CN110105912B - 汽车内饰用水性聚氨酯胶粘剂及其制备方法 - Google Patents

汽车内饰用水性聚氨酯胶粘剂及其制备方法 Download PDF

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CN110105912B
CN110105912B CN201910389147.7A CN201910389147A CN110105912B CN 110105912 B CN110105912 B CN 110105912B CN 201910389147 A CN201910389147 A CN 201910389147A CN 110105912 B CN110105912 B CN 110105912B
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polyurethane adhesive
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尹成勇
周其平
姚郑生
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Wuxi Wanli Adhesion Materials Co ltd
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Abstract

本发明涉及一种汽车内饰用水性聚氨酯胶粘剂及其制备方法，属于粘合剂技术领域。其将聚酯多元醇、聚醚多元醇、松香树脂抽真空脱水后加入抗氧剂、二异氰酸酯、交联剂、和亲水性扩链剂并加入催化剂有机锡反应得到预聚体，然后加入丙酮降粘和中和剂调节pH值，最后在高速剪切搅拌下分散到去离子水中化再滴加扩链剂扩链，减压蒸出丙酮即可得到本产品。本发明操作简单易实施，得到的产品有机溶剂含量低，味道小，稳定性好，初粘力好。

Description

汽车内饰用水性聚氨酯胶粘剂及其制备方法
技术领域
本发明涉及一种汽车内饰用水性聚氨酯胶粘剂及其制备方法，属于粘合剂 技术领域。
背景技术
汽车内部装饰大多数使用人造革、聚氨酯泡沫塑料、塑料壁纸、乳胶海绵、 人造地毯、布、丝绒和木材等材料，增加车内美观。例如顶蓬、地毯、门板、 仪表盘等。目前在国内汽车内饰大多还是使用易燃、有毒、污染环境的溶剂型 胶粘剂，如氯丁胶胶粘剂。溶剂型胶粘剂不仅造成资源严重浪费，严重污染环 境，而且对施工人员的健康造成很大威胁。使用溶剂型胶粘剂装饰的汽车，在 很长一段时间内溶剂不断地缓慢释放出来，使司乘人员受到伤害，汽车质量也 受到影响。而水基胶粘剂由于以水为溶剂，不含有毒溶剂，甚至可以做到VOC 几乎为0。因此近年来在汽车工业上，水基胶粘剂正在取代传统的溶剂型粘合剂， 开始用于汽车内饰，并且增长速度很快。目前世界上汽车顶棚内衬水性胶粘剂 的比例已超过1/3。以日本汽车为例，目前汽车内饰胶几乎全部实现水性化。今 后水基聚氨酯胶粘剂的年增长估计保持在8％-10％。
在我国，随着经济的持续高速发展，汽车进入家庭步伐的加快，汽车车内 环境污染问题也越来越引起人们的关注。而这些污染的主要来源于胶粘剂，尤 其是，车内空间较室内更为狭小，其危害将更大。目前，车内空气污染问题已 引起社会各界与政府有关部门的广泛重视，国家有关法规对车内污染物及VOC 含量做了严格的规定。可以预料，这些标准的制定与实施，将促进我国水性胶 粘剂等环保型产品在汽车上的使用。
在水基胶粘剂中，水性聚氨酯胶粘剂与其它水系材料相比，具有强度高、 弹性好、耐低温和抗磨性能优良，胶膜物性可调节范围大等特点。而且在特定 条件下，水性聚氨酯大分子上所含的羧基、羟基等基团也可参与固化反应，使 大分子交联，从而获得优良的粘接效果。由于在结构中具有较多的极性基团,如 氨酯键、脲键、离子键以及羧基、羟基等基团，因此对许多合成材料特别是极 性材料、多孔性材料如汽车内饰件用PVC人造革、聚氨酯软泡沫、纤维布复合 材料、塑料壁纸、乳胶海绵、布、丝绒和木材、ABS、聚丙烯纤维板、织物、乙烯基塑料等具有良好的粘接性能，因而在汽车的仪表板、车门与顶棚内衬、 座椅以及杂物箱内饰件等部位上得到应用，具有诱人的发展前景。
