CN111925483A - 一种笼型倍半硅氧烷改性丙烯酸酯-聚氨酯复合材料及其制法 - Google Patents
一种笼型倍半硅氧烷改性丙烯酸酯-聚氨酯复合材料及其制法 Download PDFInfo
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Abstract
本发明涉及聚氨酯技术领域，且公开了一种笼型倍半硅氧烷改性丙烯酸酯‑聚氨酯复合材料，含烯基的聚氨酯、甲基丙烯酸甲酯和八聚乙烯基笼型倍半硅氧烷通过烯基自由基共聚反应，制备得到一种笼型倍半硅氧烷改性丙烯酸酯‑聚氨酯复合材料，由于甲基丙烯酸甲酯为硬单体，与聚氨酯中的硬段极性相似，并且可以形成氢键，因而具有更好的相容性，同时通过化学聚合反应，将八聚乙烯基笼型倍半硅氧烷的引入到聚氨酯共聚物的分子链中，笼型倍半硅氧烷独特的笼状形貌，以及易迁移的特性改变了涂层表面的化学物质组成，赋予了材料优异的物理机械性能，进一步改善了丙烯酸酯‑聚氨酯复合材料的力学拉伸性能。
Description
技术领域
本发明涉及聚氨酯技术领域，具体为一种笼型倍半硅氧烷改性丙烯酸酯-聚氨酯复合材料及其制法。
背景技术
聚氨酯材料是由多异氰酸酯和多元醇反应而得到的含有若干个氨基甲酸酯链段的有机高分子材料，性能较为全面，具有优异的声学、电学和耐化学介质性能，可以制成如塑料、胶黏剂、橡胶、涂料、纤维等材料，被广泛应用于建筑、交通、服装、家具、医疗等众多产业领域。
聚倍半硅氧烷是较为特殊的一类硅氧烷聚合物，其聚合物主体组成为(RSiO1.5)n，有梯形、树枝型和笼型等结构，与高聚物分子有良好的结合性和相容性，逐渐成为近年来聚合物的研究热点，目前研究重点多集中于涂料、塑料和树脂等领域，具有非常广泛的应用。
但是聚氨酯材料的韧性和拉伸等机械性能不高，极大限制了聚氨酯材料在某些方面的应用，目前可以将水性丙烯酸酯和水性聚氨酯复合，最大程度地发挥聚氨酯和丙烯酸酯的优势，对材料的性能有显著的提高，因此通过对聚氨酯材料进行改性处理来增强聚氨酯材料的力学拉伸性能就显得很有必要。
(一)解决的技术问题
针对现有技术的不足，本发明提供了一种笼型倍半硅氧烷改性丙烯酸酯-聚氨酯复合材料及其制法，解决了聚氨酯材料力学拉伸性能较差的问题。
(二)技术方案
为实现上述目的，本发明提供如下技术方案：一种笼型倍半硅氧烷改性丙烯酸酯-聚氨酯复合材料，所述笼型倍半硅氧烷改性丙烯酸酯-聚氨酯复合材料制备方法如下：
(1)向三口烧瓶中加入体积比为480-550:70-100:100的丙酮、浓盐酸和蒸馏水的混合溶剂及乙烯基三乙氧基硅烷，用磁力搅拌器搅拌，冷凝管回流，在50-60℃的条件下反应20-30h，过滤掉溶剂，丙酮洗涤产物并干燥，制备得八聚乙烯基笼型倍半硅氧烷；
