CN116751533B - 一种非后固化型环氧胶带及其制备方法 - Google Patents
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Abstract
本发明涉及胶黏剂技术领域,公开了一种非后固化型环氧胶带及其制备方法,沿厚度方向,所述环氧胶带由下至上依次包含基材层、环氧胶膜层及离型膜层,所述环氧胶膜层所采用的原料按照重量份数计,包含以下组分:双酚A型环氧树脂70‑100份、二元醇二缩水甘油醚50‑80份、增韧剂0‑20份、固化剂5‑15份、丁酮50‑100份、N,N‑二甲基甲酰胺15份,所述固化剂由脂环胺和双氰胺混合而成,所述双氰胺经N,N‑二甲基甲酰胺溶解后与脂环胺混合。本发明的环氧胶带具有粘接强度高,耐温性好的优点,且在制备过程中无需后固化,制备周期短、粘接速度快。
Description
技术领域
本发明涉及胶黏剂技术领域,具体涉及一种非后固化型环氧胶带及其制备方法。
背景技术
环氧胶黏剂因其具有高粘接强度、低收缩、化学性质稳定、电绝缘性优异等优点一直备受关注,可用于金属、塑料等常见材料的结构性粘接。在电子产品、汽车、建筑等行业得到了极为广泛的应用。例如,在新的柔性电路生产制程中,通过预先将铜箔按照线路布局要求进行裁切,然后在裁切后的电路两侧贴合PI基材环氧胶带,进而完成柔性电路的生产,该制程取代了原有刻蚀生产制程,有效降低了柔性电路的生产成本和生产效率,备受关注和发展。
目前现有的环氧胶带通常需要进行高温预贴合,且预贴合后粘接强度普遍不高,同时由于普遍使用了粉末形态的潜伏性固化剂(如双氰胺,酸酐等)进行后固化,需要在较高的温度下经历0.5-2h的后固化过程,以达到足够的贴合强度和耐高温要求。这势必会严重降低相关产品的生产效率,导致生产成本大幅增加。同时粉末性固化剂的使用也会给胶带生产过程中的分散均匀性、涂布均匀性及外观等带来了挑战及不确定性。并且,现有的环氧胶带由于往往使用潜伏性固化剂,为保证其性能稳定,往往需要在10℃以下进行低温储存,这大大限制了其运输灵活性,同时抬升了成本。
因此,需要开发一款生产简便、无需后固化,且可常温储存的环氧胶带,以满足日益迫切的应用需求。
发明内容
本发明的目的是克服现有技术的不足,提供一种非后固化型环氧胶带。
为达到上述目的,本发明采用的技术方案是:一种非后固化型环氧胶带,其特征在于,沿厚度方向,所述环氧胶带由下至上依次包含基材层、环氧胶膜层及离型膜层,所述环氧胶膜层所采用的原料按照重量份数计,包含以下组分:双酚A型环氧树脂70-100份、二元醇二缩水甘油醚50-80份、增韧剂0-20份、固化剂5-15份、丁酮50-100份、N,N-二甲基甲酰胺15份,所述固化剂由脂环胺和双氰胺混合而成,所述双氰胺经N,N-二甲基甲酰胺溶解后与脂环胺混合。
作为一种具体的实施方式,原料中所采用的所述双酚A型环氧树脂的环氧当量介于700-2500之间,所述二元醇二缩水甘油醚的环氧当量介于100-400之间,其中环氧树脂的环氧当量对胶带的最终性能有较大影响,环氧当量过低会造成胶膜柔韧性不佳和基材附着性差,产生脱基风险;环氧当量过高则会造成环氧树脂溶解困难,不利于涂布。
作为一种具体的实施方式,所述增韧剂采用了环氧化二烯烃,其环氧当量介于100-300之间。
作为一种具体的实施方式,所述双酚A型环氧树脂采用了南亚塑胶工业股份有限公司(以下简称南亚塑胶)生产的型号为NPES-903H、NPES-907、NPES-909中的至少一种。
作为一种具体的实施方式,所述的二元醇缩水甘油醚购自日本三洋化成工业,具体型号为GLYCI-ALE PP-300P。
作为一种具体的实施方式,所述增韧剂采用了大赛璐贸易(上海)有限公司生产的型号为DAICEL PB-3600的环氧化聚丁二烯。
