CN101550324A - 可逆的干粘合剂 - Google Patents

可逆的干粘合剂 Download PDF

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CN101550324A
CN101550324A CNA2008100929506A CN200810092950A CN101550324A CN 101550324 A CN101550324 A CN 101550324A CN A2008100929506 A CNA2008100929506 A CN A2008100929506A CN 200810092950 A CN200810092950 A CN 200810092950A CN 101550324 A CN101550324 A CN 101550324A
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T·谢
X·肖
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Abstract

本发明涉及可逆的干粘合剂。本发明的一个实施方案包括含有弹性环氧干粘合剂的产品，所述弹性环氧干粘合剂从基材的拉脱强度为1－200N/cm2，且通过小于1N/cm的剥离力可以可逆的脱附。

Description

可逆的干粘合剂
[0001]本申请要求2007年4月20日提交的美国临时申请No.60/925,418的利益。
技术领域
[0002]本申请一般涉及的领域包括环氧干粘合剂的组合物(composition of epoxy dry adhesives)。
背景技术
[0003]壁虎足垫，在其上具有纳米毛(nanohair)结构，为灵活的干粘合剂的实例。壁虎粘附的工作原理是该纳米毛结构允许脚垫与相对表面最大接触，与其粗糙度和化学组成无关。这是由纳米毛实现的，纳米毛较长且从脚垫以一定角度突出以便相邻的纳米毛可以接触相对表面，无论所述相对表面的地形结构如何。最大接触进一步使壁虎脚垫和相对表面之间可以累积数百万个小的范德华(在微牛顿的范围内)相互作用，导致整个粘附力(拉脱力(pull-off force))为约10N/cm2。然而，当该脱附力(detaching force)以剥离的方式(in a peel-off mode)应用时，通过克服相应于非常小的面积的小粘附力逐渐地实现完全脱附。因此，粘附容易逆转。总的来说，壁虎粘附的吸引力在于如下组合：粘附强度(10N/cm2)、可逆性和适合于就表面粗糙度和组成而言的各种表面的能力。壁虎粘附的上述独特特征刺激了制备合成的、灵活的干粘合剂的科学研究的努力，所述粘合剂使用与壁虎足部相同的原理工作。迄今为止，两种最好的合成壁虎粘合剂显示出对玻璃的最大拉脱粘合强度为3和10N/cm2。在仅仅一次或两次附着/脱附循环后，这两种粘合剂都遭受严重的粘附损失，这是因为纳米结构的破坏和侧向坍塌(lateral collapse)，后者指壁虎脚垫的相邻纳米毛彼此结合。另外，合成的壁虎粘合剂生产费用高，并且事实上大批生产十分困难。
发明内容
[0004]本发明的一个实施方案包括类似于壁虎足垫起作用的干粘合剂。
[0005]本发明的一个实施方案包括产品，含有弹性环氧干粘合剂(elastomeric epoxy dry adhesive)，其从不锈钢304合金基材(SS304)的拉脱强度为1-200N/cm2。
[0006]本发明的一个实施方案包括含有脂肪族二环氧化物(aliphatic diepoxy)和二胺固化剂(diamine curing agent)的组合物。