(2)向烧瓶中加入聚四氢呋喃醚二醇和二羟甲基丙酸，搅拌升温至110-130℃，进行除水5-15min，降温至55-65℃，然后加入异佛尔酮二异氰酸酯，在80-95℃的条件下反应2-3h，加入丙烯酸羟乙酯，继续反应2-3h，反应完成后加入丙酮进行稀释，加入三乙胺进行中和，搅拌5-20min，将得到的预聚体在水溶剂中分散扩链反应2-4h，制备得水性聚氨酯乳液；
(3)向烧瓶中加入水性聚氨酯乳液，在70-80℃的条件下滴加甲基丙烯酸甲酯和八聚乙烯基笼型倍半硅氧烷，以过氧化二苯甲酰为引发剂，恒温反应2-4h，制备得一种笼型倍半硅氧烷改性丙烯酸酯-聚氨酯复合材料。
优选的，所述步骤(1)中的磁力搅拌装置包括基底，所述基底的内壁底部固定连接有轴承座，所述轴承座的顶部转动连接有转轴，所述转轴的外壁活动链接有履带，所述履带的内部活动连接有轴承杆，所述轴承杆的底部固定连接有锥齿轮一，所述锥齿轮一的底部活动链接有支杆，所述锥齿轮一的右侧活动链接有锥齿轮二，所述锥齿轮二的右侧固定连接有旋转杆，所述旋转杆的右侧固定连接有电机，所述电机的右侧固定连接有开关，所述转轴的顶部固定连接有托板。
优选的，所述步骤(3)中的聚四氢呋喃醚二醇、二羟甲基丙酸、异佛尔酮二异氰酸酯和三乙胺的质量比为100:10-13:32-35:6-9。
优选的，所述步骤(4)中的水性聚氨酯乳液的固体组分、甲基丙烯酸甲酯和笼型倍半硅氧烷的质量比为100:6-8:1-5。
(三)有益的技术效果
与现有技术相比，本发明具备以下有益的技术效果：
该一种笼型倍半硅氧烷改性丙烯酸酯-聚氨酯复合材料，首先以丙酮、浓盐酸和蒸馏水的混合溶剂及乙烯基三乙氧基硅烷为原料制备得八聚乙烯基笼型倍半硅氧烷，再以聚四氢呋喃醚二醇和异佛尔酮二异氰酸酯为聚合单体、丙烯酸羟乙酯作为支链，得到含烯基的聚氨酯，在过氧化二苯甲酰引发作用下，含烯基的聚氨酯、甲基丙烯酸甲酯和八聚乙烯基笼型倍半硅氧烷通过烯基自由基共聚反应，制备得到一种笼型倍半硅氧烷改性丙烯酸酯-聚氨酯复合材料。
由于甲基丙烯酸甲酯为硬单体，与聚氨酯中的硬段极性相似，并且可以形成氢键，因而具有更好的相容性，因此共聚形成的丙烯酸酯-聚氨酯复合材料具有更好的力学拉伸性能，同时通过化学聚合反应，将八聚乙烯基笼型倍半硅氧烷的引入到聚氨酯共聚物的分子链中，笼型倍半硅氧烷独特的笼状形貌，以及易迁移的特性改变了涂层表面的化学物质组成，赋予了材料优异的物理机械性能，进一步改善了丙烯酸酯-聚氨酯复合材料的力学拉伸性能。
附图说明
图1是磁力搅拌器剖视图；
图2是磁力搅拌器俯视图；
图3是锥齿轮啮合示意图。
1-基底；2-轴承座；3-转轴；4-履带；5-轴承杆；6-锥齿轮一；7-支杆；8-锥齿轮二；9-旋转轴；10-电机；11-开关；12-托板。
具体实施方式
为实现上述目的，本发明提供如下具体实施方式和实施例：一种笼型倍半硅氧烷改性丙烯酸酯-聚氨酯复合材料，笼型倍半硅氧烷改性丙烯酸酯-聚氨酯复合材料制备方法如下：
(1)向三口烧瓶中加入体积比为480-550:70-100:100的丙酮、浓盐酸和蒸馏水的混合溶剂及乙烯基三乙氧基硅烷，用磁力搅拌器搅拌，冷凝管回流，在50-60℃的条件下反应20-30h，过滤掉溶剂，丙酮洗涤产物并干燥，制备得八聚乙烯基笼型倍半硅氧烷；
