CN108517194A - 一种高阻隔铝塑材料专用双组分无溶剂型聚氨酯胶粘剂及其制备方法 - Google Patents

一种高阻隔铝塑材料专用双组分无溶剂型聚氨酯胶粘剂及其制备方法 Download PDF

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CN108517194A
CN108517194A CN201810233622.7A CN201810233622A CN108517194A CN 108517194 A CN108517194 A CN 108517194A CN 201810233622 A CN201810233622 A CN 201810233622A CN 108517194 A CN108517194 A CN 108517194A
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顾嘉卫
周锦君
钟树良
蔡炳照
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JIANGSU LIHE ADHESIVE CO Ltd
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Abstract

本发明公开了一种高阻隔铝塑材料专用双组分无溶剂型聚氨酯胶粘剂，由A胶和B胶配制而成，其中，A胶以聚醚多元醇、TDI、IPDI和六亚甲基二异氰酸酯三聚体为原料；B胶以二聚酸、多元醇、1,3‑丁二醇、葵二酸、间苯二甲酸为原料，以钛酸四丁酯为催化剂得特定酸价和羟值的聚酯多元醇；再用聚酯多元醇与聚醚多元醇和端羟基聚丁二烯混合制得B胶；A胶和B胶以10:7混合得到无溶剂聚氨酯胶粘剂。这种胶水对于高阻隔铝塑材料具有良好的粘合牢度，制备工艺的参数易于控制，制备过程无排放，属于环境友好型生产方案。