[0007]本发明的另一个实施方案包括方法，其包括固化组合物，所述组合物包含脂肪族二环氧化物和二胺固化剂，以提供能粘附到表面的弹性环氧干粘合剂，其从SS304基材的拉脱强度大于10N/cm2，且从相同基材的剥离力为1N/cm或更小。
[0008]本发明的另一个实施方案包括方法，其包括提供由包含脂肪族二环氧化物和二胺固化剂的组合物制成的弹性环氧干粘合剂，将该粘合剂放置在表面上，用力使该粘合剂预先加上载荷以便该粘合剂具有从SS304基材的大于10N/cm2的拉脱强度，使用1N/cm2或更小的剥离力从相同的基材上剥离该粘合剂，并重复所述附着和剥离步骤超过六次。
[0009]本发明的其它示例性实施方案将根据下文提供的详细说明变得显而易见。应当理解本发明的详细说明和具体实施例虽然公开了本发明的示例性实施方案，但仅仅是用于阐述目的，而不意味着限制本发明的范围。
附图说明
[0010]根据详细说明和附图将更充分地理解本发明的示例性实施方案，其中：
[0011]图1图解了Jeffamine D-230和NGDE的化学结构。
[0012]图2图解了在干环氧粘合剂的刚性背层上的拉脱力。
[0013]图3为拉脱强度对附着/脱附循环数的关系图。
[0014]图4图解了干粘合剂的剥离力。
[0015]图5图解了EPON 826和十八烷基胺的化学结构。
具体实施方式
[0016]下述实施方案的描述本质上仅仅是示例性的，决不意味着限制本发明、其应用或用途。
[0017]本发明的一个实施方案包括具有类似于壁虎足垫功能的干粘合剂。在一个实施方案中，所述干粘合剂可具有玻璃转化温度Tg为从-90至25℃。
[0018]本发明的一个实施方案包括产品，含有弹性环氧干粘合剂，其从SS304基材的拉脱强度为1-200N/cm2。关于拉脱强度，本发明不限于从SS304基材的拉脱强度。可使用多种基材获得1-200N/cm2的拉脱强度。
[0019]本发明的一个实施方案包括包含脂肪族二环氧化物和二胺固化剂的组合物。
[0020]本发明的另一个实施方案包括方法，所述方法包括固化组合物，所述组合物包含脂肪族二环氧化物和二胺固化剂，以提供能粘附到表面的弹性环氧干粘合剂，其从SS304基材的拉脱强度大于10N/cm2，且从相同基材的剥离力为1N/cm或更小。
[0021]本发明的另一个实施方案包括一种方法，其包括提供由包含脂肪族二环氧化物和二胺固化剂的组合物制备的弹性环氧干粘合剂，将该粘合剂放置在表面上，用力对该粘合剂预先施加载荷以便该粘合剂从SS304基材的拉脱强度为大于10N/cm2，使用1N/cm或更小的剥离力从相同的基材上剥离该粘合剂，并重复所述附着和剥离步骤超过六次。
[0022]在本发明的一个实施方案中，制备弹性环氧干粘合剂。在一个实施方案中，将4.32g的新戊二醇二环氧甘油醚(NGDE)与2.3g的Jeffamine D-230混合，Jeffamine D-230为固化剂聚(丙二醇)二(2-氨基丙基)醚。Jeffamine D-230为聚醚胺，其为双官能的伯胺，平均分子量为约230。伯胺基位于脂肪族聚醚链末端的仲碳上。NGDE可以从TCI America获得，Jeffamine D-230可以从Huntsman获得。Jeffamine D-230和NGDE的化学结构显示在图1中。将4.32g的NGDE和2.3g的Jeffamine D-230的液体混合物倾入铝模中。在100℃，在烘箱中固化该混合物约1.5小时。然后，将该混合物在130℃后固化约1小时。
[0023]脱模所固化的环氧干粘合剂，并切成约1cmx1cm的片。为了测定拉脱力，将1cmx1cm环氧干粘合剂片10的一面结合到刚性基材或背层12比如刚性环氧化物上。将所述环氧干粘合剂片的另一面放置在基材14例如SS304上。通过将载荷16施加在朝上的刚性基材表面上而施加4N的预载荷力，所述干环氧粘合剂面朝下对着基材14，如图2所示。