作为一种具体的实施方式,所述固化剂由脂环胺和双氰胺按照质量比1-5:1配置而成,所述脂环胺采用了孟烷二胺、异佛尔酮二胺两者中的至少一种,所述脂环胺为液体,所述双氰胺为粉末状。
本发明的另一个目的是提供一种非后固化型环氧胶带的制备方法,用于制备上述非后固化型环氧胶带,包含以下步骤:
1)将双酚A型环氧树脂与丁酮按照比例进行混合,在高速搅拌机中快速搅拌直至环氧树脂全部溶解,然后依次将二元醇二缩水甘油醚和增韧剂加入到完全溶解的环氧树脂中,继续搅拌20min至混合均匀;
2)将双氰胺溶解在N,N-二甲基甲酰胺中,然后将脂环胺和溶解后的双氰胺依次加入到上述混合均匀的胶液中,高速搅拌10-15min;
3)通过刮刀或涂布机将步骤2)中配置完成的胶液在适用期内涂布在50μm的聚酰亚胺(PI)基材上,放入高温烘箱,135℃烘烤5min,去除溶剂,并完成初步固化反应,保证干胶厚度在30μm±1μm之间,而后再贴附离型膜,并在60℃温度条件下放置72h,确保固化剂反应完全,从而完成所述环氧胶带的制备。
这里将潜伏性粉末固化剂双氰胺提前溶解在溶剂中,大大降低了胶液分散不均引起的外观不良及粘接性能风险,并且在保证充足的胶水适用期以保证涂布稳定性的同时,提高了相关潜伏性固化剂的反应活性,确保涂布后的环氧胶在一定时间内固化反应完全,从而提高了其常温储存稳定性。
作为一种具体的实施方式,所述基材采用了PI基材。
由于上述技术方案的运用,本发明与现有技术相比具有下列优点:
1)与现有产品相比,采用本发明配方的环氧胶带,其在应用时不需要进行耗时的后固化过程,只需在一定温度(150℃)下和压力(0.4Mpa)下,5-8min即可达到高的粘接强度,贴合后220℃下30min无起泡溢胶,耐温性佳;
2)本发明中固化剂采用了脂环胺和双氰胺搭配使用,避免了固体双氰胺粉末分散所需的繁杂费时过程,且常温下具有长达6h以上的适用期,保证了涂布的稳定性和生产的可行性,脂环胺体系固化的环氧树脂其热变形温度相对较高,可达150℃左右,具有较好的耐温性,且常温下具有相对合适的适用期,双氰胺固化的环氧树脂热变形温度相对较低,在相对较低的热压温度和较短的时间内即可实现一定的粘接强度,双氰胺本身粉末形态时可以作为潜伏性固化剂,固化所需温度很高(180℃以上),本发明通过将双氰胺提前溶解加入到环氧体系中,其反应活性大幅增加,失去潜伏效果,在较低的温度下和较短的时间内即可完成反应固化,通过两种固化剂体系固化后的热变形温度调控,在应用时只需较低的贴合温度和贴合时间,即可在短时间内达到高的粘接强度,为贴合材质提供粘接和保护功能;
3)本发明制备得到的环氧胶带在制备过程中无需后固化过程,反应完全后无潜伏性固化剂存在,不需要进行常规高温后固化过程,此外,本发明通过合理的增韧剂体系,胶厚在30μm时, 仍能在PI基材上保持良好的附着性和柔韧性。
具体实施方式
下面结合具体实施例来对本发明的技术方案作进一步的阐述。
实施例1
本例中提供一种非后固化型环氧胶带,其制备方法如下:
1)将100份双酚A型环氧树脂(NPES-909)溶于100份丁酮中,使用高速搅拌机搅拌至环氧树脂完全溶解,而后依次加入50份GLYCI-ALE PP-300P,15份环氧化聚丁二烯,继续搅拌20min至混合均匀;
2)将粉末状的双氰胺固化剂溶解在15份N,N-二甲基甲酰胺中,然后将溶解后的2.5份双氰胺和3.5份溶液状孟烷二胺依次加入到上述混合胶液中,继续搅拌15-20min, 确保混合均匀;
3)将上述制备好的原胶通过刮刀涂布在50μm的PI基材上,放入高温烘箱,135℃烘烤5min,干胶厚度至30μm,取出冷却后贴附离型膜,然后将其放入80℃烘箱中72h确保反应完全。
