合性能。
由对比例1-9与实施例3的性能对比可以看出，对比例1-3分别用碳化二亚胺改性MDI、MDI-50、MDI代替IPDI，其黄变指数大幅增大，耐黄变性能变差；对比例4没有添加丙烯酸树脂，其初粘力由原来的0.5变为0.18，初粘强度显著变小；对比例5-6分别用松香树脂、萜烯树脂代替丙烯酸树脂，不但初粘力和最终粘接强度出现了较大幅度的下降，而且因其本身带有颜色，其黄变指数大于8，出现了较大的变色；对比例7用Tg低于50℃的AC1420代替/>2013，其初粘力由原来的0.5变为0.29，初粘强度明显变小；对比例8没有添加潜固化剂，固化速度明显变慢，且最终粘接强度变差，这可能与无潜固化剂的PUR体系湿固化反应较慢，且会释放较多CO2，使胶层有气泡产生，导致粘接缺陷所致；对比例9没有添加粘合促进剂，其最终粘接强度较差。可见，本发明的各原料组分按照特定种类和配比配合才能同时获得高透明度、耐黄变性好、初粘力大、固化速度快和最终粘接强度高的综合性能。
以上所述实施例的各技术特征可以进行任意的组合，为使描述简洁，未对上述实施例中的各个技术特征所有可能的组合都进行描述，然而，只要这些技术特征的组合不存在矛盾，都应当认为是本说明书记载的范围。
以上所述实施例仅表达了本发明的几种实施方式，其描述较为具体和详细，但并不能因此而理解为对发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。因此，本发明专利的保护范围应以所附权利要求为准。
Claims (7)
1.一种高透明反应型聚氨酯热熔胶，其特征在于，由以下重量份的原料制备而成：无定形聚酯多元醇38～42份，聚醚多元醇25～30份，异氰酸酯12～16份，丙烯酸树脂15～20份，粘合促进剂1.8～2.2份，潜固化剂1.8～2.2份，催化剂0.05～0.15份，紫外光吸收剂0.7～1.0份，抗氧剂1.0～1.4份；
所述异氰酸酯为异佛尔酮二异氰酸酯；
所述丙烯酸树脂为2013；
所述粘合促进剂为3-异氰酸酯丙基三甲氧基硅烷；
所述潜固化剂为3-羟乙基-1,3-恶唑烷；
所述无定形聚酯多元醇为7130；
所述聚醚多元醇为聚氧化丙烯二醇。
2.根据权利要求1所述的高透明反应型聚氨酯热熔胶，其特征在于，所述聚氧化丙烯二醇的数均分子量为1800-2200。
3.根据权利要求2所述的高透明反应型聚氨酯热熔胶，其特征在于，所述聚氧化丙烯二醇的数均分子量为2000。
4.根据权利要求1所述的高透明反应型聚氨酯热熔胶，其特征在于，由以下重量份的原料制备而成：无定形聚酯多元醇7130 39～41份，数均分子量为2000的聚氧化丙烯二醇26～28份，异佛尔酮二异氰酸酯13～15份，丙烯酸树脂/>2013 17～19份，3-异氰酸酯丙基三甲氧基硅烷1.9～2份，3-羟乙基-1,3-恶唑烷1.9～2份，催化剂0.05～0.15份，紫外光吸收剂0.7～1.0份，抗氧剂1.0～1.4份。
5.根据权利要求4所述的高透明反应型聚氨酯热熔胶，其特征在于，由以下重量份的原料制备而成：无定形聚酯多元醇7130 40份，数均分子量为2000的聚氧化丙烯二醇27份，异佛尔酮二异氰酸酯14份，丙烯酸树脂/>2013 18份，3-异氰酸酯丙基三甲氧基硅烷2份，3-羟乙基-1,3-恶唑烷2份，催化剂0.1份，紫外光吸收剂0.8份，抗氧剂1.2份。
6.根据权利要求1-5任一项所述的高透明反应型聚氨酯热熔胶，其特征在于，所述催化剂为二月桂酸二丁基锡、三亚乙基二胺和二吗啉基二乙基醚中的至少一种；和/或，
所述抗氧剂为四[β-(3,5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯和2,6-二叔丁基对甲基苯酚中的至少一种；和/或，
所述紫外光吸收剂为UV-123、UV-328、UV-770、UV-928和UV-1130中的至少一种。
7.一种权利要求1-6任一项所述的高透明反应型聚氨酯热熔胶的制备方法，其特征在于，包括以下步骤：
(1)将所述无定形聚酯多元醇、聚醚多元醇、丙烯酸树脂投入反应容器中，加热至100℃～130℃，在搅拌下真空脱水60分钟～180分钟，真空度为-0.095MPa～-0.05MPa；
(2)投入所述异氰酸酯，在氮气或者惰性气体的保护下于100℃～120℃搅拌反应60分钟～120分钟；
(3)投入所述潜固化剂，在氮气或者惰性气体保护下于100℃～120℃搅拌反应10分钟～30分钟；
(4)依次投入所述粘合促进剂、催化剂、抗氧剂、紫外吸收剂，在氮气或者惰性气体保护下于100℃～120℃搅拌混合20分钟～40分钟；
(5)于100℃～120℃下抽真空至无气泡出现，出料，即得。
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