CN112376279B - 一种用于生产玻璃纤维连续毡浸润剂的制备方法 - Google Patents

一种用于生产玻璃纤维连续毡浸润剂的制备方法 Download PDF

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CN112376279B
CN112376279B CN202011283423.0A CN202011283423A CN112376279B CN 112376279 B CN112376279 B CN 112376279B CN 202011283423 A CN202011283423 A CN 202011283423A CN 112376279 B CN112376279 B CN 112376279B
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顾柔坚
费海燕
赵建元
缪李鹏
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Abstract

本发明公开了一种用于生产玻璃纤维连续毡浸润剂的制备方法，包括硅烷接枝聚辛二酸‑丁烯酸‑乙二醇酯的制备以及通过硅烷接枝聚辛二酸‑丁烯酸‑乙二醇酯制备浸润剂。本发明优点在于，通过硅烷与低分子成膜剂接枝合成，生成一种含硅烷的水性成膜剂，在此基础上制得浸润剂，减少了常用偶联剂用冰醋酸水解的过程，简化人工操作，大幅度降低了工人因冰醋酸产生的皮肤过敏现象；又解决了常用偶联剂高温易分解挥发问题，同时增加了成膜剂的韧性，更好的增强了玻璃纤维与树脂的界面结合力，从而提高复合材料力学性能。

Description

一种用于生产玻璃纤维连续毡浸润剂的制备方法
技术领域
本发明属于玻璃纤维增强复合材料技术领域，具体涉及一种用于生产玻璃纤维连续毡浸润剂的制备方法。
背景技术
玻璃纤维浸润剂是玻璃纤维生产特有的一种表面处理剂，不仅能改变玻璃纤维的表面性能，满足玻纤原丝后道工序加工性能的要求，而且在复合材料中还能促进玻璃纤维增强体与高分子聚合物基体的结合，是决定玻璃纤维增强复合材料最终性能的重要因素。浸润剂通常由成膜剂、偶联剂、抗静电剂、润滑剂等组成，尤其以成膜剂和偶联剂最为关键。
一般浸润剂用硅烷偶联剂，需要先将偶联剂进行水解分散。通常方法是先用冰醋酸调节水解酸值再加入偶联剂，才能让硅烷偶联剂在水中充分分散。而冰醋酸的使用，极易造成拉丝工人皮肤过敏现象。连续玻璃纤维毡制作工艺需要在高温200-220℃烘干固化，而普通硅烷偶联剂在此过程中易挥发、黄变等问题，一定程度上降低偶联剂的作用，影响玻纤与树脂的结合力，使得后期复合材料力学性能下降。选用耐高温偶联剂，但价格昂贵。
发明内容
本发明的目的在于提供一种用于生产玻璃纤维连续毡浸润剂的制备方法，已解决背景技术中所存在的问题。
为实现上述目的，本发明提供如下技术方案：一种用于生产玻璃纤维连续毡浸润剂的制备方法，所述浸润剂的制备方法包括如下步骤：
S1：依次向反应釜内加入聚乙二醇600以及辛二酸与顺丁烯二酸酐的混合物，搅拌混合，混合物中辛二酸与顺丁烯二酸酐的摩尔比为3-4:1，聚乙二醇600与混合物的摩尔比1.2-1.4:1；
S2：向S1中的物料内通N2，在160—190℃下聚合3小时；
S3：开启真空泵，将S2中的物料脱除水分2h；
S4：S3中脱除水分后，将釜内温度下降至130℃，加入0.1-0.3％二月硅酸二丁基锡，再将硅烷慢慢滴加到釜内，硅烷添加量为1-3％，直至釜内物料酸值为10-20mgKOH/g，即得到硅烷接枝聚辛二酸-丁烯酸-乙二醇酯；
S5：配置浸润剂：按各组分及其质量百分比的2.5-3.5％硅烷接枝聚辛二酸-丁烯酸-乙二醇酯、1.5-2.5％E44改性环氧乳液、0.5-1.0％醚类润滑剂E02、0.01-0.03％阳离子抗静电剂、余量为去离子水制得浸润剂。
进一步地，S1中釜内搅拌速度为30Hz。
优选地，S2中釜内升温反应的顺序为：温度升温至160℃，反应1h，升温至170℃，反应1h，升温至180℃反应0.5h，升温至190℃下反应0.5h。
优选地，S4中硅烷为3-氨丙基三乙氧基硅烷、3-氨丙基三甲氧基硅烷、N-(2-氨乙基-3-氨丙基)三甲氧基硅烷、3-(甲基丙烯酰氧)丙基三乙氧基硅烷中的任意一种。
优选地，S4中硅烷滴加完成时间为2h。
进一步地，S4中的硅烷接枝聚辛二酸-丁烯酸-乙二醇酯的粘度为1000-2000mPa·s。
与现有技术相比，本发明的有益效果是：通过硅烷与低分子成膜剂接枝合成，生成一种含硅烷的水性成膜剂，再制得浸润剂。既避免了常用偶联剂用冰醋酸水解的过程，简化人工操作，同时大幅度降低了工人因冰醋酸产生的皮肤过敏现象。又解决了常用偶联剂高温易分解挥发问题，同时增加了成膜剂的韧性，更好的增强了玻璃纤维与树脂的界面结合力，从而提高复合材料力学性能。
具体实施方式
下面将结合实施例对本发明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做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
制备用于生产玻璃纤维连续毡浸润剂的步骤如下：
1、依次向反应釜内加入420kg聚乙二醇600、75kg辛二酸和19kg顺丁烯二酸酐，搅拌速度开启30Hz，向釜内通N2，将釜内温度升温至160℃，反应1h，170℃，反应1h，180℃反应0.5h，在190℃下反应0.5h后，慢慢地开启真空泵，脱除水分2小时后，将釜内温度下降至130℃，加入13g二月硅酸二丁基锡，将5kg的3-氨丙基三甲氧基硅烷以慢慢滴加到釜内，2h滴加结束，得到硅烷接枝聚辛二酸-丁烯酸-乙二醇酯。
取样测试，釜内酸值10-20mgKOH/g。
表1：硅烷接枝聚辛二酸-丁烯酸-乙二醇酯检测指标
检测项目 检测方法 检测指标
外观 目测 黄色至棕色液体
粘度 NDJ-1旋转粘度计 1000～2000mPa·s
酸值 10～20mgKOH/g
水溶性 聚合物：水＝1：9 全溶透明
2、将制得的硅烷接枝聚辛二酸-丁烯酸-乙二醇酯共聚物按照组分和配比配置浸润剂。
表2：实施例和对比例
Figure BDA0002781544990000031
Figure BDA0002781544990000041
按照表2中的配置的浸润剂用于玻璃纤维拉丝作业，经过施胶、高温烘干和收卷等工段制成玻璃纤维连续毡。通过连续毡铺层、真空灌注环氧树脂工艺，制成玻璃纤维连续毡增强环氧板材，按照性能测试要求制作样条。性能测试如表3所示。
表3：玻璃纤维连续毡增强环氧树脂板材性能
性能指标 实施例 对比例
外观 表面平整 表面平整
弯曲强度/MPa 232.2 215.8
冲击强度(简支梁)/kJ/m2 58 45
拉伸强度/MPa 125.6 127.2
从表3中可见，使用本发明浸润剂生产的连续毡增强环氧树脂板在弯曲强度和冲击强度均明显高于用普通硅烷偶联剂的浸润剂配方。这说明硅烷接枝聚辛二酸-丁烯酸-乙二醇酯共聚物成膜剂的使用，一定程度上提高了玻纤的韧性，增强了玻纤与树脂的结合力。同时，使用本发明的配方，不需要使用冰醋酸，避免了工人因冰醋酸产生的皮肤过敏现象。
实施例1中硅烷还可以选择3-氨丙基三乙氧基硅烷、N-(2-氨乙基-3-氨丙基)三甲氧基硅烷或3-(甲基丙烯酰氧)丙基三乙氧基硅烷，制得浸润剂的性能指标及应用的效果与使用3-氨丙基三甲氧基硅烷最终的结果相同。
尽管已经示出和描述了本发明的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由所附权利要求及其等同物限定。

