CN115029097B - 一种易挤出双组份聚氨酯中空玻璃密封胶及其制备方法 - Google Patents
一种易挤出双组份聚氨酯中空玻璃密封胶及其制备方法 Download PDFInfo
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Abstract
本发明属于密封胶技术领域，具体涉及一种易挤出双组份聚氨酯中空玻璃密封胶及其制备方法，所述密封胶包括重量比为100:35～45的A组份和B组份；其中，A组份由如下重量份的成份组成：30～40份支化聚氨酯预聚物、5～15份液态超支化树脂、40～65份填料、1～3份触变剂、0.5～1份润滑剂；B组份由如下重量份的成份组成：10～20份固化剂、15～30份填料、0.5～1份润滑剂、0.01～0.05份催化剂。支化聚氨酯预聚物由聚丙二醇、聚丙三醇、二异氰酸酯和封端剂合成，聚丙三醇/聚丙二醇当量比0.2～0.4。支化聚氨酯预聚物和超支化树脂均可以降低分子链缠结程度、降低粘度，复配有机盐类润滑剂，可有效降低挤出过程中的阻力。该方案能解决秋冬季节中空玻璃密封胶挤出性差、生产效率降低的难题。
Description
技术领域
本发明涉及一种易挤出双组份聚氨酯中空玻璃密封胶及其制备方法，属于密封胶技术领域。
背景技术
中空玻璃第二道密封采用的材料以双组份硅酮胶居多，虽然硅酮胶具有出色地耐候性能，但长期暴露会出现硅油渗出，污染基材、影响美观。双组份聚氨酯密封胶，固化成型速度快、固化后强度高，特别适合高速流水线操作。但是与双组份硅酮胶相比，聚氨酯分子间作用力大，粘度受温度影响较大，在低于0℃条件下，聚氨酯预聚物粘度较大，导致用聚氨酯预聚物制得的聚氨酯密封胶粘度增大，其挤出性受到较大影响。一方面，增大施胶的挤出压力则影响出胶量的稳定性，另一方面，维持稳定的低出胶量则降低施胶效率，使中空玻璃流水线的生产效率降低。因此提升双组份聚氨酯密封胶在低温下的挤出性，对其在中空玻璃密封胶的应用具有重要意义。
发明内容
本发明的目的在于克服上述现有技术的不足之处而提供一种易挤出双组份聚氨酯中空玻璃密封胶及其制备方法。
为实现上述目的，本发明采用如下所述的技术方案：一种易挤出双组份聚氨酯中空玻璃密封胶，包括重量比为100:35～45的A组份和B组份。
所述A组份由如下重量份的成份组成：
支化聚氨酯预聚物30～40份
液态超支化树脂5～15份
填料40～65份
触变剂1～3份
润滑剂0.5～1份。
所述B组份由如下重量份的成份组成：
固化剂10～20份
填料15～30份
润滑剂0.5～1份
催化剂0.01～0.05份。
所述支化聚氨酯预聚物由聚丙二醇、聚丙三醇、二异氰酸酯和封端剂合成。
所述聚丙二醇数均分子量为2000～4000g/mol，聚丙三醇数均分子量为300～600g/mol，聚丙三醇/聚丙二醇当量比为0.2～0.4，二异氰酸酯为甲苯二异氰酸酯TDI、二苯基甲烷-4-4’-二异氰酸酯MDI、多苯基多亚甲基多异氰酸酯PAPI中的一种或多种混合物，异氰酸根/羟基当量比等于2。
所述封端剂为己内酰胺、对氯苯酚、邻氯苯酚、对溴苯酚、对硝基苯酚、2-吡啶酚、3-羟基吡啶、8-羟基喹啉、苯硫酚、2-巯基吡啶、三氟乙醇、三氯乙醇、2-乙基己醇、N,N-二丁基羟基乙酰胺、N-羟基琥珀酰亚胺、N-吗啉代乙醇、2,2'-二甲基-1,3-二氧戊环-4-甲醇、3-噁唑烷乙醇、2-羟乙基吡啶、甲乙酮肟、乙酰苯胺、N-甲基乙酰胺、2-甲基咪唑、N-乙基-4-甲基咪唑、3,5-二甲基吡唑中的一种或多种混合物，封端剂与聚丙二醇和聚丙三醇混合物的当量比为2.4。
所述液态超支化树脂为液态超支化聚酯或液态超支化环氧树脂，优选为HyPerU102或HyPer E102。
所述填料为纳米碳酸钙、活性重钙、钛白粉、炭黑、颜料中的一种或多种混合物。
所述触变剂为气相二氧化硅。