本例中,双酚A型环氧树脂购自南亚塑胶工业股份有限公司(以下简称南亚)NPES-909,其环氧当量约1800-2400;二元醇二缩水甘油为三洋化成工业的GLYCI-ALE PP-300,其环氧当量约为296;所述增韧剂为大赛璐贸易(上海)有限公司的DAICEL PB-3600,其环氧当量约为196,该增韧剂与双酚A型环氧树脂具有极佳的相容性。
实施例2
本例中提供一种非后固化型环氧胶带,其制备方法与实施例1相同,其与实施例1不同点在于,本例中用于制备环氧胶带的组分和含量变更为:
20份NPES-903H,80份NPES-909,70份GLYCI-ALE PP-300P,15份环氧化丁二烯,3份双氰胺,6份异佛尔酮二胺,丁酮90份,N,N-二甲基甲酰胺15份。
本例中,所述双酚A型环氧树脂采用了南亚NPES-903H和NPES-909两种型号,NPES-903H的环氧当量在740-780,NPES-909的环氧当量在1800-2400。
实施例3
本例中提供一种非后固化型环氧胶带,其制备方法与实施例1相同,其与实施例1不同点在于,本例中用于制备环氧胶带的组分和含量变更为:
100份NPES-907, 60份GLYCI-ALE PP-300P,18份环氧化丁二烯,3份双氰胺,4.5份孟烷二胺,丁酮80份,N,N-二甲基甲酰胺15份。
本例中,所述双酚A型环氧树脂采用了南亚环氧树脂NPES-907,其环氧当量在1500-1800。
实施例4
本例中提供一种非后固化型环氧胶带,其制备方法与实施例1相同,其与实施例1不同点在于,本例中用于制备环氧胶带的组分和含量变更为:
100份NPES-907,60份GLYCI-ALE PP-300P,2.5份双氰胺,4份异佛尔酮二胺,丁酮90份,N,N-二甲基甲酰胺15份。
实施例5
本例中提供一种非后固化型环氧胶带,其制备方法与实施例1相同,其与实施例1不同点在于,本例中用于制备环氧胶带的组分和含量变更为:
100份NPES-903H, 80份GLYCI-ALE PP-300P,20份环氧化丁二烯,3份双氰胺,10份孟烷二胺,丁酮50份,N,N-二甲基甲酰胺15份。
实施例6
本例中提供一种非后固化型环氧胶带,其制备方法与实施例1相同,其与实施例1不同点在于,本例中用于制备环氧胶带的组分和含量变更为:
100份NPES-903H, 80份GLYCI-ALE PP-300P,5份环氧化丁二烯,3份双氰胺,10份孟烷二胺,丁酮60份,N,N-二甲基甲酰胺15份。
对比例1
本例中提供一种非后固化型环氧胶带,其制备方法与实施例5相同,其与实施例5不同点在于,本例中用于制备环氧胶带的组分和含量变更为:
100份NPES-903H,45份GLYCI-ALE PP-300P,20份环氧化丁二烯,3份双氰胺,10份孟烷二胺,丁酮50份,N,N-二甲基甲酰胺15份。
对比例2
本例中提供一种非后固化型环氧胶带,其制备方法与实施例5相同,其与实施例5不同点在于,本例中用于制备环氧胶带的组分和含量变更为:
100份NPES-903H, 80份GLYCI-ALE PP-300P,20份环氧化丁二烯,13份双氰胺,丁酮70份,N,N-二甲基甲酰胺15份。
对比例3
本例中提供一种非后固化型环氧胶带,其主体组分和含量与实施例5相同,制备方法过程也与实施例5大体类似,其与实施例5不同点在于制备方法第2)步:不需将双氰胺提前溶解在N,N-二甲基甲酰胺,而是将双氰胺以原始粉末形式直接加入到混合胶液中。
对比例4
本例中提供一种非后固化型环氧胶带,其制备方法与实施例5相同,其与实施例1不同点在于,本例中用于制备环氧胶带的组分和含量变更为:
100份南亚NPES-901,其环氧当量为450-500,80份GLYCI-ALE PP-300P,20份环氧化丁二烯,3份双氰胺,10份孟烷二胺,丁酮50份,N,N-二甲基甲酰胺15份。
对实施例1至6及对比例1至4中所得到的环氧胶带进行以下测试:
1)剥离力及破坏模式测试
将所述PI环氧胶带贴附在30微米铜箔上,在热压机150℃,0.4Mpa条件下热压5min,取出冷却后,然后按照GB2792-2014测试胶带从铜箔上180°剥离的剥离力,记录破坏模式。
2)溢胶及起泡测试
将所述PI环氧胶带按照上述一样方式贴合铜箔后,用夹子固定两端,在220℃烘箱中放置30min, 冷却后取出,观察是否有溢胶和起泡现象。
3)胶膜在PI基材表面外观及柔韧性测试
将制备好的环氧胶带裁切成5cm*5cm的方块,撕除离型膜,将其向PI基材一侧完全对折,观察胶膜是否有裂纹以及是否从基材上脱离。
测试结果见表1。
表1:
从表1中我们可以看出,本发明的实施例具有高的剥离强度,耐高温性好,在PI基材上具有良好的柔韧性和附着性能。
上述实施例只为说明本发明的技术构思及特点,其目的在于让熟悉此项技术的人士能够了解本发明的内容并据以实施,并不能以此限制本发明的保护范围。凡根据本发明精神实质所作的等效变化或修饰,都应涵盖在本发明的保护范围之内。
Claims (6)
1.一种非后固化型环氧胶带,其特征在于,沿厚度方向,所述环氧胶带由下至上依次包含基材层、环氧胶膜层及离型膜层,所述环氧胶膜层所采用的原料按照重量份数计,包含以下组分:双酚A型环氧树脂70-100份、二元醇二缩水甘油醚50-80份、增韧剂0-20份、固化剂5-15份、丁酮50-100份、N,N-二甲基甲酰胺15份,所述固化剂由脂环胺和双氰胺混合而成,所述双氰胺经N,N-二甲基甲酰胺溶解后与脂环胺混合,
其中,原料中所采用的所述双酚A型环氧树脂的环氧当量介于700-2500之间;
所述增韧剂采用了环氧化二烯烃,其环氧当量介于100-300之间;
所述的二元醇缩水甘油醚购自日本三洋化成工业,具体型号为GLYCI-ALE PP-300P。
2.根据权利要求1所述的非后固化型环氧胶带,其特征在于,所述双酚A型环氧树脂采用了南亚塑胶工业股份有限公司生产的型号为NPES-903H、NPES-907、NPES-909中的至少一种。
3.根据权利要求1所述的非后固化型环氧胶带,其特征在于,所述增韧剂采用了大赛璐贸易(上海)有限公司生产的型号为DAICEL PB-3600的环氧化聚丁二烯。
4.根据权利要求1所述的非后固化型环氧胶带,其特征在于,所述固化剂由脂环胺和双氰胺按照质量比1-5:1配制而成,所述脂环胺采用了孟烷二胺、异佛尔酮二胺两者中的至少一种。
5.一种非后固化型环氧胶带的制备方法,用于制备如权利要求1至4中任一权利要求所述的非后固化型环氧胶带,其特征在于,包含以下步骤:
1)将双酚A型环氧树脂与丁酮按照比例进行混合,在高速搅拌机中快速搅拌直至环氧树脂全部溶解,然后依次将二元醇二缩水甘油醚和增韧剂按比例加入到完全溶解的环氧树脂中,继续搅拌20min至混合均匀;
2)将双氰胺溶解在N,N-二甲基甲酰胺中,然后将脂环胺和溶解后的双氰胺依次加入到上述混合均匀的胶液中,高速搅拌10-15min;
3)通过刮刀或涂布机将步骤2)中配制完成的胶液在适用期内涂布在50μm的基材上,放入高温烘箱,135℃烘烤5min,去除溶剂,并完成初步固化反应,保证干胶厚度在30μm±1μm之间,而后再贴附离型膜,并在80℃温度条件下放置72h,确保固化剂反应完全,从而完成所述环氧胶带的制备。
6.根据权利要求5所述的非后固化型环氧胶带的制备方法,其特征在于,所述基材采用了PI基材。
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