CN112646532A - 一种耐蒸煮的水性聚氨酯胶粘剂的制备方法 - Google Patents

一种耐蒸煮的水性聚氨酯胶粘剂的制备方法 Download PDF

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CN112646532A
CN112646532A CN202011559479.4A CN202011559479A CN112646532A CN 112646532 A CN112646532 A CN 112646532A CN 202011559479 A CN202011559479 A CN 202011559479A CN 112646532 A CN112646532 A CN 112646532A
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parts
preparation
polyol
chain extender
diol
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CN112646532B (zh
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周忠武
张军
伏阳
张红军
郭培荣
杨凡凡
梁裕波
何建忠
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Jiangsu Zhongjin Matai Medicinal Packaging Co Ltd
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Abstract

本发明公开了水性聚氨酯胶粘剂技术领域的一种耐蒸煮的水性聚氨酯胶粘剂的制备方法，制备方法包括以下步骤：（1）复合多元醇60‑80份，二异氰酸酯10‑20份，前扩链剂3‑5份，后扩链剂6‑8份，交联剂7‑9份，三乙胺3‑5份，二甲基乙醇胺1‑2份，去离子水130‑150份，增稠剂6‑8份；（2）将复合多元醇、二异氰酸酯、前扩链剂加入到反应器中，并加入二甲基乙醇胺，在氮气保护下升温至75‑85℃，保温4‑5h；（3）向反应器中加三乙胺，搅拌后得到聚合物；（4）将去离子水、后扩链剂和交联剂放入反应器中与聚合物混合，高速搅拌后加入增稠剂继续搅拌，即得目标产物；本发明通过对原料进行合理的选择和配比，并优化制备方法，得到的水性聚氨酯胶粘剂性能较为优良。

Description

一种耐蒸煮的水性聚氨酯胶粘剂的制备方法
技术领域
本发明涉及水性聚氨酯胶粘剂技术领域，具体为一种耐蒸煮的水性聚氨酯胶粘剂的制备方法。
背景技术
随着人们的安全和环保意识的加强，水性聚氨酯胶黏剂的研究得以迅速发展。水性聚氨酯胶黏剂是指将聚氨酯溶于水或分散于水中而形成的胶粘剂，与溶剂型相比具有无溶剂、无污染、成膜性好、粘接力强、和其他聚合物尤其是乳液型聚合物易掺混有利于改性等优点。90年代后已逐渐在汽车内饰物粘接、厨房用品制造、复合薄膜制造、鞋底鞋帮粘接、服装加工等方面得到应用。但是还存在许多缺点，需要通过各种改性，完善其功能。
中国于20世纪70年代初就开始了对水性聚氨酯的研究。PU在中国最早用于制备电泳漆，随后人们研制出了织物整理用水溶性PU以及用作皮革涂饰剂的PU乳液。进入20世纪80年代后，中国对PU胶粘剂的研究速度加快，但与国外系列化、工业化的水平相比，仍处于起步阶段，存在原料和制备方法单一、品种少、理论研究不足和应用研究不够深入等问题，现有技术中的水性聚氨酯胶粘剂的耐高温性能较为一般，导致其应用受到限制。