Description

一种高阻隔铝塑材料专用双组分无溶剂型聚氨酯胶粘剂及其 制备方法
技术领域
本发明涉及一种高阻隔铝塑材料专用双组分无溶剂型聚氨酯胶粘剂及其制备方法，属于聚氨酯胶黏剂材料研究领域。
背景技术
相比于传统的溶剂型聚氨酯胶黏剂，无溶剂聚氨酯胶粘剂存在无溶剂挥发、操作简便、原料利用率高软硬段可调等优势，这使得其更具有研究和开发价值。然而普通的无溶剂聚氨酯胶粘剂对于高阻隔铝塑材料不具备良好的复合牢度，主要体现在复合强度不高，且伴随着胶水固化后，复合膜内存在大量的气泡，这将严重影响胶水的使用性能，为了克服现有产品存在的不足，满足市场的要求，申请人开发了一种高阻隔铝塑材料专用双组分无溶剂型聚氨酯胶粘剂。
发明内容
本发明的目的是提供一种高阻隔铝塑材料专用双组分无溶剂型聚氨酯胶粘剂及其制备方法。
本发明采取的技术方案如下：
一种高阻隔铝塑材料专用双组分无溶剂型聚氨酯胶粘剂，由A胶和B胶配制而成，具体制备步骤如下：
第一步，A胶的制备：
分别取345～355g分子量为1000～2000的聚醚多元醇、148～152g TDI、148～152gIPDI和99～101g六亚甲基二异氰酸酯三聚体于四口烧瓶中，升温至80～90℃的条件下反应6h，然后升温至100～120℃并在真空度为-0.1MPa的条件下，脱水2小时，检测体系含水量少于0.05％为合格，降温至40℃，即得A胶；
第二步，B胶的制备：
分别取69～71g二聚酸、99～101g多元醇、138～142g 1,3-丁二醇、189～191g葵二酸、139～141g间苯二甲酸于1000mL四口烧瓶中，滴加0.1～0.25g钛酸四丁酯催化剂之后，搅拌并缓慢升温至160℃，此时反应出水，然后缓慢升温至240℃并保温两小时，此时取样测酸价，若酸价低于15mg KOH/g,则酯化反应结束，然后在温度为220～230℃以及压力为-0.1Mpa的条件下下抽真空5小时，得到酸价≤1mg KOH/g以及羟值为250±5mg KOH/g的聚酯多元醇；取100g上述得到的聚酯多元醇与197～203g分子量为400～700的聚醚多元醇(羟基的官能度为4.5)、以及44～46g分子量为2800～3500的端羟基聚丁二烯混合，在120℃条件下真空脱水至体系含水量少于0.05％，降温至40℃，即为B胶。
第三步，高阻隔铝塑材料专用双组分无溶剂型聚氨酯胶粘剂的配制：
A胶和B胶以10:7混合得到无溶剂聚氨酯胶粘剂。
进一步，在A胶的制备过程中，聚醚多元醇的质量为70g，TDI的质量为150g，IPDI的质量为150g，六亚甲基二异氰酸酯三聚体的质量为100g。
进一步，在B胶的制备过程中，二聚酸的质量为120g，多元醇的质量为100g，1,3-丁二醇的质量为140g，葵二酸的质量为190g，间苯二甲酸的质量为140g；聚酯多元醇的质量为100g，聚醚多元醇的质量为300g，端羟基聚丁二烯的质量为45g。
这种高阻隔铝塑材料专用双组分无溶剂型聚氨酯胶粘剂的优点：
该款胶水对于高阻隔铝塑材料具有良好的粘合牢度。
这种制备方法的优点：
制备工艺的参数易于控制，制备过程无排放，属于环境友好型生产方案。
具体实施方式
现在结合具体实施例对本发明做进一步说明，以下实施例旨在说明本发明而不是对本发明的进一步限定。
实施例1：
高阻隔铝塑材料专用双组分无溶剂型聚氨酯胶粘剂，由A胶和B胶组成，具体制备步骤如下：
第一步，A胶的制备：
分别取350g分子量为1000～2000的聚醚多元醇、150g TDI、150g IPDI和100g六亚甲基二异氰酸酯三聚体于四口烧瓶中，升温至80～90℃的条件下反应6h，然后升温至100～120℃并在真空度为-0.1MPa的条件下，脱水2小时，检测体系含水量少于0.05％为合格，降温至40℃，即得A胶。
第二步，B胶的制备：
分别取70g二聚酸、100g多元醇、140g 1,3-丁二醇、190g葵二酸、140g间苯二甲酸于1000mL四口烧瓶中，滴加0.1～0.25g钛酸四丁酯催化剂之后，搅拌并缓慢升温至160℃，此时反应出水，然后缓慢升温至240℃并保温两小时，此时取样测酸价，若酸价低于15mgKOH/g,则酯化反应结束，然后在温度为220～230℃以及压力为-0.1Mpa的条件下下抽真空5小时，得到酸价≤1mg KOH/g以及羟值为250±5mg KOH/g的聚酯多元醇；取100g上述得到的聚酯多元醇与300g分子量为400～700的聚醚多元醇(羟基的官能度为4.5)以及45g分子量为2800～3500的端羟基聚丁二烯混合，在120℃条件下真空脱水至体系含水量少于0.05％，降温至40℃，即为B胶。
第三步，无溶剂型双组分聚氨酯胶粘剂的制备：A胶和B胶以10:7混合得到无溶剂聚氨酯胶粘剂。
为了考查TDI的量对复合材料剥离强度的影响，因此，分别调节TDI和IPDI的质量比为0.6:1、0.8:1.、1.0:1、1.2:1、1.4:1。将制得的无溶剂聚氨酯胶粘剂加入到无溶剂覆膜机的上胶系统中，上胶量为2.0g/m2，以PET和铝膜为基材，制备得到铝塑复合材料，进一步熟化之后，根据GB/T2791-1995的步骤测试其剥离强度，结果表1所示，随着TDI的比例升高，剥离强度先增加，后减小，并在摩尔比为1.0:1时，剥离强度达到最高。剥离强度上升是因为：TDI的比例提高会提升胶水的硬度，从而剥离强度升高；而剥离强度下降是因为：TDI的比例过高而使得聚氨酯粘度快速提升，从而降低了A胶和B胶之间的兼容性，从而出现部分胶膜不干，这一现象导致熟化后强度降低。
表1
实施例2：
溶剂型双组分聚氨酯胶粘剂的制备过程与实施例1相同。
为了考查多元醇的量对复合材料耐水煮性能的影响，因此，分别调节多元醇和1,3-丁二醇的质量比为1:1.8、1:1.6、1:1.4、1:1.2、1:1.0。将制得的无溶剂聚氨酯胶粘剂加入到无溶剂覆膜机的上胶系统中，上胶量为2.0g/m2，以PET和PA为基材，制备得到铝塑复合材料，进一步熟化之后，根据GB/T2791-1995的步骤测试其剥离强度，结果表1所示，随着多元醇的比例升高，剥离强度先增加，后减小，并在摩尔比为1:1.4时，剥离强度达到最高。剥离强度上升是因为：多元醇的比例提升会提高胶水的内交联度，从而剥离强度升高；而剥离强度下降是因为：多元醇的比例过高而使得聚氨酯粘度快速提升，从而降低了A胶和B胶之间的兼容性，从而出现部分胶膜不干，这一现象导致熟化后强度降低。
表2
实施例3：
溶剂型双组分聚氨酯胶粘剂的制备过程与实施例1相同。
将制得的无溶剂聚氨酯胶粘剂加入到无溶剂覆膜机的上胶系统中，上胶量为2.0g/m2，以PET和PA为基材，分别制备得到PET/PA、PET/PET和PA/PA复合材料，进一步熟化之后，根据GB/T2791-1995的步骤测试其剥离强度，结果表3所示，发现该款胶水对于三种铝塑复合均具备良好的粘合牢度。
表3
PET/PA PET/PET PA/PA
剥离强度(N.15mm) 4.1 4.4 3.9
本发明制备得到的溶剂型双组分聚氨酯胶粘剂，该款胶水对于高阻隔铝塑材料具有良好的粘合牢度，且制备工艺的参数易于控制，制备过程无排放，属于环境友好型生产方案。

