CN111303827B - 一种uv-湿气双重固化聚氨酯密封胶及其制备方法 - Google Patents

一种uv-湿气双重固化聚氨酯密封胶及其制备方法 Download PDF

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CN111303827B
CN111303827B CN202010244355.0A CN202010244355A CN111303827B CN 111303827 B CN111303827 B CN 111303827B CN 202010244355 A CN202010244355 A CN 202010244355A CN 111303827 B CN111303827 B CN 111303827B
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刘志培
王建斌
陈田安
解海华
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Abstract

本发明公开了一种UV‑湿气双重固化聚氨酯密封胶，包括以下重量份的组分：聚氨酯预聚体100份、邻苯二甲酸二辛酯稀释剂10‑50份、填料50‑100份、钛白粉0‑10份、触变剂2‑4份、恶唑烷类除水剂2‑5份、附着力促进剂2‑5份、催化剂1‑3份、光引发剂1‑3份。本发明UV‑湿气双重固化聚氨酯密封胶可通过UV辐射或湿气固化，结合了UV辐射固化与湿气固化的优点，解决了双组份聚氨酯密封胶操作复杂、适用期短的难题，克服了传统单组份湿气固化聚氨酯密封胶固化速度慢，易起泡的缺点，同时解决了传统UV胶挡光区无法固化的缺陷，实现快速固化的同时有效拓宽了应用范围。

Description

一种UV-湿气双重固化聚氨酯密封胶及其制备方法
技术领域
本发明涉及聚氨酯密封胶，尤其涉及一种UV-湿气双重固化聚氨酯密封胶及其制备方法。
背景技术
密封胶是汽车等工业生产中重要的工艺材料之一，聚氨酯密封胶、硅酮和聚硫密封胶构成了合成密封胶的三大品种，因聚氨酯密封胶具有性能可调节范围宽、适应性强、耐磨、耐油、低温弹性好，使用寿命长，粘接强度高等优点，已成为目前发展最快的汽车制造业中的高档密封材料。但是传统单组份湿固化体系存在固化速度慢、交联过程中容易起泡导致粘结效果差，双组份固化体系存在操作复杂、使用期短等问题。
发明内容
单组份聚氨酯密封胶粘结效果不理想，双组份的使用不便，针对该问题，本发明提供一种UV-湿气双重固化聚氨酯密封胶及其制备方法。
本发明解决上述技术问题的技术方案如下：一种UV-湿气双重固化聚氨酯密封胶，包括以下重量份的组分：聚氨酯预聚体100份、邻苯二甲酸二辛酯稀释剂10-50份、填料50-100份、钛白粉0-10份、触变剂2-4份、恶唑烷类除水剂2-5份、附着力促进剂2-5份、催化剂1-3份、光引发剂1-3份。
其中，所述聚氨酯预聚体由20wt％-50wt％的聚氨酯预聚体A和50wt％-80wt％的聚氨酯预聚体B组成；所述聚氨酯预聚体A由500-510重量份的HDI三聚体、185-190重量份的扩链剂、150-160重量份甲基丙烯酸异氰基乙酯和0.5-1.5重量份的阻聚剂组成；所述聚氨酯预聚体B由15-36重量份的聚醚多元醇、6-18重量份的聚酯多元醇和5-15重量份的异氰酸酯组成；所述填料为纳米碳酸钙、重质碳酸钙、滑石粉中的一种或几种的组合；所述触变剂为气相二氧化硅和有机膨润土中的一种或两种；所述附着力促进剂为迈图A-187；所述催化剂为二月桂酸二丁基锡、辛酸亚锡、双吗啉二乙基醚或三乙烯二胺中的一种或两种的组合；所述光引发剂为184光引发剂或1173光引发剂中的一种或两种的组合；所述阻聚剂为对苯二酚、对叔丁基邻苯二酚或苯甲酚中的一种过多种的组合；所述聚醚多元醇为数均分子量为2000-4000的二官能度聚氧化丙烯醚；所述聚酯多元醇为数均分子量为1000-3000的二官能度聚己内酯或聚碳酸酯多元醇；所述异氰酸酯为二苯基甲烷二异氰酸酯、甲苯二异氰酸酯或异氟尔酮二异氰酸酯中的一种或两种的组合。