因此提出一种耐蒸煮的水性聚氨酯胶粘剂的制备方法以解决上述问题。
发明内容
本发明的目的在于提供一种耐蒸煮的水性聚氨酯胶粘剂的制备方法，以解决上述背景技术中提出问题。
为实现上述目的，本发明提供如下方案予以实现：
本发明提供了一种耐蒸煮的水性聚氨酯胶粘剂的制备方法，具体包括以下步骤：
（1）称取以下重量份原料：复合多元醇60-80份，二异氰酸酯10-20份，前扩链剂3-5份，后扩链剂6-8份，交联剂7-9份，乙二胺3-5份，二甲基乙醇胺1-2份，三乙胺3-5份，去离子水130-150份，增稠剂6-8份；
（2）将复合多元醇、二异氰酸酯、前扩链剂加入到反应器中，并加入二甲基乙醇胺，在氮气保护下升温至75-85℃，保温4-5h；
（3）向反应器中加三乙胺，以1000-1500r/min的转速搅拌15-20min，得到聚合物；
（4）将去离子水、后扩链剂和交联剂放入反应器中与聚合物混合，高速搅拌后加入增稠剂继续搅拌，即得目标产物。
优选的，复合多元醇包括杂化多元醇A、杂化多元醇B、聚己二酸1，4丁二醇酯二醇和聚己二酸新戊二醇酯二醇、聚己二酸乙二醇酯二醇、聚己二酸一缩二乙二醇酯二醇 、聚碳酸酯二醇 、聚己内酯二醇 、聚丁二烯二醇 、丙烯酸酯多元醇 、聚氧化丙烯二醇 、聚氧化丙烯三醇、聚四氢呋喃二醇或四氢呋喃－氧化丙烯共聚二醇中的三种或四种，且由杂化多元醇A、杂化多元醇B以及上述其它2种多元醇按质量比1:1:1:1混合。
优选的，所述杂化多元醇A的制备方法如下：将苯酐、对苯二甲酸、1,4环已烷二甲醇和环已烷二甲酸按质量比1:1:3.2:1放入反应器中，在温度140-220℃下反应8-10h，抽真空后得到杂化多元醇A。
优选的，所述杂化多元醇B的制备方法如下：将新戊二醇、乙二醇、癸二酸和间苯二甲酸二甲酸按质量比2:1:1:1放入反应器中，在温度140-220℃下反应8-10h，抽真空后得到杂化多元醇B。
优选的，所述前扩链剂为二羟甲基丙酸、二羟甲基丁酸、1,4丁二醇、新戊二醇、乙二醇中的一种或多种混合。
优选的，所述后扩链剂为乙二胺、二亚乙烯三胺、三亚乙烯四胺、四亚乙烯五胺中一种或多种混合。
优选的，所述交联剂为三羟甲基丙烷、甘油中的一种或来两种混合。
优选的，所述增稠剂为增稠剂EXP300。
本发明的有益效果是：
本发明通过加入复合多元醇，复合多元醇包括杂化多元醇A、杂化多元醇B、聚己二酸1，4丁二醇酯二醇和聚己二酸新戊二醇酯二醇、聚己二酸乙二醇酯二醇、聚己二酸一缩二乙二醇酯二醇 、聚碳酸酯二醇 、聚己内酯二醇 、聚丁二烯二醇 、丙烯酸酯多元醇 、聚氧化丙烯二醇 、聚氧化丙烯三醇、聚四氢呋喃二醇或四氢呋喃－氧化丙烯共聚二醇中的三种或四种，且由杂化多元醇A、杂化多元醇B以及上述其它2种多元醇按质量比1:1:1:1混合，其中杂化多元醇A由苯酐、对苯二甲酸、1,4环已烷二甲醇和1,4环已烷二甲酸共混，杂化多元醇B由新戊二醇、乙二醇、癸二酸和间苯二甲酸共混，利用多种醇的酯化缩聚，得到的复合多元醇和二异氰酸酯聚合生成的水性聚氨酯胶粘剂。复合多元醇之间的化学键产生协同作用，制得的高分子聚合物产生化学键的交联，提高了胶粘剂的耐热性，热稳定性分析表明其耐高温蒸煮性能较好 。
本发明通过对原料进行合理的选择和配比，并优化制备方法，得到的水性聚氨酯胶粘剂性能较为优良。
具体实施方式
下面将结合本发明实施例，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例，都属于本发明保护的范围。
实施例1
一种耐蒸煮的水性聚氨酯胶粘剂的制备方法，具体包括以下步骤：