(2)向烧瓶中加入聚四氢呋喃醚二醇和二羟甲基丙酸，搅拌升温至110-130℃，进行除水5-15min，降温至55-65℃，然后加入异佛尔酮二异氰酸酯，在80-95℃的条件下反应2-3h，加入丙烯酸羟乙酯，继续反应2-3h，反应完成后加入丙酮进行稀释，加入三乙胺进行中和，其中聚四氢呋喃醚二醇、二羟甲基丙酸、异佛尔酮二异氰酸酯和三乙胺的质量比为100:10-13:32-35:6-9，搅拌5-20min，将得到的预聚体在水溶剂中分散扩链反应2-4h，制备得水性聚氨酯乳液；
(3)向烧瓶中加入水性聚氨酯乳液，在70-80℃的条件下滴加甲基丙烯酸甲酯和八聚乙烯基笼型倍半硅氧烷，其中水性聚氨酯乳液的固体组分、甲基丙烯酸甲酯和笼型倍半硅氧烷的质量比为100:6-8:1-5，以过氧化二苯甲酰为引发剂，恒温反应2-4h，制备得一种笼型倍半硅氧烷改性丙烯酸酯-聚氨酯复合材料。
实施例1
(1)向三口烧瓶中加入体积比为480:70:100的丙酮、浓盐酸和蒸馏水的混合溶剂及乙烯基三乙氧基硅烷，用磁力搅拌器搅拌，冷凝管回流，在50℃的条件下反应20h，过滤掉溶剂，丙酮洗涤产物并干燥，制备得八聚乙烯基笼型倍半硅氧烷；
(2)向烧瓶中加入聚四氢呋喃醚二醇和二羟甲基丙酸，搅拌升温至110℃，进行除水5min，降温至55℃，然后加入异佛尔酮二异氰酸酯，在80℃的条件下反应2h，加入丙烯酸羟乙酯，继续反应2h，反应完成后加入丙酮进行稀释，加入三乙胺进行中和，其中聚四氢呋喃醚二醇、二羟甲基丙酸、异佛尔酮二异氰酸酯和三乙胺的质量比为100:10:32:6，搅拌5min，将得到的预聚体在水溶剂中分散扩链反应2h，制备得水性聚氨酯乳液；
(3)向烧瓶中加入水性聚氨酯乳液，在70℃的条件下滴加甲基丙烯酸甲酯和八聚乙烯基笼型倍半硅氧烷，其中水性聚氨酯乳液的固体组分、甲基丙烯酸甲酯和笼型倍半硅氧烷的质量比为100:6:1，以过氧化二苯甲酰为引发剂，恒温反应2h，制备得一种笼型倍半硅氧烷改性丙烯酸酯-聚氨酯复合材料。
实施例2
(1)向三口烧瓶中加入体积比为550:100:100的丙酮、浓盐酸和蒸馏水的混合溶剂及乙烯基三乙氧基硅烷，用磁力搅拌器搅拌，冷凝管回流，在60℃的条件下反应30h，过滤掉溶剂，丙酮洗涤产物并干燥，制备得八聚乙烯基笼型倍半硅氧烷；
(2)向烧瓶中加入聚四氢呋喃醚二醇和二羟甲基丙酸，搅拌升温至130℃，进行除水15min，降温至65℃，然后加入异佛尔酮二异氰酸酯，在95℃的条件下反应3h，加入丙烯酸羟乙酯，继续反应3h，反应完成后加入丙酮进行稀释，加入三乙胺进行中和，其中聚四氢呋喃醚二醇、二羟甲基丙酸、异佛尔酮二异氰酸酯和三乙胺的质量比为100:13:35:9，搅拌20min，将得到的预聚体在水溶剂中分散扩链反应4h，制备得水性聚氨酯乳液；