本发明的有益效果是：1)本发明UV-湿气双重固化聚氨酯密封胶可通过UV辐射或湿气固化，结合了UV辐射固化与湿气固化的优点，解决了双组份聚氨酯密封胶操作复杂、适用期短的难题，克服了传统单组份湿气固化聚氨酯密封胶固化速度慢，易起泡的缺点，同时解决了传统UV胶挡光区无法固化的缺陷，实现快速固化的同时有效拓宽了应用范围；2)本发明通过接枝反应将不饱和双键接到异氰酸酯的分子链中，体系中不存在游离的不饱和双键，与传统的UV-湿气双固化体系相比，解决了丙烯酸酯与聚氨酯体系不相容的问题，提高了密封胶的储存稳定性、机械性能和耐候性。
进一步，所述扩链剂具有如下分子结构：
Figure BDA0002433581610000021
该扩链剂具有稳定的六元环结构和长链的醚键，使密封胶具有较好的耐候性、粘接强度和回弹性，还能够与MOI进行接枝，改善MOI的脆性且不降低其力学性能和耐候性。
本发明还涉及上述UV-湿气双重固化聚氨酯密封胶的制备方法，包括以下步骤：
1)按重量份称取各物质，将扩链剂在110-120℃和真空度为0.08-0.1MPa的状态下脱水2.5h，降温至50℃后，加入甲基丙烯酸异氰基乙酯与阻聚剂，升温至70-75℃反应2h，加入HDI三聚体，继续反应2h，得聚氨酯预聚体A，将聚醚多元醇和聚酯多元醇在110-120℃和真空度为0.08-0.1MPa的状态下脱水2.5h，降温至50℃后，加异氰酸酯，升温至80-85℃反应2-3h，得聚氨酯预聚体B，将所得聚氨酯预聚体A和聚氨酯预聚体B按比例混合均匀得聚氨酯预聚体，充氮气保存；
2)将邻苯二甲酸二辛酯、填料、钛白粉和触变剂在真空度0.08-0.1MPa及110-115℃条件下搅拌1.5-2h，搅拌速度为500-1000r/min，再加入步骤1)所得聚氨酯预聚体和恶唑烷类除水剂，继续真空搅拌30-60min，搅拌速度为200-500r/min，最后加入附着力促进剂、催化剂和光引发剂，继续真空搅拌30-60min，搅拌速度为200-500r/min，即得。
具体实施方式
以下结合实例对本发明进行描述，所举实例只用于解释本发明，并非用于限定本发明的范围。
实施例1
一种UV-湿气双重固化聚氨酯密封胶的制备方法：
1)取扩链剂187份在120℃和真空度为0.08MPa的状态下脱水2.5h，降温至50℃后，加155份甲基丙烯酸异氰基乙酯与1份对叔丁基邻苯二酚，在70-75℃下反应2h，反应结束后加505份HDI三聚体在75℃下继续反应2h，既得聚氨酯预聚体A；
2)取分子量2000二官能度聚氧化丙烯醚15份，分子量1000的二官能度聚己内酯6份在120℃和真空度为0.08MPa的状态下脱水2.5h，降温至50℃后，加异氟尔酮二异氰酸酯5份，在85℃下反应3h，既得聚氨酯预聚体B；
3)将50份邻苯二甲酸二辛酯、20份轻质碳酸钙、80份重质碳酸钙、10份钛白粉、4份气相硅在真空度及110-115℃条件下搅拌1.5-2h，搅拌速度为1000r/min，降温，得到混合物料；向混合料中加50份聚氨酯预聚体A、50份聚氨酯预聚体B、5份恶唑烷类除水剂，真空搅拌30min，搅拌速度为200r/min，得到混合物料；向混合物料中快速加入A-1875份、二月桂酸二丁基锡1份、双吗啉二乙基醚催化剂2份、184光引发剂3份，真空搅拌60min，搅拌速度为200r/min，制得UV-湿气双重固化体系聚氨酯密封胶。
实施例2
一种UV-湿气双重固化聚氨酯密封胶的制备方法：