（1）称取以下重量份原料：复合多元醇60份，二异氰酸酯10份，前扩链剂3份，后扩链剂6份，交联剂7份，三乙胺3份，二甲基乙醇胺1份，去离子水130份，增稠剂6份；
（2）将复合多元醇、二异氰酸酯、前扩链剂加入到反应器中，并加入二甲基乙醇胺，在氮气保护下升温至75℃，保温4h；
（3）向反应器中加三乙胺，以1000r/min的转速搅拌15min，得到聚合物；
（4）将去离子水、后扩链剂和交联剂放入反应器中与聚合物混合，高速搅拌后加入增稠剂继续搅拌，即得目标产物。
复合多元醇包括杂化多元醇A、杂化多元醇B、聚碳酸酯二醇 、聚己内酯二醇 ，且杂化多元醇A、杂化多元醇B、聚碳酸酯二醇 、聚己内酯二醇 按摩尔比1:1:1:1混合；
杂化多元醇A的制备方法如下：将苯酐、对苯二甲酸、1,4环已烷二甲醇和1,4环已烷二甲酸按摩尔比1:1:3.2:1放入反应器中，在温度140℃下反应2h，抽真空后得到杂化多元醇A；杂化多元醇B的制备方法如下：将新戊二醇、乙二醇、癸二酸和间苯二甲酸按摩尔比2:1:1:1放入反应器中，在温度140℃下反应2h，抽真空后得到杂化多元醇B。
前扩链剂为二羟甲基丙酸；后扩链剂为乙二胺；交联剂为三羟甲基丙烷；增稠剂为增稠剂EXP300。
实施例2
一种耐蒸煮的水性聚氨酯胶粘剂的制备方法，具体包括以下步骤：
（1）称取以下重量份原料：复合多元醇65份，二异氰酸酯15份，前扩链剂3.5份，后扩链剂6.5份，交联剂7.5份，三乙胺3.5份，二甲基乙醇胺1份，去离子水130份，增稠剂6.5份；
（2）将复合多元醇、二异氰酸酯、前扩链剂加入到反应器中，并加入二甲基乙醇胺，在氮气保护下升温至82℃，保温4.5h；
（3）向反应器中加三乙胺，以1200r/min的转速搅拌15min，得到聚合物；
（4）将去离子水、后扩链剂和交联剂放入反应器中与聚合物混合，高速搅拌后加入增稠剂继续搅拌，即得目标产物。
复合多元醇包括杂化多元醇A、杂化多元醇B、聚四氢呋喃二醇和聚已二酸新戊二醇酯二醇，且杂化多元醇A、杂化多元醇B、聚四氢呋喃二醇和聚已二酸新戊二醇酯二醇按摩尔比1:1:1:1混合；
杂化多元醇A的制备方法如下：将苯酐、对苯二甲酸、1,4环已烷二甲醇和1,4环已烷二甲酸按摩尔比1:1:1:1放入反应器中，在温度180℃下反应1.5h，抽真空后得到杂化多元醇A；杂化多元醇B的制备方法如下：将已二酸、乙二醇、癸二酸和间苯二甲酸按摩尔比2:1:1:1放入反应器中，在温度180℃下反应1.5h，抽真空后得到杂化多元醇B。
前扩链剂为二羟甲基丁酸；后扩链剂为乙二胺；交联剂为三羟甲基丙烷；增稠剂为增稠剂EXP300。
实施例3
一种耐蒸煮的水性聚氨酯胶粘剂的制备方法，具体包括以下步骤：
（1）称取以下重量份原料：复合多元醇70份，二异氰酸酯18份，前扩链剂4份，后扩链剂7份，交联剂8份，三乙胺3.5份，二甲基乙醇胺1.5份，去离子水140份，增稠剂6.5份；
（2）将复合多元醇、二异氰酸酯、前扩链剂加入到反应器中，并加入二甲基乙醇胺，在氮气保护下升温至80℃，保温4.5h；
（3）向反应器中加三乙胺，以1200r/min的转速搅拌18min，得到聚合物；
（4）将去离子水、后扩链剂和交联剂放入反应器中与聚合物混合，高速搅拌后加入增稠剂继续搅拌，即得目标产物。
复合多元醇包括杂化多元醇A、杂化多元醇B、聚已二酸1，4丁二醇酯二醇和聚己二酸乙二醇酯二醇，且杂化多元醇A、杂化多元醇B、聚已二酸1，4丁二醇酯二醇和聚己二酸乙二醇酯二醇按摩尔比1:1:1:1混合；
杂化多元醇A的制备方法如下：将苯酐、对苯二甲酸、1,4环已烷二甲醇和1,4环已烷二甲酸按摩尔比1:1:3.3:1放入反应器中，在温度200℃下反应1.8h，抽真空后得到杂化多元醇A；杂化多元醇B的制备方法如下：将新戊二醇、乙二醇、癸二酸和间苯二甲酸二甲酸按摩尔比2:1:1:1放入反应器中，在温度200℃下反应1.8h，抽真空后得到杂化多元醇B。
