CN115260969B - 一种铝塑膜用热熔复合胶黏剂及其制备方法和应用 - Google Patents

一种铝塑膜用热熔复合胶黏剂及其制备方法和应用 Download PDF

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CN115260969B
CN115260969B CN202211050263.4A CN202211050263A CN115260969B CN 115260969 B CN115260969 B CN 115260969B CN 202211050263 A CN202211050263 A CN 202211050263A CN 115260969 B CN115260969 B CN 115260969B
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composite adhesive
plastic film
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关秋
井光辉
袁功道
莫丽丽
戴平翔
徐秋春
戴晓兵
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Jiangxi Shengwei Material Co ltd
Zhuhai Smoothway Electronic Materials Co Ltd
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Abstract

本发明公开了一种铝塑膜用热熔复合胶黏剂及其制备方法，按质量百分数计，包括聚酯多元醇20.0‑60.0％、聚己内酯二元醇10.0‑30.0％、二异氰酸酯5.0‑15.0％、热塑性树脂5.0‑15.0％、扩链剂0‑5.0％、增塑剂0‑5.0％、填料0‑3.0％、催化剂0.05‑1.0％、功能助剂0‑8.0％，制备所述聚酯多元醇的二元酸为间苯二甲酸和癸二酸。本发明还提供一种铝塑膜用热熔复合胶黏剂用于铝塑膜中保护膜与铝箔之间的粘结。将本发明的热熔复合胶黏剂用于铝塑膜中保护膜与铝箔之间的粘结，使得铝塑膜具有良好的冲深性能和较高的高温剥离强度，抗高温分层性好。