1)取扩链剂185份在120℃和真空度为0.08MPa的状态下脱水2.5h，降温至50℃后，加160份甲基丙烯酸异氰基乙酯与0.5份对苯二酚，在70℃下反应2h，反应结束后加500份HDI三聚体在70℃下继续反应2h，既得聚氨酯预聚体A；
2)取分子量4000二官能度聚氧化丙烯醚36份，分子量2000的二官能度聚碳酸酯18份在120℃和真空度为0.1MPa的状态下脱水2.5h，降温至50℃后，加异氟尔酮二异氰酸酯5份，二苯基甲烷二异氰酸酯10份，在80℃下反应2h，既得聚氨酯预聚体B；
3)将10份邻苯二甲酸二辛酯、30份重质碳酸钙、20份滑石粉、2份有机膨润土在真空度及115℃条件下搅拌2h，搅拌速度为1000r/min，降温，得到混合物料；向混合料中加20份聚氨酯预聚体A、80份聚氨酯预聚体B、1份恶唑烷类除水剂，真空搅拌30min，搅拌速度为500r/min，得到混合物料；向混合物料中快速加入A-1872份、辛酸亚锡0.5份、双吗啉二乙基醚催化剂0.5份、1173光引发剂1份，真空搅拌60min，搅拌速度为500r/min，制得UV-湿气双重固化体系聚氨酯密封胶。
实施例3
一种UV-湿气双重固化聚氨酯密封胶的制备方法：
1)取扩链剂190份在120℃和真空度为0.1MPa的状态下脱水2.5h，降温至50℃后，加150份甲基丙烯酸异氰基乙酯与1份苯甲酚，在70℃下反应2h，反应结束后加510份HDI三聚体在75℃下继续反应2h，既得聚氨酯预聚体A；
2)取分子量3000二官能度聚氧化丙烯醚25份，分子量3000的二官能度聚碳酸酯15份在120℃和真空度为0.1MPa的状态下脱水2.5h，降温至50℃后，加异氟尔酮二异氰酸酯5份，甲苯二异氰酸酯3份，在80℃下反应3h，既得聚氨酯预聚体B；
3)将30份邻苯二甲酸二辛酯、40份重质碳酸钙、20份滑石粉、10份轻质碳酸钙、3份有机膨润土在真空度及110℃条件下搅拌2h，搅拌速度为500r/min，降温，得到混合物料；向混合料中加30份聚氨酯预聚体A、70份聚氨酯预聚体B、4份恶唑烷类除水剂，真空搅拌60min，搅拌速度为200r/min，得到混合物料；向混合物料中快速加入A-1873份、双吗啉二乙基醚催化剂1.5份、1173光引发剂2份，真空搅拌30min，搅拌速度为200r/min，制得UV-湿气双重固化体系聚氨酯密封胶。
实施例1-3所用扩链剂具有如下结构：
Figure BDA0002433581610000051
将实施例1-3所得聚氨酯密封胶用胶枪打出后，于常温下分别进行UV固化和UV-湿气固化，并进行如下检测，结果如表1和表2所示。
表1UV固化指标
Figure BDA0002433581610000061
表2.UV+湿气固化指标
Figure BDA0002433581610000062
注：
表1和表2检测执行标准如下：
1、UV固化时间：将样品放置于距灯源10cm的正下方照射，紫外光强度为55mW/cm2，直至样品表面不发粘所需的时间。
2、硬度：按GBT2411-2008测试。
3、拉伸强度及断裂伸长率：按GB/T30776-2014测试。将模具放置箔纸上，用胶枪将密封胶注入模具里，用刮刀刮平，去掉多余的密封胶，从箔纸上取下模具，胶层厚度为2.5～3.0mm。在紫外光下固化30s或先在紫外光下固化30s，后在温度(23士1)℃、湿度(50士5)％RH的条件下固化168h，取出胶片，将其切成规定尺寸的哑铃形试片。以(5士0.2)mm/s的拉伸速度，测试常温拉伸强度和伸长率。
4、拉伸剪切强度：按GB/T7124-2008测试。标准试样的搭接长度是(12.5士0.25)mm，粘接层厚度为0.2mm。玻璃钢试片需用刚玉砂布均匀打磨，用乙酸乙醋擦干净，于105～110℃烘干，放入干燥器中备用。紫外光下固化30s或先在紫外光下固化30s，后在温度(23士1)℃、湿度(50士5)％RH的条件下固化168h固化后进行测试。