前扩链剂为二羟甲基丁酸；后扩链剂为二亚乙烯三胺；交联剂为甘油；增稠剂为增稠剂EXP300。
实施例4
一种耐蒸煮的水性聚氨酯胶粘剂的制备方法，具体包括以下步骤：
（1）称取以下重量份原料：复合多元醇75份，二异氰酸酯20份，前扩链剂4.5份，后扩链剂7份，交联剂9份，三乙胺4份，二甲基乙醇胺1.5份，去离子水145份，增稠剂7份；
（2）将复合多元醇、二异氰酸酯、前扩链剂加入到反应器中，并加入二甲基乙醇胺，在氮气保护下升温至80℃，保温5h；
（3）向反应器中加三乙胺，以1500r/min的转速搅拌18min，得到聚合物；
（4）将去离子水、后扩链剂和交联剂放入反应器中与聚合物混合，高速搅拌后加入增稠剂继续搅拌，即得目标产物。
复合多元醇包括杂化多元醇A、杂化多元醇B、聚已二酸1，4丁二醇酯二醇和聚己二酸一缩二乙二醇酯二醇，且杂化多元醇A、杂化多元醇B、聚已二酸1，4丁二醇酯二醇和聚己二酸一缩二乙二醇酯二醇按摩尔比1:1:1:1混合；
杂化多元醇A的制备方法如下：将苯酐、对苯二甲酸、1,4环已烷二甲醇和1,4环已烷二甲酸按摩尔比1:1:3.2:1放入反应器中，在温度200℃下反应1.8h，抽真空后得到杂化多元醇A；杂化多元醇B的制备方法如下：将新戊二醇、乙二醇、癸二酸和间苯二甲酸二甲酸按摩尔比2:1:1:1放入反应器中，在温度200℃下反应1.8h，抽真空后得到杂化多元醇B。
前扩链剂为二羟甲基丁酸；后扩链剂为三亚乙烯四胺和四亚乙烯五胺，按质量1:1混合；交联剂为甘油；增稠剂为增稠剂EXP300。
实施例5
一种耐蒸煮的水性聚氨酯胶粘剂的制备方法，具体包括以下步骤：
（1）称取以下重量份原料：复合多元醇80，二异氰酸酯20份，前扩链剂5份，后扩链剂8份，交联剂9份，三乙胺5份，二甲基乙醇胺2份，去离子水140份，增稠剂8份；
（2）将复合多元醇、二异氰酸酯、前扩链剂加入到反应器中，并加入二甲基乙醇胺，在氮气保护下升温至85℃，保温5h；
（3）向反应器中加三乙胺，以1500r/min的转速搅拌20min，得到聚合物；
（4）将去离子水、后扩链剂和交联剂放入反应器中与聚合物混合，高速搅拌后加入增稠剂继续搅拌，即得目标产物。
复合多元醇包括杂化多元醇A、杂化多元醇B、聚碳酸酯二醇 和聚已二酸新戊二醇酯二醇，且杂化多元醇A、杂化多元醇B、聚碳酸酯二醇和聚已二酸新戊二醇酯二醇按摩尔比1:1:1:1混合；
杂化多元醇A的制备方法如下：将苯酐、对苯二甲酸、1,4环已烷二甲醇和1,4环已烷二甲酸按摩尔比1:1:3.1:1放入反应器中，在温度220℃下反应2h，抽真空后得到杂化多元醇A；杂化多元醇B的制备方法如下：将新戊二醇、乙二醇、癸二酸和间苯二甲酸二甲酸按摩尔比2:1:1:1放入反应器中，在温度220℃下反应2h，抽真空后得到杂化多元醇B。
前扩链剂为二羟甲基丁酸；后扩链剂为三亚乙烯四胺和四亚乙烯五胺，按质量2:1混合；交联剂为甘油；增稠剂为增稠剂EXP300。
结果检测
1、试验方法：采用美国TA Instruments公司的TGA 2050型热重分析仪进行水性聚氨酯乳胶膜的热重分析(TG)测试。取各实施例中10mg左右的样品在氮气氛围下进行测试，升温速率为10℃/min，温度区间为30℃-600℃；根据GB 19340-2014《鞋和箱包用胶粘剂》及HG/T 2815-1996《鞋用胶粘剂耐热性试验方法蠕变法》，在实验温度为100℃、砝码重量为1.5kg的情况下，测定通过实施例中的产品粘结在一起的两个PET塑料试片完全剥离经历的时间。具体检测结果如表1所示。