Description

一种铝塑膜用热熔复合胶黏剂及其制备方法和应用
技术领域
本发明涉及热熔胶技术领域，更具体地涉及一种铝塑膜用热熔复合胶黏剂及其制备方法和应用。
背景技术
铝塑膜是软包装电池的重要材料，比其他包装材料拥有如电池轻量化、高能量密度、尺寸灵活等独特优点，得到了广泛的应用。目前铝塑膜制造业普遍采用干法复合工艺，虽然设备简单成本较低，但是VOC的排放需要购买设备如RTO进行治理，否则排放超标致病致害的问题会引起社会的广泛关注。
热熔复合从根本上避免了制造过程的溶剂排放，其100％固体含量，不含任何有机溶剂，不造成环境污染，为环境友好材料。但是传统的热熔胶在高温下的性能减弱，导致铝塑膜的冲深性能不佳及抗高温分层能力弱。
发明内容
为了克服现有技术的缺陷，本发明的目的是提供一种铝塑膜用热熔复合胶黏剂，将其用于铝塑膜中保护膜与铝箔之间的粘结，使得铝塑膜具有良好的冷冲深性能和较高的高温剥离强度，抗高温分层性好。
为了实现上述目的，本发明公开了一种铝塑膜用热熔复合胶黏剂，按质量百分数计，包括聚酯多元醇20.0-60.0％、聚己内酯二元醇10.0-30.0％、二异氰酸酯5.0-15.0％、热塑性树脂5.0-15.0％、扩链剂0-5.0％、增塑剂0-5.0％、填料0-3.0％、催化剂0.05-1.0％、功能助剂0-8.0％；
其中，制备所述聚酯多元醇的二元酸为间苯二甲酸和癸二酸。
相应地，本发明还提供一种铝塑膜用热熔复合胶黏剂的制备方法，包括步骤：将聚酯多元醇、聚己内酯二元醇、热塑性树脂、填料、增塑剂、功能助剂加入反应容器中，在100-140℃下真空熔融干燥0.5-2小时，在氮气保护下，加入二异氰酸酯与催化剂，滴加扩链剂，检测NCO含量为0.5％-5％，得到热熔复合胶黏剂。
相应地，本发明还提供一种铝塑膜用热熔复合胶黏剂用于铝塑膜中保护膜与铝箔之间的粘结。
本发明的有益之处在于：本发明的铝塑膜用热熔复合胶黏剂为单组份反应性聚氨酯热熔胶，不需组配，无计量失误之虞，可确保施工质量，快速粘接，粘接时无须胶带或夹具固定，简化了操作，加热后冷凝硬化即可到达一般热塑性热熔胶的物理粘接强度，常温下后续反应交联固化，粘接强度大幅度提高，优良的耐水、耐溶剂及耐低温性能。尤其是将其用于铝塑膜中保护膜与铝箔之间的粘结，使得该铝塑膜初始剥离强度高，冷冲深性能好，抗高温分层性能好。且对比现有的干法复合工艺，本发明可采用挤出流延复合工艺避免了制造过程大量有机溶剂排放、收集与后处理设备，制造过程更加高效环保。
具体实施方式
为详细说明本发明的技术内容、构造特征、所实现目的及效果，以下结合实施方式详予说明。
本发明提供一种铝塑膜用热熔复合胶黏剂，按质量百分数计，包括聚酯多元醇20.0-60.0％、聚己内酯二元醇10.0-30.0％、二异氰酸酯5.0-15.0％、热塑性树脂5.0-15.0％、扩链剂0-5.0％、增塑剂0-5.0％、填料0-3.0％、催化剂0.05-1.0％、功能助剂0-8.0％。
其中，聚酯多元醇由二元羧酸与二元醇通过缩聚反应得到，在本发明中，聚酯多元醇的二元酸为间苯二甲酸和癸二酸，制得的聚酯多元醇耐高温、耐湿热性较优，更优选地，聚酯多元醇由间苯二甲酸、癸二酸、新戊二醇和乙二醇制得，制得的聚酯多元醇不仅耐高温、耐湿热，还有较好的柔韧性，有利于冲深。而对于通过间苯二甲酸、癸二酸、新戊二醇和乙二醇制备聚酯多元醇的方法属于本领域对聚酯多元醇的常规制备方法，在此不进行阐述。
在一较佳实施例中，聚酯多元醇的重均分子量为400-2000。
在一较佳实施例中，聚酯多元醇的羟值为50-200mgKOH/g。
在一较佳实施例中，聚酯多元醇的酸值为0.1-1.0mgKOH/g。
示例地，聚酯多元醇的含量可为但不限于20.0％、30.0％、40.0％、50.0％、60.0％。
在一较佳实施例中，聚己内酯二元醇的重均分子量为400-2000。
示例地，聚己内酯二元醇的含量可为但不限于10.0％、15.0％、20.0％、25.0％、30.0％。
在一较佳实施例中，二异氰酸酯选自MDI，TDI，HDI，HMDI中的至少一种。
示例地，二异氰酸酯的含量可为但不限于5.0％、8.0％、10.0％、12.0％、15.0％。
在一较佳实施例中，所述热塑性树脂为醛酮树脂、松香树脂、萜烯树脂、丙烯酸树脂中的任意一种。因松香树脂的耐热性较差，因此，更为优选地，热塑性树脂为醛酮树脂、萜烯树脂、丙烯酸树脂中的任意一种。进一步地，萜烯树脂可为但不限于萜烯酚醛树脂。
示例地，热塑性树脂的含量可为但不限于5.0％、8.0％、10.0％、12.0％、15.0％。
在一较佳实施例中，所述扩链剂选自1，4一丁二醇、1，6一己二醇、甘油、三羟甲基丙烷、二甘醇、三甘醇、新戊二醇、山梨醇、二乙氨基乙醇、腰果酚改性聚醚二醇中的至少一种。扩链剂是能与线型聚合物链上的官能团反应而使分子链扩展、分子量增大的物质，提升产品物化性能。更为优选地，腰果酚改性聚醚二醇柔软性佳，故而，扩链剂采用腰果酚改性聚醚二醇可使得铝塑膜的冲深性能得到有效提升。
示例地，扩链剂的含量可为但不限于0％、1％、2％、3％、4％、5％。优选地，扩链剂的含量为0.05-5.0％。
在一较佳实施例中，增塑剂选自邻苯二甲酸酯、脂肪族二元酸酯、脂肪酸酯、苯多酸酯、多元醇酯、环氧烃类、烷基磺酸酯中的任意一种。
示例地，增塑剂的含量可为但不限于0％、1％、2％、3％、4％、5％。优选地，增塑剂的含量为0.05-5.0％。
在一较佳实施例中，填料选自高岭土、硅藻土、滑石粉、石墨、炭黑、氧化铝粉、玻璃粉、石棉粉、云母粉、石英粉、碳纤维、粉末状软木、金刚砂中的至少一种。
示例地，填料的含量可为但不限于0％、1％、2％、3％。优选地，填料的含量为0.05-3.0％。
在一较佳实施例中，催化剂选自有机铋催化剂。
示例地，催化剂的含量可为但不限于0.05％、0.08％、1％。
功能助剂包括但不限于抗氧剂，附着力促进剂，抗水解剂等。