发明内容
本发明的目的是克服上述不足之处，提供一种汽车内饰用水性聚氨酯胶粘 剂及其制备方法，其活化温度低、初粘力好、低气味、无污染。
本发明的技术方案，汽车内饰用水性聚氨酯胶粘剂，配方比例按重量份计 如下：聚酯多元醇10-15份和聚醚多元醇6-8份、松香树脂4-8份、异氰酸酯 8-13份、亲水性扩链剂0.2-0.6份、内交联剂0-0.3份、扩链剂0.1-0.3份、中和 剂0.14-0.36份、催化剂0.001-0.1份、抗氧剂0.001-0.01份、有机溶剂1-5份和 去离子水40-70份。
进一步的，所述聚酯多元醇为平均分子量在500-5000之间的聚己二酸丁二 醇酯二醇、聚己二酸乙二醇酯二醇、聚己内酯二醇、聚碳酸1，6-己二醇酯二醇 及蓖麻油中的一种或几种物质的混合物。
进一步的，所述聚醚多元醇为平均分子量在500-5000之间的聚氧化丙烯二 醇、聚氧化乙烯二醇、聚四氢呋喃二醇中的一种或几种物质的混合物。
进一步的，所述松香树脂是氢化松香、歧化松香、聚合松香、马来松香和 水白松香中的一种或几种物质的混合物。
进一步的，所述异氰酸酯为1，6-己二异氰酸酯、异佛尔酮二异氰酸酯、氢 化二苯基甲烷二异氰酸酯、苯二亚甲基二异氰酸酯中的一种或几种物质的混合 物。
进一步的，所述亲水性扩链剂为含有羧酸基的二羟甲基丙酸或磺酸基的乙 二胺基乙磺酸钠水溶性小分子化合物；
所述扩链剂为乙二胺、己二胺、二乙烯三胺、三乙烯四胺中的一种或两种 物质的混合物。
进一步的，所述内交联剂为三羟甲基丙烷、甘油或1,2,6-己三醇中的一种 或几种物质的混合物；
进一步的，所述中和剂为三乙胺、氨、碳酸钠、碳酸氢钠、二甲基乙醇胺 中的一种或两种物质的混合物；
进一步的，所述抗氧剂为抗氧剂1010；
进一步的，所述催化剂为二月桂酸二丁基锡；
进一步的，所述有机溶剂为丙酮、丁酮、N-甲基吡咯烷酮、乙酸乙酯中的 一种或几种物质的混合物。
所述汽车内饰用水性聚氨酯胶粘剂的制备方法，具体步骤如下：
(1)预聚体的制备：聚酯多元醇10-15份和聚醚多元醇6-8份、松香树脂 4-8份、0.001-0.01份抗氧剂加入反应釜中，在氮气的保护下升温至120-140℃， 抽真空脱水0.5-1.5h；
降温冷却至50-60℃，加入8-15份异氰酸酯和0.1-0.3份亲水性扩链剂，在 60-70℃反应1.5-2.5h；继续加入0.001-0.1份催化剂、0-0.3份内交联剂和剩余的 0.1-0.3份亲水性扩链剂，升温至75-85℃，反应3-3.5h得到预聚体；
(2)降粘：将步骤(1)所得预聚体降温至50-60℃，加入1-5份有机溶剂 以降低预聚体粘度，然后再加入0.14-0.36份中和剂反应8-12min；
(3)反应：最后在1500-2000r/min的高速剪切力下将步骤(2)所得降粘 的预聚体分散乳化到40-70份去离子水中，并逐滴加入0.1-0.3份扩链剂搅拌 30-60min，在50℃下抽真空脱去溶剂即得到汽车内饰小扶手用水性聚氨酯胶粘 剂。
进一步的，所述异氰酸酯的加入量应满足R值即NCO/OH值为1.5-1.8。
进一步的，所述亲水性扩链剂为含有羧酸基的二羟甲基丙酸时，二羟甲基 丙酸的加入量占异氰酸酯的重量百分比为3％-5％。
本发明的有益效果：本发明操作简单易实施，得到的产品有机溶剂含量低， 味道小，稳定性好，初粘力好。
具体实施方式
实施例1
汽车内饰小扶手用水性聚氨酯胶粘剂，配方如下：7份聚己内酯二醇、8份 聚碳酸1，6-己二醇酯二醇、6份蓖麻油、6份松香树脂、4份异佛尔酮二异氰 酸酯、6.8份1，6-己二异氰酸酯、0.36份亲水性扩链剂DMPA、0.12份内交 联剂三羟甲基丙烷、0.1份扩链剂乙二胺、0.22份中和剂三乙胺、0.004份催化 剂二月桂酸二丁基锡、0.004份抗氧剂、4份有机溶剂丙酮和57份去离子水。
汽车内饰小扶手用水性聚氨酯胶粘剂的制备方法，步骤如下