所述润滑剂为硬脂酸钙、硬脂酸锌、硬脂酸镁、硬脂酸钡中的一种或多种混合物。
所述固化剂为650#低分子聚酰胺树脂。
所述催化剂为二月桂酸二丁基锡、四甲基丁二胺、三亚乙基二胺、辛酸亚锡中的一种或多种混合物。
本发明还提供了易挤出双组份聚氨酯中空玻璃密封胶的制备方法：(1)往反应釜中投入1.0当量份聚丙二醇和聚丙三醇混合物，升温至105～120℃，控制真空度不大于-0.095MPa，除水1～2小时后降温至70～80℃，投入设定量二异氰酸酯，投入0.002％质量分数的二月桂酸二丁基锡，氮气保护下搅拌2～4小时得到异氰酸酯根封端树脂，投入设定量封端剂，氮气保护下搅拌至少2小时直至NCO红外特征峰消失，得到支化聚氨酯预聚物；(2)投入设定量液态超支化树脂、填料、触变剂和润滑剂，控制物料温度≤50℃，氮气保护下搅拌混合1～2小时，计量出料、密封包装得A组份；(3)将设定量固化剂、填料、润滑剂和催化剂加入双行星高速搅拌机中，控制物料温度≤50℃，氮气保护下搅拌混合1～2小时，计量出料、包装得B组份。
与现有技术相比，本发明的有益效果如下：支化聚氨酯预聚物比线性结构预聚物分子链缠结弱，可有效降低粘度，引入超支化树脂进一步降低支化聚氨酯预聚物的分子链缠结，比邻苯二甲酸酯类增塑剂降低粘度效果更环保，引入有机盐类润滑剂，一方面促进填料在液体体系中的分散，另一方面可降低挤出过程中的阻力，该方案能解决秋冬季节中空玻璃密封胶挤出性差、生产效率降低的难题。
具体实施方式
为更好的说明本发明的目的、技术方案和优点，下面将结合具体实施例对本发明作进一步说明。
本发明实施例及对比例中实验所用的原料如下，但是不限于以下原料，本发明只是以下原料为具体例子来进一步具体说明本发明中所述易挤出双组份聚氨酯中空玻璃密封胶的效果：
液态超支化树脂：HyPer U102，武汉超支化树脂科技有限公司。
聚丙二醇：DL2000D，数均分子量为2000g/mol，山东蓝星东大。
聚丙三醇：C305，数均分子量为500g/mol，山东一诺威。
二异氰酸酯：MDI-50，烟台万华。
封端剂：对氯苯酚。
触变剂：气相二氧化硅，Waker HDKN20，德国瓦克。
填料：活性重钙、纳米碳酸钙，重量比4:1。
润滑剂：硬脂酸锌，济南腾岳化工。
固化剂：650#低分子量聚酰胺树脂，河南汇能。
催化剂：二月桂酸二丁基锡DBTDL，上海新典。
本发明设置实施例1～5，制备方法如下：(1)往反应釜中投入0.8当量份聚丙二醇DL2000D、0.2当量份聚丙三醇C305混合物，升温至110℃，控制真空度不大于-0.095MPa，除水1小时后降温至75℃，投入2.2当量份二异氰酸酯MDI-50，投入0.002％质量分数的二月桂酸二丁基锡，氮气保护下搅拌2小时得到异氰酸酯根封端树脂，投入2.4当量份的封端剂对氯苯酚，氮气保护下搅拌2小时得到支化聚氨酯预聚物，记为树脂1；(2)投入设定量液态超支化树脂HyPer U102、填料、触变剂气相二氧化硅和润滑剂硬脂酸锌，控制物料温度≤50℃，氮气保护下搅拌混合1小时，计量出料、密封包装得A组份；(3)将设定量固化剂650#、填料、润滑剂硬脂酸锌和催化剂二月桂酸二丁基锡加入双行星高速搅拌机中，控制物料温度≤50℃，氮气保护下搅拌混合1小时，计量出料、包装得B组份。
本发明设置对比例1～4，制备方法如下：(1)往反应釜中投入1.0当量份聚丙二醇DL2000D，升温至110℃，控制真空度不大于-0.095MPa，除水1小时后降温至75℃，投入2.0当量份二异氰酸酯MDI-50，投入0.002％质量分数的二月桂酸二丁基锡，氮气保护下搅拌2小时得到异氰酸酯根封端树脂，投入2.2当量份的封端剂对氯苯酚，氮气保护下搅拌2小时得到线性聚氨酯预聚物，记为树脂2；(2)投入设定量填料、触变剂气相二氧化硅和润滑剂硬脂酸锌，控制物料温度≤50℃，氮气保护下搅拌混合1小时，计量出料、密封包装得A组份；(3)将设定量固化剂650#、填料、润滑剂硬脂酸锌和催化剂二月桂酸二丁基锡加入双行星高速搅拌机中，控制物料温度≤50℃，氮气保护下搅拌混合1小时，计量出料、包装得B组份。