Claims (3)

1.一种高阻隔铝塑材料专用双组分无溶剂型聚氨酯胶粘剂，其特征是：由A胶和B胶配制而成，具体制备步骤如下：
第一步，A胶的制备：
分别取345～355g分子量为1000～2000的聚醚多元醇、148～152g TDI、148～152gIPDI和99～101g六亚甲基二异氰酸酯三聚体于四口烧瓶中，升温至80～90℃的条件下反应6h，然后升温至100～120℃并在真空度为-0.1MPa的条件下，脱水2小时，检测体系含水量少于0.05％为合格，降温至40℃，即得A胶；
第二步，B胶的制备：
分别取69～71g二聚酸、99～101g多元醇、138～142g 1,3-丁二醇、189～191g葵二酸、139～141g间苯二甲酸于1000mL四口烧瓶中，滴加0.1～0.25g钛酸四丁酯催化剂之后，搅拌并缓慢升温至160℃，此时反应出水，然后缓慢升温至240℃并保温两小时，此时取样测酸价，若酸价低于15mg KOH/g,则酯化反应结束，然后在温度为220～230℃以及压力为-0.1Mpa的条件下下抽真空5小时，得到酸价≤1mg KOH/g以及羟值为250±5mg KOH/g的聚酯多元醇；取100g上述得到的聚酯多元醇与197～203g分子量为400～700的聚醚多元醇(羟基的官能度为4.5)、以及44～46g分子量为2800～3500的端羟基聚丁二烯混合，在120℃条件下真空脱水至体系含水量少于0.05％，降温至40℃，即为B胶。
第三步，高阻隔铝塑材料专用双组分无溶剂型聚氨酯胶粘剂的配制：
A胶和B胶以10:7混合得到无溶剂聚氨酯胶粘剂。
2.根据权利要求1所述高阻隔铝塑材料专用双组分无溶剂型聚氨酯胶粘剂，其特征是：在A胶的制备过程中，聚醚多元醇的质量为70g，TDI的质量为150g，IPDI的质量为150g，六亚甲基二异氰酸酯三聚体的质量为100g。
3.根据权利要求1所述高阻隔铝塑材料专用双组分无溶剂型聚氨酯胶粘剂，其特征是：在B胶的制备过程中，二聚酸的质量为120g，多元醇的质量为100g，1,3-丁二醇的质量为140g，葵二酸的质量为190g，间苯二甲酸的质量为140g；聚酯多元醇的质量为100g，聚醚多元醇的质量为300g，端羟基聚丁二烯的质量为45g。
CN201810233622.7A 2018-03-21 2018-03-21 一种高阻隔铝塑材料专用双组分无溶剂型聚氨酯胶粘剂及其制备方法 Pending CN108517194A (zh)

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