表1 性能检测
Figure DEST_PATH_IMAGE002
在本说明书的描述中，参考术语“一个实施例”、“示例”、“具体示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中，对上述术语的示意性表述不一定指的是相同的实施例或示例。而且，描述的具体特征、结构、材料或者特点可以在任何的一个或多个实施例或示例中以合适的方式结合。
以上公开的本发明优选实施例只是用于帮助阐述本发明。优选实施例并没有详尽叙述所有的细节，也不限制该一种高强度制动钳密封件的制备方法仅为所述的具体实施方式。显然，根据本说明书的内容，可作很多的修改和变化。本说明书选取并具体描述这些实施例，是为了更好地解释本发明的原理和实际应用，从而使所属技术领域技术人员能很好地理解和利用本发明。本发明仅受权利要求书及其全部范围和等效物的限制。

Claims (8)

1.一种耐蒸煮的水性聚氨酯胶粘剂的制备方法，其特征在于，制备方法包括以下步骤：
（1）称取以下重量份原料：复合多元醇60-80份，二异氰酸酯10-20份，前扩链剂1-1.5份，后扩链剂6-8份，交联剂7-9份，三乙胺3-5份，二甲基乙醇胺1-2份，去离子水130-150份，增稠剂6-8份；
（2）将复合多元醇、二异氰酸酯、前扩链剂加入到反应器中，并加入二甲基乙醇胺，在氮气保护下升温至75-85℃，保温4-5h；
（3）向反应器中加三乙胺，以1000-1500r/min的转速搅拌15-20min，得到聚合物；
（4）将去离子水、后扩链剂和交联剂放入反应器中与聚合物混合，高速搅拌后加入增稠剂继续搅拌，即得目标产物。
2.根据权利要求1所述的一种耐蒸煮的水性聚氨酯胶粘剂的制备方法，其特征在于，所述复合多元醇包括杂化多元醇A、杂化多元醇B、聚己二酸1，4丁二醇酯二醇和聚己二酸新戊二醇酯二醇、聚己二酸乙二醇酯二醇、聚己二酸一缩二乙二醇酯二醇 、聚碳酸酯二醇 、聚己内酯二醇 、聚丁二烯二醇 、丙烯酸酯多元醇 、聚氧化丙烯二醇 、聚氧化丙烯三醇、聚四氢呋喃二醇或四氢呋喃－氧化丙烯共聚二醇中的三种或四种，且由杂化多元醇A、杂化多元醇B以及上述其它2种多元醇按质量比1:1:1:1混合。
3.根据权利要求2所述的一种耐蒸煮的水性聚氨酯胶粘剂的制备方法，其特征在于，所述杂化多元醇A的制备方法如下：将苯酐、对苯二甲酸、1,4环已烷二甲醇和环已烷二甲酸按质量比1:1:3.2:1放入反应器中，在温度140-220℃下反应8-10h，抽真空后得到杂化多元醇A。
4.根据权利要求2所述的一种耐蒸煮的水性聚氨酯胶粘剂的制备方法，其特征在于，所述杂化多元醇B的制备方法如下：将新戊二醇、乙二醇、癸二酸和间苯二甲酸放入反应器中，在温度140-220℃下反应8-10h，抽真空后得到杂化多元醇B，分子量1500－4000。
5.根据权利要求1所述的一种耐蒸煮的水性聚氨酯胶粘剂的制备方法，其特征在于，所述前扩链剂为二羟甲基丙酸、二羟甲基丁酸、1,4丁二醇、新戊二醇、乙二醇中的一种或多种混合。
6.根据权利要求1所述的一种耐蒸煮的水性聚氨酯胶粘剂的制备方法，其特征在于，所述后扩链剂为乙二胺、二亚乙烯三胺、三亚乙烯四胺、四亚乙烯五胺中一种或多种混合。
7.根据权利要求1所述的一种耐蒸煮的水性聚氨酯胶粘剂的制备方法，其特征在于，所述交联剂为三羟甲基丙烷、甘油中的一种或两种混合。
8.根据权利要求1所述的一种耐蒸煮的水性聚氨酯胶粘剂的制备方法，其特征在于，所述增稠剂为增稠剂EXP300。
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