Claims (4)

1.一种用于生产玻璃纤维连续毡浸润剂的制备方法，其特征在于，所述浸润剂的制备方法包括如下步骤：
S1：依次向反应釜内加入聚乙二醇600以及辛二酸与顺丁烯二酸酐的混合物，搅拌混合，混合物中辛二酸与顺丁烯二酸酐的摩尔比为3-4:1，聚乙二醇600与混合物的摩尔比1.2-1.4:1；
S2：向S1中的物料内通N2，在160—190℃下聚合3小时；釜内升温反应的顺序为：温度升温至160℃，反应1h，升温至170℃，反应1h，升温至180℃反应0.5h，升温至190℃下反应0.5h。
S3：开启真空泵，将S2中的物料脱除水分2h；
S4：S3中脱除水分后，将釜内温度下降至130℃，加入0.1-0.3％二月桂酸二丁基锡，再将硅烷慢慢滴加到釜内，硅烷添加量为1-3％，直至釜内物料酸值为10-20mgKOH/g，即得到硅烷接枝聚辛二酸-丁烯酸-乙二醇酯；
S5：配置浸润剂：按各组分及其质量百分比的2.5-3.5％硅烷接枝聚辛二酸-丁烯酸-乙二醇酯、1.5-2.5％E44改性环氧乳液、0.5-1.0％醚类润滑剂E02、0.01-0.03％阳离子抗静电剂、余量为去离子水制得浸润剂。
2.根据权利要求1所述的一种用于生产玻璃纤维连续毡浸润剂的制备方法，其特征在于：S4中硅烷为3-氨丙基三乙氧基硅烷、3-氨丙基三甲氧基硅烷、N-(2-氨乙基-3-氨丙基)三甲氧基硅烷、3-(甲基丙烯酰氧)丙基三乙氧基硅烷中的任意一种。
3.根据权利要求1所述的一种用于生产玻璃纤维连续毡浸润剂的制备方法，其特征在于：S4中硅烷滴加完成时间为2h。
4.根据权利要求1所述的一种用于生产玻璃纤维连续毡浸润剂的制备方法，其特征在于：S4中的硅烷接枝聚辛二酸-丁烯酸-乙二醇酯的粘度为1000-2000mPa·s。
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