(3)向烧瓶中加入水性聚氨酯乳液，在80℃的条件下滴加甲基丙烯酸甲酯和八聚乙烯基笼型倍半硅氧烷，其中水性聚氨酯乳液的固体组分、甲基丙烯酸甲酯和笼型倍半硅氧烷的质量比为100:8:5，以过氧化二苯甲酰为引发剂，恒温反应4h，制备得一种笼型倍半硅氧烷改性丙烯酸酯-聚氨酯复合材料。
实施例3
(1)向三口烧瓶中加入体积比为500:80:100的丙酮、浓盐酸和蒸馏水的混合溶剂及乙烯基三乙氧基硅烷，用磁力搅拌器搅拌，冷凝管回流，在55℃的条件下反应24h，过滤掉溶剂，丙酮洗涤产物并干燥，制备得八聚乙烯基笼型倍半硅氧烷；
(2)向烧瓶中加入聚四氢呋喃醚二醇和二羟甲基丙酸，搅拌升温至120℃，进行除水10min，降温至60℃，然后加入异佛尔酮二异氰酸酯，在90℃的条件下反应2.5h，加入丙烯酸羟乙酯，继续反应2.5h，反应完成后加入丙酮进行稀释，加入三乙胺进行中和，其中聚四氢呋喃醚二醇、二羟甲基丙酸、异佛尔酮二异氰酸酯和三乙胺的质量比为100:12:24:8，搅拌15min，将得到的预聚体在水溶剂中分散扩链反应3h，制备得水性聚氨酯乳液；
(3)向烧瓶中加入水性聚氨酯乳液，在75℃的条件下滴加甲基丙烯酸甲酯和八聚乙烯基笼型倍半硅氧烷，其中水性聚氨酯乳液的固体组分、甲基丙烯酸甲酯和笼型倍半硅氧烷的质量比为100:7:3，以过氧化二苯甲酰为引发剂，恒温反应3h，制备得一种笼型倍半硅氧烷改性丙烯酸酯-聚氨酯复合材料。
实施例4
(1)向三口烧瓶中加入体积比为520:85:100的丙酮、浓盐酸和蒸馏水的混合溶剂及乙烯基三乙氧基硅烷，用磁力搅拌器搅拌，冷凝管回流，在60℃的条件下反应25h，过滤掉溶剂，丙酮洗涤产物并干燥，制备得八聚乙烯基笼型倍半硅氧烷；
(2)向烧瓶中加入聚四氢呋喃醚二醇和二羟甲基丙酸，搅拌升温至130℃，进行除水10min，降温至60℃，然后加入异佛尔酮二异氰酸酯，在90℃的条件下反应2h，加入丙烯酸羟乙酯，继续反应2.5h，反应完成后加入丙酮进行稀释，加入三乙胺进行中和，其中聚四氢呋喃醚二醇、二羟甲基丙酸、异佛尔酮二异氰酸酯和三乙胺的质量比为100:12:35:9，搅拌10min，将得到的预聚体在水溶剂中分散扩链反应3h，制备得水性聚氨酯乳液；
(3)向烧瓶中加入水性聚氨酯乳液，在70℃的条件下滴加甲基丙烯酸甲酯和八聚乙烯基笼型倍半硅氧烷，其中水性聚氨酯乳液的固体组分、甲基丙烯酸甲酯和笼型倍半硅氧烷的质量比为100:8:3，以过氧化二苯甲酰为引发剂，恒温反应4h，制备得一种笼型倍半硅氧烷改性丙烯酸酯-聚氨酯复合材料。
对比例1
(1)向三口烧瓶中加入体积比为450:50:100的丙酮、浓盐酸和蒸馏水的混合溶剂及乙烯基三乙氧基硅烷，用磁力搅拌器搅拌，冷凝管回流，在30℃的条件下反应10h，过滤掉溶剂，丙酮洗涤产物并干燥，制备得八聚乙烯基笼型倍半硅氧烷；
(2)向烧瓶中加入聚四氢呋喃醚二醇和二羟甲基丙酸，搅拌升温至90℃，进行除水25min，降温至80℃，然后加入异佛尔酮二异氰酸酯，在60℃的条件下反应1h，加入丙烯酸羟乙酯，继续反应5h，反应完成后加入丙酮进行稀释，加入三乙胺进行中和，其中聚四氢呋喃醚二醇、二羟甲基丙酸、异佛尔酮二异氰酸酯和三乙胺的质量比为100:20:46:14，搅拌2min，将得到的预聚体在水溶剂中分散扩链反应10h，制备得水性聚氨酯乳液；