[0024]用测力计测定粘附力，对应于相同的样品的多个附着/脱附循环的最大拉脱力显示在图3中。在图3中的数据显示出在六次附着/脱附循环后拉脱力不降低，平均的拉脱力为约60N/cm2。
[0025]为了测定剥离力，通过负载16施加的4N预载荷，将不含刚性背层的干粘合剂10压在SS304表面14上，以剥离方式施加分离力并用测力计测量，如在图4中所示。所述剥离力小于1N/cm。在一个实施方案中，弹性干粘合剂可以进行多次附着和脱附循环，而没有粘附损失。
[0026]在另一个实施方案中，以在下述表1中列出的比例混合NGDE和Jeffamine D-230。在100℃固化该混合物1.5小时，并在130℃后固化其1小时。在NGDE对Jeffamine D-230的各种摩尔比下得到的拉脱强度显示在下表1中。
表1.样品1-7的拉脱强度
Figure A20081009295000071
[0027]在另一个实施方案中，保持胺基的总数为环氧基总数的两倍，以不同的比例混合EPON 826(双酚A环氧单体的二环氧甘油醚)、Jeffamine D-230和十八烷基胺(CH3(CH2)17NH2，示例性的脂肪单胺)。EPON 826和十八烷基胺的化学结构显示在图5中。EPON 826可以从Hexion获得。在100℃固化该混合物1.5小时，并在130℃后固化其1小时。当Jeffamine D-230和十八烷基胺的摩尔比从0变至无限大时，从固化的环氧化物获得的从SS304基材的拉脱强度落入1N/cm2至100N/cm2的范围。
[0028]在根据本发明各种实施方案的组合物中使用的胺可以是脂肪族胺、支链的胺或芳香族胺。
[0029]一个实施方案包括方法，其包括固化组合物，所述组合物包含至少一种多官能环氧化物(脂肪族或芳香族)、和固化剂(例如芳香族或脂肪族酐，或芳香族或脂肪族多胺)或者催化剂的至少一种，以提供从SS304基材的拉脱强度为1-100N/cm2的弹性环氧干粘合剂。
在各个实施方案中，弹性环氧干粘合剂的组分可包括刚性环氧化物和柔性增充剂(flexible extender)。可用于获得弹性环氧干粘合剂的可能的交联化学品的范围可包括α，ω-二氨基烷烃、有机多羧酸、酸酐或催化的(如咪唑类型中)交联反应物(crosslinking reaction)。存在许多获得分子性质之间的适当关系的不同方式。例如，所述弹性环氧干粘合剂可包括刚性环氧化物、环氧增充剂和交联剂；或刚性环氧化物、柔性交联剂和柔性环氧化物；或刚性环氧化物、刚性交联剂和柔性环氧化物；或刚性环氧化物、柔性环氧化物和催化固化剂；或刚性环氧化物、交联剂和稀释剂；或柔性环氧化物、交联剂和稀释剂；或刚性环氧化物和柔性交联剂；或柔性环氧化物和催化固化剂；或柔性环氧化物和交联剂；和其中，所述刚性环氧化物为具有至少两个环氧基的芳香族环氧化物，所述柔性环氧化物为具有至少两个环氧基的脂肪族环氧化物，所述环氧化物增充剂具有一个环氧基，且所述交联剂为多胺、有机多羧酸或酸酐中的一种，所述稀释剂为单胺或单羧酸。在各个实施方案中，所述催化固化剂(或催化固化物)促进环氧基-至-环氧基或环氧基-至-羟基的反应。所述催化固化剂可包括但不限于叔胺、胺盐、三氟化硼络合物或硼酸胺。所述干粘合剂的组分可以以一定量存在，当所述组合物固化时，该量足够提供具有低于室温的玻璃转化温度和从基材的拉脱强度为1-200N/cm2的弹性环氧干粘合剂。
[0030]本发明实施方案的上述说明本质上仅仅是示例性的，因此，其变化不能被认为是背离本发明的精神和范围。