示例地，功能助剂的含量可为但不限于0％、1％、2％、3％、4％、5％、6％、7％、8％。优选地，功能助剂的含量为0.05-8.0％。
本发明还提供一种铝塑膜用热熔复合胶黏剂用于铝塑膜中保护膜与铝箔之间的粘结。
在一较佳实施例中，保护膜可以为但不限于尼龙膜、聚酯膜、聚偏氯乙烯膜、乙烯乙烯醇膜中的一种。
下面通过几个具体的优选实施例来进一步阐述本发明的铝塑膜的制备方法，但并不因此而限定本发明的保护范围。
部分原料如下：
聚酯多元醇，XCP-2000IPS，旭川化学
聚己内酯二元醇，PCL 230N，DIC
扩链剂，NX-9203，卡德莱化工(珠海)有限公司
热塑性树脂，松香TSR-901，广西藤县通轩立信化学有限公司
热塑性树脂，萜烯酚醛树脂803L，日本荒川
催化剂，BCAT-E20，广州优润
抗氧剂，Irganox168，巴斯夫
色素炭黑，MA7，日本三菱
增塑剂，DINCH，伊士曼
二苯基甲烷二异氰酸酯(MDI)，MDI-50，万华化学
甲苯二异氰酸酯(TDI)，TDI-80，陶氏化学
二环己基甲烷二异氰酸酯(HMDI)，万华化学
其中，实施例中所用原料未列出的，均属于市售。
实施例1
一种铝塑膜用热熔复合胶黏剂的制备方法，包括如下步骤：
在3L不锈钢反应釜中，加入1054g聚酯多元醇XCP-2000IPS、527g聚己内酯二元醇PCL 230N、264g萜烯酚醛树脂803L、79g的填料MA7、131g的增塑剂DINCH、0.3g的催化剂BCAT-E20、26g抗氧剂Irganox168，在140℃下真空熔融搅拌干燥1小时，在氮气保护下，加入285g二苯基甲烷二异氰酸酯(MDI)、滴加132g扩链剂腰果酚改性聚醚二醇NX-9203、检测NCO含量为1.0％，获得热熔复合胶黏剂；
在氮气保护下，将反应釜中熔融物料，通过直径22mm双螺杆挤出机挤出，设置机筒温度140-200℃，600目过滤网，模头温度170℃，狭缝间隙为0.02mm，涂布量为15±5g/m2，基材为铝箔，与尼龙膜复合，复合温度100℃，得到尼龙膜/铝箔复合膜。
将尼龙膜/铝箔复合膜与CPP膜复合得到铝塑膜。
实施例2
一种铝塑膜用热熔复合胶黏剂的制备方法，包括如下步骤：
在3L不锈钢反应釜中，加入1318g聚酯多元醇XCP-2000IPS、263g聚己内酯二元醇PCL 230N、264g萜烯酚醛树脂803L、79.1g的填料MA7、131g的增塑剂DINCH、0.3g的催化剂BCAT-E20、26g抗氧剂Irganox168，在140℃下真空熔融搅拌干燥1小时，在氮气保护下，加入185g甲苯二异氰酸酯(TDI)、滴加132g扩链剂腰果酚改性聚醚二醇NX-9203、检测NCO含量为0.4％，获得热熔复合胶黏剂；
其余步骤与实施例1相同，在此不进行阐述。
实施例3
一种铝塑膜用热熔复合胶黏剂的制备方法，包括如下步骤：
在3L不锈钢反应釜中，加入791聚酯多元醇XCP-2000IPS、791g聚己内酯二元醇PCL230N、264g萜烯酚醛树脂803L、79.1g的填料MA7、131g的增塑剂DINCH、0.3g的催化剂BCAT-E20、26g抗氧剂Irganox168，在140℃下真空熔融搅拌干燥1小时，在氮气保护下，加入324g二环己基甲烷二异氰酸酯(HMDI)、滴加132g扩链剂腰果酚改性聚醚二醇PCL 230N、检测NCO含量为1.3％，获得热熔复合胶黏剂；
其余步骤与实施例1相同，在此不进行阐述。
实施例4
该实施例4与实施例1基本相同，不同在于：实施例4中扩链剂为1，4-丁二醇，而实施例1中扩链剂为腰果酚改性聚醚二醇NX-9203。
其余与实施例1相同，在此不再阐述。
实施例5
该实施例5与实施例1基本相同，不同在于：实施例5中热塑性树脂为松香增粘树脂TSR-901，而实施例1中热塑性树脂为萜烯酚醛树脂803L。
其余与实施例1相同，在此不再阐述。
对比例1
该对比例1与实施例1基本相同，不同在于：对比例1中聚酯多元醇为分子量2000的聚己二酸丁二醇型聚酯二元醇PBA2000，而实施例1中聚酯多元醇为XCP-2000IPS(聚间苯二甲酸-癸二酸-新戊二醇-乙二醇型聚酯多元醇)。
其余与实施例1相同，在此不再阐述。
参考例
采用市售干法复合聚氨酯胶粘剂进行铝箔与尼龙膜复合，涂布量5.0g/m2，复合烘道温度：50℃～60℃、60℃～70℃、70℃～80℃；熟化条件70℃*7天。
将尼龙膜/铝箔复合膜与CPP膜复合得到铝塑膜。
将实施例、对比例和参考例的铝塑膜进行剥离强度、单坑冲深深度，测试结果见表3。
其中，剥离强度的测试方法为：GB/T 8808-1988软质复合塑料材料剥离试验方法，测试速度100mm/min，单位N/15m；
单坑冷冲深的测试方法为：冲头形状为60mm*110mm，R角＝1.0mm，间隙0.3mm，深度3.75mm；40个；
湿热老化的测试方法为：温度85度&湿度85％R.H.&7天，查看是否存在白线分层，气泡分层，面分层，褶皱等情况。
表3试验结果
由表3的数据可知，实施例1-5制得的产品均具有较好的初始剥离强度和冲深性能。
实施例1与实施例4相比，实施例4中因扩链剂为1，4-丁二醇，使得冲深破损12.5％，可能的原因是1，4-丁二醇合成的聚氨酯较硬，而腰果酚改性聚醚二醇合成的聚氨酯比较柔软。
实施例1与实施例5相比，实施例5的产品初始剥离强度和冲深性能均良好，但湿热老化后100％线分层，可能的原因是松香增粘树脂的耐湿热较差，
实施例1与对比例1相比，对比例1的产品冲深破损50％，且湿热老化后50％线分层，可能的原因是聚己二酸丁二醇型聚酯多元醇不够柔软且耐高温性不佳。
从实施例1和参考例比较来看，本发明的技术方案几乎可以达到其效果，且初始剥离强度效果更好，尤其是本发明无需溶剂挥发，对环境友好。
以上所揭露的仅为本发明的优选实施例而已，当然不能以此来限定本发明之权利范围，因此依本发明申请专利范围所作的等同变化，仍属本发明所涵盖的范围。