(1)预聚体的制备：7份聚己内酯二醇、8份聚碳酸1，6-己二醇酯二醇、 6份蓖麻油、6份松香树脂和0.004份抗氧剂加入到反应釜中，在氮气的保护下， 升温至120℃，真空脱水1小时，冷却至60℃，加入4份异佛尔酮二异氰酸酯、 6.8份1，6-己二异氰酸酯和0.18份的亲水性扩链剂DMPA，在60℃反应2小时， 然后加入催化剂0.004份、内交联剂三羟甲基丙烷0.12份和剩余的0.18份亲水 性扩链剂DMPA，升温至80℃反应3小时得到预聚体。
(2)降粘：将步骤(1)所得预聚体降温至50℃，加入有机溶剂丙酮4份 以降低预聚体粘度，然后再加入0.22份中和剂三乙胺反应10分钟。
(3)反应：最后在2000r/min高速剪切力下将步骤(2)所得的预聚体分散 乳化到57份去离子水中，并逐滴加入0.1份扩链剂乙二胺，搅拌30分钟抽真空， 在50℃下脱去丙酮，即得到水性聚氨酯胶粘剂。
制备所得产品具体性能测试结果如表1所示。
实施例2
汽车内饰小扶手用水性聚氨酯胶粘剂，配方如下：7份聚己二酸乙二醇酯二 醇、8份聚碳酸1，6-己二醇酯二醇、8份蓖麻油、6份松香树脂、11份异佛尔 酮二异氰酸酯、0.46份亲水性扩链剂乙二胺基乙磺酸钠、0.1份内交联剂甘油、 0.1份扩链剂乙二胺、0.25份中和剂三乙胺、0.003份催化剂二月桂酸二丁基锡、 0.003份抗氧剂、4份有机溶剂丙酮、55份去离子水。
汽车内饰小扶手用水性聚氨酯胶粘剂的制备方法，步骤如下：
(1)预聚体的制备：将7份聚己二酸乙二醇酯二醇、8份聚碳酸1，6-己二 醇酯二醇、6份松香树脂、8份蓖麻油和0.003份抗氧剂加入到反应釜中，在氮 气的保护下，升温至140℃，真空脱水0.5小时，冷却至60℃，加入11份异佛 尔酮二异氰酸酯(IPDI)和0.23份亲水性扩链剂乙二胺基乙磺酸钠，在70℃反 应2小时，然后加入0.003份催化剂、0.1份内交联剂甘油和剩余的亲水性扩链 剂0.23份乙二胺基乙磺酸钠，升温至75℃反应3.5小时得到预聚体。
(2)降粘：将步骤(1)所得预聚体降温至60℃，加入4份有机溶剂丙酮 以降低预聚体粘度，然后再加入0.25份中和剂三乙胺，反应12分钟。
(3)反应：最后在1500r/min高速剪切力下将步骤(2)所得预聚体分散乳 化到55份去离子水中，并逐滴加入0.1份扩链剂乙二胺，搅拌60分钟，抽真空 在50℃下脱去丙酮，即得到水性聚氨酯胶粘剂。
制备所得产品具体性能测试结果如表1所示。
实施例3
汽车内饰小扶手用水性聚氨酯胶粘剂，配方如下：15份聚己内酯二醇、6 份聚四氢呋喃二醇、6份松香树脂、6份异佛尔酮二异氰酸酯、6份1，6-己二异 氰酸酯、0.34份的亲水性扩链剂DMPA、0.1份扩链剂乙二胺、0.2份中和剂三 乙胺、0.002份催化剂二月桂酸二丁基锡、0.002份抗氧剂、4份有机溶剂丙酮、 52份去离子水。
汽车内饰用水性聚氨酯胶粘剂的制备方法，步骤如下：
(1)预聚体的制备：将15份聚己内酯二醇(平均分子量为2000)和6份 聚四氢呋喃二醇1(平均分子量为2000)6份松香树脂、和抗氧剂0.002份加 入到反应釜中，在氮气的保护下，升温至130℃，真空脱水1小时，冷却至60℃， 加入6份异佛尔酮二异氰酸酯(IPDI)和6份1，6-己二异氰酸酯(HDI)和0.17 份亲水性扩链剂DMPA，在65℃反应2小时，然后加入0.002份催化剂和剩余 的0.17份亲水性扩链剂DMPA，升温至85℃反应3小时得到预聚体。
(2)降粘：将步骤(1)所得预聚体降温至55℃，加入4份有机溶剂丙酮 以降低预聚体粘度，然后再加入0.2份中和剂三乙胺反应10分钟。
(3)反应：最后在1800r/min高速剪切力下将上面所得的预聚体分散乳化 到52份去离子水中，并逐滴加入0.1份扩链剂乙二胺，搅拌45分钟，抽真空在 50℃下脱去丙酮，即得到水性聚氨酯胶粘剂。
制备所得产品具体性能测试结果如表1所示。
表1
Figure BDA0002055857220000041
根据上表1所得数据可知，本发得到的产品稳定性好，初粘力好，最终强 度大，耐高低温性能优良，具有优异的耐热性。