(3)向烧瓶中加入水性聚氨酯乳液，在120℃的条件下滴加甲基丙烯酸甲酯和八聚乙烯基笼型倍半硅氧烷，其中水性聚氨酯乳液的固体组分、甲基丙烯酸甲酯和笼型倍半硅氧烷的质量比为100:12:7，以过氧化二苯甲酰为引发剂，恒温反应7h，制备得一种笼型倍半硅氧烷改性丙烯酸酯-聚氨酯复合材料。
使用YG028H型万能材料试验机测试实施例和对比例中的笼型倍半硅氧烷改性丙烯酸酯-聚氨酯复合材料的拉伸强度，测试标准GB/T 19250-2013。
Claims (4)
1.一种笼型倍半硅氧烷改性丙烯酸酯-聚氨酯复合材料，其特征在于：所述笼型倍半硅氧烷改性丙烯酸酯-聚氨酯复合材料制备方法如下：
(1)向体积比为480-550:70-100:100的丙酮、浓盐酸和蒸馏水的混合溶剂中加入乙烯基三乙氧基硅烷，搅拌并回流，在50-60℃的条件下反应20-30h，过滤并干燥产物，制备得八聚乙烯基笼型倍半硅氧烷；
(2)向聚四氢呋喃醚二醇中加入二羟甲基丙酸，搅拌升温至110-130℃，进行除水5-15min，降温至55-65℃，然后加入异佛尔酮二异氰酸酯，在80-95℃的条件下反应2-3h，加入丙烯酸羟乙酯，继续反应2-3h，加入丙酮进行稀释，加入三乙胺进行中和，搅拌5-20min，将得到的预聚体在水溶剂中分散扩链反应2-4h，制备得水性聚氨酯乳液；
(3)在70-80℃的条件下，向水性聚氨酯乳液中滴加甲基丙烯酸甲酯和八聚乙烯基笼型倍半硅氧烷，以过氧化二苯甲酰为引发剂，反应2-4h，制备得一种笼型倍半硅氧烷改性丙烯酸酯-聚氨酯复合材料。
2.根据权利要求1所述的一种笼型倍半硅氧烷改性丙烯酸酯-聚氨酯复合材料，其特征在于：所述步骤(1)中的磁力搅拌装置包括基底，所述基底的内壁底部固定连接有轴承座，所述轴承座的顶部转动连接有转轴，所述转轴的外壁活动链接有履带，所述履带的内部活动连接有轴承杆，所述轴承杆的底部固定连接有锥齿轮一，所述锥齿轮一的底部活动链接有支杆，所述锥齿轮一的右侧活动链接有锥齿轮二，所述锥齿轮二的右侧固定连接有旋转杆，所述旋转杆的右侧固定连接有电机，所述电机的右侧固定连接有开关，所述转轴的顶部固定连接有托板。
3.根据权利要求1所述的一种笼型倍半硅氧烷改性丙烯酸酯-聚氨酯复合材料，其特征在于：所述步骤(2)中的聚四氢呋喃醚二醇、二羟甲基丙酸、异佛尔酮二异氰酸酯和三乙胺的质量比为100:10-13:32-35:6-9。
4.根据权利要求1所述的一种笼型倍半硅氧烷改性丙烯酸酯-聚氨酯复合材料，其特征在于：所述步骤(3)中的水性聚氨酯乳液的固体组分、甲基丙烯酸甲酯和笼型倍半硅氧烷的质量比为100:6-8:1-5。
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