从表1和表2数据可以看出，本发明的UV-湿气双重固化聚氨酯密封胶，在光辐射下几十秒之内即可获得较高的拉伸剪切强度，大大节省了固化夹固时间；再经湿气固化后具有优异的力学性能，不饱和双键的加入并没有使体系的力学性能和分子柔韧性降低。
以上所述仅为本发明的较佳实施例，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (7)

1.一种UV-湿气双重固化聚氨酯密封胶，其特征在于，包括以下重量份的组分：
聚氨酯预聚体100份、邻苯二甲酸二辛酯稀释剂10-50份、填料50-100份、钛白粉0-10份、触变剂2-4份、恶唑烷类除水剂2-5份、附着力促进剂2-5份、催化剂1-3份、光引发剂1-3份；
其中，所述聚氨酯预聚体由20wt％-50wt％的聚氨酯预聚体A和50wt％-80wt％的聚氨酯预聚体B组成；所述聚氨酯预聚体A由500-510重量份的HDI三聚体、185-190重量份的扩链剂、150-160重量份甲基丙烯酸异氰基乙酯和0.5-1.5重量份的阻聚剂组成；所述聚氨酯预聚体B由15-36重量份的聚醚多元醇、6-18重量份的聚酯多元醇和5-15重量份的异氰酸酯组成；
所述附着力促进剂为迈图A-187；所述聚醚多元醇为数均分子量为2000-4000的二官能度聚氧化丙烯醚；所述聚酯多元醇为数均分子量为1000-3000的二官能度聚己内酯或聚碳酸酯多元醇；所述异氰酸酯为二苯基甲烷二异氰酸酯、甲苯二异氰酸酯或异氟尔酮二异氰酸酯中的一种或两种的组合；
所述扩链剂具有如下分子结构：
Figure FDA0003341678790000011
2.根据权利要求1所述的UV-湿气双重固化聚氨酯密封胶，其特征在于，所述填料为纳米碳酸钙、重质碳酸钙、滑石粉中的一种或几种的组合。
3.根据权利要求1所述的UV-湿气双重固化聚氨酯密封胶，其特征在于，所述触变剂为气相二氧化硅和有机膨润土中的一种或两种。
4.根据权利要求1所述的UV-湿气双重固化聚氨酯密封胶，其特征在于，所述催化剂为二月桂酸二丁基锡、辛酸亚锡、双吗啉二乙基醚或三乙烯二胺中的一种或两种的组合。
5.根据权利要求1所述的UV-湿气双重固化聚氨酯密封胶，其特征在于，所述光引发剂为184光引发剂或1173光引发剂中的一种或两种的组合。
6.根据权利要求1所述的UV-湿气双重固化聚氨酯密封胶，其特征在于，所述阻聚剂为对苯二酚、对叔丁基邻苯二酚或苯甲酚中的一种过多种的组合。
7.一种如权利要求1-6任一项所述的UV-湿气双重固化聚氨酯密封胶的制备方法，其特征在于，包括以下步骤：
1)按重量份称取各物质，将扩链剂在110-120℃和真空度为0.08-0.1MPa的状态下脱水2.5h，降温至50℃后，加入甲基丙烯酸异氰基乙酯与阻聚剂，升温至70-75℃反应2h，加入HDI三聚体，继续反应2h，得聚氨酯预聚体A，将聚醚多元醇和聚酯多元醇在110-120℃和真空度为0.08-0.1MPa的状态下脱水2.5h，降温至50℃后，加异氰酸酯，升温至80-85℃反应2-3h，得聚氨酯预聚体B，将所得聚氨酯预聚体A和聚氨酯预聚体B按比例混合均匀得聚氨酯预聚体，充氮气保存；
2)将邻苯二甲酸二辛酯、填料、钛白粉和触变剂在真空度0.08-0.1MPa及110-115℃条件下搅拌1.5-2h，搅拌速度为500-1000r/min，再加入步骤1)所得聚氨酯预聚体和恶唑烷类除水剂，继续真空搅拌30-60min，搅拌速度为200-500r/min，最后加入附着力促进剂、催化剂和光引发剂，继续真空搅拌30-60min，搅拌速度为200-500r/min，即得。
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