Claims (8)

1.汽车内饰用水性聚氨酯胶粘剂的制备方法，其特征是具体步骤如下：
（1）预聚体的制备：聚酯多元醇10-15份、聚醚多元醇6-8份、松香树脂4-8份、0.001-0.01份抗氧剂加入反应釜中，在氮气的保护下升温至120-140℃，抽真空脱水0.5-1.5h；
降温冷却至50-60℃，加入8-13份异氰酸酯和0.1-0.3份亲水性扩链剂，在60-70℃反应1.5-2.5h；继续加入0.001-0.1份催化剂、0-0.3份内交联剂和剩余的0.1-0.3份亲水性扩链剂，升温至75-85℃，反应3-3.5h得到预聚体；
所述异氰酸酯的加入量应满足 R 值即 NCO/OH 值为1.5-1.8；
所述亲水性扩链剂为含有羧酸基的二羟甲基丙酸时，二羟甲基丙酸的加入量占异氰酸酯的重量百分比为3%-5%；
（2）降粘：将步骤（1）所得预聚体降温至 50-60℃，加入1-5份有机溶剂以降低预聚体粘度，然后再加入0.12-0.36份中和剂反应8-12min；
（3）反应：最后在1500-2000r/min的高速剪切力下将步骤（2）所得降粘的预聚体分散乳化到40-70份去离子水中，并逐滴加入0.1-0.3份扩链剂搅拌 30-60min，在50℃下抽真空脱去溶剂即得到汽车内饰用水性聚氨酯胶粘剂。
2.如权利要求1所述汽车内饰用水性聚氨酯胶粘剂的制备方法，其特征是：所述聚酯多元醇为平均分子量在 500-5000之间的聚己二酸丁二醇酯二醇、聚己二酸乙二醇酯二醇、聚己内酯二醇和聚碳酸 1，6-己二醇酯二醇中的一种或几种物质的混合物。
3.如权利要求1所述汽车内饰用水性聚氨酯胶粘剂的制备方法，其特征是：所述聚醚多元醇为平均分子量在 500-5000之间的聚氧化丙烯二醇、聚氧化乙烯二醇和聚四氢呋喃二醇中的一种或几种物质的混合物。
4.如权利要求1所述汽车内饰用水性聚氨酯胶粘剂的制备方法，其特征是：所述松香树脂是氢化松香、歧化松香、聚合松香、马来松香和水白松香中的一种或几种物质的混合物。
5.如权利要求1所述汽车内饰用水性聚氨酯胶粘剂的制备方法，其特征是：所述异氰酸酯为1，6-己二异氰酸酯、异佛尔酮二异氰酸酯、氢化二苯基甲烷二异氰酸酯和苯二亚甲基二异氰酸酯中的一种或几种物质的混合物。
6.如权利要求1所述汽车内饰用水性聚氨酯胶粘剂的制备方法，其特征是：所述亲水性扩链剂为含有羧酸基的二羟甲基丙酸或磺酸基的乙二胺基乙磺酸钠水溶性小分子化合物；
所述扩链剂为乙二胺、己二胺、二乙烯三胺和三乙烯四胺中的一种或两种物质的混合物。
7.如权利要求1所述汽车内饰用水性聚氨酯胶粘剂的制备方法，其特征是：所述内交联剂为三羟甲基丙烷、甘油和1,2,6- 己三醇中的一种或几种物质的混合物；
所述中和剂为三乙胺、氨、碳酸钠、碳酸氢钠和二甲基乙醇胺中的一种或两种物质的混合物；
所述抗氧剂为抗氧剂1010；
所述催化剂为二月桂酸二丁基锡；
所述有机溶剂为丙酮、丁酮、N- 甲基吡咯烷酮和乙酸乙酯中的一种或几种物质的混合物。
8.权利要求1-7之一方法制备所得的汽车内饰用水性聚氨酯胶粘剂。
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