Claims (8)

1.一种铝塑膜用热熔复合胶黏剂的制备方法，其特征在于，包括步骤：
将聚酯多元醇、聚己内酯二元醇、热塑性树脂、填料、增塑剂、功能助剂加入反应容器，在100-140℃下真空熔融干燥0.5-2小时，在氮气保护下，加入二异氰酸酯与催化剂，滴加扩链剂，检测NCO含量为0.5％-5％，得到热熔复合胶黏剂，
其中，所述铝塑膜用热熔复合胶黏剂，按质量百分数计，包括聚酯多元醇20.0-60.0％、聚己内酯二元醇10.0-30.0％、二异氰酸酯5.0-15.0％、热塑性树脂5.0-15.0％、扩链剂0-5.0％、增塑剂0-5.0％、填料0-3.0％、催化剂0.05-1.0％、功能助剂0-8.0％，制备所述聚酯多元醇的二元羧酸为间苯二甲酸和癸二酸，所述热塑性树脂为萜烯树脂。
2.如权利要求1所述的铝塑膜用热熔复合胶黏剂的制备方法，其特征在于，所述聚酯多元醇由间苯二甲酸、癸二酸、新戊二醇和乙二醇制得。
3.如权利要求1所述的铝塑膜用热熔复合胶黏剂的制备方法，其特征在于，所述聚酯多元醇的重均分子量为400-2000。
4.如权利要求1所述的铝塑膜用热熔复合胶黏剂的制备方法，其特征在于，所述聚酯多元醇的羟值为50-200mgKOH/g，所述聚酯多元醇的酸值为0.1-1.0mgKOH/g。
5.如权利要求1所述的铝塑膜用热熔复合胶黏剂的制备方法，其特征在于，所述聚己内酯二元醇的重均分子量为400-2000。
6.如权利要求1所述的铝塑膜用热熔复合胶黏剂的制备方法，其特征在于，所述二异氰酸酯选自MDI、TDI、HDI、HMDI中的至少一种。
7.如权利要求1所述的铝塑膜用热熔复合胶黏剂的制备方法，其特征在于，所述扩链剂选自1，4一丁二醇、1，6一己二醇、甘油、三羟甲基丙烷、二甘醇、三甘醇、新戊二醇、山梨醇、二乙氨基乙醇、腰果酚改性聚醚二醇中的至少一种。
8.一种如权利要求1-7任一项所述的铝塑膜用热熔复合胶黏剂的制备方法制得的热熔复合胶黏剂用于铝塑膜中保护膜与铝箔之间的粘结。
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