Claims (20)

1.弹性环氧干粘合剂组合物，其包括：
刚性环氧化物或柔性环氧化物的至少一种；和
交联剂或催化固化剂的至少一种；
其中所述刚性环氧化物为具有至少两个环氧基的芳香族环氧化物，所述柔性环氧化物为具有至少两个环氧基的脂肪族环氧化物，且所述交联剂为多胺、有机多羧酸或酸酐中的一种；和
其中所述组分以一定量存在，当所述组合物固化时，该量足够提供具有低于室温的玻璃转化温度和从基材的拉脱强度为1-200N/cm2的弹性环氧干粘合剂。
2.如权利要求1所述的弹性环氧干粘合剂组合物，其进一步包括具有一个环氧基的环氧增充剂。
3.如权利要求1所述的弹性环氧干粘合剂组合物，其进一步包括稀释剂，其中所述稀释剂为单胺或单羧酸。
4.如权利要求1所述的弹性环氧干粘合剂组合物，其中所述弹性环氧干粘合剂从基材的拉脱强度为10-100N/cm2。
5.如权利要求1所述的弹性环氧干粘合剂组合物，其中所述弹性环氧干粘合剂能够粘合至基材，从所述基材的剥离力小于1N/cm。
6.如权利要求1所述的弹性环氧干粘合剂组合物，包括脂肪族二环氧化物和二胺。
7.如权利要求6所述的弹性环氧干粘合剂组合物，进一步包括芳香族二环氧化物。
8.如权利要求1所述的弹性环氧干粘合剂组合物，其中所述芳香族环氧化物为环氧当量为180的双酚A环氧单体的二环氧甘油醚。
9.如权利要求1所述的弹性环氧干粘合剂组合物，其中所述脂肪族环氧化物为NGDE。
10.如权利要求1所述的弹性环氧干粘合剂组合物，其中所述多胺为平均分子量为230的聚(丙二醇)二(2-氨基丙基)醚。
11.如权利要求3所述的弹性环氧干粘合剂组合物，包括芳香族二环氧化物、二胺和单胺。
12.如权利要求1所述的弹性环氧干粘合剂组合物，其中所述柔性环氧化物的分子量等于或大于216。
13.方法，包括固化包含如下组分的组合物：
多官能脂肪族环氧化物或多官能芳香族环氧化物的至少一种；和
至少一种固化剂，其中所述固化剂为芳香族酸酐、脂肪族酸酐、芳香族多胺或脂肪族多胺中的一种；
以提供弹性环氧干粘合剂，其从基材的拉脱强度为1-100N/cm2。
14.如权利要求13所述的方法，其中所述弹性环氧干粘合剂能够粘合至基材，从基材的剥离力为1N/cm2或更少。
15.如权利要求13所述的方法，其中所述弹性环氧干粘合剂的玻璃转化温度低于室温。
16.方法，包括提供由包含脂肪族二环氧化物和二胺的组合物制备的弹性环氧干粘合剂，将该粘合剂放置在基材上，用力为该粘合剂预先施加载荷以便所述粘合剂从所述基材的拉脱强度大于10N/cm2，和使用1N/cm或更小的剥离力从所述相同的基材上剥离所述粘合剂。
17.如权利要求16所述的方法，进一步包括重复所述附着和剥离步骤超过六次。
18.弹性环氧干粘合剂，包括：
刚性环氧化物或柔性环氧化物的至少一种和交联剂或催化固化剂的至少一种的反应产物；
其中所述刚性环氧化物为具有至少两个环氧基的芳香族环氧化物，所述柔性环氧化物为具有至少两个环氧基的脂肪族环氧化物，且所述交联剂为多胺、有机多羧酸或酸酐中的一种；和
其中所述弹性环氧干粘合剂的玻璃转化温度低于室温，且从基材的拉脱强度为1-200N/cm2。
19.如权利要求18所述的弹性环氧干粘合剂，进一步包括具有一个环氧基的环氧增充剂的反应产物。
20.如权利要求18所述的弹性环氧干粘合剂，进一步包括稀释剂的反应产物，其中所述稀释剂为单胺或单羧酸。
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