挤出性测试：参考GB-T 13477.3-2017规定的方法进行测试，挤出筒以及混合前A组份、B组份在-5℃和25℃三种温度下调节6小时，然后AB组份按100:40的重量比调制混合物进行打胶。
表1：实施例1～5及对比例1～4配方
表2：实施例1～5及对比例1～4挤出性能
挤出性大于20克/分钟的双组份密封胶，在自动打胶流水作业中施加中等压力即可获得合适稳定的出胶速度。实施例1～5采用支化聚氨酯预聚物和液态超支化树脂，低温和室温下的挤出性明显优于对比例1～4。对比例1和对比例2仅采用支化聚氨酯预聚物，而对比例3和对比例4仅采用线性聚氨酯预聚物，分子链缠结严重，导致挤出性降低。
以上所述仅为本发明的实施例而已，并不用于限制本发明。本发明可以有各种合适的更改和变化。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 (1)
1.一种易挤出双组份聚氨酯中空玻璃密封胶，其特征在于，包括重量比为100:35~45的A组份和B组份，所述A组份由如下重量份的成份组成：30~40份支化聚氨酯预聚物、5~15份液态超支化树脂、40~65份填料、1~3份触变剂、0.5~1份润滑剂；所述B组份由如下重量份的成份组成：10~20份固化剂、15~30份填料、0.5~1份润滑剂、0.01~0.05份催化剂；
其中，所述支化聚氨酯预聚物由聚丙二醇、聚丙三醇、二异氰酸酯和封端剂合成，所述聚丙二醇数均分子量为2000~4000 g/mol，聚丙三醇数均分子量为300~600 g/mol，聚丙三醇/聚丙二醇当量比为0.2~0.4；
所述二异氰酸酯为甲苯二异氰酸酯TDI、二苯基甲烷-4-4’-二异氰酸酯MDI中的一种或多种混合物，异氰酸根/羟基当量比等于2；
所述封端剂为己内酰胺、对氯苯酚、邻氯苯酚、对溴苯酚、对硝基苯酚、2-吡啶酚、3-羟基吡啶、8-羟基喹啉、苯硫酚、2-巯基吡啶、三氟乙醇、三氯乙醇、2-乙基己醇、N,N-二丁基羟基乙酰胺、N-羟基琥珀酰亚胺、N-吗啉代乙醇、2,2'-二甲基-1,3-二氧戊环-4-甲醇、3-噁唑烷乙醇、2-羟乙基吡啶、甲乙酮肟、乙酰苯胺、N-甲基乙酰胺、2-甲基咪唑、N-乙基-4-甲基咪唑、3,5-二甲基吡唑中的一种或多种混合物，封端剂与聚丙二醇和聚丙三醇混合物的当量比为2.4；
所述液态超支化树脂为HyPer U102，触变剂为气相二氧化硅；
所述固化剂为650#低分子聚酰胺树脂，催化剂为二月桂酸二丁基锡、四甲基丁二胺、三亚乙基二胺、辛酸亚锡中的一种或多种混合物；
所述A组份和B组份中，填料为纳米碳酸钙、活性重钙、钛白粉、炭黑中的一种或多种混合物，润滑剂为硬脂酸钙、硬脂酸锌、硬脂酸镁、硬脂酸钡中的一种或多种混合物；
所述易挤出双组份聚氨酯中空玻璃密封胶的制备方法，包括如下步骤：
（1）往反应釜中投入1.0当量份聚丙二醇和聚丙三醇混合物，升温至105~120℃，控制真空度不大于-0.095 MPa，除水1~2小时后降温至70~80℃，投入设定量二异氰酸酯，投入0.002%质量分数的二月桂酸二丁基锡，氮气保护下搅拌2~4小时得到异氰酸酯根封端树脂，投入设定量封端剂，氮气保护下搅拌至少2小时直至NCO红外特征峰消失，得到支化聚氨酯预聚物；
（2）投入设定量液态超支化树脂、填料、触变剂和润滑剂，控制物料温度≤50℃，氮气保护下搅拌混合1~2小时，计量出料、密封包装得A组份；
（3）将设定量固化剂、填料、润滑剂和催化剂加入双行星高速搅拌机中，控制物料温度≤50℃，氮气保护下搅拌混合1~2小时，计量出料、包装得B组份。
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